UNIT

Metallography
1.18 Microscopy and Macroscopy :

Metallography is a study of the structural characteristics or constitution of a

alloy, in relation toits physical and mechanical properties. metal o
There are two examination methods in metallography :
1.
Microscopy
2. Macroscopy ".

1.18.1 Microscopy :
In microscopy, the examination is done with the prepared metal specimens,
emplovino
magnifications with the optical metallurgical microscope, from 100X to high as 2000X
of magnification.
In microstructural study of metals, provide information about the morphology and
distribution of phases present in the metal, due to which sometimes properties at the
metal can also determined.
Microstructural examination can provide quantitative information about the following
parameters :
(i) The grain sizeof specimen
(ü) The amnount of interfacial area per unit volume.
(iii) The dimension of constituent phases.
(iv) The amount and distribution of phases.
1.18.2 Macroscopy:
In case of macroscopic examination the nature of inhomogenities and flow lines n a
metal by unaided dye or with the help of low
power
The general distribution and variation in size of magnifying glass.
of structure, the location and non-metallic inclusions, the unifomy
extent of segregation, flow lines etc. can be
macroscopy and these cannot be examined by exame
microscopy.
Microscopic examination can provide the following
(i) information:
Crystalline heterogeneity i.e. manner of solidification and the crystalline growth
of the metal or alloy.
(iü) Chemical heterogeneity i.e. impurities in a metal or alloy, segregation of certain
chemical constituents (like sulphur or
phosphorus).
1.20 Preparation of Samples :

Specimen preparation is necessary to study it's microstructure as metallurgical

microscope makes use of the principle of reflection of light to obtain image of the metal
structure.

A satisfactory image of the microstructure can be obtained only when the specimen has
been carefully prepared.
Even the most expensive microscope will not reveal the metal structure, if the specimen
has been poorly prepared.
The procedure to be followed in the preparation of a specimen is simple but the
technique gets develop only after practice.
The final objective is toproduce a flat, scratch free and a mirror like finish surface.
The procedure for preparing the specimen for both microscopy and macroscopy
examination is the same except that in the case of microscopy the final surface finish is
more important.
The steps required to prepare a metallographic specimen are as under :
1. Selection of specimen 2. Cutting of specimen
3. Rough grinding 4. Mounting of specimen
5. Fine grinding 6. Polishing
7. Etching

1.20.1 Selection of Specimen :

Specimen should be selected from, that area of a metal, which can be taken as
representative of the metal that is being studied.
 Incase of study of failures, specimen should be taken as close as possible to the fracture
or to the initiation of the failure.
Generally in many cases, specimens are required to be taken from a sound area for a
comparison of structure and properties.
After deciding the location of the specimen, the type of section to be examined must be
decided. The location of surface examined should always be given in reporting results.
Size of specimen be proper for handling during all sample preparation techniques.
If the specimen sample is too small, then it should be mounted on the mounting press,
along with thermosetting resign or cold mounting process.
1.20.2 Cutting ofSpecimen :
After selecting a particular area, the specimen may be removed from the metallic piece
by sawing or cutting using abrasive wheel which is carried out on abrasive wheel cutting
machine as shown in Fig. 1.20.1.

Fig, 1.20.1 : Abrasive cut-off wheel

The specimen shallbe kept coolduring the cutting operation. While cutting, care must
be taken to minimize, altering the micro-structure of the metal.
1.20.3 Rough Grinding :
After cutting, a soft specimen may be made flat by slowly moving it up and back across
the surface of a smooth file, and hard specimens may be rough ground on a belt grinder
(as shown in Fig. 1.20.2).
 Fig. 1.20.2: Belt grinder
Rough grinding is continued until all scratches due tothe hacksaw or cutoff wheel are
no longer visible and the surface is flat.
Due to rough grinding surface damages, created by cutting discs, are reduced by
grinding.The belt grinding paper is made up of silicon carbide abrasive.
1.20.4 Mountingof Specimen :

(a) Mounting press

(b) Specimen duly mounted
Fig. 1.20.3
 arried out for convenience in handling it during the subsequent steps of
metallographic preparation and examination. For this the specimen is mounted.
Compression mounting involves molding around the specimen by a material like
Bakelite. acrylic resins, by application of heat and pressure. This is known as hot
mounting process.
Enoxy or polyester resins are used for cold molding, and this is known as cold mounting
[Mounting
process.[N press and duly mounted specimen is as shown in Fig. 1.20.3].
Also due to mounting of metallurgical specimen, serves for protection of the specimen
edges and improvement of it's irregular shape, which become more con venient during
grinding and polishing.
1.20.5 Fine Grinding :
After rough grinding the specimen is finely ground using fine abrasive paper (grit sizes
from 180 mesh to 600 mesh).
This abrasive grit size is as per ANSIstandards (American National Standards Institute)
system units.

Fine grinding is generally carried out on many papers, of grades from 01 to 04. i.e. 01 is
coarse grained and it's fineness goes on increasing towards 04.

The 04 grade number is very fine many papers. Special grinding table equipped with
clamps for grinding paper are used for manual graining [As shown in Figs. 1.20.4
and 1.20.5].

Fig. 1.20.4 : Emerry papers

This fine grinding is carried out on a series of stages with increasing the fineness of the
paper i.e. from 01 to 04.
Each grinding operation on a paper, will remove the marks, produced in the previous
operation.
 After each grinding stage the specimen should be thoroughly washed in order to prevent
carry over the coarser grit to the next grinding paper.
The grinding direction during each stage should be change by 90° relative to the
direction of the previous stage.

Fig. 1.20.5 : Polishing on emerry paper

This makes easier indication of completion of the grinding stage (removal of the
scratches from the previous stage).
1.20.6 Polishing:
The fine scratches caused by final grinding operation are removed by
polishing.
Polishing is carried out on single disc or double disc polisher (As shown in Figs. 1.20.6
and 1.20.7).

Fig. 1.20.6 : Single disc polishing machine

The time consumed and the success of polishing depends
largely upon the care that Was
taken during fine grinding.
 The final approximately flat scratch free surface is obtained by use of a wet rotating
wheel covered with special cloth, charged with abrasive particles,
specimen is rotated in a direction, counter to the rotation of the
During polishing, the
During
polishing wheel.
In addition the specimen is continuously moved back and forth between the centre and
odge of the wheel, thereby ensuring even distribution of the abrasive and uniform wear
of the polishing cloth.
A wide range of abrasives is available. Generally alpha grade of aluminium oxide is
used for rough polishing on one polishing wheel while gamma grade of aluminium
Oxide is used for fine polishing on other polishing wheel.
After polishing i.e. after obtaining a mirror finish image on the specimen surface, the
other alcohol
specimen is washed in warm running water, rinsed with methanol or any
that does not leave a residue, and dried in a stream of warm air.

Fig, 1.20.7- Double disc polishing machine

1.20.7 Etching :
polishing the next step is etching, etching is a selective chemical attack of
ler
specimen surface.
characteristics of the metal or alloy.
epurpose of etching is to make visible structural chemical
This is achieved by a use of an appropriate etching reagent which carTy out
action on a polished surface.
rubbing the
Etching is done by immersing the polished surface in the reagent or by
Poished surface gentlv witha cotton swab, wetted with the etching reagent.
 After etching the specimen is again washed thoroughly and dried. Now the specimen
can be studied under a microscope.
The selection of the appropriate etching reagent is determined by the metal or alloy and
the specificstructure desired for viewing.
The common etching reagents used for various metals and alloys are as under. [Refer
Table 1.20.1]
Table 1.20.1: Various etching reagents with their applications
Etching reagent Composition Use
Nitric acid White4 nitric acid "1 to 5 ml Ethyl Carbon steels and cast iron
or methyl alcohol" 100 ml (95% or
absolute)(also amyl alcohol)
Picric acid (picral) Picric acid 4 g Ethyl or methyl| Carbon steels
alcohol" 100 ml (95% or absolute)
Ferric chloride and Ferric chloride 5 g Hydrochloric Structure of austenitic
hydrochloric acid acid 50 ml water 100 ml nickel stainless steels.
Ammonium hydroxide Ammonium hydroxide 5 parts Copper and its alloys
and hydrogen peroxide water 5 parts Hydrogen peroxide
2 to 5 parts
Ammonium per Ammonium per sulphate 10 g Copper, brass, bronze.
sulphate water 90 ml aluminum silver, nickel
Palmerton reagent Chromic oxide 200 g sodium Zinc and its alloys
sulfate 15 g water 1000 ml
Ammonium molybdate Molybdic acid (85%) 100 g| Lead and its alloys
ammonium hydroxide (sp. gr. 0.9)
140ml water 240ml filter and add
tonitric acid sp. gr. 1.32) 60 ml
Hydrofluoric acid
Hyarofluoric acid (concentrated) Aluminium and its alloy
0.5 ml
 1.22 Electrolytic Etching :
Electrolytic etching is used when the specimen does not respond to conventional
chemical etching reagents.
The specimen is immersed in the acid and etching is enhanced by electric current. The
etched specimen (anode) is immersed in an acidic electrolyte.
1.23 Electrolytic Polishing :
During metallographic sample preparation techniques, even most care is taken during
mechanical polishing, some disturbed metal however will remain after preparation of a
metallographic specimen.
 If the specimen is to be examined in the as polished condition, however, or if no surface
disturbance can be accepted or tolerated, either electrolytic polishing or chemical
polishing is preferred.

Thermometer
Stirrer
Anode

Timer
Specimen

Electrolyte DC SOurce

Cathode

Cooling
Bath

Fig. 1.23.1 :Electrolytic polishing

As shown in the Fig. 1.23.1, an electrolytic reaction cell containing a liquid electrolyte
with two electrodes, an anode and cathode.
The sample to be polished/etched forms an anode. The electrodes are connected to an
external power supply and voltage applied to cause reaction within the cell.:
Inelectrolytic polishing the specimen is the anode in an electrolytic cell. Direct current
from an external cell is applied to the clectrolytic cell under specific conditions, and
anodicdissolution results in a leveling and brightening of the specimen surface.
Electrolytic polishing does not disturb any metal on the specimen surface and therefore
ideally suitable for the metallographic preparation of soft metals, most single phase
alloys, alloys that work harden readily.
The disadvantages of electrolytic polishing includes, chemical atack in multiphase
alloys due difference in electrical potential between phases.
As shown in the Fig. 1.23.2 shows the correct voltage and current for getting a best
polishing on a metal surface.
Control of the voltage and current density at the anode, plus electrolytic composition,
temperature and agitation are all critical in achieving the desired polishing surface.
 E
Acm
in
density
Current
D

best polishing; OXygenfomation

formation of viscOUs
electrolyte layer

etching polishing
voltage in V
Fig. 1.23.2 : Graphical representation of Electrolytic polishingetching
 1.19
Microscope Principle (Microstructural Exam):

Metallurgical microscope is the optical microscope which is different from the other
microscopes in the method of specimen illumination.
light
Since metals are opaque substances those must be illuminated reflected
mechanism, therefore the source of light is 1located within the microscope tube, as shown
in Fig. 1. 19.1.
This is achieved by plain glass reflector installed in the tube. The optical system of
metallurgical microscope is as shown in Fig. 1.19.1.
Also as shown in the simplified ray diagram also Fig. 1.19.2, it is clearly seen that the
--
metallurgical microscopes are differ in the manner by which the specimen is
illuminated.

Eyepiece

Light source
Plain glass
reflector

Condensing system

Objective

Specimen

Fig. 1.19.1l :Optical system of metallurgical microscope

Since metallographic samples are opaque to light, there for the samples must be
illuminated by reflected light.
The prepared metallurgical specimens are placed perpendicular to the optical axis of the
microscope and illuminated through the objective lenses by light from the source, which
is focused by the condenser into a beam that is made approximately parallel to the
optical axis of the microscope by the plane glass reflector.
The light is then reflected from the surface of the specimen. This light which is reflected
from the specimen, will be magnified in passing through the objective lens and will
continue upward through the plane glass reflector and gets magnified again by the
eyepiece.
The image quality and it's resolving power are mainly determined by the quality of the
objective.
The objective magnification depends on it'sfocal length (i.e. the shorter focal length,
the higher magnification).
Eye

Eyepiece

First image
plane

Light sOurce
Plane Glass
Reflector

Condenser lens

Objective lens

Specimen

Fig. 1.19.2 : Ray diagram of metallurgical microscope

 The eyepiece is the lens nearest the eye. The image is magnified by eye piece in
Xó, A0
or X10. The total magnification of the microscope is the product of
magnifying power
of objective multiplied by the magnifying power of eyepiece as given below :
1 Magnifying power of objective = 20X
2. Magnifying power of eyepiece = 10X
Therefore the total magnification will be 20X x 10X = 200X. The common
magnification of metallurgical microscope is in the range of 50X to 1000X.
1.19.1 Metallography :

Metallography is related to the methods of studying structure of metals and alloys.

Microstructures have a strong influence on the properties and successful application of
metals and alloys. Hence the primary objective of metallographic study is to find out the
constituents and structure of a metal or an alloy.
It is also useful in failure analysis and in research and development.
Metallographic study is divided into two types as:
1.19.1.1 Macro Examination or Macroscopy:

It is a method of examination of large regions of the specimen surface or fractured

section, allowing to determine character of the structure, defects and segregation of alloying
elements with the naked eyes or under low magnification.
1.19.1.2 Micro Examination or Microscopy :
It is the method of studying of micro-structure constituents (like grains, phases, non
hetallic inclusions, micro cracks, etc.) under high magnification, generally more than 50 or
100 X.
Some important parameter with the microscopy are :
Bright field illumination:
It is used for producing images with bright back round and dark non-flat structure
Leatures (e.g. pores, edges, etched grain boundaries).
(0) Dark field illumination :
It is used for producing images with dark background and bright non flat structure
Teatures (e.g. pores, edges, etched grain boundaries).
The structure of polished and etched metals as revealed by a microscope at a
magnification greater than ten diameters is called microstructure.
1.25.1 Sulphur Printing :
ImpuritieS may eXiSt in steel products, It is desirable that their amount
should be
minimal and homogenously distributed within the steel
product.
These impurities may degrade the mechanical properties of the steel,
content in steel makes it brittle.
especially sulphur
Sulphur may exist chemically in steel one or two forms., either as
manganese sulpnlde of
as iron sulphide. Sulphur printing detects and permanently record the distribution of
sulphur in steel.
It is used to determine distribution of sulphur impurity in the steel sample.
Sulphur
impurity has the effect of inducing brittleness in the steel or the distribution of such
impurities in the steel is very important.
Because if these impurities gets segregated at any point, may lead to local weakness, by
stress concentration at that point.
Therefore a standard method for revealing the sulphur distribution is by a chemical
method known as sulphur printing. In this method the surface to be examined is
smoothly ground.
Ensuring that the surface to be examined should be flat and smoothly polished. Then a
sheet of ordinary photographic silver bromide paper is soaked in 2% sulphuric acid
(Approximately for three minutes) the paper is then removed from the acid bath. and
hold vertically to drain out excess acid.
Then emulsion side of the paper is laid firmly on the prepared specimen surface, being
investigated. The photographic paper is rubbed smooth to remove air bubbles and to
ensure intimate contact between paper and specimen surface.
The sulphides on the steel surface react with the acid, giving off hydrogen sulphide to
Teact with the silver bromide on the paper.
This results in the appearance of dark brown spot on the paper, depending upon the
disposition of sulphide inclusions on the steel surface.
 The bromide paper is removed after 1 to 2 minutes washed and dried. The pattern es
dark brown stains indicates the way in which sulphur impurities are distributed.
The following reaction takes place during contact with photographic paper.
FcS (From steel) + H,SO, (from paper) ’ FeSO, + H,S
MnS (from steel) + H,SO,(from paper) ’ MnSO, + H,S
H,S + 2AgBr (emulsion on paper)’Ag,S+ 2HBr
This Ag,S gives a brown colour on the paper at that particular spot where the sulphide
inclusion exists.
Sulphur printing gives a permanent record of the distribution of sulphur in steel. The
specimen surface should be prepared smoothly on or 0 or 00 enemy paper, so that the
surface should be free from oil, grease, dirt and scale etc.
After polishing the paper should be thoroughly washed and dried again. This entire
process of sulphur printing can be carried out in day light, no dark roomn is needed.
The typical sulphur printing photographs at different magnification are shown in
Fig. 1.25.1 and Fig..1.25.2.

Fig. 1.25.1 : Optical micrograph showing Fig. 1.25.2: Electron micrograph showing
inclusions in the steel at 30x (lower
magnification)
inclusions in the steel, at 1000x (highersulphur
magnification)
1.25.2 Flow Lines Observations:
It issometimes desirable to determine whether or not a finished piece has
or cast into shape. Flow lines are revealed by been forged,
A macroetched forged material shows a
macroetching of forged components.
directional flow pattern consisting of streakS
and striations. The orientation of this pattern, with
respect to the plane of the prepareo
surface indicates the direction of metal flow during
deformation.
The flow lines are made visible because the
elongated inclusions of impurities, such a
oxides, sulphides are selectively attacked by the etching
reagent.
 Generally low lines are seen in forged components only. Components whicn are
manufactured by forging operation, can show enhanced mechanical properties, impact
strength, and high fatigue limit.
Which increases the service life of a component (e.g, - crank shaft, gears, cam
Shart,
rocker arm etc), several times than the samne component if manufactured by casting or
machining operation.
Therefore many components of automotive industry, aerospace industry are
manufactured by only forging process., because of grain flow in forged components.
1.25.2.1 Procedure :

Fig. 1.25.3:Sections etched to reveal flow lines : (left) original forged gear,
(right) gear do not forged as it is not showing flow lines

The specimen surface on which, a flow lines is to be observe, should by polished on 0

and '00' enemy papers.
Followed by washing and drying. Then macro etching is carried out by dipping the
Surface in a 50% aqueous solution of hydrochloric acid at a temperature of 60 to 70°C
for 5 to 10 minutes. Then the surface is washed and dried, for the observation of flow
lines.
For forged components macro-etched surface will clearly show the directional flow
pattern. The orientation of these patterns indicates the direction of metal flow during
forging.
With reference to Fig. 1.25.3, which shows original gear had been forged before the
where tha
teeth were cut. that can be seen clearly with flow lines. While in other sample
lines.
gear is mnachined directly from round bar, that do not show any flow
Fig, 1.25.4 also clearly show the pattern of flow lines in a crane hook. Fig. 1.25.5 showe
three samples, which are manufactured by three different methods.
After preparing for macro-etching, the etching surface will show the pattern like :
(a) For casting
(b) For machining and
(c) For forging, flow line pattern.

Fig.1.25.4 : Flow lines in a forged part

(a) Casting (No grain flow) (b) Machining (Parallel)

(c) Forging (Grain flow follows contour)

Fig. 1.25,5 : Macroetched specimens
 1.9.3 Electron Microscopy
Light microscopes can achieve a resolution up to 0.2 mm.
X-ray microscopes are also available to
Super-resolution light microscopy allows going beyond this limit and afew
have higher resolution.
Electron Microscopes are capable of producing very high resolution up to 1
Instrumentation
microscopes (SEM) and
Electron Microscopes are basically classified into two main types, scanning electron
transmission electron microscopes (TEM).
reflected of
SEM is a reflection microscope. Electron beam falls on the surface of the sample and reflected off. This
electrons iscollected by the scan coils" and transmitted to the computer.
TEM is transmission microscope. Electron beam passes through the -Electron gun
sample towards the fluorescent screen and camera chamber.

a 1.9.3.1 Transmission Electron Microscopy

Condenser lenses

It has an electron gun, which consists of an electron source

(a filament to produces a cloud of electrons), a Wehnelt cylinder Condenser aperture
(to form the beam) and an anode (to accelerate the beam). Objective lens
Sample
The beanm of electrons passes through the electromagnetic Objective aperture
condenser lenses. Function of condenser lenses is to focus the Intermediate lens
beam towards the condenser aperture. LAIIntermediate aperture

Apertures are thin plates of molybdenum with several small bores SProject lernses
(usually a range of 10-300 um in diameter). Apertures are used to
control the coherence of the beam, which affects resolution, and
Fluorescent screen
the amount of contrast in the signal.
Camerachamber
The condensed beam of electrons passes through the objective lenses and objective aperture, and focused onto the
sample.
The intermediate lenses and projector lenses magnify the beam and project it onto the camera (or fluorescent screen)
or projector screen to form a large image.
Advanced TEMS are capable of producing a resolution less than 2 nm.
1.9.3.2 Scanning Electron Microscopy
It has an electron gun, which consists of an electron source (a filament that produces a cloud of electrons), a Wehnelt
cylinder (to form the beam) and an anode (to accelerate the beam). Electron gun
The beam of electrons passes through the electromagnetic
condenser lenses. Function of condenser lenses is to focus
the beam towards the condenser aperture.
Condenser lenses
Apertures are thin plates of molybdenum with several
small bores (usually a range of 10-300 um in diameter).
Apertures are used to control the coherence of the beam, Scan coils
which affects resolution, and the amount of contrast in the Condenser aparture
signal.
Objective lens
The condensed beam of electrons passes through the
objective lenses and objective aperture, and focused Objective aperture
onto the sample. Detector

Electron beam falls on the surface of the sample and -Detector

reflected off. This reflected of electrons is collected by
the scan coils and detectors and transmitted to the Sample
computer.
Fig. 1.9.3