ACCENT TM

ECV Pro
Electrochemical C-V Profiler

User Manual
Issue 1.0
Copyright © 2003 Accent Optical Technologies, Inc. Printed in the UK. All rights reserved. No
part of this manual may be used, reproduced, or transmitted in any form or by any means
without prior written permission of Accent. All information containes herein is to be considered
Accent Confidential.

EXCEPTION: This manual, in whole or in part, may be reproduced by purchasers of an Accent

ECV Pro for training their personnel only. Release of any information to any outside party for any
reason is expressly forbidden.

Trademarks, such as product and service names, mentioned herein are owned by Accent or by
third parties. Microsoft is a registered trademark, and Windows NT is a trademark of Microsoft
Corporation.

Other product and company names mentioned in this document are the property of their
respective owners.

Part number: 9PROF-UM01 (printed copy)

Software release: 1.nn

Headquarters:

Accent Optical Technologies, Inc.

131 NW Hawthorne
Bend, Oregon 97701
www.accentopto.com

ECV Pro development:

Accent Optical Technologies (U.K.) Ltd.

222 Maylands Avenue
Hemel Hempstead
Herfordshire HP2 7DF, England

ACCENT TM
Table of Contents

Chapter 1. Introduction
1.1 ECV Pro . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
1.2 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
1.2.1 Shock Hazard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
1.2.2 Chemical Hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
1.2.3 UV light source hazards (UV option only) . . . . . . . . . . . . . . . . . . . . . . . . 1-5
1.2.3.1 Light . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
1.2.3.2 High-Voltage trigger. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
1.2.3.3 Lamp replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
1.2.3.4 Inhibition of removal and modification . . . . . . . . . . . . . . . . . 1-5
1.2.3.5 Vibration and impacts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
1.3 Manual conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-6

Chapter 2. Theory
2.1 Theory of Electrochemical CV (ECV) profiling . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
2.1.1 Etching . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
2.1.2 Method of measurement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
2.2 Specimen modeling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-7
2.3 Factors and Terms. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
2.3.1 Excess Area Compensation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
2.3.1.1 Inaccurate area declarations . . . . . . . . . . . . . . . . . . . . . . . . . 2-10
2.3.2 Debye spreading. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-10
2.3.3 Dissipation factor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
2.3.4 Series Resistance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-13
2.3.5 Flatband potential. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-14
2.3.6 Ohmic contact quality . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-14
2.3.6.1 Indications of poor ohmic contact . . . . . . . . . . . . . . . . . . . . 2-15
2.3.6.2 Improving ohmic contacts . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15

Chapter 3. Installation & Startup

3.1 Installing the ECV Pro . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
3.2 Starting the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3

ECV Pro User Manual iii

9PROF-UM01 Issue 1.0
Table of Contents

Chapter 4. Profiler Software

4.1 System Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-1
4.2 Jobs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-4
4.2.1 Mount/Demount Sample. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-4
4.2.2 Rest Potential . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5
4.2.3 IV Curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
4.2.3.1 Measure Setup. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
4.2.3.2 Graph Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8
4.2.3.3 Mouse Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8
4.2.3.4 Print . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
4.2.3.5 Save . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
4.2.3.6 SaveAs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
4.2.3.7 Read . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
4.2.4 CV Curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-10
4.2.4.1 Measure Setup. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-11
4.2.4.2 Graph Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-12
4.2.4.3 Mouse Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-12
4.2.4.4 Print . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-13
4.2.4.5 Save . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-13
4.2.4.6 SaveAs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-13
4.2.4.7 Read . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-13
4.2.5 Spot Measure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-14
4.2.6 Etch Profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-16
4.2.6.1 Measure Setup. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-16
4.2.6.2 Graph Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-16
4.2.6.3 Mouse Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-18
4.2.6.4 Print . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-18
4.2.6.5 Save . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-18
4.2.6.6 SaveAs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-18
4.2.6.7 Read . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-18
4.2.7 Etch Control Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-19
4.2.7.1 Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-20
4.2.8 Depletion Profile. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-25
4.2.8.1 Measure Setup. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-26
4.2.8.2 Graph Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-27
4.2.8.3 Mouse Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-27
4.2.8.4 Print . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-28
4.2.8.5 Save . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-28
4.2.8.6 SaveAs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-28
4.2.8.7 Read . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-28
4.2.9 Check Contacts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-28
4.3 System. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-29
4.3.1 Equipment Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-30
4.3.2 Manual Control. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-30
4.3.3 Condition Electrodes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-30
4.4 Recipes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-31
4.4.1 Recipe List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-31
4.4.2 Create Recipe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-32
4.4.3 Backup Recipe List. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-33

iv ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Table of Contents

4.5 Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-34

4.5.1 Material . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-35
4.5.2 Reagent Handling. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-35
4.5.2.1 Select . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-35
4.5.2.2 Flush . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-37
4.5.3 Sealing Rings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-37
4.5.4 Capacitance Params . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-39
4.5.5 Users. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-41
4.5.6 Printer & Page Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-41
4.5.7 Multi-Graph . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-42
4.5.8 Configure Warning Tower . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-42
4.6 Datalog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-43
4.6.1 Activity Log . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-43
4.6.2 Auto-Save Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-44
4.7 Alarms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-44
4.8 Help . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-44

Chapter 5. Samples
5.1 About the sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
5.2 Sample size. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
5.3 Sample cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2

Chapter 6. Electrolytes
6.1 Electrolytes and applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-2
6.2 Electrolyte preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
6.2.1 Ammonium bifluoride solution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
6.2.2 Ammonium tartrate solution in ammonium hydroxide . . . . . . . . . . . . . . . 6-3
6.2.3 Hydrochloric acid electrolyte, HCl, Sulfuric Acid H2SO4 . . . . . . . . . . . . 6-4
6.2.4 Diaminoethane (Ethylene Diamine), EDTA . . . . . . . . . . . . . . . . . . . . . . . 6-4
6.2.5 Sodium fluoride : sulfuric acid. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4
6.2.6 Sodium hydroxide : EDTA. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-5
6.2.7 Tiron electrolyte . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-5

Chapter 7. The Electrochemical Cell

7.1 The cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
7.2 The sealing ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-2
7.3 Removing/inserting the cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3
7.4 Inserting/replacing the sealing ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-4
7.5 Problems with sealing rings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-4
7.5.1 Leaking. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-4
7.5.2 Large excess area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5
7.6 Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-6
7.6.1 When to calibrate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-6

ECV Pro User Manual v

9PROF-UM01 Issue 1.0
Table of Contents

7.6.2 Blue slice calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-6

7.6.2.1 Making a blue slice . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-7
7.6.2.2 Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-7
7.6.2.3 Measuring the areas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-8
7.6.3 Alternative calibration method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-9
7.6.4 Entry of calibration data into the software . . . . . . . . . . . . . . . . . . . . . . . . 7-9

Chapter 8. Etching a sample at Operator user level

8.1 Overview. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-1
8.2 Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-2
8.3 Emergency stop. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-3
8.4 Keyboard function keys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-4
8.5 Load a Recipe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-4
8.6 Prepare to mount the sample. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-5
8.7 Mount the sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-7
8.8 Checking Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-15
8.8.1 Rest Potential . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-15
8.8.2 IV Plot. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-16
8.8.3 CV Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-17
8.8.4 Spot Measure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-18
8.9 Etch Profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-19
8.9.1 Start etch profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-19
8.9.2 Interrupting a profile. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-22
8.9.3 Restarting a paused profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-22
8.10 Demount the sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-23
8.10.1 ECVision. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-26
8.10.1.1 Stage 1 - image fitting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-26
8.10.1.2 Stage 2 - updating . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-28

Chapter 9. Supervisor Level Operation

9.1 Preparatory Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9-1
9.2 IV Plot. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9-5
9.3 CV Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9-9
9.4 Spot measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9-13
9.5 Depletion profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9-15
9.6 Etch profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9-17
9.6.1 Setting up conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-17
9.6.2 Pause a Profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-21
9.6.3 Restart a paused profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-21
9.6.4 Ending the Profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-21
9.6.5 Saving the data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-21
9.7 Save the recipe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9-21

vi ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Table of Contents

9.8 Check Contacts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-22

Chapter 10. Maintenance

10.1 Etching problems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-1
10.1.1 Material related etching problems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-2
10.1.1.1 Etching GaAs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-3
10.1.1.2 Etching AlGaAs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-4
10.1.1.3 Etching InGaAs and InGaAsP . . . . . . . . . . . . . . . . . . . . . . . 10-4
10.1.1.4 Etching GaN and AlGaN . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-4
10.1.1.5 Etching InP . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-5
10.2 Electrode conditioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-5
10.3 Halogen lamp replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-6
10.4 UV lamp replacement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-9
10.4.1 Replacing the UV lamp . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-9
10.4.2 Resetting the lamp operation time . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-12
10.5 Changing front contacts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-13
10.6 Changing back contact pins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-13
10.7 Replacing the cell O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-15
10.8 System fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-16

Chapter 11. Using the Etch Reprocessing Program

11.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-1
11.2 Starting Reprocessing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-2
11.3 The Etch Reprocessing screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-3
11.4 Graph scaling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-8
11.5 Regions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-9
11.5.1 Multiple Regions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-9
11.6 Alternative Graphs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-10
11.7 Global parameters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-12
11.8 Reprocessing data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-13
11.8.1 Etched depth calculation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-13
11.8.2 Electrolyte resistance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-13
11.8.3 Deleting points . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-13
11.8.4 Excess area compensation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-13

Appendix A. Etch Examples

A.1 Example 1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1
A.2 Example 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-2
A.3 Example 3 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-3
A.4 Example 4 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-4

ECV Pro User Manual vii

9PROF-UM01 Issue 1.0
Table of Contents

viii ECV Pro User Manual

9PROF-UM01 Issue 1.0
Chapter 1: Introduction

Electronic devices are engineered by selectively introducing impurities into substrate

semiconductor materials or by depositing (growing) new layers epitaxially onto the
surface of the bulk. The properties of the device are determined by the nature of the
impurities and substrate and by the carrier concentration and spatial distribution of the
various regions. Processes used to engineer these structures are often complex, and the
results are highly dependent on purity of starting materials and the processing route. As
device operation depends on the electrical activity of the species and not on their
chemical concentration it is appropriate to evaluate the material by measurement of its
electrical characteristics. Among the many parameters that can be measured, carrier
concentration versus depth is one of the most useful and widely used.

The major techniques used for determining the 'electrical' carrier concentration as a
function of depth are capacitance/voltage (C-V) measurements, spreading resistance, and
differential hall. Spreading resistance involves a lot of time consuming sample
preparation and complex data processing, and the results are highly dependent on the
skill of the operator. On the other hand C-V measurements employing a Schottky contact
are relatively straightforward. The principal limitation is the depth of profiling which is
constrained by the reverse breakdown voltage of the Schottky diode. This is a serious
consideration in materials with high carrier concentrations where the depletion layer is
very narrow.

The Electrochemical C-V Profiler (ECV) overcomes this limitation by employing an

electrochemical etching system. By making use of a well defined electrochemical
dissolution reaction, the material can be profiled to any depth at a controlled and
calculated rate. The semiconductor/electrolyte interface behaves as a Schottky diode and
thus permits carrier concentration measurements to be made in the conventional manner.

By using an electrolyte to both etch and form a Schottky contact with the semiconductor,
the ECV Profiler is the most effective method of determining the efficiency and success
of a process prior to device manufacture.

ECV Pro User Manual 1-1

9PROF-UM01 Issue 1.0
Introduction
ECV Pro

1.1 ECV Pro

Cell viewing
cover

Electrolyte
vacuum
Manifold
vapour trap

Emergency Off Splash guard

button

Fluid bottles
Cell

Bottle tray

Sample stage
Keyboard on pull-out
drawer

Front door catch

Figure 1-1: The Production Profiler

The ECV Pro is designed for use by both experienced physisists and relatively
inexperienced operators:

• Mounting wafers, obtaining good ohmic contacts and debubbling the cell are all part
of an easy-to use Mount Sample wizard.

• Parameters for IV, CV and etch profiling can be determined by the physisist then
stored in a recipe so that an operator can recall predefined settings.

• Capturing an etch pit image, monitoring the ring size (if ECVision is installed) and
demounting the wafer is performed by a wizard.

1-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Introduction
Safety

1.2 Safety

The information provided in this section is designed to give a new user of the ECV Pro
an overview of safety aspects of the system. Recommendations given are meant as a
guide only. The operator should consult with the laboratory safety officer for specific
instruction on safety practices.

IMPORTANT
It is important to read this section before attempting to operate the system.

1.2.1 Shock Hazard

• This system should be operated from the type of power source indicated on the back
panel label. If you are not sure of the type of power available, consult your
electrician

• This system is equipped with 3-wire grounding-type plugs (plugs having a third
'grounding' pin). These plugs will only fit into a grounding-type power outlets. This
is a safety feature. If you are unable to insert these plugs into the outlets, contact
your electrician for advice

• Always unplug the system from the wall outlet before opening or removing covers

• Do not attempt to service this product yourself. Refer all servicing to qualified
service personnel

• Unplug the system from the wall outlet and refer servicing to qualified service
personnel under the following conditions:
- If a liquid has been spilled into the system
- If the system has been exposed to rain or water
- If the system (or part of the system) has been dropped or the casing damaged.

IMPORTANT
Always replace blown fuses with a UL approved fuse of the same type and
current rating. If the fuse continues to blow, contact qualified service
personnel.

ECV Pro User Manual 1-3

9PROF-UM01 Issue 1.0
Introduction
Safety

1.2.2 Chemical Hazards

The chemicals used with this system are potentially hazardous. Anyone using the system,
or who could potentially come into contact with these chemicals should discuss the
following safety guidelines with the safety officer.

• Make a list of all the chemicals that you use with this system

• Obtain, and make available to anyone who could potentially come into contact with
these chemicals, the Material Safety Data Sheets (MSDS) for each chemical

• Discuss the practical implications of the MSDS for each chemical with your safety
officer

• Make available written spill clean up procedures

• Make sure that the chemicals, and prepared electrolytes, are properly labelled

• Make sure all chemicals are stored carefully

• Consult a qualified chemist for instructions on preparing the electrolytes

• Prepare only the minimum quantity necessary of each electrolyte

• Consult a qualified chemist on the correct method for discarding used or old
electrolytes and chemicals

• Discard any electrolyte or chemical that has been stored for any time exceeding its
shelf life.

• Discard any electrolyte or chemical with an ambiguous or unreadable label

• Take extra care when using parts of the system labeled as follows:

• Follow carefully any warnings included in the operating instructions.

The conventions for these are described in Section 1.3.

1-4 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Introduction
Safety

1.2.3 UV light source hazards (UV option only)

1.2.3.1 Light

CAUTION
This equipment emits very strong ultraviolet light which is harmful to eyes and
the skin. Also, as the light emanating from the light guide connection aperture
contains infrared light in addition to ultraviolet light, its irradiation will cause
heat generation.
Be sure to observe following instructions for operation of the equipment.
• Never look directly into the light guide connection aperture or at the light emanating
from the light guide. Strong ultraviolet light can damage eyesight.
• Do not allow light to come into contact with skin. Contact with skin may cause
sunburn-grade inflammation. Always wear safety glasses, gloves, and other
appropriate protective gear when operating this equipment.
• Never allow light from the light guide to radiate onto flammable material.
• The light source unit includes an interlock that prevents the lamp from lighting
while the lamp cover is open. Never attempt to override the interlock function by
manually depressing the switch, as this may result in uncontrolled release of
dangerous ultraviolet light.

1.2.3.2 High-Voltage trigger

The mercury-xenon lamp used is started by a high-voltage (30 kV) pulse applied at the
lamp electrodes. As protection against accidental electrical shock hazard, the light source
unit design includes an interlock switch that disables lamp operation while the lamp
cover is open.
Never attempt to turn on the lamp by blocking the sensor window of the interlock
switch.

1.2.3.3 Lamp replacement

The inside of the lamp housing becomes extremely hot during lamp operation. Before
replacing the lamp, switch it off and run the cooling fan for at least 15 minutes. Always
exercise due caution when handling or replacing a lamp. A lamp contains high-pressure
gas [approximately 1 MPa (10 atmospheres) at room temperature, approximately 4 MPa
(40 atmospheres) during operation] and may burst if dropped or otherwise impacted.
The average service life of the lamp is 3000 hours. The lamp life is monitored and once it
reaches 3000 hours a message is displayed the next time an illuminated measurement is
requested. Lamps may burst if used for longer than 3000 hours so no further illuminated
measurements will be allowed until the lamp is changed and the lifetime reset.

1.2.3.4 Inhibition of removal and modification

Do not remove the top cover or under cover unless absolutely necessary and never touch
any of the screws inside the unit. As the internal components of this unit have been
precisely adjusted, disassembling or modifying the equipment can cause problems with
the unit, fire and electrical shock.

1.2.3.5 Vibration and impacts

Handle the unit with care. Sharp impact or strong vibration can break the lamp or other
fragile components, or disrupt the precise adjustment of internal mechanisms.

ECV Pro User Manual 1-5

9PROF-UM01 Issue 1.0
Introduction
Manual conventions

1.3 Manual conventions

The following table lists abbreviations and symbols used throughout this document:

A Effective contact or etch area M Molecular weight

B Susceptance (wC) N Carrier concentration

C Capacitance Φ 'Built In' or contact potential

Cp Parallel capacitance ρ Density

Cs Series capacitance q Charge of the electron

D Dissipation factor Rs Series resistance

ε0 Permittivity of free space Rp Parallel resistance

εr Relative permittivity of the V Applied voltage (negative in

semiconductor reverse bias sense)

Eg Energy gap between the conduction Wr Etched depth

and valence bands

f Frequency Wd Depletion depth

F Faraday constant ω Radial frequency

G Conductance Xc Reactance

h Planck's constant Y Admittance

Z Impedance

Table 1-1: Nomenclature

Convention Definition and Use

Bold Boldfaced text highlights functions and important

concepts.

italics Highlights text that you need to consider.

SMALL CAPS Indicates a menu item in the top menu bar or in a

subsequent drop down menu.

Indicates additional information to help the user better

NOTE understand something or obtain optimum
performance. Notes are not safety-related to the
equipment or personnel and do not contain required
reading.

Table 1-2: Conventions (Sheet 1 of 2)

1-6 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Introduction
Manual conventions

Convention Definition and Use

Indicates information that is significant to an operation

IMPORTANT being performed. Important information is not safety-
related for the equipment or personnel, but is required
reading.

Indicates a potentially hazardous situation which, if

CAUTION not avoided, could result in moderate or minor injury
or damage to the equipment.

Table 1-2: Conventions (Sheet 2 of 2)

ECV Pro User Manual 1-7

9PROF-UM01 Issue 1.0
Introduction
Manual conventions

1-8 ECV Pro User Manual

9PROF-UM01 Issue 1.0
Chapter 2: Theory

2.1 Theory of Electrochemical CV (ECV) profiling

If a semiconductor is placed in contact with an electrolyte, charge exchange takes place.

In a well designed electrochemical system charge transfer from the semiconductor to the
electrolyte (anodic current) will be supported by carriers (holes) in the valence band of
the semiconductor. The dissolution reactions for two common semiconductor materials,
silicon and gallium arsenide, are as follows:

Si + 4⊕ ⇒ Si4+

GaAs + 6⊕ ⇒ Ga3+ + As3+

The dissolution process results in an increasing separation of electric charge. Equilibrium

is eventually achieved when the decrease in chemical free energy, as a result of
dissolution, is balanced by the increase in electrical energy associated with the separation
of charge. This system of charges is called the Helmholtz electrical double layer, and the
potential drop across the layer is referred to as the equilibrium electrode potential. At
equilibrium the anodic dissolution current is balanced by charge transfer from the
electrolyte to the semiconductor (cathodic current) supported by carriers (electrons) in
the conduction band.

In practice the situation is more complex. The limited availability of carriers in the
semiconductor means that exchange currents are invariably dwarfed by mixed potential
currents. Consequently, measured potentials are not single electrode potentials, but
mixed potentials.

The main difference between semiconductor and metal electrodes is their respective
charge carrier densities. Because the charge carrier density in a metal is so high
(>1022cm-3), charge is transferred with negligible penetration into the metal. Any
externally applied potential is completely dropped across the Helmholtz layer. However,
the lower carrier densities of semiconductors (1013 - 1019 cm-3) result in a much larger
field-affected region. Depending on the charge of the ions in solution adjacent to the
interface, carriers may be attracted (accumulation) or repelled (depletion) in the field-
affected region.

ECV Pro User Manual 2-1

9PROF-UM01 Issue 1.0
Theory
Theory of Electrochemical CV (ECV) profiling

To measure carrier concentration by CV methods, conditions must be such that a region

depleted of carriers is formed. For a p-type semiconductor, where the majority carriers
are holes, this condition is satisfied by positive ions in solution, as in Figure 2-1 (a).

Small leakage Semiconductor/Electrolyte Small leakage Semiconductor/Electrolyte

-ve +ve current +ve -ve
current

-
A- D+
+
Si Si Si Si Si Si
+ -
-
+

Si Si A- Si + Si - Si D+ Si -
+ +
-
+ - -
A- D+
+
Si Si Si Si Si Si
+ -
-
+

A- A-
+ +
Si Si + D Si Si D -

Depletion Zone Depletion Zone

(a) (b)
p-type semiconductor n-type semiconductor
Reverse Bias Reverse Bias

Figure 2-1: Depletion regions for p-type and n-type samples

By making the semiconductor more negative than its equilibrium value, positive ions are
attracted to the interface and the holes are repelled. For an n-type semiconductor, where
the majority carriers are electrons, negative ions are required and thus the semiconductor
must be made more positive than its equilibrium value, as in Figure 2-1 (b).

Providing the electrolyte is fairly concentrated (0.1M), field penetration into the
electrolyte is negligible and the semiconductor/electrolyte interface behaves as a one-
sided or Schottky junction. In this case the potential drop across the Helmholtz layer is
constant and the remaining applied potential is dropped across the depletion layer. The
well known equations for depletion width (Wd) and capacitance (C) for a
metal/semiconductor junction therefore apply to this system.

1
---
2 ( Φ – V )ε 0 ε r 2 (1)
Wd = --------------------------------
qN

1
---
qNε 0 ε r 2 (2)
C = A ----------------------
2(Φ – V )

2-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Theory
Theory of Electrochemical CV (ECV) profiling

2.1.1 Etching
The advantages of using an electrolyte are apparent when the dissolution process is
considered. Dissolution (etching) of semiconductor materials depends on the presence of
holes. For p-type materials holes are plentiful and dissolution is readily achieved by
forward biasing the semiconductor/electrolyte junction, as illustrated in Figure 2-2 (a).
For n-type materials, in which electrons are the majority charge carriers, holes have to be
created for dissolution to take place. By illuminating the semiconductor/electrolyte
junction with light of a wavelength short enough to generate electron hole pairs. For this
to occur, the wavelength, λ, must obey the condition:

hc
λ ≤ ------
Eg

Etching Etching
current current
+ Semiconductor/Electrolyte Semiconductor/Electrolyte
+ve -ve +ve -ve
-

-
Si A- Si Si Si D+ Si Si
-
+ - -
+

A- D+ -
+
Si Si Si Si - Si Si
- +
+ +
+
+ -
+
+ -
A- Si + Si
Si Si Si D Si
+ 4+ -
- 4+
Si Si
A- A-
+ +
Si Si D Si Si D -

Depletion Zone

(a) (b)
p-type semiconductor n-type semiconductor
Forward Bias Reverse Bias with illumination

Figure 2-2: Dissolution of p-type and n-type samples

Etching of n-type materials takes place under conditions of reverse bias, as illustrated in
Figure 2-2 (b). Forward biasing would deposit ions from solution. The holes created by
illumination give rise to an appreciable leakage current through the depleted region. This
current is a function of the density of the minority carriers and is therefore only
controlled by the level of illumination.

ECV Pro User Manual 2-3

9PROF-UM01 Issue 1.0
Theory
Theory of Electrochemical CV (ECV) profiling

2.1.2 Method of measurement

There are four stages in obtaining an ECV profile:

1. Obtain an IV plot, from which it is possible to derive a suitable bias voltage range
for the capacitance measurement.

2. Using the bias voltage range derived from the IV plot, obtain a CV plot, and analyze
this to derive the measurement bias condition required to create etching conditions.

3. Measure the depletion profile using the bias voltage range derived from the IV plot.

4. Using information obtained above, perform the etch profile.

The IV plot shows the consequence for a given sample of departure from the equilibrium
state. Figure 2-3 and Figure 2-4, which are IV plots for n- and p-type materials
respectively, both exhibit characteristic diode behavior. It is essential to bear in mind that
these potentials are measured in an electrochemical system, and they are therefore
displaced in voltage with respect to the more familiar absolute scale based on zero
potential for an electron in vacuum at infinite distance from the source.

Etching is carried out by appropriate choice of electrode potential. For p-type material
this will be in the forward bias region, i.e. the working electrode (the sample) must be
more positive than the rest potential. For n-type material, reverse bias is used and the
working electrode is illuminated.

As the etching process depends on the flow of charge, the etching rate is, in the ideal
case, proportional to the current flowing between the working and counter electrodes.
The amount of material removed and consequently the etched depth Wr is given by
Faraday's law of electrolysis as follows:

M 2
W r = ------------- ∫ I dt (3)
zFρa 0

Carrier concentration determination requires the semiconductor electrode to be reverse

biased. As carrier density is measured at the edge of the depletion layer, the
corresponding depth is equal to the sum of the etch depth and the depletion depth.

ε0 εr A
PROFILED DEPTH = Wr + Wd where W d = --------------
C

The charge carrier density N at the edge of the depletion layer is given by:

3
1 C
N = -------------------2- ⋅ ---------------- (4)
qε 0 ε r A dC/dV

2-4 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Theory
Theory of Electrochemical CV (ECV) profiling

I-V .00 µm
1
Light
Dark

.5

Illuminated I-V curve

-.5
Dark I-V curve

-1
-2 -1 0 1 2
VOLTAGE

Figure 2-3: IV curve of n-type GaAs (4E17cm-3) with Tiron electrolyte

I-V .00 µm
1
Light
Dark

.5

Dark I-V curve

-.5 Illuminated I-V curve

-1
-2 -1 0 1 2
VOLTAGE

Figure 2-4: IV curve of p-type GaAs (4E17cm-3) with Tiron electrolyte

For n-type semiconductors the capacitance of the depletion layer will decrease as the
semiconductor is made more positive than its rest potential. Consequently dC/dV and
hence N will be negative. For p-type semiconductors the capacitance of the depletion
layer will decrease as the semiconductor is made more negative than its rest potential,
hence dC/dV and N will be positive. The CV characteristics of the semiconductor/
electrolyte junction for p- and n-type materials are exhibited in Figure 2-5 and Figure 2-6
respectively. The measurement bias condition employed is chosen using these plots.

ECV Pro User Manual 2-5

9PROF-UM01 Issue 1.0
Theory
Theory of Electrochemical CV (ECV) profiling

Equation (4) is particularly useful as it provides an elegant experimental method for

determining carrier density. Parameters C and dC/dV are obtained by using a slowly
modulated high frequency voltage. The electrochemical cell, along with a reference
(termination) resistor and various stray admittances, form a potential divider.

C-V .00 µm
250 2
C(nF/cm2)
1/C2
parallel D
series I
200 S
S
C I
A P
P A
A T
C I
I 150 O
T N
A 2
N 1/C curve C-V curve
1
C
E
100 F
A
C
T
O
R

50
Dissipation curve

0 0
-4 -3 -2 -1 0 1
VOLTAGE

Figure 2-5: CV plot of p-type GaAs with Tiron electrolyte

C-V .00 µm
120 2
C(nF/cm2)
1/C2
parallel 2 D
100 series 1/C curve I
S
S
C I
A P
P A
A 80 T
C I
I O
T N
A
N
C 60 C-V curve 1
E
Dissipation
F
curve A
C
40 T
O
R

20

0 0
-1 -.5 0 .5 1 1.5 2
VOLTAGE

Figure 2-6: CV plot of n-type GaAs with Tiron electrolyte

2-6 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Theory
Specimen modeling

2.2 Specimen modeling

An equivalent circuit for a specimen mounted on an electrochemical cell may be thought

of as an ideal Schottky capacitor (diode) with some parallel leakage Rr and series
resistance Rs caused by the ohmic contact, semiconductor resistances and electrolyte
resistance. By measuring at two frequencies, one is able to calculate all circuit values. In
some cases, the specimen may not conform to the 3-element model because it contains
distributed elements (e.g. sheet resistance across the junction surface) or frequency-
dependent elements (e.g. trap response times). Thus results obtained using different
frequency pairs may be inconsistent.

1
The complex admittance at the carrier frequency is: Y = --- + iωC
R

The differential admittance is: dY = dY

-------
dV

Admittance and differential admittance are calculated as follows:

ωC ωdC
Parallel Im(Y) Im(dY)

Series –1
( I m ( Y ) ) ⋅ I m  --------
-------------- 2 -dY-
2
I m  ---
1 Y
Y

where Im = Imaginary.

The 3-Term model is a generalized calculation. It is intended to remove most of the series
resistive effect of a weak electrolyte (such as 0.1M Tiron or 0.075M NH4HF2) when
measuring high carrier concentration material. This helps increase the measurable carrier
concentration range.

ECV Pro User Manual 2-7

9PROF-UM01 Issue 1.0
Theory
Factors and Terms

2.3 Factors and Terms

This section discusses some important factors that affect the appearance or accuracy of
the results obtained by ECV profiling. Some of these factors will have different effects
on different structures, but an understanding of when and how they affect your results
will be beneficial before you attempt serious use of the system.

Also discussed will be some of the terms used in the software such as Flatband potential
and D-Factor. It is important to understand these terms in order to make educated choices
when setting up profiling conditions.

2.3.1 Excess Area Compensation

Calibration of the electrolyte contact areas is the only calibration necessary for accurate
measurements (see Section 7.6). This involves accurate measurement of the wetted
contact area (p-type etch area) and the illuminated (n-type) etch area, using an anodized
piece of n-type GaAs called a blue slice. The annular ring of material revealed in the blue
slice calibration as the difference between the wetted and illuminated areas is known as
the excess area. It is caused by the slight shadow formed by the O-ring.

It is important to understand the effect of miscalibration on the carrier concentration

profile. Normally, because n-type material requires illumination before it can be etched,
the excess area does not etch because it is in the dark. It does, however, have a
capacitance, the magnitude of which depends on the area and carrier concentration. To
compensate for this, the capacitance associated with this area is calculated at the first
total capacitance measurement, and then subtracted from each subsequent measurement.
This is important in hi-lo, n-type structure profiles, as the illuminated area capacitance
can drop to a level similar to the excess area capacitance.

The following notations are used in subsequent explanations:

CX0 = excess capacitance measured at surface

CX = actual excess capacitance at current step (electrolyte spreading, side walls, etc.)
Cs = capacitance of illuminated area
Ctot = capacitance of total wetted area
C = capacitance used in calculations
Awet = wetted area
Aill = illuminated area

A wet – A ill
At the surface: CX0 = C tot -------------------------
A wet

where: Ctot = Cs+ CX

calculate: C = Ctot - CX0

= Cs + CX - CX0

if: CX ≈ CX0 then C ≈ Cs

2-8 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Theory
Factors and Terms

It is apparent from these relationships and Equation 4 on page 2-4 that as the profile
changes from a region of higher to lower carrier concentration, CS becomes much
smaller. CX, on the other hand is a constant. It is therefore evident that any errors in the
area calculations will assume greater importance. If the errors in area calculation are
large, CS and measured depletion depth can go negative and the carrier concentration to
appears to change carrier type.

An important practical point to note here is that since wetted areas vary from one
electrolyte to another, it is essential to recalibrate whenever a different electrolyte or
sealing ring is used.

Figure 2-7: Correct area compensation

Figure 2-8: Slight over compensation

ECV Pro User Manual 2-9

9PROF-UM01 Issue 1.0
Theory
Factors and Terms

Figure 2-9: Gross over compensation

2.3.1.1 Inaccurate area declarations

If the wetted and illuminated area values (entered by selecting the Ring option from the
Specimen menu) are incorrect, there will be an error in CX0, and excess area
compensation will lead to errors in the profile. You can avoid this by:
• Discard old sealing rings that have a significantly enlarged excess area
• Measuring areas carefully with the blue slices and keep the ring data file updated
(see Section 7.6)
• If in doubt, avoid excess area compensation altogether by declaring your material as
p-type before starting the profile. In the case of hi-lo structures, the 'lo' layer will
measure too high. The correct excess area compensation values can later be applied
in the Etch Reprocessing program.

2.3.2 Debye spreading

Capacitance techniques provide a measure of the free carrier density at the depletion
edge (which is assumed to be abrupt). However, because free charges diffuse a few
Debye lengths (Ld) into adjacent regions (including the depletion region), they will not
accurately reflect the impurity distribution near an abrupt discontinuity in a sample.
Features will appear 'spread-out' over several Debye lengths, giving a fundamental
resolution limit to the measurement (see Figure 2-10). The effect is most pronounced in
sharply varying hi-lo structures such as shallow ion implants, in which the total thickness
may only be a few Debye lengths. The ion implant's peak height may appear reduced and
the tail will appear extended.
1 ε 0 ε r kT 1⁄2
L d = --- ----------------
q N
Depth resolution is ≈ 3Ld

NOTE
This resolution does not take into account etch non-uniformity.

2-10 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Theory
Factors and Terms

1017

Simulated implanted profile, LSS

Concentration
1016

Measured profile

15
10

0 0.4 0.8
Depth

Figure 2-10: Ion implant profile showing effects of Debye spreading

The following table of Debye length values and consequent resolution limits is obtained
from the expression above.

Log N Debye Length Ld Resolution R (µm)

20 0.0004 0.0013
19 0.0013 0.004
18 0.004 0.013
17 0.013 0.04
16 0.04 0.13
15 0.13 0.4
14 0.4 1.3
13 1.3 4.0

Computer simulations of step profiles which incorporate the Debye spreading effect have
been generated. These show that:

• The measured profiles will differ depending on the direction in which the profile is
performed (lo-hi or hi-lo)

• Profiles measured by depletion profiling (ramping voltage) differ from profiles

obtained by ECV (constant voltage)

• Abrupt lo-hi steps may show a regression in depth or foldback.

ECV Pro User Manual 2-11

9PROF-UM01 Issue 1.0
Theory
Factors and Terms

2.3.3 Dissipation factor

The dissipation factor (D) is used in the ECV Pro as an indication of the quality of the
electrochemical 'Schottky' diode. It is used by the Spot Measure facility to assist in
selection of the measurement conditions. Its measured value also appears in the CV
curves and on the data log printout for each point of the etch profile.

The dissipation factor is the inverse of the quality factor (Q) of the model circuit of the
semiconductor/electrolyte interface, and is defined as follows:

1 XC
X c = -------- Rs
ωC

ω = 2πf = 20000 rad/sec @ 3.2kHz Rp

1
R p = ----
G

B = ωC B

Rs
Series circuit D = ----- = R s ωC
Xc
G 1
Parallel circuit D = ---- = --------------
B R p ωC

The value of D depends on material resistivity, carrier concentration, sealing ring size,
type of ohmic contact and measuring frequency. Its main use is as an indicator of the
effect of series or parallel resistance on the quality of the measurement.

D should not exceed about 0.4 and will ideally be much lower. One criterion in selecting
measurement conditions is therefore to minimize the D value. The factors affecting series
resistance are described in the next section.

2-12 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Theory
Factors and Terms

2.3.4 Series Resistance

Series resistance is an important factor affecting the results of samples measured by
depletion or etch CV techniques. Samples with thin epitaxial layers and ion implanted
layers on semi-insulating or opposite carrier type substrates are especially susceptible.

Sealing
ring

Electrolyte

Ohmic Ohmic
contact contact

Epitaxial
layer
Semi-insulating
substrate

Series
resistance

Figure 2-11: Source of series resistance

Series resistance arises from the following sources:

• Bulk resistivity of the material (Rb)

• Sheet resistivity of a surface layer (Rs)

• Spreading resistance of a point contact (Rp)

• Electrolyte resistance between specimen and platinum electrode (Re).

Many structures are grown on semi-insulating substrates or contain one or more p-n
junctions. Front contacts must be used for such structures.
For other structures, either front, back or both contacts may be used.

ECV Pro User Manual 2-13

9PROF-UM01 Issue 1.0
Theory
Factors and Terms

2.3.5 Flatband potential

The flatband (or built-in) potential of a Schottky diode is a physical property of the
semiconductor-electrolyte contact and can be calculated from the capacitance
measurement. The calculated flatband potential is displayed in the Spot Measure dialog
box (see Section 4.2.5) and etch profiles. This can be used as a confidence indicator
when setting up the measurement conditions and for checks of the results obtained.

The capacitance of a Schottky contact in uniformly doped material is:

2
2 A qε 0 ε r N
C = ------------------------
2(Φ – V )

where Φ is the flatband potential.

The ECV Pro uses the following differential formula:

3
C 2
------------------ = A qε 0 ε r N
dC ⁄ dV

and is valid for non-uniformly doped material. This avoids the need to know Φ, but
requires an additional measurement of dC/dV by use of a modulation signal.

For a reverse biased Schottky diode with a uniformly doped depletion region, the two
equations should yield the same result for carrier concentration. Equating, we obtain the
relationship:
C -
----------------- = 2( Φ – V )
dC ⁄ dV

This is the equation used to derive Φ by extrapolation of the 1/C2 curve back to the
voltage axis.

So, the flatband potential displayed in the Spot Measure dialog box and Etch Profile
control panel indicates how closely the measurements of C and dC/dV conform to the
Schottky equation, and hence how closely the junction models a Schottky diode.

2.3.6 Ohmic contact quality

The quality of the ohmic contact can greatly affect the results obtained by ECV profiling.
Normally, the ECV Pro contact blasting facility will form sufficiently good ohmic
contact for measurements on the following samples:

• Epitaxial layers grown on the same carrier type, moderately to heavily doped
substrates

• Thick (>0.25 mm) layers grown on or ion-implanted into semi-insulating, low

doped, or opposite carrier type substrates.

Sample types that typically will not form good ohmic contacts by use of the contact
blasting facility are:

• Low doped layers on semi-insulating or opposite carrier type substrates

• Low doped bulk samples

2-14 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Theory
Factors and Terms

• Samples with isolated layers, e.g. n-p-n or n-p-semi-insulating substrate

• Low doped or thin layers on conducting substrates with insulating oxide on the back
surface or highly compensated (insulating) interface regions

• Thin (<0.25 mm) layers grown on semi-insulating substrates.

2.3.6.1 Indications of poor ohmic contact

• Some indications of poor ohmic contact are:

• High forward and reverse resistances indicated in the Check Contacts dialog box
(see Section 4.2.9)

• IV curves that show flat (zero current) regions in the forward bias direction

• Low, flat CV curves

• Larger than expected depletion widths.

Suspected poor ohmic contacts can be checked with a curve tracer. Any rectifying quality
will be cause for concern. The ability to form ohmic contact to a thin layer is related to its
resistivity. This is in turn dependent on the material (GaAs, Si, InP, etc), the carrier
concentration and resistivity (see table) of the layer and the condition of the surface.
Certain materials such as p-type InP and AlGaAs are well known to cause problems in
ohmic contact formation.

Resistivity (Ω-cm @ 300K)

N (cm-3) n-type Si p-type Si n-type GaAs p-type GaAs
20
10 0.0007 0.001 0.0001 0.0015
1019 0.006 0.009 0.0004 0.008 Blast contact
1018 0.02 0.04 0.002 0.03 normally OK
1017 0.08 0.2 0.02 0.25
1016 0.5 1.5 0.15 2.0
1015 4.0 15.0 1.5 20 Alloyed contacts
1014 40 150 10 200 increasingly necessary
1013 400 1500

2.3.6.2 Improving ohmic contacts

If the electrochemical cell fails to form a good ohmic contact, other techniques must be
employed before a reliable measurement can be achieved. The method of choice is
usually the use of a large area metal contact.

Gallium - Indium eutectic (liquid at room temperature) can be painted on an oxide free
surface to form an ohmic link between the semiconductor and the contact pins. Scratch
the surface of the sample to remove any oxide before painting on the Ga-In.

NOTE
This will normally short out the pins, resulting in very low indicated resistance
(as displayed in the Check Contacts dialog box). Evaporated metal contacts

ECV Pro User Manual 2-15

9PROF-UM01 Issue 1.0
Theory
Factors and Terms

will often be the only alternative for very low doped compound semiconductor
layers.

Examples:

1. AuGe-Ni is a suitable choice for n-type GaAs

2. Au-Zn is often used for p-type InP or p-type GaAs

3. The area of the contact metal (evaporated or painted) should be large (> electrolyte
area) so that capacitive coupling into the semiconductor is sufficient.

2-16 ECV Pro User Manual

9PROF-UM01 Issue 1.0
Chapter 3: Installation & Startup

CAUTION
Components within the Instruments can be damaged by electrostatic discharge.
Observe precautions for handling electrostatic discharge sensitive devices. You
are advised to ground yourself to a suitably earthed point with a proprietary
ESD wrist strap.

3.1 Installing the ECV Pro

1. Move the ECV Pro so that it is standing in the location where it is to be used.
Rotate the orange wheel clockwise, on each castor, to lower the wheels to the
castors rolling positions. Once at the working location, rotate the orange wheels
anti-clockwise to raise the wheels off the floor and return the castors to their stable
positions.

Rolling position Stable position

Rotate orange wheel clockwise to Rotate orange wheel anti-clockwise
lower wheel to raise the wheel off the floor

Figure 3-1: Moving the instrument

2. Open the front door and remove the inside front panel (see Figure 3-5).

ECV Pro User Manual 3-1

9PROF-UM01 Issue 1.0
Installation & Startup
Installing the ECV Pro

3. Remove the tie wrap holding the PC in place.

Figure 3-2: Tie wrap on PC

4. Ensure that the pump power switch is in the On position.

Figure 3-3: Vacuum pump power switch in On position

5. Replace the inside front panel.

6. If you have an extraction unit, connect this to the fume outlet at the back of the
instrument (see Figure 3-4).

Fume outlet

Figure 3-4: Extraction unit connector

7. The ECV Pro is supplied with standard 2m mains cables. Plug this in to the power
socket.

The ECV Pro is now installed and ready for use.

3-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Installation & Startup
Starting the instrument

3.2 Starting the instrument

1. Turn the power On at the power socket.

2. Open the front door and press the Green button to turn the instrument on. You
should now hear the pump operating.

Instrument Off button

Instrument On button

PC On/Off button

Inside front panel

Figure 3-5: Inside the front door

3. Press the PC power button to turn the PC on.

4. Close the front door.

Due to the extremely low signals measured by the ECV Pro some noise may be observed
on the data during disturbances associated with external events such as Fast transients or
ESD. However, these errors are trapped by the software warning you of the nature and
cause of the error, allowing you the option to either continue or wait until the disturbance
has passed.

ECV Pro User Manual 3-3

9PROF-UM01 Issue 1.0
Installation & Startup
Starting the instrument

3-4 ECV Pro User Manual

9PROF-UM01 Issue 1.0
Chapter 4: Profiler Software

4.1 System Startup

Double click on the shortcut to ProdProf on the desktop or on the ProdProf.exe file to
start the program. The initial screen allows, as shown in Figure 4-1, for the possibility
that the software may have last been terminated when the tool was in the middle of a
measuring cycle.

Figure 4-1: Login screen

If a sample is still mounted, click on Demount.

If there is a chance that the cell may not be in its correct starting position, click on
Initialize.

If it is known that all is ready to start a new sample, click on Cancel.

ECV Pro User Manual 4-1

9PROF-UM01 Issue 1.0
Profiler Software
System Startup

The first action must be to Login. Click once on Login, in the top right-hand corner of the
screen, to display the following dialog box:

Figure 4-2: Entering User name and password

Valid user name and password entries must be set in the system at Supervisor level.
Details are given in Section 4.5.5. There are two user levels:

• Operator
gives restricted access to functions (see Figure 4-3) and is intended for profiling
samples using installed recipes.
While an Operator is logged in, it can be seen in Figure 4-3 that a Supervisor can
also login so that minor adjustments may be made to settings to enable small
deviations from recipe limits to be accepted during a measurement.

• Supervisor
allows full access to program functions.

Figure 4-3: Initial Profiler screen with an Operator logged in

Having logged in, some of the bottom function keys become available.
In Operator mode, Jobs (once a recipe has been selected), Recipe, Alarms and Help are
available for use.
In Supervisor mode all are available for use.

4-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
System Startup

The Profiler conforms largely to the SEMI E95-0200 interface specification, so the
display is divided into consistent functional areas. In general, you can navigate freely
between areas and functions. However, in some cases Wizards or Modal Dialog boxes
are used. These must be completed or exited before you can navigate elsewhere.

Top Bar
This bar includes:

• Network communication status,

• Current date and time,

• The coordinations of the cursor in a graphical window,

• The title of the current view,

• Prompt and Message strings,

• Login / Logout buttons.

Navigation Bar
This contains a series of buttons along the bottom of the screen which give access to
the main functional areas within the Profiler application. The buttons are:

• Jobs – functions used to etch and measure a profile (Section 4.2)

• System – various maintenance functions (Section 4.3)

• Recipes – selection and management of defined parameter sets for etching

samples (Section 4.4).

• Setup – manual entry of parameters and program configuration (Section 4.5).

• Datalog – the storage of system and sample data files (Section 4.6)

• Alarms - not yet available

• Help – not yet available

Sub-Navigation Bar
This is a column of buttons located on the left side of the screen that varies
according to the Navigation Bar function selected (as shown, for example, in
Figure 4-4).

Command Bar
Further functions may appear in the Command Bar in the right-hand column of the
screen when a Sub-Navigation function is selected (see Figure 4-5).

Information Panel
The central area of the screen. This may contain command features as well as
information.

ECV Pro User Manual 4-3

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

4.2 Jobs

The Jobs screen is available to all users.

Figure 4-4: Jobs screen

Sub-Navigation functions available are:

• Mount/Demount Sample (Section 4.2.1)

• Rest Potential (Section 4.2.2)

• IV Curve (Section 4.2.3)

• CV Curve (Section 4.2.4)

• Spot Measure (Section 4.2.5)

• Etch Profile (Section 4.2.6)

• Depletion Profile (Section 4.2.8)

• Check Contacts (Section 4.2.9)

4.2.1 Mount/Demount Sample

A series of screens will take you through the process of mounting or demounting a
sample, as appropriate. These screens are described in detail in Section 8.7 and
Section 8.10 respectively.

4-4 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

4.2.2 Rest Potential

This is the open circuit voltage of the semiconductor contacts with reference to the sense
electrode. It is measured both in the dark and illuminated conditions. The difference in
these voltages gives an indication of the carrier type.

Rest potentials give assurance that the sample mounting, contact formation and filling
procedures have been carried out correctly. For example, if there is still a bubble
isolating the sample from the electrolyte, the dark potential will be unusual and lack
repeatability.

Rest potential measurements can also be misleading if the structure contains p-n
junctions, very high doping levels, or is highly compensated.

Figure 4-5: Rest Potential screen

Measure
Measures the dark and light rest potentials.The measurement can be repeated, but
you should wait for about 15 seconds to allow the electrodes to recover. Some drift
is often seen initially due to the adjustment of the semiconductor or sense electrode
to a new electrochemical environment.

The shutter will click open and closed, illuminating the sample for a short time. The
Dark and Light voltages will be displayed, along with the apparent Type of the
material under test.
Typical values of Vrest(dark):
Electrolyte Volts
Tiron -0.3 to -0.7
NaOH -0.7 to -1.2
HCl -0.1 to -0.6
If the result is n-type, you should use illumination and excess area compensation
when etch profiling.

ECV Pro User Manual 4-5

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

4.2.3 IV Curve
The IV curve reveals where the forward and reverse bias limits sit, where the reverse
breakdown occurs, and whether there is a photo response. You can identify etching
conditions and a range of possible measuring voltages. Constant voltage (Vetch) or
constant current (Ietch) is displayed on the screen as a red line. Figure 4-6 shows that a
constant voltage of 0.2V has been set.

Figure 4-6: IV Curve screen

Command bar functions available with this sub-navigation function are:

• Measure Setup (Section 4.2.3.1)

• Graph Options (Section 4.2.3.2)

• Mouse Mode (Section 4.2.3.3)

• Print (Section 4.2.3.4)

• Save (Section 4.2.3.5)

• SaveAs (Section 4.2.3.6)

• Read (Section 4.2.3.7)

4-6 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

4.2.3.1 Measure Setup

Before measuring, you must set the range of measuring voltages (X), current density
limits (Y) and, if required, choose the illumination and set the lamp intensity.

Figure 4-7: IV Measurement Options dialog box

Current Limits
Normal +0.1 mA/cm2 (large ring)
+0.5 mA/cm2 (small ring)
Current must not exceed 2.5 mA in total.

Some samples may be damaged by excessive current, and you must use lower
limits. To view photo current on n-type samples, you will usually have to set a
higher positive current limit.

Voltage Range
Normal +2 volts
Maximum +10.235 volts

Slow Measurement
Imposes a short delay period between measurements.

Illumination

Clear and do:

Dark - measures with no illumination and creates a new graph
Dark + Light - measures both with and without illumination and creates a new
graph
Family of curves - measures without illumination and five curves with
differing lamp intensities up to a maximum of the value specified at Lamp,
producing a new graph with six curves plotted.

Add Curve:
Dark - measures with no illumination and adds the curve to the displayed graph
Light - measures with illumination and adds the curve to the displayed graph

Lamp
Set the level of illumination to be used for a Light measurement.

Measure
Click on this button to start the measurement.
Use the Stop button that appears to abort the procedure.

ECV Pro User Manual 4-7

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

An IV measurement only takes a few seconds to complete. The measurement

always starts at the rest potential (zero current) and proceeds cathodically (to the
left). It then returns to the rest potential and proceeds anodically (to the right). This
ensures that any material plated onto the sample in the cathodic region is cleaned
away before proceeding.

Measure also stores the values in the box as described for Apply, below.

Apply
Stores the values set in the box ready for saving in the recipe. The values will be lost
if you exit from the program or load a different recipe before saving to the recipe.

Cancel
Revert to the recipe or previously applied values.

4.2.3.2 Graph Options

To view an area of graph defined by specific coordinate ranges, set the coordinate ranges
for X and Y then click on Set Fixed Scale. To return to the default full scale view, click
on Auto-Scale to Data.

Note that the grid lines can be toggled on/off using the keyboard key F9.

Figure 4-8: IV Graph Options dialog box

4.2.3.3 Mouse Mode

The current mouse mode setting is displayed under the title of the button. Available
modes and the function keys that may be used to select them are:

Normal (F1)
Provides normal mouse pointing and clicking functions.

Zoom (F2)
Move the cursor to one corner of the desired region, press the Left button, and
drag to the opposite corner. When you release the Left button, the graph will
rescale to the defined rectangle. To return to default scaling select the Graph
Options and Auto-Scale to Data.

Line Draw (F3)

Hold the left mouse button down and drag the mouse across a graph to draw a
line. These lines may be drawn for illustrative purposes. Only one line at a
time can be drawn and it is not transferred to the printer.

4-8 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

Set Value (F4)

Sets the value of Vetch if constant voltage is selected, or Ietch if constant current
is selected.
Note that the value can not be changed at Operator user level.

Add Text (F5)

The point where you click the Left button becomes the origin of a comment to
be added to the graph. Enter your comment in the dialog which appears.
Comments follow the graph scaling and are transferred to the printer.
To enter another comment, you must select the Add Text function again.

Delete Text
Select this mode to delete all text that has been added to the graph using the
Add Text function.

4.2.3.4 Print
Sends the currently displayed graph to the printer.

4.2.3.5 Save
Writes data from the active graph to file. The name will be as specified when the sample
was opened. The extension will be made up from a two character type identifier, and a
sequence character.

4.2.3.6 SaveAs
Writes data from the active graph to a file name that must be specified.

4.2.3.7 Read
Displays a graph from previously saved data.

ECV Pro User Manual 4-9

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

4.2.4 CV Curve
After completing the IV measurement, the CV curve provides the next step in evaluating
diode quality and measurement conditions. It is also an important tool in deciding which
of the three circuit models to use. The red horizontal line indicates the width of the
measuring signal (set in Capacitance Params see Section 4.5.4). The short vertical tick in
the centre indicates the current measuring potential Vmeas.

Figure 4-9: CV Curve screen

Command bar functions available with this sub-navigation function are:

• Measure Setup (Section 4.2.4.1)

• Graph Options (Section 4.2.4.2)

• Mouse Mode (Section 4.2.4.3)

• Print (Section 4.2.4.4)

• Save (Section 4.2.4.5)

• SaveAs (Section 4.2.4.6)

• Read (Section 4.2.4.7)

4-10 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

4.2.4.1 Measure Setup

Before measuring, you must set the range of measuring voltages (X) and maximum
expected capacitance (Y).

Figure 4-10: CV Measurement Options dialog box

C-Max
The capacitance scale can be set approximately as shown in the Junction Data table
(Table 9-1) to enable you to view measurements in real-time. The graph is
automatically auto-scaled on completion.

Voltage Range
Use the reverse bias range determined in the IV section. A convenient way to set
this range is to use the zoom facility in IV to view only the flat portion of the curve,
excluding forward and reverse breakdown regions. Then transfer this range into CV
with the ‘Get IV Graph Range’ button provided here.

Slow Measurement
Imposes a short delay period between measurements.

Measure
Click on this button to start measuring. Use the Stop button that appears to abort the
procedure.

CV measurement takes about a minute to complete. The measurement takes place

from the rest potential, first cathodically, then anodically as in the IV curve. If a
discontinuity is seen at the rest potential, this is probably due to significant cathodic
current having plated a film onto the sample surface. It is desirable to avoid
deposition by reducing the cathodic voltage range or reducing the current limit.

Measure also stores the values in the box as described for Apply, below.

Apply
Stores the values set in the box ready for saving in the recipe. The values will be lost
if you exit from the program or load a different recipe before saving to the recipe.

Cancel
Revert to the recipe or previously applied values.

ECV Pro User Manual 4-11

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

4.2.4.2 Graph Options

To view an area of graph defined by specific coordinate ranges, set the coordinate ranges
for X and Y then click on Set Fixed Scale. To return to the default full scale view, click
on Auto-Scale to Data.

Note that the grid lines can be toggled on/off using the keyboard key F9.

Figure 4-11: CV Graph Options dialog box

Show Curves
Select the curves you wish to see displayed on the graph.

4.2.4.3 Mouse Mode

The current mouse mode setting is displayed under the title of the button. Available
modes and the function keys that may be used to select them are:

Normal (F1)
Provides normal mouse pointing and clicking functions.

Zoom (F2)
Move the cursor to one corner of the desired region, press the Left button, and
drag to the opposite corner. When you release the Left button, the graph will
rescale to the defined rectangle. To return to default scaling select the Graph
Options and Auto-Scale to Data.

Line Draw (F3)

Hold the left mouse button down and drag the mouse across a graph to draw a
line. These lines may be drawn for illustrative purposes. Only one line at a
time can be drawn and it is not transferred to the printer.

Set Value (F4)

Sets the value for Vmeas. This can not be changed at Operator user level.

Add Text (F5)

The point where you click the Left button becomes the origin of a comment to
be added to the graph. Enter your comment in the dialog which appears.
Comments follow the graph scaling and are transferred to the printer.
To enter another comment, you must select the Add Text function again.

4-12 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

Delete Text
Select this mode to delete all text that has been added to the graph using the
Add Text function.

4.2.4.4 Print
Sends the currently displayed graph to the printer.

4.2.4.5 Save
Writes data from the active graph to file. The name will be as specified when the sample
was opened. The extension will be made up from a two character type identifier, and a
sequence character.

4.2.4.6 SaveAs
Writes data from the active graph to a file name that must be specified.

4.2.4.7 Read
Display a graph from previously saved data.

ECV Pro User Manual 4-13

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

4.2.5 Spot Measure

The purpose of spot measurement is to preview different choices of Vmeas.

Although the CV plot gives a visual presentation of the diode's electrical characteristics,
it performs measurements in a different way: using a ramping DC voltage and no
modulation signal. In cathodic regions, films may form on the surface to give misleading
results.

Spot measure performs measurements in exactly the same way as etch profiling, and
gives a full set of information for all three models in numerical form. You can therefore
accurately evaluate prospective values of Vmeas and your choice of circuit model.

A measuring current limit should have been preset in the Capacitance Measuring Signals
dialog box (Section 4.5.4). Excessive current can damage the sample. Current is
measured first and the procedure is aborted at an early stage if it exceeds the current limit
setting.

Figure 4-12: Spot Measure screen

Bias Voltage
The value set in the recipe will be displayed, change this if necessary.

I-meas.
If the current measured is higher than the current limit, a message will appear here
and the sequence will be aborted.
If the measured current is within range, the measured value will appear here.

4-14 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

Results
The results of the measurement at the set bias voltage are displayed here. The
information displayed is:
- Freq. two measurement frequencies, F1 (primary) and F2 (secondary), as
set in the Capacitance Measuring Signals dialog box
(Section 4.5.4)(Hz)
- Dissipation dissipation at Vmeas
-C measured capacitance (nF)
-G measured conductance (µS)
- Rs series resistance (ohms)
- dC/dV slope of the CV curve at Vmeas (nF/V)
- dG/dV slope of the GV curve at Vmeas (µS/V)
- FBP measured flatband potential (Volts)
- Depl. depletion width at Vmeas (µm)
-N carrier concentration measured (cm-3)

The lower results box builds a history of results for measurements at selected Vmeas
values.

Measure
Press this button to start a measurement. The measurement process may take up to
10 sec. Status or error information may appear on the status line.

Print
Use this button to copy the table to the log printer.

ECV Pro User Manual 4-15

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

4.2.6 Etch Profile

Use this screen to set up some of the measurement parameters and to obtain an etch
profile.

Figure 4-13: Etch Profile screen

Command bar functions available with this sub-navigation function are:

• Measure Setup (Section 4.2.6.1)

• Graph Options (Section 4.2.6.2)

• Mouse Mode (Section 4.2.6.3)

• Print (Section 4.2.6.4)

• Save (Section 4.2.6.5)

• SaveAs (Section 4.2.6.6)

• Read (Section 4.2.6.7)

4.2.6.1 Measure Setup

This button opens the Etch Control Panel, which is described in Section 4.2.7.

4.2.6.2 Graph Options

To view an area of graph defined by specific coordinate ranges, set the coordinate ranges
for X and Y then click on Set Fixed Scale. To return to the default full scale view, click
on Auto-Scale to Data.

4-16 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

Figure 4-14: Etch Graph Options

Note that the grid lines can be toggled on/off using the keyboard key F9.

Reference File
If the sample has been etched before, this etch can be used as a reference file.
Repeat etches are compared for conformity with a specified reference file. Readings
that fall within the specified error band of the reference file are accepted.

Action
This is the action to be taken if a ready falls outside the specified error band.
None - ignore the condition and continue
Log Warning - log a warning in the datalog file and continue
Pause & Alarm -

Figure 4-15: Etch compared with a reference etch

ECV Pro User Manual 4-17

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

4.2.6.3 Mouse Mode

The current mouse mode setting is displayed under the title of the button. Available
modes and the function keys that may be used to select them are:

Normal (F1)
Provides normal mouse pointing and clicking functions.

Zoom (F2)
Move the cursor to one corner of the desired region, press the Left button, and
drag to the opposite corner. When you release the Left button, the graph will
rescale to the defined rectangle. To return to default scaling select the Graph
Options and Auto-Scale to Data.

Line Draw (F3)

Hold the left mouse button down and drag the mouse across a graph to draw a
line. These lines may be drawn for illustrative purposes. Only one line at a
time can be drawn and it is not transferred to the printer.

Add Text (F5)

The point where you click the Left button becomes the origin of a comment to
be added to the graph. Enter your comment in the dialog which appears.
Comments follow the graph scaling and are transferred to the printer.
To enter another comment, you must select the Add Text function again.

Delete Text
Select this mode to delete all text that has been added to the graph using the
Add Text function.

4.2.6.4 Print
Sends the currently displayed graph to the printer.

4.2.6.5 Save
Writes data from the active graph to file. The name will be as specified when the sample
was opened. The extension will be made up from a two character type identifier, and a
sequence character.

4.2.6.6 SaveAs
Resave the active graph data with a new file name.

4.2.6.7 Read
Display a graph from previously saved data.

4-18 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

4.2.7 Etch Control Panel

This screen displays a panel on the right-hand side that gives control of all conditions
before and during the measurement sequence. You need to change settings on this panel
during the etch process.

If you have not previously set the measuring and etch voltages (with the cursor in IV and
CV graphs), set these now. For n-type material, if you have previously determined a
lamp intensity, you can set it now, otherwise start at zero and ramp it up during the first
etch step until the etch current is satisfactory. You must also choose an initial resolution
or depth step.

Note that all of these values can be changed dynamically during the profiling process.

A single button serves to start, pause, and continue the etch process. Note that you may
not exit this window unless the process is paused. Also, other acquisition functions are
disabled while this window is open. You may however, re-scale, adjust configuration,
view other graphs, read Help files, or jump to other applications during acquisition.

Figure 4-16: Etch measuring screen

Close
Click here to close the etch control panel.

Start
Click here to start the etch measurement process. While the etch is active this button
will change to PAUSE.

Options
Click here to open the Etch Measurement Options dialog box (see Section 4.2.7.1).

ECV Pro User Manual 4-19

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

4.2.7.1 Options
When this function is selected the Edit Measurement Options dialog box opens where:

Scale & End, Meas. Options and Etch Options

Supervisors can view and change any of the parameters on these pages
Operators can view but cannot change the parameters on these pages

Change Reagent
This page is available to all users to change the electrolyte in use in the middle
of an etch process.

Functions that are common to all pages of the dialog box are:

OK
Stores the values set in the pages of the dialog box ready for saving in the recipe.
The values will be lost if you exit from the program or load a different recipe before
saving to the recipe.

Cancel
Revert to the recipe or previously applied values.

Scale & End page

Use this page to set the etch depth and the scale for the etch graph.

Figure 4-17: Etch Measurement Options dialog box - Scale & End page

log N
Sets the scale for the y-axis.

End Depth
Enter the required depth here and specify whether it is:
- Etch Depth (the calculated depth of the actual etch)
or
- Total Depth (the sum of the calculated etch depth and the depletion depth).

4-20 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

Measure Options page

Use this page to set the measurement parameters.

Figure 4-18: Etch Measurement Options dialog box - Measure Options page

V Meas
The value displayed here is that selected by the placement of the red cursor bar in
the CV screen. It can be manually changed here if necessary.

Settling
After the switch from etching to measuring conditions, the system needs time to
come to equilibrium. When the forward bias etching current and illumination are
switched off to measure admittance, anodic films that haven't completely dissolved,
or discharging deep levels, may cause capacitance to change for several seconds.
The Settling time defines this pre-measurement delay period.

Fixed Delay
Fixed time from 1 to 10 seconds, during which the specimen is open circuit.
For most samples, 3-6 seconds are sufficient but this is very sample dependent
and requires experimentation.

Auto, using Capacitance meas and Delta

Capacitance readings are made until a stable result is obtained.
Delta - is the error band within which measurements are accepted.

ECV Pro User Manual 4-21

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

Etch Options page

The parameters on this page set the etch controls.

Figure 4-19: Etch Measurement Options dialog box - Etch Options page

Step Size
Step Size indicates in mm how much of the sample will be etched between each
measurement. The setting will depend on the sample and the data required. A step
size of 0.01 mm is typical. The step size appears in the etch control panel as the
Resolution.

I-etch Limit
This controls the maximum current drawn during etching. Although some current
needs to be drawn to etch at a reasonable rate, this must not be excessive as it may
cause the bottom of the etch hole to become pitted or uneven due to insufficient
removal of dissolution products. The maximum etch current that can be drawn
without such problems is sample dependent and can be set accurately only by trial
and error.

Circulation Pump
It is often beneficial to ensure that the electrolyte is refreshed by pumping it through
the contact area. This also helps to remove soluble dissolution products from the
sample surface. Some semiconductor materials such as silicon can generate gas at
the etching surface, while others such as compounds containing aluminium can
form difficult-to-remove films. Using the pump helps mitigate these concerns.

Etching Modes
This enables the selection of either constant current or constant voltage for etching.

With constant current the etch rate is not structure dependent. Do not select this
facility if you wish to monitor changes in etching current as an indication of
otherwise undetectable changes in crystal quality or a hetero-junction where the
doping level remains constant.

With constant voltage the etch rate is structure dependent and this can be used to
stop the etching at a certain point in the structure.

4-22 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

NOTE
The field shown in Figure 4-19 as I-etch Target will change to I-etch Constant
or I-etch Limit according to the etch mode selected.

Constant Current (p-type)

Set a value in I-etch Constant.
The drive circuitry is put in constant current mode at the set current. Etching is
timed, I-etch is not measured.

Uncontrolled
Set a value in V-etch.
Set a value in I-etch Limit that is above the maximum Ietch required.
The value entered for V-etch and Lamp are held constant and the etch current is
allowed to vary. If I-etch exceeds I-etch Limit, the process pauses.

Lamp Control (n-type)

Set a value for V-etch.
Set a target current in I-etch Target.
This option maintains a constant I-etch by adjusting the lamp automatically. If
the lamp reaches 100%, the process pauses.

V-etch Control (p-type)

Set a value for V-max.
Set a value for I-etch Target.
This option maintains a constant I-etch by adjusting V-etch automatically.

Etch Area
For n-type material this parameter causes the surface capacitance values for the
excess (wetted-illuminated) area to be subtracted from each reading. The software
automatically calculates the capacitance of this annular excess area from the ring
areas (specified in the Sealing Rings dialog box Section 4.5.3). At each subsequent
point, the excess capacitance is subtracted from the total wetted capacitance to
obtain the correct carrier concentration profile.
It is possible to correct data for excess area compensation after the data is acquired
using the Reprocessing program.

ECV Pro User Manual 4-23

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

Change Reagent

This page is available to all users. Its purpose is to allow a change of electrolyte
when the etch shows that a layer of a different material has been reached. The user
will need to PAUSE the etch so that the OPTIONS button becomes available. The
instructions and progress messages on screen are self explanatory.

Figure 4-20: Etch Measurement Options dialog box - Change Reagent page

4-24 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

4.2.8 Depletion Profile

For low to moderately doped samples, you can explore the concentration profile within
the available depletion region without etching the surface. This facility can be used in
the following ways:

- for non-destructive profiling of suitable samples

- to obtain as near-surface data as possible

- to anticipate results during etch profiling

to assist the selection of a suitable Vmeas for samples of all concentrations. This, together
with the CV curve, is similar to an automated spot-measure.

Figure 4-21: Depletion Profile screen

Command bar functions available with this sub-navigation function are:

• Measure Setup (Section 4.2.8.1)

• Graph Options (Section 4.2.8.2)

• Mouse Mode (Section 4.2.8.3)

• Print (Section 4.2.8.4)

• Save (Section 4.2.8.5)

• SaveAs (Section 4.2.8.6

• Read (Section 4.2.8.7)

ECV Pro User Manual 4-25

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

4.2.8.1 Measure Setup

Before measuring, you must set the range of measuring voltages (X) and carrier
concentrations (Y). Generally, use a wide concentration scale and a voltage X-axis to be
sure results appear in real-time. The graph is automatically auto-scaled on completion.

Figure 4-22: Depletion Measurement Options dialog box

N Range
Enter the expected carrier concentration range.

Voltage Range
There are two methods for setting the voltage scale:

• Enter the voltage directly.

• Use the well-behaved diode range determined in the CV curve.

Normally, a CV curve will have been acquired over a suitable voltage range
and the same range can be selected for the depletion profile. Set the graph scale
on the CV curve to view only the diode region then transfer this range into the
Depletion Scale dialog box by clicking on Get CV Graph Range.

Direction
It is best to select the direction of profiling according to type as indicated, as the
measurement then proceeds from the inside towards the surface, that is from reverse
towards forward bias.

Measure
Click here to save the values as in Apply, below, and start the measurement.
Depletion measurement takes about two minutes to complete. It will terminate
early if the current limit is exceeded. Use the Stop button that appears, to abort the
procedure.

Apply
Stores the values set in the dialog box ready for saving in the recipe. The values will
be lost if you exit from the program or load a different recipe before saving to the
recipe.

Cancel
Revert to the recipe or previously applied values.

4-26 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Jobs

4.2.8.2 Graph Options

To view an area of graph defined by specific coordinate ranges, set the coordinate ranges
for X and Y then click on Set Fixed Scale. To return to the default full scale view, click
on Auto-Scale to Data.

Note that the grid lines can be toggled on/off using the keyboard key F9.

Figure 4-23: Depletion Graph Options dialog box

4.2.8.3 Mouse Mode

The current mouse mode setting is displayed under the title of the button. Available
modes and the function keys that may be used to select them are:

Normal (F1)
Provides normal mouse pointing and clicking functions.

Zoom (F2)
Move the cursor to one corner of the desired region, press the Left button, and
drag to the opposite corner. When you release the Left button, the graph will
rescale to the defined rectangle. To return to default scaling select the Graph
Options and Auto-Scale to Data.

Line Draw (F3)

Hold the left mouse button down and drag the mouse across a graph to draw a
line. These lines may be drawn for illustrative purposes. Only one line at a
time can be drawn and it is not transferred to the printer.

Add Text (F5)

The point where you click the Left button becomes the origin of a comment to
be added to the graph. Enter your comment in the dialog which appears.
Comments follow the graph scaling and are transferred to the printer.
To enter another comment, you must select the Add Text function again.

Delete Text
Select this mode to delete all text that has been added to the graph using the
Add Text function.

ECV Pro User Manual 4-27

9PROF-UM01 Issue 1.0
Profiler Software
Jobs

4.2.8.4 Print
Sends the currently displayed graph to the printer.

4.2.8.5 Save
Writes data from the active graph to file. The name will be as specified when the sample
was opened. The extension will be made up from a two character type identifier, and a
sequence character.

4.2.8.6 SaveAs
Resave the active graph data with a new file name.

4.2.8.7 Read
Display a graph from previously saved data.

4.2.9 Check Contacts

This is a manual way of making and confirming contacts to the sample. Contacts are
checked automatically in the sample mounting procedure, but you may need to repeat
contact formation and checking in some circumstances.

Figure 4-24: Check Contacts screen

Contact selection for measurement is made when the material is specified (see
Section 4.5.1). Front and Back contacts must be selected and checked individually if
both are to be used.

The contact resistance is measured by passing a current in both directions between the
contact pair, and measuring the voltage. Resistance values will vary according to the
sample charactistics, but in general should be less than a few 100 ohms.
Contact Blasting uses inductive flyback pulses to form contacts. Each pulse is of fixed
energy, which you can set. Repetetive pulses can be generated.

4-28 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
System

4.3 System

The System screen is only available to Supervisor level users.

Figure 4-25: System screen

Sub-Navigation functions available are:

• Equipment Status (Section 4.3.1)

• Manual Control (Section 4.3.2)

• Condition Electrodes (Section 4.3.3)

ECV Pro User Manual 4-29

9PROF-UM01 Issue 1.0
Profiler Software
System

4.3.1 Equipment Status

Shows information about the system configuration, self-test results, and sample data.

Figure 4-26: Equipment Status screen

4.3.2 Manual Control

CAUTION
Unsupervised use of these functions could lead to equipment and sample
damage. This sub-menu allows the operation of individual items for testing
purposes. It is present so that a service engineer may ask a supervisor to
perform manual operations to achieve diagnostics over the phone.

4.3.3 Condition Electrodes

It may be necessary to manually electrolyze the platinum electrodes if they become badly
contaminated in use. About 15 seconds in each direction should be sufficient. A short
conditioning takes place automatically at the start of each measurement function.

Figure 4-27: Electrode Conditioning dialog box

4-30 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Recipes

4.4 Recipes

The recipes are available at both Operator and Supervisor levels. At Operator level,
however, access is restricted to selecting an existing menu.

4.4.1 Recipe List

When this sub-navigation function is selected, a list of all recipes stored in the system
will be displayed.

Figure 4-28: Recipe List screen

To Select a recipe for application to a measurement,

click on the recipe name to highlight it then click on Select.

To Delete a recipe (Supervisor level only)

click on the recipe name to highlight it then click on Delete. You will be prompted

Click on Yes or No as appropriate.

Before deleting, a backup copy of the recipe will automatically be made.

ECV Pro User Manual 4-31

9PROF-UM01 Issue 1.0
Profiler Software
Recipes

4.4.2 Create Recipe

Available at Supervisor level only.

Figure 4-29: Create Recipe screen

Enter the name for the new recipe and (optionally) a useful description. Click on Save to
save the current settings under the entered name.

To amend a recipe, make the changes in the settings then create a new recipe with the
same file name. You will be prompted with

Reply Yes or No as appropriate.

4-32 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Recipes

4.4.3 Backup Recipe List

Available at Supervisor level only.

Figure 4-30: Backup Recipe List screen

Enables previously deleted or overwritten recipes to be restored to the same or a new

name.

To restore a recipe to its original name:

Click on the recipe to highlight it.
Click on Restore.

To restore a recipe to a new name:

Click on the recipe to highlight it.
Enter a name in the Restore to: box.
Click on Retsore.

To delete a recipe from the backup list:

Click on the recipe to highlight it.
Click on Delete. You will be prompted

Click on Yes or No as appropriate.

ECV Pro User Manual 4-33

9PROF-UM01 Issue 1.0
Profiler Software
Setup

4.5 Setup

The Setup screen is available to Supervisor level users only.

Figure 4-31: Setup screen

Sub-Navigation functions available are:

• Material (Section 4.5.1)

Select the semiconductor material, and the contacts to be used.

• Reagent Handling (Section 4.5.2)

Select the electrolyte to be used and set the parameters for filling, flushing and
debubbling the cell.

• Sealing Rings (Section 4.5.3)

Define the effective sealing ring areas.

• Capacitance Params (Section 4.5.4)

Configure the capacitance measurement parameters

• Users (Section 4.5.5)

Maintain the list of users of this system

• Printer & Page Setup (Section 4.5.6)

Select the printer, and set the page orientation and margins.

• Multi-Graph (Section 4.5.7)

Print several small graphs per sheet of paper.

4-34 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Setup

• Configure Warning Tower (Section 4.5.8)

Configure the warning tower signals.

4.5.1 Material

Figure 4-32: Material Selection dialog box

Semiconductor Material
Specify the semiconductor material of your sample.
For simple binary semiconductors, the Fraction value should be zero.
For ternary materials, enter the fraction and select the name of the second material.
For example GaAs + InAs = InGaAs.

Dielectric and etching constants are obtained from the system database. Linear
interpolation is used to obtain values for ternary materials.

Contacts
Select which contacts to use as appropriate for the sample to be measured.
Specify a maximum contact resistance (greater than zero) to be used for routine
contact verification.

4.5.2 Reagent Handling

4.5.2.1 Select
Select the electrolyte to be used. This applies the filling and circulating control settings
entered for the electrolyte.

The initial set of electrolytes are the base set, they cannot be amended or deleted. New
electrolytes can be added, amended and deleted as required. A detailed description of
electrolytes can be found in Chapter 6.

The Prime, Drain and Clean Settings

These control various components of the manifold and drain routines. Values set
have been established as a good working set. Only in the event of an untried
electrolyte, for which these settings do not seem suitable, should the settings be
changed, and then only following consultation with Accent.

ECV Pro User Manual 4-35

9PROF-UM01 Issue 1.0
Profiler Software
Setup

Circ. Pump Volts

Sets the speed of the circulation pump that can be used during the etch measurement
(see Figure 4-19).

Rinse Cycles
Increase this value if the cell and manifold require longer rinse cycles to remove the
remnants of the electrolyte.

Figure 4-33: Reagent handling screen - Select

To select an electrolyte:
simply click on the electrolyte to highlight it then click on OK.

To add an electrolyte:
- insert a name for the electrolyte,
- enter the debubbling and rinse settings,
- click on Save.

To amend a user entered electrolyte:

- click on the electrolyte to select it,
- enter the new debubbling and rinse settings,
- click on Save.

To delete a user entered electrolyte:

- click on the electrolyte to select it,
- click on Delete.

4-36 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Setup

4.5.2.2 Flush
Use this page when it is necessary to change to a different electrolyte. Move the
electrolyte dip tube into a small bottle of DI water then click on Flush Reagent. The
routine will flush the system through with clean water several times until the bottle of
water is empty.

Figure 4-34: Reagent handling screen - Flush

4.5.3 Sealing Rings

Several complete ring assemblies may be available for different purposes, e.g. specific
electrolytes. It is convenient to measure these rings when they are first installed, and
store the areas together with an identifying name in a database of rings.

The Wetted and Illuminated area values can be entered manually in the Areas section
(see Figure 4-35) or they may be calculated by the software after entering the coordinates
in the Measuring Microscope Method section. The Measuring Microscope Method
section also provides a simple way to check whether there has been any deterioration in
your sealing ring.

Sealing Ring Name

For an existing ring - select a sealing ring from the list.
The areas will automatically appear. The Excess area is (Awet - Aillum)/Aillum.
For a new ring - enter the name in this box.

Areas
Enter in the wetted and illuminated areas manually.

ECV Pro User Manual 4-37

9PROF-UM01 Issue 1.0
Profiler Software
Setup

Figure 4-35: Sealing Rings dialog box

Measuring Microscope Method
Enter coordinates obtained from a measuring microscope while examining a blue
slice. Data entry boxes are arranged pictorially, and you may enter either horizontal
or vertical co-ordinates, or both.

When you click on the Calculate button, the results will be placed in the area boxes
if no error occurs. A status message indicates any errors. Check that the areas and
excess percentage are reasonable values.

OK
Click on OK to exit from the dialog box to use the areas displayed.
You can carry on measurements using the data displayed without saving it to the
database.

Cancel
Click on OK to exit from the dialog box with the previously selected sealing ring
still selected.

Delete Ring
Deletes the selected ring from the database. This action cannot be cancelled.

Save Ring
Modifies the areas of an exisiting entry, or creates a new entry if necessary. This
action cannot be cancelled.

4-38 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Setup

4.5.4 Capacitance Params

Figure 4-36: Capacitance Measuring Parameters dialog box

Primary Frequency (Hz)
The admittance measuring system uses a sine wave to measure capacitance. The
traditional frequency is 3 kHz, but a wide range is available from 300 Hz to 50 kHz.
Choosing the proper frequency is important as the frequency has a significant effect
on the measurements. Some criteria for selecting a frequency are:
· where series resistance is high (as can be seen in either spot measurement or the
CV curve), try a lower frequency.
· where parallel leakage is high, try a higher frequency.
· to determine a suitable model, you need results from two or more frequencies.
· to check for contaminated electrodes

The secondary frequency is shown below the Primary frequencies.

Amplitude
The default amplitude of the sine wave is 200 mV. This may be increased for low
doped samples with a large diode region available. It should be reduced for high
doped samples where the diode region is narrow.
The amplitude can be seen on the CV curve, where you must check that it does not
extend into regions where 1/C2 is not linear. On the IV curve, check that the
amplitude does not extend into an area of leakage current.

dV
The differential capacitance (dC/dV) is obtained by applying a small DC bias above
and below the set bias level. The value of dV is the total voltage of this
perturbation.

Model
Admittance measurements can be interpreted in three ways in deriving doping
concentration information:
Parallel - generally used for epi-layers on conducting substrates.
Series - generally used for implants and epi-layers on insulating substrates.
3-Term - this is the best generic model and is recommended for use in most cases.
Model selection affects Etch and Depletion measurements.
CV curves can show models superimposed so that you can see what effect model
selection has as a function of bias.

ECV Pro User Manual 4-39

9PROF-UM01 Issue 1.0
Profiler Software
Setup

Adjust dV (applicable to 3-Term only)

Calculates the actual voltage drop across the semiconductor/electrolyte
interface by removing any voltage drop across the series resistance.
The model on which the calculation is based is represented in Figure 4-37.

Rs

Rp

Figure 4-37: 3-Term circuit representing the semi-conductor/electrolyte junction

I-meas Limit
The current drawn when measuring the sample's admittance should be kept to a
minimum. I-meas Limit sets a maximum current value that stops the measurement,
if the measurement current is exceeded during a CV, Depletion, Etch or Spot
measurement. This is to protect the sample from drawing excess current which may
remove or deposit layers of material.

For IV graphs, the current limits are equal to the measurement scale range.

Set Defaults
These buttons provide sets of default values for high, medium and low doped
samples. It will still be necessary to select the Model and set the I-Meas Limit.

IMPORTANT
These defaults are only guideline values. Tests using IV, CV and spot
measurements are still necessary to achieve good results.

4-40 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Setup

4.5.5 Users

Figure 4-38: User List Maintenance dialog box

To set up a new user:
- enter the name in the User List box
- enter a password (if required) in the Password box
- specify the authority level of the user
Operator gives restricted access intended for processing using installed recipes
Supervisor allows full access to program functions
- click on Save User.
If the password is left blank, then the user can log in without entering any password.

Modify Existing User

Select the user from the User List, modify the password and/or level, then click on
Save User.

Delete User
Select the user from the User List, then click on Delete User.

4.5.6 Printer & Page Setup

This is the standard Windows page setup dialog box. You can select the printer, paper
orientation, and margins for your graphs.

Figure 4-39: Page Setup dialog box

ECV Pro User Manual 4-41

9PROF-UM01 Issue 1.0
Profiler Software
Setup

4.5.7 Multi-Graph

Not yet available

4.5.8 Configure Warning Tower

You can configure the Warning Tower to operate acording to your own scheme. The
events which cause warnings are listed, and by selecting one you can view or change the
color and state of the warning signal.

Figure 4-40: Warning Tower Setup dialog box

The Save button writes the complete scheme to the system database, which will become
the startup default.

4-42 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Profiler Software
Datalog

4.6 Datalog

4.6.1 Activity Log

Events occurring in the program are automatically recorded and appended to the end of
the file, so they appear in chronologon8coarso th, earso dat(l)8.6(e)-1. &so tey

ECV Pro User Manual 4-43

9PROF-UM01 Issue 1.0
Profiler Software
Alarms

4.6.2 Auto-Save Options

When the Save option is selected, graph data files that are selected in this dialog box will
be automatically saved with a numerically incremented file name based on that specified
when the sample was loaded.

Figure 4-43: Datalog - Auto Save Options screen

4.7 Alarms

Not yet available

4.8 Help

Not yet available

4-44 ECV Pro User Manual

9PROF-UM01 Issue 1.0
Chapter 5: Samples

5.1 About the sample

NOTE
For novice users, it is strongly recommended that the first samples attempted
be as simple as possible. Moderately doped n- and p-type substrates would be
a good choice.

Before mounting the sample, important choices need to be made, such as selecting an
electrolyte. The following table lists a number of sample features and the hardware and
software setup choices they influence. Each of these topics is discussed in greater detail
in subsequent subsections.

Sample feature Hardware and software setup

Semiconductor material Electrolyte choice

Safety concerns

Software 'material' settings

Substrate type Front or back contacts

Software 'model' settings

5.2 Sample size

The minimum sample size is 15mm x 10mm. This allows for 12mm between front
contacts and a 5mm diameter vacuum hole.

The maximum sample size is up to 6 inch diameter.

ECV Pro User Manual 5-1

9PROF-UM01 Issue 1.0
Samples
Sample cleaning

5.3 Sample cleaning

The sample must be as clean as possible before attempting the ECV profile. Surface
contamination and oxide can cause the following problems:

• difficult ohmic contact formation

• difficult bubble removal

• uneven etching.

The sample should be cleaned using normal techniques. For example, GaAs samples can
be cleaned with alcohol. If a native oxide is suspected, remove using a strong
hydrochloric acid (5 M) clean for 30 - 60 seconds.

Always inspect the sample surface for defects and marks. Select an area for profiling that
is as clean as possible.

5-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
Chapter 6: Electrolytes

CAUTION
The electrolytes used with this system are potentially hazardous. Refer to the
section on Safety (Section 1.2) and consult your safety officer before preparing
or using these electrolytes. Data sheets for chemicals supplied by Accent are
available on request.

The electrolyte has a double function in ECV:

• It forms an electrical contact to the semiconductor, similar to a Schottky diode.

• Under the correct conditions it will have a controlled electrochemical dissolution

reaction with the semiconductor, removing a given thickness of material per unit
charge passed.

The electrolyte must be transparent to the illumination used for etching, non corrosive to
the plastics used in the construction of the cell and be reasonably safe to handle.

ECV Pro User Manual 6-1

9PROF-UM01 Issue 1.0
Electrolytes
Electrolytes and applications

6.1 Electrolytes and applications

Three basic categories of electrolyte are used in ECV profiling:

• acidic

• basic

• complexing

Electrolytes that have been successfully used with different materials are:

Semiconductor 1st Electrolyte Choice 2nd Electrolyte Choice

GaAs (>1018 cm-3) Diaminoethane:EDTA Tiron
n-GaAs (<1018 cm-3), Tiron Diaminoethane:EDTA
HiLo structures
AlGaAs (<50% Al) Diaminoethane:EDTA Tiron
GaAsP/GaP Diaminoethane:EDTA Ammonium Tartrate/NH4
InAs Diaminoethane:EDTA Ammonium Tartrate/NH4
InP Diaminoethane:EDTA Ammonium Tartrate/NH4
InGaAsP Diaminoethane:EDTA Ammonium Tartrate/NH4
InGaAs/InP Diaminoethane:EDTA Ammonium Tartrate/NH4
InGaAs/GaAs Diaminoethane:EDTA Ammonium Tartrate/NH4
GaInSb Tiron NaOH:EDTA
GaN H2SO4 (0.2M) KOH (0.002M)
GaSb Tiron NaOH:EDTA
Si NaF/H2SO4 Ammonium Bifluoride (0.1M)
Ge NaOH (0.5M)
CdTe NaOH (0.5M)
AlGaInAs Diaminoethane:EDTA Tiron
AlGaInP Diaminoethane:EDTA Tiron
AlGaN H2SO4 (0.2M) KOH (0.002M)

6-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Electrolytes
Electrolyte preparation

6.2 Electrolyte preparation

CAUTION
Read MSDS sheets before attempting to prepare electrolytes. Use safety eye
wear, rubber gloves and protective clothing as appropriate. Prepare all
electrolytes under a fume hood.

Ensure that all electrolytes are correctly labeled.

6.2.1 Ammonium bifluoride solution

(I. Mayes, Accent/Bio-Rad application note #202, March 1985)

Prepare a 0.1M solution of ammonium bifluoride (NH4F.HF (FW57.04)) in deionized

water. A small quantity of a wetting agent such as Triton X-100TM can be added to
reduce the surface tension and assist in bubble removal.

The shelf life of the solution, without wetting agent and stored in a plastic container, is
about one month. Solutions with wetting agent should not be stored.

6.2.2 Ammonium tartrate solution in ammonium hydroxide

Dissolve 110g of ammonium tartrate (NH4)2C4O6 (FW184.15) in a minimum volume of
deionized water.

Carefully in a fume hood and while cooling the mixing vessel, add concentrated
ammonium hydroxide (minimum 28% NH4) to the ammonium tartrate solution to give a
total volume of 1000 ml.

The pH of the final solution should be 11.5 or higher.

Store the electrolyte in a glass bottle with a tight fitting stopper. The shelf life of this
solution is two months or when the pH drops below 11.5.

This electrolyte has an obnoxious smell and for this reason is not commonly used. The
1M NaOH electrolyte has equivalent properties.

ECV Pro User Manual 6-3

9PROF-UM01 Issue 1.0
Electrolytes
Electrolyte preparation

6.2.3 Hydrochloric acid electrolyte, HCl, Sulfuric Acid H2SO4

(T. Ambridge, D.J. Ashen, 'Automatic electrochemical profiling of carrier concentration
in InP', Electronic Letters, Vol 15, No 20, pp 647-648, Sept 1979)

Prepare a 0.5M solution of HCl or 1M H2SO4 in deionized water.

CAUTION
Always add acid slowly to water. NEVER add water to acid. Avoid breathing
fumes.

0.5M hydrochloric acid and 1M sulfuric acid have a six month shelf life when stored in a
tightly closed bottle.

6.2.4 Diaminoethane (Ethylene Diamine), EDTA

(Bio-Rad information sheet, ‘Characterization of InP and related materials’, July 1990)

This electrolyte can be used with GaAs and InP and possibly other III-V materials. The
excess area can be large, so use with a large sealing ring.

Prepare a 0.2M EDTA solution and add 10% Diaminoethate (Ethylene Diamine). Shelf
life 1 month.

6.2.5 Sodium fluoride : sulfuric acid

(W.Y. Leong, R.A.A. Kubiak, E.C. Parker, 'Dopant profiling of Si MBE material using
electrochemical C-V technique', Proc. of the first international symposium on MBE
silicon, Toronto, Canada, Vol 85-7, pp 140-148, The Electrochemical Society 1985)

CAUTION
Avoid inhaling NaF dust.

Into a 0.05M H2SO4 solution, add sufficient NaF powder to make the solution 1M NaF.
Stir until the NaF is completely dissolved.

This solution is usually used diluted with deionized water in the ratio 1 part NaF solution
: 2 parts deionized water.

A wetting solution such as Triton X-100TM is also often added to the diluted solution to
assist in bubble removal.

The stock solution has a shelf life of one month when stored in a plastic bottle. Do not
store the diluted solution, or a solution with a wetting agent added.

6-4 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Electrolytes
Electrolyte preparation

6.2.6 Sodium hydroxide : EDTA

(G. Cabaniss, 'Compound semiconductor characterization by electrochemical C-V
analysis', Solecon Laboratories Inc, application note No 201, 2241 Paragon Drive, San
Jose, Ca 95131)

Prepare a 0.2M sodium hydroxide (NaOH) solution in deionized water. Into 250 ml of
the 0.2M NaOH solution, add 9.3g of disodium ethylenediamine tetra acetate
(FW372.24). Stir until completely dissolved.

The NaOH : EDTA should be stored in a suitable plastic container, in which its shelf life
is two months.

6.2.7 Tiron electrolyte

(T. Ambridge, J. Stevenson, M. Redstall, 'Applications of electrochemical methods for
semiconductor characterization', J. Electrochem. Soc. Solid State Science and
Technology, Vol 127, no 1, pp222-228)

Tiron is 1,2 dihydroxybenzene-3,5-disulphonic acid disodium salt

C6H2(OH)2(SO3Na)2.H2O (FW332.22).

ECV Pro User Manual 6-5

9PROF-UM01 Issue 1.0
Electrolytes
Electrolyte preparation

6-6 ECV Pro User Manual

9PROF-UM01 Issue 1.0
Chapter 7: The Electrochemical Cell

IMPORTANT
Please read this chapter before you attempt to run any sample on your system.

7.1 The cell

The electrochemical cell (referred to as the cell) is one of the most important parts of
your system. Treat it with care.

Figure 7-1: The electrochemical cell

The functions of the cell are:

• To contain and isolate the electrolyte that is used to etch and form electrical contact
to the sample

• To house the electrodes and provide an electrical interface to the rest of the system

• To remove bubbles from the sample surface

• To allow uniform illumination of the semiconductor : electrolyte interface.

ECV Pro User Manual 7-1

9PROF-UM01 Issue 1.0
The Electrochemical Cell
The sealing ring

7.2 The sealing ring

As with all capacitance-voltage techniques, contact area definition is critically important

for obtaining accurate carrier concentration results. With electrochemical C-V, the
accuracy of the etch depth is also dependent on the correct area being used in the
calculations.

Of the possible methods of defining an area of electrolyte contact onto a semiconductor

surface, the convenience and flexibility of the sealing ring makes it the best choice.

The ECV technique requires that the area of the electrolyte contact to the semiconductor,
necessary for C-V measurements, is etched to profile through the sample. Since etching
of n-type material requires illumination, the sealing ring acts as a mask, allowing
(ideally) the total wetted area to be illuminated.

To perform these functions, the sealing ring is made of an opaque material that is resilient
enough to form a seal to contain the electrolyte, yet also be hard enough to form a knife
edge seal allowing illumination over the total wetted area.

The sealing ring defines the area reproducibly and allows illumination of typically 98%
of the total wetted area. The small ring of material that is in contact with the electrolyte,
but not illuminated is called the ‘excess area’. The large majority of the area, which is
illuminated, is called the ‘illuminated area’.

As p-type material does not need light to etch:

wetted area = p-type etch area

illuminated area = n-type etch area

Capacitance is measured over the total wetted area, whether the material is n-type or
p-type. When n-type material is etched, the annular excess area that contributes to the
capacitance but does not etch will cause an error in the measurement, unless it is
compensated for.

The software will compensate for excess area when profiling n-type material. However,
the wetted and illuminated areas should be measured accurately and entered into the
Sealing Rings dialog box (select SEALING RINGS in the sub-navigation bar of SETUP, see
Section 4.5.3). For a detailed discussion of how excess area compensation works and the
effects of miscalibration, see Section 2.3.

The contact areas used in ECV are typically much larger than those used in conventional
C-V. This is because:
• The electrolytes used in ECV process are generally aqueous and exhibit high
surface tension
• As the technique requires etching into the material, the contact area needs to be
large compared to the side wall of the etch hole. This is especially important when
profiling hi-lo structures.
• As the excess area becomes proportionately smaller as the area increases, the areas
are more accurately defined for larger contact areas
• It is physically easier to remove bubbles from the larger contact areas.

7-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 The Electrochemical Cell
Removing/inserting the cell

7.3 Removing/inserting the cell

When the cell is installed it is locked into position as shown in Figure 7-2.

Figure 7-2: Cell locked into position

To remove the cell, pull the lever forward slightly then move the lever down to the
position shown in Figure 7-3. The cell is pushed out and can then easily be removed from
the profiler.

Figure 7-3: Cell in the unlocked position

To insert the cell, reverse the process, making sure that the lever is initially in the down
position as shown in Figure 7-3.

ECV Pro User Manual 7-3

9PROF-UM01 Issue 1.0
The Electrochemical Cell
Inserting/replacing the sealing ring

7.4 Inserting/replacing the sealing ring

IMPORTANT
Removing/inserting the sealing ring holder from/into the cell requires firm
pressure. It is imperative that the cell is removed from the instrument before
attempting to change the ring. Failure to conform to this practice is likely to
adversely affect the alignment of the cell.

The sealing ring is fixed in a holder. When it is necessary to change the sealing ring , the
complete holder must be removed and replaced.

Figure 7-4: The cell with a sealing ring inserted

To remove a sealing ring:

- insert your thumb into the hole and pull the holder horizontally out of the fixing.

To insert a sealing ring:

- ensure that the ring is completely clean using clean water and ultrasonic cleaning
- slide the holder into the slot and push it in until it is hard against the cell moulding.

7.5 Problems with sealing rings

7.5.1 Leaking
Assuming that the sample is correctly mounted, electrolyte will only leak from the seal
if:

• there is gross damage to the sealing area

• there is a very poor sample surface

• the sealing area is too close to the sample edge

• the profiler mechanism has failed to move the cell fully forward onto the sample.

7-4 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 The Electrochemical Cell
Problems with sealing rings

Ring Etch hole Profile

Normal ring and etch hole

Compressed ring base causing shadowing

Damaged sealing edge causing leakage

Trapped bubble

Worn sealing edge causing large excess area

Figure 7-5: Ring and etch problems

7.5.2 Large excess area

The excess area is usually expressed as a percentage of the wetted area and is due to the
spread of electrolyte into a shaded region of the sealing area. The degree to which the
electrolyte penetrates under the sealing edge of the ring depends on:

- the surface tension of the electrolyte : semiconductor surface

- the roughness of the semiconductor surface
- the condition of the sealing edge of the ring
- the pressure by which the sample is held in place.

When the cell is set up correctly and the sealing ring is in good condition, typical
percentage excess areas are:

Tiron 1-3%
HCl 3-5%
EDTA:NaOH 5-7%

If the excess area percentages increase much above these levels, examine the sealing
edge of the ring for damage or excessive flattening. Typically, a damaged sealing edge
will show up as a leakage mark when calibrating with a blue slice. An increase in
percentage excess area uniformly around the diameter is usually due to a worn sealing
edge.

ECV Pro User Manual 7-5

9PROF-UM01 Issue 1.0
The Electrochemical Cell
Calibration

7.6 Calibration

The only calibration required for the ECV Pro is that of the wetted and illuminated
contact areas to the semiconductor surface. These areas must be measured accurately
before accurate carrier concentration and depth measurements can be made with the
system.

Apart from giving inaccurate results in terms of absolute values, miscalibration can also
distort profiles of certain sample structures due to the effects of the excess area
capacitance. Samples particularly susceptible to this distortion are hi-lo n-type structures
(MESFETs) and samples with 'spikes' in the profile. To see the effects of miscalibration,
see Section 2.3.

7.6.1 When to calibrate

It will be necessary to calibrate the sealing ring:

• Whenever you replace or re-insert the sealing ring

• If you use different electrolytes with a sealing ring (because the different surface
tension will cause different electrolyte spread)

• On a regular basis (dependent on use) to monitor sealing ring wear.

How frequently calibration is necessary depends on several factors:

• How often the system is used. Obviously, sealing rings wear out faster if the system
is heavily used

• Generally, the greater the number of users of the system the more often the system
will need to be calibrated. In most cases the best solution is for each individual users
to have their own sealing rings, that they are responsible for calibrating

• If the type of samples that are run on the system are of a hi-lo, n-type nature, it will
be necessary to keep the system in calibration with a greater degree of precision
than for samples of uniform doping

• If the system is left unused for a long period of time and the ring dries out, the ring
should be recalibrated

• If a new batch of electrolyte is prepared the ring should be recalibrated.

7.6.2 Blue slice calibration

The calibration procedure involves profiling a ‘blue slice’, just as you would a normal
sample and then measuring the wetted and illuminated areas using a measuring
microscope. The 'blue slice' is a piece of polished, n-type GaAs substrate that has been
anodized to grow an approximately 50 nm thick anodic oxide. This oxide is blue in color,
giving the sample its name. The illuminated area will be clearly visible, as n-type
material etches in the light. Although the wetted area does not usually etch with n-type
material, it is clearly visible with a blue slice run because the blue anodic oxide is
chemically removed by the electrolyte.

7-6 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 The Electrochemical Cell
Calibration

Blue slices can be purchased from Accent as part PN4116, but it is also possible to make
them yourself following the instructions in Section 7.6.2.1.

7.6.2.1 Making a blue slice

Blue slices can be prepared from polished n-type GaAs substrates (double side polished
wafers are best) as follows:

1. Carefully clean a polished substrate wafer of n-type (-1E17 to -5E18 cm-3) GaAs.

2. Prepare a solution of 0.2M EDTA (see Section 6.2) in deionized water.

3. Select a cathode of similar area to the wafer. Carbon, platinum or other non-reactive
conductors are suitable.

4. Make the substrate wafer the anode by forming an ohmic contact to the edge.
Connect a plastic coated wire to the contact and protect the exposed metal contact
with silicone rubber. No metal should be exposed to the solution.

5. Apply between 30 and 50V DC between the non-reactive cathode and the wafer
anode. The current supply should be limited to about 30 mAcm-2. As the anodic
film forms, the current will drop. Wait until the current drops to about 500 µA.

6. Remove the wafer and disconnect the wire. Wash the anodized wafer carefully in
deionized water.

7. Dice the wafer into approximately 1 cm squares.

40V DC
Anode Cathode

0.2M EDTA

Silicone
rubber

Figure 7-6: Setup for blue slice preparation

7.6.2.2 Procedure
To mimic as accurately as possible the conditions used when running a real sample, the
sample should be mounted exactly as it will normally (see Section 8.7). In addition, note
the following:

• Take extra care to clean and dry the sample before the run

• Take extra care to clean and dry the sealing ring before the run

ECV Pro User Manual 7-7

9PROF-UM01 Issue 1.0
The Electrochemical Cell
Calibration

• Etch into the sample only the minimum amount necessary to see the illuminated
etch area (typically about 0.5 mm). Any additional etching may give an exaggerated
excess area

• Before removing the sample, flush the cell several times to remove electrolyte from
the sample surface. Any electrolyte left on the sample when it is removed will
spread on the surface, increasing the excess area

• Remove the sample as soon as possible after the run

• Wash the sample immediately after removing it.

7.6.2.3 Measuring the areas

The best way to measure the wetted and illuminated areas is by measuring the etched
blue slice under a microscope. There are several ways to do this, the best method in each
case being dependent on the equipment available.

Excess area
Illuminated
etch edge
Wetted etch
edge

Figure 7-7: An etched blue slice showing the excess area

Measuring microscope method

This method requires access to a measuring microscope, or to a microscope with
cross hair eye pieces and drum vernier caliper stages. Slide vernier caliper stages are
not precise enough. To be able to distinguish the blue anodized region of the sample,
the microscope must also have through-the-lens illumination.

The procedure involves taking measurements, preferably in metric, across two

diameters of the etched blue slice. As long as the results are in metric they can be
entered directly into the ECV Pro software for automatic calculation of the areas -
see Section 7.6.4.

7-8 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 The Electrochemical Cell
Calibration

Microscope with camera

Microscopes fitted with cameras are suitable if the magnifications available are
sufficient. Usually one photograph of the whole etched area is necessary to measure
the total wetted area. Higher magnification photographs of different parts of the
excess area region (on different quadrants of the sample) are necessary to measure
the excess area and calculate the illuminated area. It is essential to calibrate the
microscope/camera carefully at each magnification used.

7.6.3 Alternative calibration method

It is also possible to calibrate the wetted and illuminated areas by etching, in two separate
runs, an n-type sample (requiring illumination), and a p-type sample (etching with
voltage alone, no illumination). This method is best suited for continual monitoring of
the cell's calibration over a period of time, between blue slice calibrations.

The region actually etched with p-type profiling may not reflect leakage due to a
damaged or worn sealing edge. The resistive path created by the sealing ring's pressure
against the sample could be sufficient to limit etching current outside the ring's normal
perimeter, and hence make the leak invisible on the etched p-type sample.

7.6.4 Entry of calibration data into the software

The wetted and illuminated areas can be entered directly into the ECV Pro software as
follows:

1. Select the SEALING RING from the sub-navigation bar of the SETUP function to
display the Sealing Rings dialog box (see Section 4.5.3).

2. Select the ring name for which you want to define the areas or enter a new name in
the Sealing Ring Name field.

3. Enter the new Wetted area and Illum. area values into the appropriate field of Areas,
or in the Measuring Microdscope Method section enter the measurements then click
on Calculate to have the software calculate the areas for you.

4. Click on Save Ring to store the values for the named sealing ring.

5. When you have finished, click on OK to exit.

ECV Pro User Manual 7-9

9PROF-UM01 Issue 1.0
The Electrochemical Cell
Calibration

7-10 ECV Pro User Manual

9PROF-UM01 Issue 1.0
Chapter 8: Etching a sample at Operator
user level

CAUTION
Running a sample on the involves the use of potentially hazardous chemicals.
Please read Section 1.2 on Safety before attempting these procedures.

This chapter takes you through the steps for making an etch profile at Operator user
level.

8.1 Overview
Once sets of parameters have been entered
into the machine and saved as recipes, Start up &
loading, etching and measuring a sample prepare machine
becomes a straight forward process. The
flowchart in Figure 8-1 illustrates the
process. The rest of the chapter describes
Prepare sample
the process in greater detail.

Procedure
Mount sample

Check
parameters

Etch

Procedure
Demount sample

End

Figure 8-1:Operator mode process flowchart

ECV Pro User Manual 8-1

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Startup

8.2 Startup

1. Open the front door of the instrument and press the large green button below the
keyboard to switch the instrument on (the large red button next to it switches the
machine off).

Instrument Off button

Instrument On button

Computer On/Off button

Figure 8-2: Inside the front door

2. Start the computer.

3. Load the ECVPro software by double-clicking the program icon . After a

few seconds the ECV Pro software will load with an Initialization dialog box within
the Login screen.

If no sample is loaded you will be requested to click on Initialize.

If a sample is still loaded from previous use you will be asked to click on Demount.

Figure 8-3: Initialize system dialog box

8-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Emergency stop

4. To Log in:
- click on Login in the top right corner of the screen
- enter your user name
- if necessary, enter a password
- click on Submit.

Figure 8-4: Login dialog box

If the login is accepted the operating screen (Figure 8-5) will appear ready for you to start
using the system.

Figure 8-5: Screen ready for starting measurement operations

8.3 Emergency stop

The large red button to the left of the wafer stage (see Figure 1-1) is the emergency off
button.

ECV Pro User Manual 8-3

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Keyboard function keys

8.4 Keyboard function keys

It is useful for the operator to be aware of the function of the following keys:

• F2 - return to normal mouse function

• F3 - zoom
Move the cursor to one corner of the desired region, press the Left button, and drag
to the opposite corner. When you release the Left button, a graph will rescale to the
defined rectangle. To return to default scaling select the Graph Options and Auto-
Scale to Data.
• F4 - line draw
Hold the left mouse button down and drag the mouse across a graph to draw a line.
These lines may be drawn for illustrative purposes. Only one line at a time can be
drawn and it is not transferred to the printer.
• F9 - toggles graph grid lines on/off
• F12 - toggles the camera view on/off

8.5 Load a Recipe

1. Select RECIPES in the navigation bar at the bottom of the screen.

2. Click on the required recipe to highlight it then click on Select in the right-hand
command bar.

8-4 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Prepare to mount the sample

8.6 Prepare to mount the sample

1. Ensure that the sample is of the correct size (minimum 12 mm2, maximum 150 mm
diameter) and is completely clean (see Section 5.3).

CAUTION
Use protective eyeware and clothing when handling chemicals or electrolytes.

2. Check that the correct electrolyte is available in the bottle rack (Figure 8-7).

3. Check that the electrolyte vacuum vapour trap is not full. If it needs empying,
unscrew the clear perspex base and dispose of the fluid safely according to local
safety regulations.

Figure 8-6: Electrolyte vacuum vapour trap

4. Check that the water bottle is in place with sufficient water and that the collection
bottle is in place with sufficient capacity for use. (A warning message is displayed
when the collection bottle is full.)

Used fluid collection bottle with

sensor attached for bottle full
notification

Clean water for flushing the

system

Electrolyte

Clean water for use when

changing electrolyte

Figure 8-7: Electrolyte and water bottle rack

ECV Pro User Manual 8-5

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Prepare to mount the sample

5. Replace the Splash Guard over the bottles as shown in Figure 8-8.

Splash guard in
place over water and
waste bottles

Figure 8-8: Splash guard

6. Ensure that a sealing ring is inserted in the cell and the cell locked in (Figure 8-9).

Figure 8-9: Sealing ring inserted into the cell and the cell locked in

7. Click on JOBS (which will now be available having selected a recipe) in the lower
navigation bar.

8-6 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Mount the sample

8.7 Mount the sample

The procedure for mounting a sample is wizard driven and is outlined in the flowchart in
Figure 8-10 . The steps are described in detail in the following paragraphs.

Enter filename details

to identify the sample

Position sample &

apply the vacuum
Check the quality &
position of the sample

Raise table &

latch into position
Remove the vacuum

Make &
No Unlatch &
check contacts.
lower table
OK?

Yes

Move cell back & Lock door &

unlock door move cell forward

Re-check
No & re-form contacts if
necessary.
OK?
Yes

No Ready to
measure?

Yes

Fill with electrolyte

& debubble

No
OK? Demount sample

Yes

End of mount sample

Figure 8-10: Flowchart of Mount Sample procedure

ECV Pro User Manual 8-7

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Mount the sample

1. Click on MOUNT SAMPLE in the JOBS sub-navigation menu bar to display:

Figure 8-11: Mount Sample - sample identification

2. Enter the following optional sample details if required:

- Wafer identifier
- Batch identifier
- Description
Click on Choose Path & Filename to display a standard windows Save dialog box as
follows:

Figure 8-12: Data file name specification

Select the storage location and enter the filename that is to identify the sample data.
Click on Save. The filename and path details will be displayed as in Figure 8-11.

8-8 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Mount the sample

3. Click on Next to continue the procedure and display the screen:

Figure 8-13: Mount Sample - sample loading

4. With the contacts raised (see Figure 8-14) place the sample on the stage so that the
area to be etched is immediately above the vacuum hole in the centre of the stage.

Contact arms

Vacuum hole

Contact arms
movement lever

Figure 8-14: Contacts raised

5. Using the Lever, lower the probes onto the sample as shown in Figure 8-15. The
vacuum will be applied automatically as the probes are lowered.

ECV Pro User Manual 8-9

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Mount the sample

Figure 8-15: Contact probes lowered onto the wafer

6. If necessary raise the probes and adjust

the position of the wafer so that the
required etch position is located as
shown in Figure 8-16.

Once vacuum is applied the Vacuum

Status box shown in Figure 8-13 will
display On and the Next button will
become available. Etch point

Figure 8-16:Position of etch relative to probes

7. When the wafer is positioned correctly, click on Next to display the Table
Movement dialog box. Initially the Door Status will show Down then, once the door
is raised, it will show Up. Finally, once the knob is turned anticlockwise to latch the
door in place, it will show Up + Locked (Figure 8-17) and Next will become
available.

Figure 8-17: Mount Sample - table movement

8-10 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Mount the sample

8. Click on Next to test the contacts. The quality of the contacts is indicated by the bar
charts. While the maximum resistance is exceeded the bar is red (Figure 8-18).

Figure 8-18: Mount Sample - make and check contacts (indication of unacceptable
ohmic contacts)

Blast until the actual resistance is less than the maximum (bar is green as shown in
Figure 8-19).

Figure 8-19: Mount Sample - make and check contacts (good contacts achieved)

Front or Back may be greyed if one is not specified to be used in the recipe.
The maximum contact resistance, as set in the recipe, is displayed between the two
bars. The actual resistance for both directions of current flow is displayed at the end
of each bar.
For a high resistance material, re-measure several times to ensure that the contact is
stable.

ECV Pro User Manual 8-11

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Mount the sample

9. Once good contacts are achieved, click on Next to display the screen for locking the
door electronically and move the cell forward onto the sample. To lock the door
click on Lock. When the door is locked and the cell moved forward, the Status will
display Ready and the Next button will become available as shown in Figure 8-20.

Figure 8-20: Mount Sample - door lock (electronically) & cell position

10. Having locked the door it is important to recheck the contacts, so when you click on
Next a repeat of the screen shown in Figure 8-19 is displayed.
11. If the contacts are acceptable and you wish to continue with the measurement, click
on Next.
12. The next screen (Figure 8-21) displays a warning to the effect that when you click
on Next in this screen, the cell will start to fill with electrolyte. This is therefore the
last point at which you can turn back without having contaminated the wafer with
electrolyte. After this point the only way to remove the wafer will be by executing
the Demount routine where the cell is drained of electrolyte and flushed with water
to cleanse it.
Click on Next when you are sure that all is ready to start filling with electrolyte.

Figure 8-21: Mount Sample - warning before filling with electrolyte

8-12 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Mount the sample

13. The screen shown in Figure 8-22 will be displayed and the cell will fill with
electrolyte. If there is insufficient electrolyte in the bottle to fill the cell or the pump
is temporarily blocked, a Refill button will appear as shown in Figure 8-23.

Figure 8-22: Mount Sample - filling with electrolyte

Figure 8-23: Mount Sample - refill button displayed

Replenish the electrolyte if necessary. Click on Refill to continue filling the cell.
When the cell is full of electrolyte the Status will display Fill Complete and the
Debubble button will become available.

14. Adjust the Lamp and Exposure so that the etch hole can be seen clearly and you may
find that you can see bubbles (see Figure 8-24).

ECV Pro User Manual 8-13

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Mount the sample

15. If bubbles are present click on Debubble.

The cell will be flushed through with recirculating electrolyte to move any bubbles.
This typically takes a few seconds and progress can be monitored on the screen.

Figure 8-24: Mount Sample - cell full but not debubbled

It will probably be necessary to click on Debubble several times. Starting at a speed

setting of 6, increase the speed to move persistent bubbles. As the process is
repeated the number of bubbles flushing away should be seen to reduce until
eventually, apart possibly for a few insignificant tiny bubbles around the perimeter,
just the flow of electrolyte may be seen. If a persistent bubble cannot be cleared,
press Drain + Refill to empty the cell and refill with electrolyte. A sufficiently
debubbled cell is shown in Figure 8-25.

Figure 8-25: Mount Sample - debubbled sufficiently

Once you are satisfied that the cell has been debubbled sufficiently, click on Finish
to exit from the Mount Sample procedure.

If debubbling is not satisfactory, click on Demount Sample so that the sample can be
removed and the problem investigated. The Demount Sample procedure is
described in Section 8.10.

8-14 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Checking Parameters

8.8 Checking Parameters

At this stage the ohmic contacts to the sample should have been formed, the cell filled
with electrolyte and any bubbles in the cell should have been cleared.

Before starting to etch the sample it is important to check that the parameters set in the
recipe are compatible with the sample.

Click on each of the following in the JOBS sub-navigation bar and check the parameters
as described.

8.8.1 Rest Potential

Click on MEASURE in the right-hand command bar. The measurement can be repeated as
many times as you wish, but it is important to wait at least ten seconds between
measurements. This allows the electrodes to fully recover.

Figure 8-26: Rest Potential screen

Check that the values displayed are within the range that you expect.

ECV Pro User Manual 8-15

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Checking Parameters

8.8.2 IV Plot
Click on MEASURE SETUP in the right-hand command bar to display the IV Measurement
Options dialog box.

Figure 8-27: IV Measurement Options dialog box

Click on Measure to start the IV data acquisition and produce a curve(s) such as that in
Figure 8-28.

NOTE
If the UV option is fitted, the message UV not stable may appear if the lamp has
not been on for approximately 7 minutes after starting the software. Continue if
the stability of the lamp is not critical at this stage.

Light curves

Dark

Figure 8-28: Typical IV curve - n-type material

Check that the curves are as you should expect.

For n-type material Vetch should lie within the flat zero current portion of the IV curve.
For p-type material Vetch should be set in the forward bias, conducting, region of the IV
curve. This value can be adjusted during profiling to give an appropriate etch current.

8-16 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Checking Parameters

8.8.3 CV Plot
16. Click on MEASURE SETUP in the right-hand command bar and display the CV
Measurement Options dialog box.

Figure 8-29: CV Measurement Options dialog box

Click on Measure to start the CV data acquisition and produce curves such as those in
Figure 8-30.

Series

Parallel

1/C2

Dissipation

Figure 8-30: Typical CV curve - n-type material

Check that the curve is as you should expect, the series and parallel curves should be
fairly close together and the dissipation should be low, typically less than 0.4.

Press the keyboard function key F3 to put the mouse in line draw mode. Draw a line on
the 1/C2 plot (as shown above) and check that the value of the concentration displayed in
the message bar is acceptable.

ECV Pro User Manual 8-17

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Checking Parameters

8.8.4 Spot Measure

Click on MEASURE in the right-hand command bar.
Check that the parameters Imeas, Dissipation, FBP and N are as expected.
Click on MEASURE several times to ensure stability.

Figure 8-31: Spot Measure screen

8-18 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Etch Profile

8.9 Etch Profile

Select ETCH PROFILE in the sub-navigation bar of JOBS.

8.9.1 Start etch profile

1. Click on MEASURE SETUP in the command bar to display the Etch screen, where the
command bar area of the screen is now replaced by an etch control panel as shown
in Figure 8-32.

Figure 8-32: Etch Control Panel screen

2. Ensure that the lamp is set at 1.

3. Click on START to begin etching and start the measurement.

The CLOSE button will be greyed and will remain so until the measurement stops or
is paused.
The START button will change to PAUSE so that the etch can be interrupted for
parameter adjustment if necessary.

4. The status bar should immediately display Measure then, after a few seconds (the
settling time), the measuring current Imeas will be displayed. Assuming that Imeas
does not exceed the Imeas limit, the measurement will proceed and the results section
will display the data from the first (Step # 0) surface measurement. The status bar
will then display ETCHING and the Ietch value, which should be small
(<0.1 ma/cm2), will be displayed.

ECV Pro User Manual 8-19

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Etch Profile

5. The Vmeas and Vetch area will initially display the relevant values set from the CV
and IV curves respectively. Once the first point has been plotted you should adjust
these values as follows:

If V-etch shows a value Const-I then the voltage will change automatically to
maintain a constant current.

If Const-I is not displayed for V-etch, then:

For n-type material

Verify that Vetch is at a value appropriate for the sample.
Slowly increase the lamp until Ie reaches a nominally low value,
dependent on the Resolution, until the % done field shows a moderate
steady rate giving an etch time of 10 - 30 seconds.
If Ie deteriorates by more than 10 - 20% over the cycle this is indication of
a film build-up on the surface of the sample. Slow the process down, by
reducing the lamp, to allow time for chemical removal of anodised film to
balance the anodisation rate.

For p-type material

Increase Vetch until Ie is approximately 0.1.
If Ie remains stable for a given Vetch then Vetch can be increased to give a
faster etch time (but do not reduce the etch time below 10 seconds).
If Ie gradually reduces for a given Vetch then reduce Vetch.

6. Once the sample has drawn sufficient etching current to have removed the
thickness of material set by the Resolution, the status bar will indicate Settling for
the time set, followed by Measure once more. The second step of measurement
data will appear in the results area (Step # 1).

7. For each measurement, a point will appear on the Log N vs. depth plot, and
another line of data will be added to the data log (if enabled).

Monitor the Dissip. and FBP values to ensure they remain at levels indicating that
the admittance values being measured are sensible.

Safe range of values

Imeas <0.1mA/cm2
Dissip. <0.4
FBP ±2.5V

8-20 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Etch Profile

To view the sample during etch, press F12 to display a camera view as shown in
Figure 8-33. Adjust the Exposure Level (in the camera dialog box) until you can see the
sample clearly.
Click on Close or press F12 again to cancel the view.

Figure 8-33: Etch profiling screen

8. If it is necessary to change to a different electrolyte at a specified point through the

etch, proceed as follows:

a. Click on PAUSE to stop the etching process.

b. Click on OPTIONS to open the Etch Options dialog box then select the Change
Reagent tab.

c. Move the dip tube from the electrolyte bottle and put it in a small bottle of DI
water.

d. Click on Start Change Sequence.

The routine will fill from the small DI water bottle and drain the electrolyte
tubes until the small bottle is empty. It will then fill from the large DI bottle,
flush the cell and wafer surface then drain the water, twice.

e. It will then instruct you to move the dip tube into the new electrolyte bottle.
Once you have done this, click on Continue. The cell will fill with electrolyte
then Finished Change will be displayed.

f. Click on OK to return to the Etch screen.

g. Press F12 to display the camera view and debubble the cell if necessary.

ECV Pro User Manual 8-21

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Etch Profile

h. Click on Start to continue the etch.

9. Once the etch procedure is complete the message bar displays End Reached
(Figure 8-34). Click on CLOSE to exit from the Etch panel and return to the Etch
Profile screen.

Figure 8-34: Completed Etch

10. Click on SAVE to save the etch graph data.

8.9.2 Interrupting a profile

To interrupt the etching process just click on PAUSE in the control panel.

If the etch is to be terminated completely:

Click on Close
Save the etch data, if necessary
Proceed to demount as described in Section 8.10.

To change parameters, at Supervisor User level only:

Click on OPTIONS to make changes to the etch options
Click on CLOSE to access screens for other parameter changes.

8.9.3 Restarting a paused profile

To restart a paused etch, click on START in the Etch panel.

8-22 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Demount the sample

8.10 Demount the sample

To remove a sample at any time after the cell has filled with electrolyte, the following
procedure wizard must be executed.

1. Select DEMOUNT SAMPLE to display:

Figure 8-35: Demount Sample - select demount routine

NOTE
Once one of the routines has been selected it is not possible to return to
the current etch.

In normal circumstances, click on Normal Demount to drain the electrolyte then

flush and clean the cell with water.

In an emergency if, for example, there is a leak, click on Quick Demount to simply
remove electrolyte quickly from the system.

The Status box displays the current activity.

If there is insufficient water available, the following message appears below the
Status box:

Figure 8-36: Demount Sample - insufficient watert

Refill the water bottle then click on Continue.

ECV Pro User Manual 8-23

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Demount the sample

Once processing is complete, the Status will display Finished and Next will become
available.

2. The next screen (Figure 8-37) presents the opportunity to clean the sample and
capture an image of the etch pit.
If the image is not required, click on Next to continue demounting at step 4 below.
If the image is required:
- lower the door and inspect the sample
- without moving the sample, carefully remove any surplus fluid
- raise and lock the door again
- click on Capture Etchpit Image.

Figure 8-37: Demount Sample - capture etch pit image

3. After clicking on ‘Capture Etchpit Image’ the screen display changes to:

Figure 8-38: Demount Sample, capture etch image

8-24 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Demount the sample

Adjust Lamp brightness and Exposure until the pit can be seen clearly then click on
Save Image to capture the image displayed. At this point, if a filename was specified
in Section 8.5 step 2, the ECVision option, if it is installed, becomes evident (see
Section 8.10.1).

Once the image is captured the camera view disappears, Status displays Finished
and Next becomes available. Click on Next to proceed with the demount process.

4. Follow the on-screen instructions, lowering the door gently to avoid damaging the
wafer.

Figure 8-39: Demount Sample - lower door and remove vacuum

5. Once the vacuum has been released, Finish will become available. Click on it to exit
from the Demount routine.

6. Remove the sample from the stage.

ECV Pro User Manual 8-25

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Demount the sample

8.10.1 ECVision
ECVision uses a high resolution camera to obtain a good image of the pit that it can use
to fit a ring to and thus calculate the ring area. It then displays a history of ring areas so
that you can decide if the ring area should be updated or if the sealing ring is no longer
adequate and should be discarded.

8.10.1.1 Stage 1 - image fitting

When the ECVision option is installed, this screen is entered once the Save Image button
is selected in Figure 8-38, provided a file name was specified in Section 8.5 step 2.

Figure 8-40: ECVision initial screen

Fitting Type
Specifies the method to be used for calculating the area of the etch pit.

Crest + Circle is the recommended method.

Once a ring has been fitted to the etch pit, a ring is placed on the image and the results are
displayed in the Results area as shown in Figure 8-41.

To accept this result and move forward to evaluate it, click on ‘Accept this result’, to
place a tick in the box, then click on Next to display the Stage 2 screen shown in
Figure 8-42.

8-26 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Demount the sample

Figure 8-41: Ring fiited to etch pit

ECV Pro User Manual 8-27

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Demount the sample

8.10.1.2 Stage 2 - updating

The purpose of the graphical plot displayed in this screen (Figure 8-42) is to help you to
decide on one of three actions:

• to continue using the ring with the current ring area values in the ring file,

• to update the ring file with the ring area results obtained at Stage 1,

• to discard the ring for being at the end of its useful life.

The plot shows all measurements, both n- (blue) and p-type (red), made with the current
ring, differentiating between those using the same electrolyte as currently in use
(diamonds) and those using other electrolytes (circles). The current measurement is
shown as a black diamond.

Figure 8-42: ECVision ring history plot screen

NOTE
When multi-layer samples are etched it is the surface layer etch that will be
used for fitting the ring. It is therefore the first electrolyte that is recorded if
more than one is used on a sample and it should be the surface material type
that should dictate the choice of n- or p-type.

Current Areas
These are the values currently stored in the ring file.

Comment
Enter any comment here that is relevant or qualifies the calculated ring area.

Hide other electrolytes

Place a tick here to remove all data from the graph of measurements made with a
different electrolyte to the one currently in use, as shown in Figure 8-43.

8-28 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etching a sample at Operator user level
Demount the sample

Figure 8-43: Ring history plot with other electrolyte data removed
Image Area
This is the area calculated following the fitting at Stage 1.

Etch Pit Type

One of these must be selected before either Update or Next are made available. This
is so that the current measurement will be saved with the correct material type and
so that the correct field is updated if Update is selected (see Update below and
Figure 8-44).

Figure 8-44: Selecting the Etch Pit Type

ECV Pro User Manual 8-29

9PROF-UM01 Issue 1.0
Etching a sample at Operator user level
Demount the sample

Update
Click on this button to update the ring data with the calculated value shown at Image
Area. It will update the Illuminated value if N-type is selected in Etch Pit Type or
Wetted if P-type is selected. Figure 8-45 shows the Illuminated ring area updated.

Figure 8-45: Illuminated ring area updated

Next
Click here to save the data and exit from the ECVision screens. The saved data is
stored in an ascii file as shown in Figure 8-46.
If Next is selected before selecting Update then the ring areas remain unchanged;
they are not updated with the newly calculated area.

Figure 8-46: Ring history data file

8-30 ECV Pro User Manual

9PROF-UM01 Issue 1.0
Chapter 9: Supervisor Level Operation

This level of operation is for setting up recipes for operator level, or for environments
where each sample is different.

It may be possible to select an existing recipe stored in the system that has similarities to
the settings you will need for a new sample. This recipe may then be modified as
necessary and the new setup may be stored as a new recipe.

In order to cover the setup of all parameters, we will assume in this chapter that we are
starting from a base recipe and that all parameters need to be set.

9.1 Preparatory Setup

1. First login as a Supervisor. The operating screen will display with all Navigation bar
functions available.

2. In RECIPE select a recipe that you wish to use as the basis for the new recipe and
save it with a new name (refer to Section 4.4.2).

3. In SETUP, MATERIAL specify the material, contacts and an initial maximum contact
resistance to be used (refer to Section 4.5.1).

Figure 9-1: Material Selection dialog box

ECV Pro User Manual 9-1

9PROF-UM01 Issue 1.0
Supervisor Level Operation
Preparatory Setup

4. In SETUP, REAGENT HANDLING specify the electrolyte to be used and modify the
parameters, if necessary (refer to Section 4.5.2).

Figure 9-2: Reagent Handling dialog box

If the chosen electrolyte is different to that previously used, select the Change tab,
move the tube inserted in the electrolyte bottle into a bottle of clean water then click
on Change (Figure 4-34). The system will flush the tubes through with clean water.
Once the routine has finished, insert the tube into the bottle of the selected
electrolyte.
5. In SETUP, SEALING RINGS specify the sealing ring that is to be used. Refer to
Section 7.6 for sealing ring calibration information.

Figure 9-3: Sealing Rings dialog box

9-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Supervisor Level Operation
Preparatory Setup

6. The AC signal that is superimposed onto the DC bias voltage (Vmeas) for
capacitance measurement is defined in the Capacitance Measuring Signals dialog
box (Figure 9-4), which is displayed when SETUP, CAPACITANCE PARAMETERS is
selected.

Figure 9-4: Capacitance Measuring Signals dialog box

Higher carrier frequencies give lower noise, but may also lead to greater leakage
current (dissipation).
The Amplitude is the magnitude of the AC measurement signal (in volts).

If it is known to be a High, Medium or Low doped sample, select default

parameters. Otherwise start with Medium.

Choose the model that you think will best suit the sample according to the following
guidelines:
Parallel:
Thick layers grown on conducting substrates without electrical junctions.
Series:
Thin layers on (or implants into) semi-insulating substrates.
3-term:
This model should cover all eventualities.
Generally it is recommended to use the 3-Term model.

Set the I-Meas Limit to 0.1 initially.

7. Prepare to mount the sample (see Section 8.6) then in JOBS select MOUNT SAMPLE
and follow the on screen instructions (see Section 8.7).

ECV Pro User Manual 9-3

9PROF-UM01 Issue 1.0
Supervisor Level Operation
Preparatory Setup

8. In JOBS, REST POTENTIAL click on Measure in the right-hand command bar then wait
10 seconds to allow the electrodes to fully recover. Repeat this several times
checking that the values displayed are stable and within acceptable limits for the
electrolyte/material combination in use (see Section 4.2.2 for details).

Figure 9-5: Rest Potential screen

The software will use the carrier type indicated in this dialog box to decide whether
to use excess area correction during etch profiling. The dark/light rest potential can
be misleading if the structure has electrical junctions, very high doping levels or is a
highly compensated material. For this reason a manual override function key is
provided in the etch profile control panel. If the result is n-type, you should
normally use illumination and excess area compensation when etch profiling.

At this stage the ohmic contacts to the sample have been formed, the cell filled with
electrolyte and any bubbles in the cell should have been cleared. The IV and CV curves
can now be plotted to test the suitability of the semiconductor/electrolyte diode for
profiling and to gather further information about the test conditions required.

9-4 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Supervisor Level Operation
IV Plot

9.2 IV Plot

Acquisition of an IV curve from the sample provides an indication of the quality of the
semiconductor/electrolyte diode. It will also highlight any possible problems due to poor
ohmic contact and will indicate the bias voltage range over which capacitance
measurements will be possible. Acquisition of an illuminated IV will indicate the
conditions required for etch profiling later.

1. In JOBS select IV CURVE.

2. Click on Measurement Setup in the right-hand command bar to display the IV

Measurement Options dialog box (see Section 4.2.3.1 for parameter details).

Figure 9-6: IV Measurement Options dialog box with initial settings

3. Before measuring, you must set the range of measuring voltages (X) and current
density limits (Y).

You will start with initial values then change the Current and Voltage ranges as
necessary to reflect the range of values required on the relevant axes. Remember
that:

• This is a 'live' measurement and the value entered for the current acts as a
current limit. The current scale should therefore be set to minimize any
potential damage, but should be sufficient to clearly define the forward and
reverse breakdown regions

• For normal samples current limits of ±0.1 mA/cm2 should be used.

The total current must not exceed 2.5 mA. Some samples may be damaged by
excessive current and you must use lower limits. To view photocurrent on
n-type specimens, you will usually have to set a higher positive current limit.

• The voltage scale should be sufficient to show the voltage range over which the
sample acts as a diode. This will help in evaluating the quality of the ohmic
contact and in setting the scales for the CV analysis.
The normal voltage range is ±2 volts. The maximum is ±10.235.

4. Set the Lamp Intensity initially to a value of 15.

5. Initially choose to plot both dark and illuminated curves.

ECV Pro User Manual 9-5

9PROF-UM01 Issue 1.0
Supervisor Level Operation
IV Plot

6. Click on Measure to start the measurement, which takes a few seconds to complete.
The measurement always starts at the rest potential (zero current). The voltage scan
proceeds, firstly in the cathodic direction (plating current can be drawn), then from
the rest potential in the anodic (etching) direction. This order of scanning the
voltage ensures that any material plated onto the sample surface is cleaned away
before proceeding.

NOTE
If the UV option is fitted, the message UV not stable may appear if the lamp has
not been on for approximately 7 minutes after starting the software. Continue if
the stability of the lamp is not critical at this stage.

7. Check the quality of the ohmic contacts.

The abruptness of the forward bias breakdown (in the bottom-left quadrant for
n-type material and in the top-left or top-right quadrants for p-type) is indicative of
the ohmic nature of the contact. It is commonly observed that if the ohmic contact is
poor, no forward breakdown is seen in the dark, but is seen under illumination.

If the forward bias breakdown cannot be seen:

a. Check the voltage range; it may be too small. +/-2 volts is recommended.

b. Check the ohmic contacts (Section 9.8).

c. Check for a large bubble by pressing F12 to obtain the camera view.

8. Adjust the scale (current and voltage) and, for n-type, the illumination (see
Figure 9-7), then re-acquire the curves until a good graph is obtained (see
Figure 9-8 and Figure 9-9).

Figure 9-7: IV Measurement Options dialog box with amended settings

Users who are familiar with 'conventional' IV curves, will notice several points:

• The electrochemical IV curve will be inverted as anodic current (dissolution

current) is always displayed as positive and cathodic current (plating current) is
displayed as negative.

• The profiler arranges the voltage axes so that the anodic and cathodic
electrochemical regions are consistently placed. The forward and reverse directions
therefore depend on doping type.

9-6 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Supervisor Level Operation
IV Plot

• There will be an offset in the voltage axis as it is measured with respect to the
voltage of the sense electrode. This adds an electrochemical potential to the usual
semiconductor built-in voltage.

• Electrochemists normally use current density as the independent variable (X-axis).

The profiler uses constant voltage (potentiostat) methods and the presentation
reflects this. Voltage is on the X-axis in IV, CV and depletion graphs.

Evaluating the IV curve

• Forward bias breakdown will occur at approximately the same voltage for different
doping levels of a given semiconductor/electrolyte combination. The voltage range
of the reverse bias, however, is determined by both the doping level of the sample
and/or its electrical quality.
Breakdown will occur at a lower voltage for more highly doped material or lower
quality material.

• To select the conditions for the etch profile:

N-type material
Etching takes place under (usually) illuminated reverse bias conditions, as the
forward bias direction will deposit ions from the solution onto the surface.
Using the reverse breakdown is undesirable, as etching would be preferential at
defects and depth resolution would be degraded. Instead, use sufficient
illumination to generate a hole current. This should be on the flat (voltage
independent) portion of the IV curve.

Figure 9-8: N-type IV curves

ECV Pro User Manual 9-7

9PROF-UM01 Issue 1.0
Supervisor Level Operation
IV Plot

P-type material
If both Light and Dark curves are acquired they will follow the same path
throughout; the light will make no difference to the current. Select Vetch (the
voltage applied to the sample during etching) in the forward bias region to give
a reasonable current density. In Figure 9-9 a highly doped sample was used and
a Vetch of about -0.17 mA/cm2 is chosen.

Figure 9-9: P-type IV curve

9-8 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Supervisor Level Operation
CV Plot

9.3 CV Plot

The purpose of acquiring the CV plot is to help in evaluating the quality of the
electrochemical diode and to select a range of possible measuring voltages, Vmeas. The
graph can display three CV curves (series, parallel and 3-term models) with their
respective 1/C2 plots and a plot of the dissipation factor against voltage.

In a sample with an electrochemical diode that conforms closely to the Schottky model,
the series, parallel and 3-term model CV curves will be superimposed over the majority
of the diode region. The plot of dissipation (D) factor will also remain low and flat
(below the 0.4 level). As the diode becomes less ideal, the three plots will separate and
the value of D will increase.

Samples that show separation of the series and parallel model CV curves will also show
different carrier concentration profiles depending on the model selected in the
Capacitance Measurement Signals dialog box. You will therefore need to try to
determine which of the models most accurately represents the sample's actual circuit.

Separation of the curves can be due to several factors:

• high series resistance

• high parallel conductance

• poor ohmic contact to the sample

• over diluted electrolyte

• measuring frequency too high

• unusual surface effects (such as surface states or films).

NOTE
Normally, you will know whether the sample is likely to exhibit high series
resistance or parallel conductance. An easy test would be to reduce the
measuring frequency and re-acquire the CV data; if the three CV plots move
closer together, then series resistance is dominant; if the plots separate further,
parallel conductance is the dominant effect.

1. In JOBS select CV CURVE.

2. Click on MEASUREMENT SETUP in the right-hand command bar to display the CV

Measurement Options dialog box (see Figure 9-10 and Section 4.2.4.1 for
parameter details).

3. The measurement voltage range may either be entered manually using the reverse
bias range (range where the curve shows zero current) determined from the IV plot,
or may be transferred automatically from the IV plot using the zoom facility on the
IV curve (see Section 4.2.4.1) and the Get IV Graph Range button shown in
Figure 9-10.

ECV Pro User Manual 9-9

9PROF-UM01 Issue 1.0
Supervisor Level Operation
CV Plot

Figure 9-10: CV Measurement Options dialog box

The capacitance scale of the CV plot (in nF/cm2) depends on the carrier
concentration of the sample. The following table can be used to select an
approximate maximum capacitance:

Table 9-1: Junction Data

Concentration Capacitance Depletion Resolution Breakdown (volts)
N (cm-3) C/A (nF/cm2) Wd (µm) 3LD (µm) GaAs Si
1020 3000 0.004 0.0013 0.09 0.06
1019 1000 0.012 0.004 0.50 0.35
18
10 300 0.04 0.013 2.7 2.0
1017 100 0.12 0.04 15 11
1016 30 0.4 0.13 88 61
1015 10 1.2 0.4 500 350
1014 3 4 1.3 2800 2000
13
10 1 12 4.0 15000 11000

4. Click on Measure to start the CV plot.

CV measurement takes about a minute to complete. The measurement takes place
from the rest potential, first cathodically, then anodically as in the IV curve. If you
see a discontinuity at the rest potential, this is probably due to significant cathodic
current having plated a film onto the sample surface. This can be avoided by
reducing the cathodic voltage range or reducing the current limit.

5. Refine the parameters to produce a CV curve as shown in the following examples.

N-type (Figure 9-11):

CV curve of the Parallel, Series and 3-Term models slope down to the right
(-ve slope), the 1/C² curve has a +ve slope. Figure 9-11 shows Parallel (blue)
and Series (green) curves with their associated 1/C² (dashed) curves and the
Dissipation (red) curve.

P-type (Figure 9-12):

CV curve slopes down to the left (+ve slope), 1/C² curve has -ve slope.
Figure 9-12 shows a Serial (green) curve, its associated 1/C² (dashed) curve
and the Dissipation (red) curve.

6. The curves and area of graph displayed are specified in the CV Graph Options
dialog box, which is displayed by clicking on GRAPH OPTIONS in the right-hand
command bar. See Section 4.2.4.2 for parameter details.

9-10 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Supervisor Level Operation
CV Plot

Figure 9-11: N-type CV curves

Figure 9-12: P-Type CV curves

ECV Pro User Manual 9-11

9PROF-UM01 Issue 1.0
Supervisor Level Operation
CV Plot

Evaluating the CV data

The CV data is acquired over the voltage range defined by the voltage scale, unless
this would cause the current limit to be exceeded. The examples show typical data
for the diode region of an n-type sample (Figure 9-11) and a p-type sample
(Figure 9-12). The Dissipation factor curve is below the dashed horizontal line that
is set at the 0.4 level. Figure 9-11 shows the series and parallel models overlapping
over the majority of the voltage scan.

The red horizontal cursor indicates the width of the measuring signal
(Amplitude + dV, set in the Capacitance Measuring Signals dialog box - see
Section 4.5.4). The short vertical tick in the centre indicates the DC bias voltage
(Vmeas) that will be used during electrochemical carrier concentration profiling.
Change this, using the left mouse button Set Value function, to a position:
where the D-factor curve is below the 0.4 dashed horizontal line
where the 1/C2 plot is a straight line
just before the forward bias.
Visually check the extremities of the cursor to ensure that they lie within these
specifications.

NOTE
1/C2 should not be straight if you are depleting into non-uniform material.

There is often a wide choice of voltages but a Vmeas close to the forward bias
breakdown is preferable as this will both minimize depletion width and be safe if the
carrier concentration increases with depth into the sample. The Spot Measure
facility, described below, can be used to obtain additional information which will
help in selecting Vmeas.

If the D-factor value is generally above the 0.4 line and the CV curves for the series
and parallel models do not fall on top of each other it is indicated that a different
carrier concentration result will be obtained depending on the model chosen. In a
case like this it will help to change the frequency (in the Capacitance Measuring
Signals dialog box) and repeat acquisition of the CV curve. If reducing frequency
causes the CV plots for the different models to move closer together, then the Series
model is indicated. If the models move further apart, then the Parallel model is
indicated.

Using the left mouse button Line Draw function, draw a line over the 1/C2 plot in
the range indicated by the cursor to obtain an estimate of the expected carrier
concentration. With the line drawn this value will appear in the top message bar.

9-12 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Supervisor Level Operation
Spot measurement

9.4 Spot measurement

This facility is used to determine the size of any variation in the carrier concentration
result caused by selecting a different Vmeas. This is necessary because, as is evident from
the CV curve in Figure 9-11, the range over which it is possible to set Vmeas is
considerable and the chosen position quite arbitrary.

CV curves are obtained by ramping the DC voltage over the selected range and
measuring capacitance using a single AC signal. However, during etch profiling, carrier
concentration results are obtained without ramping the bias voltage. When the Vmeas bias
is applied, the AC signal is modulated at a lower frequency to obtain dC/dV and hence
calculate carrier concentration at a fixed bias. The measurement of capacitance (and D
factor) in a ramped CV curve can sometimes be affected by films built up by cathodic
current plating.

The spot measurement feature measures in exactly the same way as etch profiling and
gives full information for all three models in numerical form. This makes it possible to
evaluate prospective values of Vmeas accurately and to choose the best specimen model.

1. Select SPOT MEASURE from the sub-navigation bar of JOBS to display the Spot
Measurement screen.

2. The bias voltage (Vmeas) set in the recipe will be displayed, change this if necessary.

3. A measuring current limit should have been preset in SETUP, CAPACITANCE PARAMS.
Excessive current can damage the sample. Current is measured first, and the
procedure is aborted at an early stage if it is too high.

4. Press the MEASURE. Wait - the measurement may take up to 10 sec. Status or error
information may appear on the status line.

5. Press MEASURE several times to check the stability of the results (Figure 9-13).

Evaluation

Information displayed in the results table is detailed in Section 4.2.5.

Interpretation of results is highly sample dependent. Often, there will not be an obvious
best choice of Vmeas. The following guidelines, in order of importance, should help you
decide.

1. Normally, Vmeas should be near the forward bias breakdown, but the signal width
should not encroach on the region of high conductance. This has several
advantages:

a. the depletion width is minimized

b. in samples with electrical junctions, Vmeas may also be suitable for the
underlying material (especially using NaOH:EDTA electrolyte)

ECV Pro User Manual 9-13

9PROF-UM01 Issue 1.0
Supervisor Level Operation
Spot measurement

Figure 9-13: Spot Measure dialog box

c. if the concentration increases during profiling, the reverse bias breakdown will
decrease. A low Vmeas will probably still be suitable

d. in low concentration or highly compensated samples, the CV curve may be

very flat, and the signal/noise ratio low. A low depletion voltage gives higher
capacitance signals.

2. The dissipation factor should be minimum. Results with D > 0.4 must be considered
dubious.

3. The flatband potential (FBP) should be the correct or expected value (often at a
minimum).

4. dG/dV should be minimum.

5. Imeas should be near zero (except in rare cases e.g. lo-hi silicon).

9-14 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Supervisor Level Operation
Depletion profile

9.5 Depletion profile

For low to moderately doped samples with a significant depletion region, it is possible to
explore the concentration profile within the available depletion region without etching
the surface significantly. This facility can be used in the following ways:

• For non-destructive profiling of suitable samples

• To obtain data as near to the surface as possible

• To anticipate results during etch profiling

• To assist in the selection of a suitable Vmeas for a sample. This, together with the CV
curve, is similar to an 'automated spot measure'.

To plot a depletion profile, proceed as follows:

1. Select DEPLETION PROFILE in the JOBS sub-navigation bar.

2. Click on MEASURE SETUP in the right-hand command bar to display:

Figure 9-14: Depletion Profile - Measurement Setup dialog box

3. Set the parameters as necessary (see Section 4.2.8.1).

4. Click on MEASURE to start the data acquisition process. Data points should start to
appear in the depletion graph in the voltage direction selected. Depletion
measurement takes about two minutes to complete. It will terminate early if the
current limit is exceeded. An example of a depletion profile is shown in
Figure 9-15.

5. Once the profile is complete, GRAPH OPTIONS in the right-hand command bar can be
used to rescale the graph and to select to plot either Voltage or Depletion Depth on
the x-axis.

ECV Pro User Manual 9-15

9PROF-UM01 Issue 1.0
Supervisor Level Operation
Depletion profile

Figure 9-15: Depletion profile against voltage

Evaluating the depletion data
Remember that the purpose of the depletion profile is to determine the correct Vmeas
for the electrochemical etch profile. As the cross-hair cursor is moved over a plotted
point, the coordinates of the point are displayed in the Cursor Position at the top of
the screen. This is useful for reading the Log N and Voltage value at any given point
in the window.

If the graph shows that the carrier concentration profile is mostly flat over a voltage
range then starts to change, the point of change indicates the correct Vmeas value for
the sample.

9-16 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Supervisor Level Operation
Etch profile

9.6 Etch profile

The main function of the ECV Pro is to produce a profile of concentration against sample
depth. With previous functions you have analysed the electrical characteristics of the
sample/electrolyte junction.

Before measuring, you must use the Etch OPTIONS to set the final depth (X) and range of
carrier concentrations (Y). These values may be changed during profiling if required.
The profile will terminate automatically once the final depth is reached.

9.6.1 Setting up conditions

The previous sections have shown how to use software facilities to investigate the
electrical characteristics of the electrochemical Schottky diode formed during the sample
mounting procedure. The information learned so far will help in setting up the conditions
to electrochemically etch the sample to obtain a profile of carrier concentration versus
depth that is both accurate and repeatable.

In the example used so far (Figure 9-8, Figure 9-11 and Figure 9-15), the sample is
shown to have a doping level near to the surface of about 1.33E18 n-type. We also know
that:

• Vmeas should be set from the CV curve (Figure 9-11) to a value at which the D-
factor is below 0.4 and the 1/C2 curve is an approximately straight line. It should
also be at a point on the depletion profile at which Log N does not change
significantly with voltage. For the example, we have seen in previous sections that a
Vmeas of 0.0 V should be suitable.

• Vetch should be set from the IV curve (Figure 9-8) to a value in the region of the
forward bias breakdown voltage at which the current drawn is not voltage
dependent. In the example, a starting Vetch of about -0.25 V should keep the etching
current (Ietch) less than 0.1 mA/cm2. Once etching has begun, Vetch can be gradually
increased until a suitable etch current (rate) is achieved.

It is important to realise that the electrical characteristics measured up to this point will
almost certainly have been influenced by surface effects. However, these almost always
make the electrochemical Schottky diode 'worse' than it will become after etching a few
nanometers of material from the sample. Hence the chosen Vmeas and Vetch conditions
should remain suitable as the profile proceeds. It is always permissible, however, to
pause the etch profile at any point and re-check the IV, CV, Spot Measure or Depletion
profile if you suspect that conditions may need adjustment. This is likely, for example, if
you expect the concentration to increase as you etch into the sample, as the Schottky
diode will certainly deteriorate as more heavily doped material is encountered.

ECV Pro User Manual 9-17

9PROF-UM01 Issue 1.0
Supervisor Level Operation
Etch profile

The etch profiling procedure is as follows:

1. Click on ETCH PROFILE in the JOBS sub-navigation bar and then on MEASURE SETUP
in the right-hand command bar to display the Etch control panel.

2. Click on OPTIONS to display the Etch Measurement Options dialog

box, where the etch and measurement parameters must be set (see
Section 4.2.7.1 for details).

3. Ensure that the lamp is set at 1.

4. Click on START to begin etching and start the measurement.

The CLOSE button will be greyed and will remain so until the
measurement stops or is paused.
The START button will change to PAUSE so that the etch can be
interrupted for parameter adjustment if necessary.

5. The status bar should immediately display Measure then, after a few
seconds (the settling time), the measuring current Imeas will be
displayed. Assuming that Imeas does not exceed the Imeas limit, the
measurement will proceed and the results section will display the
data from the first (Step # 0) surface measurement. The status bar
will then display Etching and the Ietch value, which should be small
(<0.1 ma/cm2), will be displayed.

6. The Vmeas and Vetch area will initially display the relevant values set
from the CV and IV curves respectively. Once the first point has
been plotted you should adjust these values as follows:

If V-etch shows a value Const-I then the voltage will change automatically to
maintain a constant current.

If Const-I is not displayed for V-etch, then:

For n-type material

Verify that Vetch is at a value appropriate for the sample.
Slowly increase the lamp until Ie reaches a nominally low value,
dependent on the Resolution, until the % done field shows a moderate
steady rate giving an etch time of 10 - 30 seconds.
If Ie deteriorates by more than 10 - 20% over the cycle this is indication of
a film build-up on the surface of the sample. Slow the process down, by
reducing the lamp, to allow time for chemical removal of anodised film to
balance the anodisation rate.

For p-type material

Increase Vetch until Ie is approximately 0.1.
If Ie remains stable for a given Vetch then Vetch can be increased to give a
faster etch time (but do not reduce the etch time below 10 seconds).
If Ie gradually reduces for a given Vetch then reduce Vetch.

7. Once the sample has drawn sufficient etching current to have removed the
thickness of material set by the Resolution, the status bar will indicate Settling for

9-18 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Supervisor Level Operation
Etch profile

the time set, followed by Measure once more. The second step of measurement
data will appear in the results area (Step # 1).

8. For each measurement, a point will appear on the Log N vs. depth plot, and
another line of data will be added to the data log (if enabled).

Monitor the Dissip. and FBP values to ensure they remain at levels indicating that
the admittance values being measured are sensible.

Safe range of values

Imeas <0.1mA/cm2
Dissip. <0.4
FBP ±2.5V

To view the sample during etch, press F12 to display a camera view as shown in
Figure 9-16. Adjust the Exposure Level (in the camera dialog box) until you can see the
sample clearly.
Click on Close or press F12 again to cancel the view.

Figure 9-16: Etch profiling screen

9. If it is necessary to change to a different electrolyte at a specified point through the

etch, proceed as follows:

a. Click on PAUSE to stop the etching process.

b. Click on OPTIONS to open the Etch Options dialog box then select the Change
Reagent tab.

ECV Pro User Manual 9-19

9PROF-UM01 Issue 1.0
Supervisor Level Operation
Etch profile

c. Move the dip tube from the electrolyte bottle and put it in a small bottle of DI
water.

d. Click on Start Change Sequence.

The routine will fill from the small DI water bottle and drain the electrolyte
tubes until the small bottle is empty. It will then fill from the large DI bottle,
flush the cell and wafer surface then drain the water, twice.

e. It will then instruct you to move the dip tube into the new electrolyte bottle.
Once you have done this, click on Continue. The cell will fill with electrolyte
then Finished Change will be displayed.

f. Click on OK to return to the Etch screen.

g. Press F12 to display the camera view and debubble the cell if necessary.

h. Click on Start to continue the etch.

10. Once the etch procedure is complete the message bar displays End Reached
(Figure 9-17). Click on CLOSE to exit from the Etch panel and return to the Etch
Profile screen.

Figure 9-17: Completed Etch

11. Click on SAVE to save the etch graph data.

12. If necessary, save the recipe (see Section 9.7).

13. Demount the sample (see Section 8.10).

9-20 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Supervisor Level Operation
Save the recipe

9.6.2 Pause a Profile

If any of the values get out of range, the profile can be suspended by clicking the PAUSE
button in the Control Panel. Once paused, the sample will not etch, unless the electrolyte/
semiconductor combination is one that results in purely chemical etching (see
Section 10.1). After pausing the profile, click CLOSE to activate other functions.

Usually, the CV and IV curves will reveal the cause for the out of range values; a
frequency change will commonly correct the problem.

9.6.3 Restart a paused profile

With the Etch screen and the Control Panel open, make any changes necessary in
OPTIONS then click START.

9.6.4 Ending the Profile

If you wish to end the profile before the final depth is reached, select PAUSE followed by
CLOSE.

If the profile is not stopped prematurely and is allowed to continue, the profile will end
automatically when the end of the depth scale is reached. At this point the status bar of
the control panel will display FINISHED. Click on CLOSE to close the Control Panel.

9.6.5 Saving the data

The etch data may be saved as often as required, whenever the etch is paused and at the
end of the etch. Click on Save to save the data to an automatically generated file name
based on that specified on loading the wafer.

Etch data can also be saved to a different filename using the Save As function.

A raw data (binary) file, which contains all the information collected during the
acquisition of the etch profile, is generated automatically. It can be reprocessed in the
Reprocessing program (refer to Chapter 11). The raw file "filename.raw" is created when
the first (surface) point is taken and the header information is written out at that time. At
each subsequent point, the file is reopened, the new data is appended and the file is then
closed. This ensures that data is never lost through file buffering or failure to close a file
at the end of a run.

9.7 Save the recipe

IMPORTANT
If you do not do save the recipe at this time then all settings that you have made
up to and during the etch will be lost.

Now that the etch is complete and you are satisfied that all parameters have been set
correctly for the sample, re-select RECIPE and save the recipe again.

ECV Pro User Manual 9-21

9PROF-UM01 Issue 1.0
Supervisor Level Operation
Check Contacts

9.8 Check Contacts

The ohmic contacts to the sample are established when mounting the sample, in the
Mount Sample wizard. Occasionally it may be necessary to check the contacts and
perhaps re-establish them later in the measurement process. Follow these steps to check
the contacts:

1. Select CHECK CONTACTS in the JOBS sub-navigation bar. The following screen will
be displayed:

Figure 9-18: Check Contacts screen

2. Click on either Back or Front Contacts in the Select & Measure box, depending on
the contact set used, to measure the current contact. (They must be selected and
checked individually if both contacts are being used.) The measurement is displayed
in the Resistance (ohms) box and should as low as possible below 100 ohms.

3. If the resistance is high, click on Blast & Measure several times until a low
resistance is shown then click on Re-Measure to ensure that the contacts are stable.
If the resistance cannot be reduced adequately, try changing the Blast Parameters.

The Blast button applies a pulse that breaks down any native oxide on the sample
surface under the contacts, and, to some extent, spot welds the contact pins to the
sample to form an ohmic contact. The success of this process depends on the carrier
concentration of the sample, the condition of the surface and the condition of the
contact set.

9-22 ECV Pro User Manual

9PROF-UM01 Issue 1.0
Chapter 10: Maintenance

10.1 Etching problems

The electrochemical dissolution process ideally produces flat bottomed etch holes with
surface quality mirroring that of the unetched surface. This ideal would produce ECV
carrier concentration profiles that exhibit the best depth resolution possible for the
electrical measuring conditions used.

In practice, the bottom of the etch hole will degrade from that of the unetched surface for
the following reasons:

• surface marks (fingerprints, grease, dust etc)

• defects or poor crystalline quality of the semiconductor material

• one or more layers of the sample are electrically isolated from the ohmic contact,
inhibiting uniform dissolution in that layer

• thin layer on an insulating substrate where series resistance causes preferential

etching around the perimeter of the etch hole

• use of non-ideal etching conditions (Vetch, illumination)

• damage to the semiconductor surface (pitting or defect revealing) from heavy

currents developed during I-V, C-V, depletion profiling and spot measurement
analysis

• bubbles on the semiconductor surface

• depletion of electrolyte at the semiconductor : electrolyte interface

• contamination or incorrect dilution of the electrolyte

• poor condition or contamination of the electrochemical cell electrodes

• poor light uniformity

• wrong electrolyte chosen for the semiconductor under test.

Many of the problems listed above can be avoided by simple maintenance of the system,
careful choice, preparation and storage of the electrolytes, and selection of the correct

ECV Pro User Manual 10-1

9PROF-UM01 Issue 1.0
Maintenance
Etching problems

measuring conditions. Other problems are less easy to avoid. The following sections
provide information which should help in obtaining the best profiles possible from your
samples.

10.1.1 Material related etching problems

Due to the lack of perfection in material growth techniques, this category of problems
will always have some effect on the quality of the etch. Obviously, if the sample has a
high level of crystalline defects, several etching problems can occur:

• defects will be revealed as pits, bumps or lines

• the dissolution current can be reduced by recombination processes; the current can
drop to zero in highly compensated materials

• dark etching current can increase due to Zener breakdown

• dark etching of the excess area region of n-type material can cause errors in etch
depth (and carrier concentration), unless p-type material (etching over entire wetted
area) is used for the excess area compensation.

Careful setting up of the etching conditions and implementation of a slow etching rate
may help to minimize revealing problems.

Figure 10-1: Photo of a good etch hole profile using Tiron in 35% Al, AlGaAs, and
corresponding stylus depth profile

10-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Maintenance
Etching problems

Stylus profile
direction

Film area

Figure 10-2: Photo and stylus depth profile of etch using Tiron in 35% Al, AlGaAs,
showing a film resulting from incorrect measuring conditions

10.1.1.1 Etching GaAs

0.1M Tiron is the electrolyte of choice for gallium arsenide with carrier concentration
<1018 cm-3, due to its tendency to produce a small excess area. In certain circumstances,
however, Diaminoethane : EDTA should be used:

• if the carrier concentration exceeds 1018 cm-3, the high resistivity of Tiron can
contribute significant series resistance leading to inaccurate results (see Section 2.3)

• with heavily zinc doped GaAs, films that can affect profiling analysis can form
during dissolution with Tiron

• if the structure contaions layers of other materials such as AlGaAs

The Diaminoethane : EDTA electrolyte does have a lower surface tension than Tiron and
this causes larger excess areas. Recalibration of the contact area is therefore required.

ECV Pro User Manual 10-3

9PROF-UM01 Issue 1.0
Maintenance
Etching problems

10.1.1.2 Etching AlGaAs

Successful profiling of AlGaAs is dependent on the quality and composition of the
material.

Material quality factors that inhibit dissolution are:

• crystalline quality

• oxygen incorporation in OMVPE growth (forming alumina)

In terms of composition, the problem is that as the percentage of aluminium increases,

the difficulty in profiling increases.

Another factor affecting the profiling of AlGaAs is the use of the GaAs cap layer. This
helps prevent atmospheric oxidation of the AlGaAs.

The recommended electrolyte is Diaminoethane : EDTA with Tiron as a second choice.

During etching with both Diaminoethane : EDTA and Tiron, a film will form on the
surface of the AlGaAs due to oxidation of the aluminium. To minimize the effects of this
film, it is best to:

• Etch as slowly as possible. If on stopping a profile for a period of time (e.g. to do a

PVS scan) and then resuming the profile, a drop in carrier concentration is noticed,
this indicates that a film is affecting the results. If necessary, increase the settling
time to give a ten second (or longer) delay between etching and measuring

• Run the pump while etching. This keeps the electrolyte in the vicinity of the sample
continually refreshed.

Other electrolytes that have been used for AlGaAs are 1M NaOH without EDTA (P.
Blood, Semiconductor Science and Technology, Vol 1, pp7-27) and ammonium tartrate
in ammonium hydroxide.

10.1.1.3 Etching InGaAs and InGaAsP

The ternary and quaternary layer etching is very dependent on the crystalline quality of
the material. Good material etches well, giving a reasonably good quality etch bottom.
Bad material will etch slowly, leaving a roughened crater.

10.1.1.4 Etching GaN and AlGaN

Sulfuric acid is the only well tested electrolyte for these materials at present.

Good material etches well, giving a reasonably good quality etch. Bad material will etch
slowly, leaving a roughened crater. Higher aluminium percentages may require special
treatment and possibly a different electrolyte.

10-4 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Maintenance
Electrode conditioning

10.1.1.5 Etching InP

Traditionally, 0.5M HCl has been used as the electrolyte for InP. It has been noted,
however, that significant chemical etching occurs in the time taken to profile typical
structures. This leads to errors in etch depth, errors in carrier concentration and loss of
resolution due to etch hole roughening. An alternative electrolyte called pear etch has
been suggested that has significantly less tendency to dark etch, and hence produces
better profiles. The published recipe calls for the use of HCl and HNO3 in 2-propanol. In
practice, methanol seems to work better.

Both HCl and pear etch require that Vetch, during photo-electrochemical etching of n-
type material, be set at about 0.5 V to ensure that the dissolution current is voltage
independent.

The recommended electrolyte isnewer electrolyte may give slightly better depth
resolution. EDTA:Diaminoethane is one of those used with some success (A.C.
Seabaugh et al.), another reported is HF: CH3COOH: H2O2: H2O in the proportions
5:1:0.5:100 (Maria Faur et al.)

10.2 Electrode conditioning

Condition Electrodes (Section 4.3.3) provides the facility to remove contamination by

performing a little electrolysis in the cell. Regular electrode conditioning will help to
maintain a high performance.

ECV Pro User Manual 10-5

9PROF-UM01 Issue 1.0
Maintenance
Halogen lamp replacement

10.3 Halogen lamp replacement

Part No. 406024144.

Replacement of the halogen bulb is straightforward and, if carried out correctly, requires
no subsequent adjustment of the optical system.

CAUTION
If the light has recently been switched on then the bulb and surrounding holder
will be very hot. Let the unit cool before attempting to change the bulb.

1. With power to the instrument turned off at the mains socket, access the lamp by
removing the four screws fixing the top panel in place (see Figure 10-3).

Top panel fixing screws

Figure 10-3: Top panel fixings

2. Remove the rear duct unit, which is fastened to the rear wall with a thumbscrew.
Remove the thumbscrew and slide the duct out of its location lugs.

Duct fixing
point

Duct fixing
thumbscrew

Duct locating lugs

Figure 10-4: Rear duct unit

10-6 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Maintenance
Halogen lamp replacement

Lamp holder

Beam-steering
mirror unit

Figure 10-5: Top cover and duct removed showing the top of the light tower
3. The lamp is held in a ceramic base, which locates on two screwed rods in the
aluminium frame (see Figure 10-5). There are two springs under the lamp base that
may push the base off once the screws are loosened. Holding the base, unscrew the
two thumbscrews and slide the lamp base off the screwed rods, ensuring that the
two springs remain in position at the base of the rods.

Thumb screws

Springs

Ceramic base

Halogen lamp

Figure 10-6: Lamp on ceramic base

4. Pull the lamp off the base and discard it.

IMPORTANT
Use rubber gloves or a tissue to handle the new lamp. Bare hands will
contaminate the glass.

5. Insert the new lamp onto the base.

ECV Pro User Manual 10-7

9PROF-UM01 Issue 1.0
Maintenance
Halogen lamp replacement

6. Press the lamp firmly into position. The lamp pins are a tight fit in the contact holes
and must be inserted fully to ensure the lamp is positioned correctly.

7. Replace the base on the two screwed rods and lightly tighten the thumbscrews.

8. Power up the instrument and start up the software, logging in at Supervisor level.

9. With the table raised (probes down) enter MANUAL CONTROL in the SYSTEM menu.
The bulb will now be illuminated.

10. Loosen the fixing screw on the Beam-steering mirror unit (see Figure 10-5 and
Figure 10-7) and swing the unit anti-clockwise away from the alignment hole.

Fixing screw

Beam alignment hole

Figure 10-7: Beam-steering mirror unit and beam alignment hole

11. Adjust the lamp holder thumb screws to move the beam so that it is positioned
centrally over the hole, as shown in Figure 10-8.

Bad lamp alignment Good lamp alignment

Figure 10-8: Lamp beam alignment

12. Swing the beam-steering mirror unit back into place and tighten the fixing screw.

13. Power down the tool and remove power from the unit. This ensures that if a screw is
accidentally dropped, it will not touch and possibly damage a live board.

14. Replace the duct and the top cover.

10-8 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Maintenance
UV lamp replacement

10.4 UV lamp replacement

Once the accumulated lamp operation time reaches 3000 hours, a message will be
displayed when the next measurement using illumination is requested. The message will
either be:

Warning: UV Lamp needs changing - can’t continue

or:

UV Lamp Alarm - can’t continue

In either case, no further measurements will be possible until the lamp has been changed
(as described in Section 10.4.1) and the operating time has been reset (as described in
Section 10.4.2).

10.4.1 Replacing the UV lamp

Part no. 406885859.

The lamp is located in the light source unit, which is located inside the inner front panel
(see Figure 3-5).
Be very careful when handling lamps as they contain high-pressure gas approximately 1
MPa (10 atmospheres) at normal temperature and may burst if dropped or otherwise
impacted.

Keep the glass section or the end of the lamp out of contact by hand. If the lamp needs to
be cleaned, wipe the glass section with a gause (soft cloth) soaked with alcohol.

IMPORTANT
Be sure to turn the lamp fixing cap until it clicks and gets locked. If the cap is
loose, the lamp will not be set at a correct position, specified light intensity will
not be obtained or the lamp will fail to light up. If the lamp cover is not closed
tightly, the interlock switch will function and the lamp will not light.

Whenever the lamp has been replaced, be sure to reset the lamp lifetime (see
Section 10.4.2).

1. Before replacing the lamp, turn it off, run the cooling fan for at least 15 minutes and
make sure that the temperature in the unit has dropped sufficiently.

2. Once the lamp temperature has dropped sufficiently, turn the power off.

ECV Pro User Manual 10-9

9PROF-UM01 Issue 1.0
Maintenance
UV lamp replacement

3. Loosen the lamp cover fixing

screw and open the lamp cover.

Lamp cover
fixing screw

Lamp cover

Figure 10-9:Open the UV lamp cover

4. Remove the lamp fixing cap by

turning it anticlockwise.
Lamp fixing screw

Figure 10-10:Remove the UV lamp fixing

5. Grasp the lamp flange and pull the

lamp gradually straight out from
the housing, taking care not to hit
the lamp against the mirror or the Lamp holder
lamp holder.
Lamp

Lamp flange

Figure 10-11:Remove the UV lamp

6. Take out the new lamp from the lamp package.

IMPORTANT
Do not touch the lamp with a bare hand.

Figure 10-12: UV lamp

10-10 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Maintenance
UV lamp replacement

7. Holding the lamp flange so that the

slit faces up, as shown, gently push
the lamp into the hole in the lamp
holder.

Slit

Figure 10-13:Insert the new UV lamp

8. After inserting the lamp fully, align

the groove in the lamp fixing cap
and the pin of the lamp holder and Pin
secure it by turning it clockwise
while pushing it.
Groove
Be sure to turn the lamp fixing cap
until it clicks and gets locked
securely.

Figure 10-14:Fix the new UV lamp into place

9. Close the lamp cover and tighten

the fixing screw.

Figure 10-15:Close the UV lamp cover

CAUTION
The lamp contains high-pressure gas, as well as mercury. Disposing of it
together with ordinary garbage is extremely dangerous. Always make sure the
lamp is disposed of properly. When sending a lamp, put it in the lamp package
box used for the new lamp to avoid any possible accident during
transportation.

ECV Pro User Manual 10-11

9PROF-UM01 Issue 1.0
Maintenance
UV lamp replacement

10. After the lamp has been replaced,

place the old lamp in the packaging Lamp package boxes
from the new lamp. Then send the
old lamp to the nearby sales office,
or have it disposed of by a waste
disposal specialist that has a
mercury disposal facility.

Figure 10-16:Place old lamp in package boxes

10.4.2 Resetting the lamp operation time

IMPORTANT
Do not reset the lamp operation time before the lamp life time runs out. If it is
reset, the alarm to indicate necessity of lamp change will not be output at the
correct time.
The control panel will revert to stand-by mode if it is left inactive for
approximately 1 minute.

SELECT [A]

SELECT [B]

[DOWN] [UP]

Figure 10-17: UV control panel

Whenever the lamp has been replaced, reset the lamp lifetime as follows:

1. In the stand-by mode, press the SELECT [B] button 10 times while pressing the
SELECT [A] button. The mode then changes to the lamp operation time resetting
mode and the operating time value flashes in the OPERATING TIME section of the
display window.

2. Press both [UP] and [DOWN] buttons simultaneously for 1 second. The lamp
operation time is then reset to “0” and the stand-by mode is restored.

10-12 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Maintenance
Changing front contacts

10.5 Changing front contacts

Part No. 5PROF00680 (set of 2).

Holding bracket
Front contacts Fixing screw

Figure 10-18: Front Contact Pins

To replace the front contact pins:

1. Remove the fixing screw and the holding bracket.

2. Lift the pins away.

3. Insert new pins by reversing these steps.

10.6 Changing back contact pins

Part No. 5PROF00631 (set of 2 tinned).

It is recommended that both back contact pins are replaced at the same time.

The instrument must be powered on and the front contact pins must be lowered with the
back contact removal disc (Part No. 2PROF40310) in place on the table. In this state the
vacuum is on and the back contacts are raised and are visible (see Figure 10-19).

Back contact pins

Back contact removal disc

Figure 10-19: Back Contact Pins

1. Using narrow jawed, snipe nose pliers, grip the top of a pin and pull upwards to
remove the pin (see Figure 10-20). Then pull the other pin out.

ECV Pro User Manual 10-13

9PROF-UM01 Issue 1.0
Maintenance
Changing back contact pins

Grip pin with pliers Pull pin out

Figure 10-20: Removing a front contact pin

2. Place a new pin into an empty hole (see Figure 10-21).

Hole for insertion

of new pin

Figure 10-21: Hole for front contact pin insertion

3. Slide the pin insertion tool (Part No. 2PROF35210) over the pin and gently, but
forcefully, push the pin fully home (see Figure 10-22).

Tool placed over pin Pin pushed fully home

Figure 10-22: Inserting a new back contact pin

4. Remove the tool.

5. Repeat step 2 to step 4 for the second pin.

10-14 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Maintenance
Replacing the cell O-ring

10.7 Replacing the cell O-ring

Part no. 354301421.

Figure 10-23: Cell and O-ring

1. Pry the O-ring out of the cell. A tweezer tip works well for this.

2. Ensure that the cell seating for the new ring is clean.

3. Gently push the new ring into the cell.

ECV Pro User Manual 10-15

9PROF-UM01 Issue 1.0
Maintenance
System fuses

10.8 System fuses

There are two sets of fuses in the instrument:

• Main power fuses

Two fuses are located in the power input socket on the back of the mains tray:

Main power fuses

Figure 10-24: Mains tray rear view

• Electronics tray fuses

Two fuses are located in the power input socket on the back of the electronics tray:

Electronics tray fuses

Figure 10-25: Electronics tray rear view

Each socket contains two fuses of the same specification. Access the fuses by opening
the rear door of the instrument. The fuses are under a small flap that should be gently
prised out, then pulled to open the fuse retaining compartment.

It is imperative that the correct fuses are

inserted:

Mains tray:
90-115V 10A anti-surge
200-240V 6.3A anti-surge

Electronics tray:
90-115V 6.3A anti-surge
200-240V 3.15A anti-surge

Figure 10-26: Fuse retaining compartment

10-16 ECV Pro User Manual

9PROF-UM01 Issue 1.0
Chapter 11: Using the Etch Reprocessing
Program

11.1 Introduction

Datafiles saved by the ECV Pro program, contain the depth and concentration values
shown on the acquisition graph. These calculated results depend on the inputs of material
and sealing ring data, the specimen circuit model declared and the application (or not) of
excess area compensation. After the measurement process is completed, it may be found
that one or more of these prior inputs was inaccurate or that the final depth does not agree
with mechanical measurement of the etch pit. Some structures may also be complex and
require different inputs for each layer or a different excess area compensation scheme.

Reprocessing is a recalculation program which converts the raw datafiles (acquired

values of charge transfer and admittance) into processed datafiles (calculated depth and
concentration) for display. Up to 12 different regions may be defined and you can input
different materials, revise sealing ring areas and circuit model selection for each region.
A more sophisticated excess area compensation scheme is available and a final etch
depth may be forced.

Additional data saved in the raw file may also be displayed. This includes etch current,
measuring voltage and current, admittance, dissipation, flatband potential and phase.

A separate package, Reprocessing, can be installed and used without the Profiler
hardware being present. The ECV Pro and Reprocessing programs may be run
concurrently.

NOTE
The Reprocessing program recalculates the raw data using all the global and
region information supplied by the user. The resulting processed data is plotted
to the existing scale. If reprocessing has shifted points off the graph, use the
Auto Scale function.

Further changes can be made to region parameters in an iterative manner. It

is not necessary to re-read the original file before reprocessing again.

ECV Pro User Manual 11-1

9PROF-UM01 Issue 1.0
Using the Etch Reprocessing Program
Starting Reprocessing

11.2 Starting Reprocessing

Run the software by double clicking on the program icon in the Accent program group.
The program opens displaying the screen shown in Figure 11-1.

Figure 11-1: Reprocessing program opening screen

Data is imported to Reprocessing from a raw data file (.raw) created by the ECV Pro
during data acquisition.

Select the file of raw data that is to be loaded (which can be a file still being written to by
the Profiler as the files are opened and immediately closed when a data point is
appended) and click on Open. The Etch Reprocessing screen will appear with a graph of
the selected raw data (see Figure 11-2).

11-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Using the Etch Reprocessing Program
The Etch Reprocessing screen

Figure 11-2: Etch Reprocessing screen with raw data file loaded

11.3 The Etch Reprocessing screen

When a file is successfully accessed, the data is processed and plotted using the original
parameters. The result should be very similar to the original acquisition graph. The
specimen description is printed at the top of the graph. The parameters are placed in the
region bar as region #1.
The following illustration shows the display after a raw data file has been loaded:
The elements of the screen and facilities available are described in the following
paragraphs.
File
Open
Use to load a new raw data file, see Section 11.2.

Save As
Use this to create a processed datafile which can be read back into the Profiler
program. Enter a suitable filename in the dialog box that is displayed. The
filename should have extension .EPn, where n is a sequence number or any
alpha-numeric character you wish.
You can also select the Save As Type = Export to Spreadsheet to save as an
ascii text file suitable for import into any spreadsheet.
If one of the alternative graphs is active, the displayed data will be saved in
ASCII text format. This can be read in by the Windows Notepad accessory or
imported into a spreadsheet or graphics program.

ECV Pro User Manual 11-3

9PROF-UM01 Issue 1.0
Using the Etch Reprocessing Program
The Etch Reprocessing screen

The depth figure in all files is the total depth (Wr+Wd).

Information
Displays file information.
Page Setup
Allows selection of the printer, paper size and layout to be used for printing
graphs.
Print Graph
Prints the displayed graph to the selected printer.
Graph
Set Scale
Select this option to display the Set Scale dialog box and change the scaling of
the graph. For full details refer to Section 11.4.
Auto Scale
Resets the scale to display the entire data set.
Features
Delete Comments
Deletes all comments that have been inserted on the graph (see Left
mouse button/Add Text).
Redraw
Simply refreshes the graph on the screen.
Copy to Clipboard
Copies the graph area of the screen to the clipboard.
Style
Gridlines
Toggles the grid lines On/Off.
Point
Displays the Data Style dialog box (Figure 11-3) where the size, shape
and colour of data points may be changed.

Figure 11-3: Data Style dialog box

11-4 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Using the Etch Reprocessing Program
The Etch Reprocessing screen

Font
Displays the Font dialog box (Figure 11-4) where the font, font size and
style for comments may be changed.

Figure 11-4: Font dialog box

log-N points
Display the default graph as points, the style of which can be changed in the
Data Style dialog box (Figure 11-3).

log-N regions
Display the default graph to show which points are within each region (see
Section 11.5).

I-etch, Vm+Im, Y+Dissip, Flat Band Pot.

Alternative graphs, see Section 11.6.

Data

Reprocess (see Section 11.8)

This causes the raw data to be recalculated using all the global (see
Section 11.7) and region (see Section 11.5) information supplied by the user.
The resulting processed data is graphed to the existing scale. If reprocessing
has shifted points off the graph, use the Auto Scale function.
Further changes can be made to region parameters in an iterative manner. It is
not necessary to re-read the original file before reprocessing again.
Reprocessing restores any hidden data points.

Reset
Resets the graph display, regions and parameters to the state when the raw data
was loaded.

ECV Pro User Manual 11-5

9PROF-UM01 Issue 1.0
Using the Etch Reprocessing Program
The Etch Reprocessing screen

Global
Display the Global Parameters dialog box where parameters applicable to the
whole specimen may be changed (see Section 11.7).

Help
Displays the Help file for the program.

Parameters
These are the parameters for the region in which the currently selected data point is
located (see Section 11.5 and Section 11.8).

Figure 11-5: Region parameters

Left mouse button functions

The toolbar contains five buttons which select the function of the Left mouse
button.

point is located
selected data
Region in which
Simple cursor

selected data point

Rubber Band
Select Point

Number of
Zoom

Add Text

on the graph
cursor position
Coordinates of

Figure 11-6: Left mouse button functions

Simple Cursor
The button selects the active window, and has no other function.

Zoom
Move the cursor to one corner of the desired region, press the Left button, and
drag to the opposite corner. When you release the Left button, the graph will
rescale to the defined rectangle. Please note that only the bottom and left-hand
scales are zoomed.

Rubber Band
These lines may be drawn for illustrative purposes. Only one line at a time can
be drawn and it is not transferred to the printer.

Select Point
When you click near a datapoint, the marking rectangle moves onto that point.
The region and point operators refer to this point. Refer to Section 11.5 for full
details about regions.

Add Text
The point where you click the Left button becomes the origin of a comment to

11-6 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Using the Etch Reprocessing Program
The Etch Reprocessing screen

be added to the graph. Enter your comment in the dialog which appears.
Comments follow the graph scaling and are transferred to the printer.
To enter another comment, you must select the Add Text function again.
To change the format of the text refer to the Font dialog box (Figure 11-4).

Right mouse button

Clicking the right mouse button anywhere on the graph presents the following
options relating to the currently selected point. To change the selected point use the
Select Point button above.

Point

Hide
Hides the currently selected point. Hidden points will be treated as deleted
points for reprocessing but will be re-displayed after Reprocess or when
Reset is selected.

Information
Displays the Point Information dialog box.

Figure 11-7: Point Information dialog box

Region
These functions are used to define regions of a graph so that different
parameters may be set for each region (see Section 11.8).

NOTE
When defining regions it is best to select the log-N regions option in
the Graph menu.

Delete
Removes the region in which the point is located (not the points).

ECV Pro User Manual 11-7

9PROF-UM01 Issue 1.0
Using the Etch Reprocessing Program
Graph scaling

Insert New
Inserts a new region starting at the selected point.

Change Start Point

Changes the start point of the region in which the currently selected point
is located to the selected point.

Change End Point

Changes the end point of the region in which the currently selected point
is located to the selected point.

11.4 Graph scaling

The optimum scale for plotting a given graph is determined by scanning the processed
data. If you wish to change the scale,

• either use the Set Scale option in the Graph menu to display the Set Scale dialog
box,

Figure 11-8: Set Scale dialog box

• or select the Zoom mouse button and zoom in on a specific area of the graph
by using the left mouse button and dragging the box to outline the area of interest.

To reset the scale to show the entire data set, use the Auto Scale option in the Graph
menu.

The Log-N scale always displays whole decades. The alternative vertical scales cannot
be changed.

11-8 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Using the Etch Reprocessing Program
Regions

11.5 Regions

When data is read in, all data points are placed in a single region and the end-of-region
square is on the final data point. The region parameters (Figure 11-5) apply to the entire
file. When you select the Reprocess menu option, the whole file will be reprocessed
using the one set of parameters, including any new parameters which have been defined.

11.5.1 Multiple Regions

You can divide the data into a maximum of 12 regions, each with its own set of
parameters.

NOTE
When defining multple regions it is best to select the log-N regions option in
the Graph menu.

To define regions use the Right mouse button (page 7) Region functions.

For each region set the parameters that are to apply before reprocessing (see
Section 11.8).

Changes can be made to region definitions and parameters at any time and in any
sequence.

ECV Pro User Manual 11-9

9PROF-UM01 Issue 1.0
Using the Etch Reprocessing Program
Alternative Graphs

11.6 Alternative Graphs

These selections, available from the Graph menu, display additional data associated with
the measurement process:

I-etch the etch current immediately prior to measurement

Vm+Im the measuring voltage and current during measurement

Y+Dissip the complex admittance in µS (1/Megohms) and dissipation factor

Yr/Yi

FBP the flatband potential (atan(dYr/dYi)).

R-series the series resistance

There is also a ‘log-N’ option to allow you to return to the default display.

These displays allow you to review the measurement conditions, view specific raw
parameters, and locate features. The depth scale is total depth (Wr+Wd) for all graph
types.

Figure 11-9 shows the log-n view of agraph followed by the variour alternatives for the
same data.

p-type n-type
layer layer
log-N points graph

I-etch graph

Figure 11-9: log-N and alternative graphs

11-10 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Using the Etch Reprocessing Program
Alternative Graphs

Vm +Im graph

Y + Dissip graph

FBP graph

Figure 11-9: log-N and alternative graphs

ECV Pro User Manual 11-11

9PROF-UM01 Issue 1.0
Using the Etch Reprocessing Program
Global parameters

11.7 Global parameters

These are sets of parameters which pertain to the specimen as a whole. They can be
entered by clicking on the Data menu and choosing Global to display the following
dialog box:

Figure 11-10: Global Parameters dialog box

Description
The phrase entered here (maximum 35 characters) will be displayed on the resulting
log-N graph and will be entered into the processed data file.

Etched Depth Calculation

The etched depth of each point is determined by integrating the charge transferred.

Mechanical measurement of etch pit depth is sometimes taken subsequently, and

can be entered to force the total etch depth to agree. Etch depths are adjusted
linearly by a fixed factor, and then the depletion depths are added to obtain the total
depths.

NOTE
As no cause for the discrepancy is assumed (eg area errors),
concentration values are not adjusted.

Electrolyte Resistance
The resistance between the platinum electrode and specimen surface is used in the
3-term model calculations. This is estimated from the measured resistance between
the platinum and counter electrodes and the sealing ring size:

R(elect)=4 x R(Pt-C) for large rings

R(elect)=15 x R(Pt-C) for small rings

11-12 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Using the Etch Reprocessing Program
Reprocessing data

11.8 Reprocessing data

To reprocess existing data, define regions and change the parameter value as required
then choose Reprocess in the menu bar. The following subsections list the items you may
wish to change before reprocessing.

11.8.1 Etched depth calculation

See Section 11.7.

11.8.2 Electrolyte resistance

See Section 11.7.

11.8.3 Deleting points

You can remove unwanted datapoints from your file or display.
Hide a data point using the Right mouse button (page 7) Point Hide function.
Hidden points are restored after each reprocessing operation. Therefore, you should hide
points just prior to saving or printing your finished results.

11.8.4 Excess area compensation

Compensation for the wetted but non-illuminated area at the edge of the sealing ring is
normally used for n-type material, especially in hi-lo structures where the remaining
surface material may contribute large capacitance values. However, the compensation
can go wildly wrong if the sealing ring areas are incorrect. It is also necessary with some
specimens (notably p-on-n) to take excess values at an underlying interface rather than at
the surface.

The reprocessing facility allows you to compensate (or not) using accurately measured
areas, and to define exactly where excess values are taken. The necessary values should
be entered in the Wetted Area and Illuminated Area fields (see Figure 11-5).

To enable excess area compensation make sure that the Excess Area Comp check box is
checked. For example, if you want compensation to be applied from the surface region,
compensation should be enabled from region 1. Compensation for subsequent regions
should normally be left ON, as it makes little physical sense to switch compensation off
once a non-etching surface is encountered.

ECV Pro User Manual 11-13

9PROF-UM01 Issue 1.0
Using the Etch Reprocessing Program
Reprocessing data

11-14 ECV Pro User Manual

9PROF-UM01 Issue 1.0
Appendix A: Etch Examples

A.1 Example 1

Figure A-1:

ECV Pro User Manual A-1

9PROF-UM01 Issue 1.0
Etch Examples

A.2 Example 2

Figure A-2:

A-2 ECV Pro User Manual

9PROF-UM01 Issue 1.0
 Etch Examples

A.3 Example 3

Figure A-3:

ECV Pro User Manual A-3

9PROF-UM01 Issue 1.0
Etch Examples

A.4 Example 4

Figure A-4:

A-4 ECV Pro User Manual

9PROF-UM01 Issue 1.0