Sample preparation

Standard preparation methods

for materialographic analysis
Practical experience ATM-Lab
2 Table of Contents

1. General Information

Grit conversion chart,

Pressure parameters and specimen size .......................................... 3

Explanation of symbols ........................................................................ 4

2. Preparation methods

Aluminum and wrought aluminum alloy ........................................... 5

Aluminum alloy ...................................................................................... 6

Carbon/glass fiber reinforced composites (CFC/GFC) ................... 7

Cast iron (GJS/GJL) ............................................................................... 8

Soft to medium-hard steel (5-35 HRC/350HV) ............................. 9

Medium-hard to hard steel (30-65 HRC/850HV) ............................ 10

Stainless steel (austenitic/ferritic) ..................................................... 11

Steel and welded steel (macro) .......................................................... 12

Nitrided steel .......................................................................................... 13

Ceramics .................................................................................................. 14

Cobalt based alloy ................................................................................. 15

Nickel based alloy .................................................................................. 16

Spray coatings (metallic) ..................................................................... 17

Magnesium .............................................................................................. 18

Printed circuit board (non assembled) .............................................. 19

Printed circuit board (assembled) ...................................................... 20

Copper and copper alloy ...................................................................... 21

Titanium (commercial pure: grade 1-4) ........................................... 22

Titanium alloys........................................................................................ 23

NOTES:
The preparation methods can be applied for proper sectioned and burred specimens. Parameters like
pressure (given as force in newton) are referred to single pressure and depend on specimen size.
For specimens ≠ 40mm these values have to be adjusted with the help of table „Pressure parameters
and specimen size”.
Instead of the Dia Complete diamond suspensions common diamond suspensions in combination with
lubricants (water or alcohol based) can be used. Mind right dosage!
The velocity of the sample holder is 100 rpm and can vary depending on the specific material.
Due to the diversity of materials and examination aims the provided standard preparation methods
might not cover all applications. In this case contact our application lab; our team will support you
with customized preparation methods.

lab@atm-m.com
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 General Information 3

Grit conversion chart

FEPA (P) grain size [µm] ANSI/CAMI grain size [µm]

60 269 60 268
80 201 80 188
100 162 100 148
120 127 120 116
180 787 180 78
240 58.5 220 66
280 52.2 240 51.8
320 46.2
360 40.5 280 42.3
400 35 320 34.3
500 30.2 360 27.3
600 25.8 400 22.1
800 21.8
1000 18.3 500 18.2
1200 15.3 600 14.5
1500 12.6 800 12.2
2000 10.3 1000 9.2
2500 8.4 1200 6.5
4000 5

Reference:
Analytical Characterization of Aluminum, Steel and Superalloys
D. Scott MacKenzie, George E. Totten
October 10, 2005 by CRC Press

ISBN: 9780824758431

Pressure parameters and specimen size

Specimen diameter [mm] 25 30 40 50 60

Divergence in pressure - (5N…10N) - 5N 0 + 5N + (5N…10N)
used in the preparation methods

NOTES:
The preparation methods can be applied for proper sectioned and burred specimen. Parameters like pressure
(given as force in newton) are referred to single pressure and depend on specimen size. For specimens ≠ 40mm
these values have to be adjusted.

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4 Explanation of Symbols

EXPLANATION OF SYMBOLS

Symbol Meaning Symbol Meaning

Cutting Single pressure

Mounting Speed grinding disc

Grinding / Polishing Speed sample holder

Grinding / Polishing ►► Sample holder clockwise

Etching ◄► Sample holder anti-clockwise

Pre-polishing Time

Polishing / diamond Dosing lubricant

Final polishing Lubricant waterbased

Lubricant alcohol based

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 Preparation Method 5

MATERIAL Aluminum (≥99,7%) and wrought aluminum alloy

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Bakelite red/black Hot mounting
KEM 20, KEM 30 Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil** H2O 250-300 ►► 20 Until plane

grinding P320 (280)

Grinding SiC-paper/foil** H2O 250-300 ►► 20 1:00

P600 (400)

Grinding SiC-paper/foil** H2O 250-300 ►► 20 1:30

P1200 (600) (change SiC
paper/foil
after 45sec)
Polishing GAMMA Dia Complete 120-150 ►► 30 6:00
Poly, 3µm

Final LAMBDA/OMEGA Eposil F 120-150 ◄► 20 2:00

polishing 0.1µm (H2O for last
30sec)
Etching Barker’s reagent 30V
(electrolyt.)

** To reduce the contamination of the specimen by SiC particles, it should be coated with paraffin wax before
grinding

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6 Preparation Method

MATERIAL Aluminum alloy

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Bakelite black/red Hot mounting
KEM 20 Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 25 Until plane

grinding P320 (280)

Pre-polishing BETA Dia Complete 120-150 ◄► 25 5:00

Poly, 9µm

Polishing SIGMA Dia Complete 120-150 ►► 30 5:00

Poly, 3µm

Final LAMBDA/OMEGA Eposil F 120-150 ◄► 20 2:00

polishing 0.1µm (H2O for last
30sec)
Etching Kroll’s reagent 0:30
(chem.)

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 Preparation Method 7

MATERIAL Carbon/glass fiber reinforced composites (CFC/GFC)

CUTTING Equipment Consumable

Brillant Cut-off wheel: diamond, metal bond (bronze)
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Pressure vessel KEM 15 plus Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 35 Until plane

grinding P320 (280)

Pre-polishing ALPHA/BETA Dia Complete 120-150 ◄► 30 5:00

Poly, 9µm

Polishing GAMMA/DELTA Dia Complete 120-150 ►► 30 5:00

Poly, 3µm

Final LAMBDA/OMEGA Eposal 120-150 ◄► 20 1:30

polishing 0.06µm (H2O for last
30sec)

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8 Preparation Method

MATERIAL Cast iron (GJS/GJL)

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Bakelite red/black Hot mounting
KEM 30 Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 30 Until plane

grinding P320 (280)

Grinding SiC-paper/foil H2O 250-300 ►► 30 1:00

P600 (400)

Grinding SiC-paper/foil H2O 250-300 ►► 30 1:00

P1200 (600)

Polishing SIGMA Dia Complete 120-150 ►► 25 5:00

Poly, 3µm

Final LAMBDA/OMEGA Eposal 120-150 ◄► 20 1:00

polishing 0.06µm (H2O for last
10sec)*
Etching Nital 0:03-0:10
(chem.)

* Rinsing with water can cause corrosion

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 Preparation Method 9

MATERIAL Soft to medium-hard steel (<35 HRC/350HV)

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Epo black, Bakelite red/black Hot mounting
KEM 15 plus Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 30 Until plane

grinding P320 (280)

Pre-polishing BETA Dia Complete 120-150 ◄► 35 5:00

Poly, 9µm

Polishing SIGMA/GAMMA Dia Complete 120-150 ►► 30 6:00

Poly, 3µm

Final LAMBDA/OMEGA Eposal 120-150 ◄► 20 1:00

polishing 0.06µm (H2O for last
30sec)
Etching Nital (micro) 0:03
(chem.) Adler’s reagent 0:03
(macro)*

* For weld analysis

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10 Preparation Method

MATERIAL Medium-hard to hard steel (35-65 HRC/850HV)

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Epo black Hot mounting
KEM 15 plus Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar GALAXY red H2O 250-300 ►► 30 Until plane

grinding

Pre-polishing BETA Dia Complete 120-150 ◄► 30 5:00

Poly, 9µm

Final IOTA Dia Complete 120-150 ◄► 30 4:00

polishing Poly, 3µm

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 Preparation Method 11

MATERIAL Stainless steel (austenitic/ferritic)

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Epo black, Bakelite red/black Hot mounting
KEM 15 plus Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 30 Until plane

grinding P320 (280)

Pre-polishing ALPHA/BETA Dia Complete 120-150 ◄► 25 5:00

Poly, 9µm

Polishing GAMMA Dia Complete 120-150 ►► 25 5:00

Poly, 3µm

Final LAMBDA/OMEGA Eposal 120-150 ◄► 20 2:00

polishing 0.06µm (H2O for last
30sec)
Etching V2A reagent 0:05-0:30
(chem.)

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12 Preparation Method

MATERIAL Steel and welded steel (macro)

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Epo black, Bakelite red/black Hot mounting
KEM 15 plus Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 30 Until plane

grinding P180 (180)

Grinding SiC-paper/foil H2O 250-300 ►► 35 1:00

P320 (280)

Etching Adler’s reagent 0:03-0:10

(chem.) (macro)

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 Preparation Method 13

MATERIAL Nitrided steel

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Epo black** Hot mounting
KEM 15 plus Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar GALAXY green H2O 250-300 ►► 25 Until plane

grinding

Pre-polishing ALPHA/BETA Dia Complete 120-150 ◄► 25 5:00

Poly, 9µm

Polishing GAMMA/DELTA Dia Complete 120-150 ►► 30 5:00

Poly, 3µm

Final LAMBDA/OMEGA Eposal 120-150 ◄► 15 1:00

polishing 0.06µm (H2O for last
30sec)
** Before hot mounting the specimen should be wrapped in aluminum foil to stabilize the nitrided layer

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14 Preparation Method

MATERIAL Ceramics

CUTTING Equipment Consumable

Brillant Cut-off wheel: diamond, metal bond (bronze)
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Vacuum KEM 90 (porous material) Castable
KEM 35 (high-density, solid
material)

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar GALAXY red H2O 250-300 ►► 30 Until plane

grinding

Grinding GALAXY blue H2O 250-300 ►► 30 2:00

Pre-polishing BETA Dia Complete 120-150 ◄► 40 6:00

Poly, 9µm +
diamond paste

Final GAMMA Dia Complete 120-150 ►► 30 5:00

polishing Poly, 3µm +
diamond paste

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 Preparation Method 15

MATERIAL Cobalt based alloy

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin or rubber bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Epo black Hot mounting
KEM 15 plus Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 30 Until plane

grinding P320 (280)

Pre-polishing BETA Dia Complete 120-150 ◄► 30 8:00

Poly, 9µm

Polishing GAMMA Dia Complete 120-150 ►► 30 6:00

Poly, 3µm

Polishing ZETA/IOTA Dia Complete 120-150 ►► 30 3:00

Poly, 1µm

Final LAMBDA/OMEGA Eposal 120-150 ◄► 20 2:00

polishing 0.06µm (H2O for last
30sec)

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16 Preparation Method

MATERIAL Nickel based alloy

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin or rubber bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Epo black Hot mounting
KEM 15 plus Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar GALAXY green H2O 250-300 ►► 30 Until plane

grinding

Pre-polishing BETA Dia Complete 120-150 ◄► 30 6:00

Poly, 9µm

Polishing GAMMA Dia Complete 120-150 ►► 30 5:00

Poly, 3µm

Final LAMBDA/OMEGA Eposal 120-150 ◄► 20 1:30-2:00

polishing 0.06µm (H2O for last
30sec)

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 Preparation Method 17

MATERIAL Spray coatings (metallic, ceramic)

CUTTING Equipment Consumable

Brillant Cut-off wheel: diamond, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Vacuum KEM 90 Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 30 Until plane

grinding P180 (180)

Grinding SiC-paper/foil H2O 250-300 ►► 30 1:30

P320 (280)

Pre-polishing ALPHA/BETA Dia Complete 120-150 ◄► 30 5:00-8:00**

Poly, 9µm

Polishing GAMMA Dia Complete 120-150 ►► 30 5:00-8:00**

Poly, 3µm

Polishing ZETA Dia Complete 120-150 ►► 20 2:00

Poly, 1µm

Final LAMBDA Eposal 120-150 ◄► 20 1:30

polishing 0.06µm (H2O for last
30sec)
** Until constant porousity å next polishing step

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18 Preparation Method

MATERIAL Magnesium

CUTTING Equipment Consumable

Brillant Cut-off wheel: diamond, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Bakelite red/black, Thermoplast, Hot mounting
KEM 20 Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil* H2O 250-300 ►► 15 Until plane

grinding P600 (400)

Polishing BETA 120-150 ►► 15 5:00

Diamond
suspension
(alcohol or oil
based) 9µm, poly

Polishing SIGMA 120-150 ►► 15 5:00

Diamond
suspension
(alcohol or oil
based) 3µm, poly

Polishing ZETA 120-150 ►► 15 5:00

Diamond
suspension
(alcohol or oil
based) 1µm, poly

Final OMEGA** Etosil E 0.06µm 120-150 ◄► 15 4:00

polishing (ethanol for last
30sec)

Etching 3% nitric acid 0:03-0:10

(chem.) (ethanol for
30sec)
* To reduce the contamination of the specimen by SiC particles, it should be coated with paraffin wax before
grinding
** Wet the polishing cloth with ethanol before polishing

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 Preparation Method 19

MATERIAL Printed circuit board (non assembled)

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Pressure vessel KEM 20 Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 30 Until plane

grinding P180 (180) (slightly before
point of interest)

Grinding SiC-paper/foil H2O 250-300 ►► 25 1:00

P800 (500) (until point of
interest)

Grinding SiC-paper/foil H2O 250-300 ►► 25 1:00

P1200 (600) (until point of
interest)

Polishing GAMMA/DELTA Dia Complete 120-150 ►► 30 3:00

Poly, 3µm

Final ZETA/LAMBDA Eposal 120-150 ◄► 25 2:00

polishing 0.06µm (LAMBDA: H2O
for last 30sec)

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20 Preparation Method

MATERIAL Printed circuit board (assembled)

CUTTING Equipment Consumable

Brillant Cut-off wheel: diamond, metal bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Vacuum KEM 90, KEM 20 Castable
Pressure vessel

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 30 Until plane

grinding P320 (280),
GALAXY green**

Grinding SiC-paper/foil H2O 250-300 ►► 30 1:00

P600 (400),
GALAXY blue**

Grinding SiC-paper/foil H2O 250-300 ►► 30 1:00

P1200 (600),
GALAXY yellow**

Pre-polishing ALPHA/BETA Dia Complete 120-150 ◄► 25 4:00

Poly, 9µm

Polishing GAMMA/DELTA Dia Complete 120-150 ►► 25 4:00

Poly, 3µm

Final ZETA/OMEGA Eposal 120-150 ◄► 20 1:30

polishing 0.06µm (LAMBDA: H2O
for last 30sec)
** For printed circuit boards with ceramic components

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 Preparation Method 21

MATERIAL Copper and copper alloy

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Bakelite red/black, Thermoplast Hot mounting
KEM 20, KEM 30 Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 30 Until plane

grinding P320 (280)

Grinding SiC-paper/foil** H2O 250-300 ►► 30 1:30

P600 (400)

Grinding SiC-paper/foil** H2O 250-300 ►► 30 1:30

P1200 (600)

Polishing SIGMA Dia Complete 120-150 ►► 30 4:00

Poly, 3µm

Final OMEGA Eposil F 120-150 ◄► 15 2:00

polishing 0.1µm** (H2O for last
30sec)
Etching Klemm’s I 0:02
(chem.) reagent

** 50ml Eposil F + 1ml H2O2 + 1ml NH3

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22 Preparation Method

MATERIAL Titanium (commercial pure: grade 1-4)

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Epo black Hot mounting
KEM 20, KEM 15 plus Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 25 Until plane

grinding P320 (280)

Pre-polishing ALPHA/BETA Dia Complete 120-150 ◄► 20 10:00

Poly, 9µm

Final LAMBDA Eposil F 120-150 ◄► 20 10:00 – 15:00*

polishing 0.1µm** (H2O for last
30sec)
Etching Kroll’s reagent 0:45
(chem.)

* Depends on grade of titanium

** Eposil F has to be mixed with hydrogen peroxide (35%) in a ratio of 5:1

(safety advice: use personal protective equipment)

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 Preparation Method 23

MATERIAL Titanium alloy

CUTTING Equipment Consumable

Brillant Cut-off wheel: corundum, resin bond
Anti-corrosion coolant

MOUNTING Equipment Consumable Method

Opal Epo black Hot mounting
KEM 20, KEM 15 plus Castable

GRINDING/ Specimen size Ø 40 mm

POLISHING

STEP MEDIUM

rpm N min

Planar SiC-paper/foil H2O 250-300 ►► 25 Until plane

grinding P320 (280)

Grinding SiC-paper/foil H2O 250-300 ►► 25 1:30

P600 (400)

Pre-polishing ALPHA/BETA Dia Complete 120-150 ◄► 20 5:00

Poly, 9µm

Final LAMBDA Eposil F 120-150 ◄► 20 5:00 – 10:00*

polishing 0.1µm** (H2O for last
30sec)
Etching Kroll’s reagent 0:45
(chem.)

* Depends on the alloy

** Eposil F has to be mixed with hydrogen peroxide (35%) in a ratio of 5:1

(safety advice: use personal protective equipment)

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2 Preparation Method

Subject to technical modification and errors ∙ Stand 04_2018

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