Unit IV

Micro & macroscopic

study of Metals
 Content
1. Macroscopy: Sulphur printing, flow line observations
2. Optical Microscopy - Introduction, Optical principles,
Instrumentation, metallographic study
3. (Various sampling techniques, specimen preparation,
specimen mounting (hot & cold mounting)
4. electrolytic polishing, etching procedure and reagents,
electrolytic etching,
5. Microscopic methods operating principle and applications of
Metallurgical microscope, Transmission Electron Microscopy
(TEM),
6. Scanning Electron Microscopy (SEM), Measurement of grain
size by different methods & effect of grain size on various
mechanical properties
Macroscopy
 Why Macroscopy
• Macro-Examination is carried out for the following
purposes:
1. To reveal size, form and arrangement of crystallites
(dendrites) in cast metals.
2. To reveal size , form & fibers in deformed metals.
3. To check manufacturing method (forging , welding ,
casting, etc..)
4. To check cavities due to gas and porosity during
solidification shrinkage.
5. To find chemical non-homogeneity during solidification.
6. To find inclusion
7. To find cause of failure
8. To find non metallic inclusions.
 Macroscopy
• Study of large area of component is done with unaided eyes or
with magnifying glass or using low powered microscope (10X)
• Sampling
– Suitable sample of material is selected (25cm X 25cm)
– Good surface finish is required (Grinding or 0 polishing)
• Etching
– Macro-etching is done under controlled conditions of temp. and time
– Surface defects, inclusions, segregated areas are selectively dissolved
by etching reagents and subsequently some visible characteristics
such as cavities, local discoloration is observed
• Observation
 Different types of etchants in macroscopy
Sr. no. Composition of Etching time Surface Observations
etchant and temp finish
required

1 HCl 15-60 min. at A or B(Avg. Segregation, porosity, hardness

71-82°C ground indentation penetration, cracks,
surface) inclusions, dendrites, flow line, soft
spot, structure and weld examination

2 10 parts of H2SO4 15-60 min at A(Saw cut) Sulphide and oxide inclusion
and 90 parts of H2O 71-82°C

3 2-25% HNO3 in 5-30min at B or C Carburization, decarburization,

water or alcohole room temp hardness indentation penetration,
cracks, Segregation, weld
examination

4 2.5 gm CuCl2.2H2O Until coppery B or C P rich areas, p banding, and general

sheen appears segregation
at room temp

5 50 gm (NH4)2S2O8 Swab until C (Polished Grain size and weld joint

500 ml H2O desired etch at surface)
room temp
 Sulphur Print
• This test is used to detect distribution of S in steel (ASTM
E1180)
• S makes steel cold or hot short and hence detrimental
• Harmful effect of S is reduced by addition of Mn
• Surface should be clean from grease, dirt and scale
• Procedure
– Photographic bromide paper is soaked for about 3-4 min. in 2% aq.
Solution of H2SO4
– Paper is taken out from the solution and excess solution is removed
– Emulsion side of the paper is placed in contact with the surface of
the specimen for about 2-3 min. under moderate pressure
– This photographic paper is removed from surface of specimen,
washed in running water and kept in photographic fixer solution for
15 min.
– It is then removed from solution and washed in running water for 1
hr and subsequently dried
• Examination of this print clearly reveals the presence of S by
dark coloured areas of silver sulphide on the paper
• Grouping of these areas shows S segregation where as
random distribution of the spot shows uniform or less harmful
distribution of S
• Reactions are as follows
FeS (from steel) + H2SO4 (from paper)  FeSO4 + H2S
MnS (from steel) + H2SO4 (from paper)  MnSO4 + H2S
H2S + 2AgBr (emulsion on paper)  Ag2S (Brown)+ 2HBr
 Flow line observations
• Forged components have superior properties than cast, rolled
and machined components
• Properties of forged component are governed by metal flow
pattern during forging
• To find out manufacturing of component, prepared surface of
component etched in 50% aq. Solution of HCl at temp of 60-
70°C for 5-10 min.
• Forged component shows directional flow pattern consisting of
streak and striations
• Orientation of this pattern w.r.t plane of prepared surface
indicates the direction of metal flow during forging
• Flow lines are seen due to attack on inclusions and other
elongated heterogeneous areas by etching reagent
• During deformation, highly stressed area gets
preferentially attacked by etching reagent
• Even after Normalizing or Annealing of
component, Flow lines are seen due to
– Presence of elongated nonmetallic inclusions
– Presence of preferred orientation areas which are
always formed due to normalizing or annealing of
cold worked metal
• Observation of flow line pattern gives idea
about mechanical working on metal

Metallography_Part_I_-_Macroscopic_Techniques.mp4
 Microscopy
• Microscopy involves study of prepared metal surface
using higher magnification
• It revels structural details such as
– Grain size,
– Shape and distribution of secondary phases,
– Non metallic inclusions
– Segregation.
• Study of microstructure also gives idea about
– The heat treatment performed on the material
– History of mechanical properties
Specimen preparation for
metallographic inspection
1) Sampling or sectioning
2) Mounting
a) Hot
b) Cold
3) Polishing
a) Rough polishing
i) Dry
ii) Wet
b) Fine polishing
4) Etching
a) Etching of single phase alloy
b) Etching of two phase alloy
5) Observation under microscope
SECTIONING
 Sectioning is the most important step in preparing specimens
for physical or microscopic analysis
 Microstructure should not be altered, but practically hot and
cold working accompany most sectioning methods.
 The damage to the specimen during sectioning
depends on
 the material being sectioned
 the nature of the cutting device
 the cutting speed and feed rate
 the amount and type of coolant used

Depth of deformation in different metals due to cutting method

SECTIONING METHODS
 Fracturing
 Breaking specimens with blows of a hammer or by steadily
applying pressure
 Not recommended, because it rarely follows desired directions
and damage from fracturing can mask inherent features
 Also lengthy coarse grinding may be required to obtain a flat
surface
 Shearing
 Low-carbon sheet steel and other thin, soft materials can be cut
to size by shearing
 The area affected by shearing must be removed by grinding
SECTIONING METHODS
 Sawing
 Using hacksaws, band saws, and wire saws
 Hand-held hacksaws or band saws generally do not generate
enough frictional heat to alter the microstructure
 Saw-cut surfaces are rough, and coarse grinding is required to
obtain a flat surface
 Electric discharge machining (EDM)
 Electric discharge machining (EDM), or spark machining, is a
process that uses sparks in a controlled manner to remove material
from a conducting workpiece in a dielectric fluid like kerosene
 The material is removed from the sample in the form of
microscopic craters
SAWING

hacksaw Band saw Wire saw

EDM

EDM schematic

EDM machine
SECTIONING METHODS
Abrasive cutting
 Abrasive cutting is the most widely used method of sectioning
 Conventional abrasive cutting using consumable wheels is fast,
accurate, and economical and most popular
 The quality of the cut surface obtained is often superior to that
obtained by other methods
ABRASIVE CUTTING

Consumable abrasive wheel

Abrasive cutting machine Non consumable abrasive wheel

 MOUNTING (Hot or Cold)
 Small or oddly shaped specimens are mounted to facilitate easy
handling during preparation and examination
 Standard mounts usually measure 25 mm (1 in.), 32 mm (1.25
in.), or 38 mm (1.5 in.) in diameter
 Bakelite and diallyl phthalate are thermosetting resins which are
most widely used as moulding material
 Transparent methyl methacrylate, polystyrene, polyvinyl chloride
(PVC)are some of the thermoplastic resins used in moulding
 Both requires heat (135-150°C) and pressure during molding.
Thermosetting molds can be ejected from the mould at the
moulding temperature, while thermoplastic resins must be cooled
to ambient temperature under pressure
MOUNTING (Hot or Cold)

Mounted specimen Hot mounting press machine

GRINDING
 To prepare the cut surface suitably for metallographic
examination as optically flat, reflective, smooth and
scratch free
 Machining
 involves the use of tools having cutting edges of controlled
shape like sawing, lathe turning, milling, and filing
 used only for the preliminary stages of preparation
 Grinding and abrasion
 uses abrasive particles whose projecting points act as the
cutting tools
 the abrasive particles are cemented together into a block whose
exposed surface is the working surface
GRINDING
 Examples are abrasive cutoff wheels, grinding wheels, abrasive
laps, and abrasive stones
 in another type, a layer of abrasive particles is cemented onto a
cloth or paper backing, creating coated abrasive products
 Emery papers are typical example for this kind
 Grinding employ high surface speeds were heating of the
surface layers may occur
 Abrasion uses low surface speeds, hence no significant
heating takes place
GRINDING WHEELS

Mechanized grinding wheels

POLISHING
 Manual polishing is done by rotating specimen by hand
against a cloth that has been charged with a fine abrasive
and an appropriate liquid, and then has been stretched
across a flat backing surface
 Diamond, alumina (Al2O3), and magnesium oxide (MgO)
are the abrasives most commonly used for polishing
 The paper or cloth is attached to the surface of a wheel
that is rotated at a comparatively low speed in a horizontal
plane
 The specimen is held against the working surface of a
wheel and rotated slowly in a direction opposite that of the
wheel
ELECTROLYTIC POLISHING
 used widely in the metallography of stainless steels, copper
alloys, aluminum alloys, magnesium, zirconium, and other metals
that are difficult to polish by conventional mechanical methods
 Electrolytic polishing can completely remove all traces of worked
metal remaining from mechanical grinding and polishing
operations used in specimen preparation
 Rough surface is made the anode of a suitable electrolytic cell,
and preferential solution of the "hills" or ridges on a rough
surface takes place
 In molded sample, only the portion of the specimen to be
polished should be in contact with the electrolyte
 High surface finish can be obtained
ELECTROLYTIC POLISHING

1. Electrolyte
2. Cathode
3. Workpiece to
polish (Anode)
4. Particle moving
from the workpiece
to the cathode
5. Surface before polishing
6. Surface after polishing

Principle Machine
ETCHING
 ETCHING is used in metallography primarily to reveal
the microstructure of a specimen under the optical
microscope
 It is procedure for achieving contrast in the
microstructure
 Nondestructive Etching is a type of etching which do not
alter the surface of the microsection
 Optical Etching uses special illumination techniques to obtain
contrast
 These optical etching techniques are dark-field illumination,
polarized light microscopy, phase contrast microscopy, and
differential interference contrast
 ETCHING
 Destructive Etching induces surface damages. They are
classified as
1. Electrochemical (Chemical) Etching
 Chemical etching
 Oldest and most commonly applied technique
 Etchant reacts with the specimen without the use of an external current
supply
 Etching proceeds by selective dissolution according to the electrochemical
characteristics of the constituents
 Proper selection of etchant and etching time is the most important criteria
which are determined experimentally and is given by ASTM E407
(Standard Practice for Micro-etching Metals and Alloys)
 Microstructure obtained is decided by etchant and etching time
 Behavior of different etchants on microstructure

Low carbon steel

Etched with 2% Nital Etched with 4% Picral Etched with Beraha’s reagent
 SOME COMMONLY USED ETCHANTS

NAME COMPOSITION USE

Nital 2 mL HNO3 and 98 mL For carbon steels; gives
ethanol or methanol maximum contrast
between pearlite and a
ferrite or cementite
network
Picral 4 g picric acid, 100 mL For all grades of carbon
ethanol or methanol steels
Beraha's reagent 3 g K2S2O5, 10 g Colours ferrite grains
Na2S2O3, and 100 mL
H2O
Aqua regia 3 parts HCl + 1 part Used with austenitic
HNO3 grades to reveal grain
structure, outline ferrite
and σ phase
Glyceregia 3 parts glycerol, 2-5 Popular etch for all
parts HCl, 1 part HNO3 stainless grades
 Electrolytic Etching
 In electrolytic (anodic) etching, electrical potential is
applied to the specimen using an external circuit
 Specimen to be etched made anode and some
suitable cathode such as platinum or graphite made
cathod
 During electrolytic etching, positive metal ions leave
the specimen surface and diffuse into the electrolyte
 Selection of electrolyte depends upon composition of
metal or alloy and constituents to be revealed in the
alloy
 Current densities are less than that required for
electro polishing
 Suitable for Al, Al alloys, high Cr steels, and
stainless steels
Basic laboratory setup for electrolytic etching
 TERMS AND DEFINITIONS
Principle
Microscopy is to get a magnified image, in which structures may be
resolved which could not be resolved with the help of an unaided eye.
Magnification
•It is the ratio of the size of an object seen
under microscope to the actual size
observed with unaided eye.
•The total magnification of microscope
is calculated by multiplying the magnifying
power of the objective lens by that of eye piece.
Resolving power
•It is the ability to differentiate two close points as separate.
•The resolving power of human eye is 0.25 mm
•The light microscope can separate dots that are 0.25µm apart.
•The electron microscope can separate dots that are 0.5nm apart.
 TERMS AND DEFINITIONS
Limit of resolution
It is the minimum distance between two points to identify them
separately.
It is calculated by Abbé equation.

Limit of resolution is inversely proportional to power or resolution.

If the wavelength is shorter then the resolution will be greater.
Working distance
•It is the distance between the objective
and the objective slide.
•The working distance decreases with
increasing magnification.
 TERMS AND DEFINITIONS
Numerical aperture(NA)
The numerical aperture of a lens is the ratio of the diameter of the lens to its
focal length. OR it is light gathering or collecting capacity of objective.
NA of a lens is an index of the resolving power.
NA can be decreased by decreasing the amount of light that passes through
a lens.

Diameter of the lens

Light microscope
 Light microscope
Parts of microscope

• Illuminator - This is the light source located below the specimen.

• Condenser - Focuses the ray of light through the specimen.
• Stage - The fixed stage is a horizontal platform that holds the specimen.
• Objective - The lens that is directly above the stage.
• Nosepiece - The portion of the body that holds the objectives over the stage.
• Iris diaphragm - Regulates the amount of light into the condenser.
• Base – Base supports the microscope which is horseshoe shaped.
• Coarse focusing knob - Used to make relatively wide focusing adjustments to
the microscope.
• Fine focusing knob - Used to make relatively small adjustments to the
microscope.
• Body - The microscope body.
• Ocular eyepiece - Lens on the top of the body tube. It has a magnification of
10× normal vision.
 WORKING PRINCIPLE OF TEM
• Electrons possess a wave like character.

• Electrons emitted into vacuum from a heated

filament with increased accelerating potential
will have small wavelength.

• Such higher-energy electrons can penetrate

distances of several microns into a solid.

• These transmitted electrons could be focused -

images with much better resolution.

• Focusing relies on the fact that, electrons also

behave as negatively charged particles and are
therefore deflected by electric or magnetic fields.
• The electron source consists of a
cathode and an anode.
• Cathode - tungsten filament which
emits electrons when being heated.
•A negative cap confines the electrons
into a loosely focused beam
• The beam is then accelerated towards
the specimen by the positive anode

Electron beam is tightly focused using

electromagnetic lens and metal
apertures.

A platform equipped with a mechanical

arm for holding the specimen and
controlling its position.

Electromagnetic lens system

Objective lens Projector lens

Phosphorescent Screen
 WORKING OF TEM
• Electron beam is produced by a heated W filament and accelerated down
the column by applying high voltage (100 to 300 kV)
• Specimen is bombarded by a beam of electrons, the primary electrons .
The bombarding electrons are focused to a bundle onto the object.
• In areas in the object where these electrons encounter atoms with a heavy
atomic nucleus, they rebound.
• In regions where the material consists of lighter atoms , the electron are
able to pass through.
• The fine pattern of electrons leaving the object , reaches the objective lens
forms the image
• It is then greatly enlarged by projector lens.
• Eventually, the traversing electrons (transmission) reach the scintillator
plate at the base of the column of the microscope.
• The scintillator contains phosphor compounds that can absorb the energy
of the stricking electrons and convert it to light flashes.
• Thus a contrasted image is formed on this plate.
 APPLICATIONS OF TEM
• Direct observations of dislocations
• Observation of stacking fault
• Formation of sub-grains without recrystallization in warm or hot deformation
• Precipitate behaviour in high temp alloy
• The fine phases causing temper brittleness in the alloy steel
• In medicine as a diagnostic tool – important in renal biopsies.
• Cellular tomography
– Tomography refers to imaging by sectioning, through the use of any kind of
penetrating wave.
– Information is collected and used to assemble a three dimensional image of the
target.
– Used for obtaining detailed 3D structures of subcellular macromolecular
objects.
• Cancer research - studies of tumor cell ultrastructure .
• Toxicology – to study the impacts of environmental pollution on the different
levels of biological organization.
 WORKING PRINCIPLE OF SEM
• Incoming (primary) electrons
– can be “reflected” (backscattered)
from a bulk specimen.
– can release secondary electrons.
• Primary electrons are focused into a
small-diameter electron probe that is
scanned across the specimen.
• Electrostatic or magnetic fields, applied
at right angles to the beam, can be used to
change its direction of travel.
• By scanning simultaneously in
two perpendicular directions, a square or
rectangular area of specimen (known as a
raster) can be covered.
• Image of this area can be formed by
collecting secondary electrons from each
point on the specimen.
 SEM WORKING
• The electron gun produces an electron beam when tungsten wire is
heated by current.
• This beam is accelerated by the anode.
• The beam travels through electromagnetic fields and lenses, which
focus the beam down toward the sample.
• A mechanism of deflection coils enables to guide the beam so that
it scans the surface of the sample in a rectangular frame.
• When the beam touches the surface of the sample, it produces:
– Secondary electrons (SE)
– Back scattered electrons (BSE)
– X - Rays...
• The emitted SE is collected by SED and convert it into signal that is
sent to a screen which produces final image.
• Additional detectors collect these X-rays, BSE and produce
corresponding images.
• A secondary electron detector attracts the scattered electrons and,
depending on the number of electrons that reach the detector,
registers different levels of brightness on a monitor.

• By reducing the size of the area scanned by the scan coils, the SEM
changes the magnification of the image.
 APPLICATIONS OF SEM
• Used to detect and analyze surface fracture, provide information in
microstructures
• Inspect surface contaminations and identify crystalline structure
• Semiconductor inspection, assembly of microchips for computers
• Virology - for investigations of virus structure
• Cryo-electron microscopy – Images can be made of the surface of
frozen materials.
• 3D tissue imaging -
– Helps to know how cells are organized in a 3D network
– Their organization determines how cells can interact.
• Forensics - SEM reveals the presence of materials on evidences that is
otherwise undetectable
• SEM renders detailed 3-D images
– extremely small microorganisms
– anatomical pictures of insect, worm, spore, or other organic
structures
 Differences between SEM and TEM
TEM SEM
Electron beam passes through thin Electron beam scans over surface of
sample. sample.

Specially prepared thin samples are Sample can be any thickness and is
supported on TEM grids. mounted on an aluminum stub.

Specimen stage halfway down Specimen stage in the chamber at

column. the bottom of the column.

Image shown on fluorescent screen. Image shown on TV monitor.

Image is a two dimensional Image is of the surface of the sample

projection of the sample.
 Grain Size Measurement
• ASTM standard E112-10

• Determination of planar grain size

• A microscopically-determined grain size of No. 1 has

1.000 grains/in2 at 100X
 Grains and Grain Boundaries
and their effects on a metal
Grain size has a significant effect on the strength of metals.
Grain boundaries have a major influence on metal behavior.
Significantly influences mechanical properties of the metal
 Large grain size is generally associated with
- Low strength
- Low hardness
- Low ductility
 Small grain size is generally the opposite
 What are grains?

• Grains- individual, randomly oriented

crystals within a metal

Grain Structure of metal alloys

 Comparis
on
procedur
e

GRAIN
SIZE
MEASU
REMEN Jefferies
Heyn’s
Intercept T Planimetr
procedur ic
e procedur
e
 Comparison Procedure
– Applicable for equiaxed grains
– Grin size is reported by ASTM grain size number
– This number is found out by measuring the number of
grains(N) per square inch at 100X (75X for copper base
alloys) by using following equation
• N = 2n-1 where n = ASTM grain size number
– Standard charts are prepared for measurement of grain
size by using ASTM E112 standard
– The grain size is compared with the size given in the
above chart at 100X and the matching number is
reported
– Matching can be done by either by focusing image on
screen and compare or by use of comparison eye piece
ASTM grain size number
 Jeffries Planimetric Procedure
– Used for measuring grain size of equiaxed grins
– In this method circle or rectangle of known area (5000 sq.mm)is drawn
on metallograph
– Adjust magnification in such a way that at least 50 grains should be
seen in the field
– Involves an actual count of the number of grains within a known area.
– Total number of grains will be sum of grains included in the above area
plus half the grains intersected by the circumference.
– Number of grains per unit area, NA, is used to determine the ASTM grain
size number, G.
– Require marking off of the grains as they are counted.

• F = Jefferis multiplier
Relationship Between Magnification Used and Jeffries’
Multiplier, f, for an Area of 5000 mm2 (f= 0.0002 M2)
 Heyn’s Intercept Procedure
– Used when grains are not equiaxed
– Consist of finding out he number of grains intercepted by a line of fixed length
– Magnification should be such that the area covered is at least 0.5 mm2 on the
actual sample
– Actual count of the number of
• grains intercepted
• grain boundary, per unit length of test line
– Lineal intercept length, used to determine the ASTM grain size number, G.
– Faster than the planimetric method for the same level of precision.
– Structures consisting of elongated grains.
– Avg. intercept length (Grain diameter) is the ratio of length of the line(in mm)
to avg. number of grains intercepted by that line
Thank You