Metallography :

Metallography Sample Preparation and Examination

Objective :- Metallography and its application, Study the
microstructure of materials. Observe grain boundaries and
phases
What is Metallography :- Metallography is the science and art of
preparing a metal surface for analysis by grinding , polishing , and
etching to show micro structural component.
Introduction:- Microstructure is the geometric arrangement of
grains and the different phases present in a material. Grain
Boundaries: is the interface between two grains in a
polycrystalline material where the crystal is disordered due to
rapid change in crystallographic directions.
Facts: -Facts Most engineering alloys are polycrystalline this
means that each piece of a metal is made up of a great number of
single crystals, or grains, each having a regular crystal structure
(for example, FCC, BCC, or HCP). Materials specialists are
interested to see the grain boundaries in order to estimate the
grain sizes. The average grain size in metals is usually in the
order of several to tens of micrometers, which can be measured
only by the use of an optical or light microscope
Application:- Application Study and characterization of materials.
Ensure that the associations between properties and structure are
properly understood. Predict properties of materials. Design alloys
with new properties. Check if the material has been correctly heat
treated.
Safety Instructions:- Safety Instructions Optical Metallography
involves the use of etchants (standard solutions containing a
variety of chemicals such as strong acids and solvents) which can
be very corrosive and poisonous.
Safety :- Safety You must wear gloves and goggles and handle
the chemicals with extreme care. You must not have direct skin or
eye contact with the etchants. Etchants must be used in well
ventilated area. Do not try to smell the etchants.

Sample Preparation:- Sample Preparation The preparation starts

by cutting a small representative piece of the metal to be studied.
Mounting . Small samples can be difficult to hold safely during
grinding and polishing operations, and their shape may not be
suitable for observation on a flat surface. They are therefore
mounted inside a polymer block or mount.
Mounting: -Mounting Cold mounting can be done using two
components resins (epoxies) which are liquid to start with but
which set solid shortly after mixing. it requires very simple
equipment consisting of a cylindrical ring which serves as a mould
and a flat piece which serves as the base of the mould. The
sample is placed on the flat piece within the mould and the
mixture poured in and allowed to set. Cold mounting takes few
hours to complete.
Mounting: -Mounting Hot-mounting the sample is surrounded by
an organic polymeric powder which melts under the influence of
heat (about 200C). Pressure is also applied by a piston, ensuring
a high quality mould free of porosity and with intimate contact
between the sample and the polymer.
Grinding: - Grinding is done using rotating discs covered with
silicon carbide paper and water. There are a number of grades of
paper, with 180, 240, 400, 1200, grains of silicon carbide per
square inch. 180 grade therefore represents the coarsest particles
and this is the grade to begin the grinding operation. Always use
light pressure applied at the centre of the sample. Continue
grinding until all the blemishes have been removed, the sample
surface is flat, and all the scratches are in a single orientation.
Wash the sample in water and move to the next grade, orienting
the scratches from the previous grade normal to the rotation
direction. This makes it easy to see when the coarser scratches
have all been removed. After the final grinding operation on 1200
paper, wash the sample in water followed by alcohol and dry it
before moving to the polishers.
Polishing: -Polishing The polishers consist of rotating discs
covered with soft cloth impregnated with a pre-prepared slurry of

hard powdery alumina particles (Al2O3, the size ranges from 0.5
to 0.03 m). Begin with the coarse slurry and continue polishing
until the grinding scratches have been removed. It is of vital
importance that the sample is thoroughly cleaned using soapy
water, followed by alcohol, and dried before moving onto the final
stage. Any contamination of the final polishing disc will make it
impossible to achieve a satisfactory polish. Examining the
specimen in the microscope after polishing should reveal mirror
like surface.
Etching: - the purpose of etching is two-fold. 1. Grinding and
polishing operations produce a highly deformed, thin layer on the
surface which is removed chemically during etching. 2. attacks
the surface with preference for those sites with the highest
energy, leading to surface relief which allows different crystal
orientations, grain boundaries, precipitates, phases and defects to
be distinguished in reflected light microscopy as demonstrated in
Figure
Etching: - Etching should always be done in stages, beginning
with light attack, an examination in the microscope and further
etching only if required. If you over etch a sample on the first step
then the polishing procedure will have to be repeated. The table
below gives the etchants for alloys that will be examined in this
experiment. Etchant Sample Kellers (2 ml HF +3 ml HCL + 5 ml
NO3+ 190 ml water) Al alloys 10 ml HNO3+90 ml water Cu-Zn
alloy (brass) Natal (2% HNO3 + 98% ethanol) Steel and cast
irons
Microscopic techniques:- Microscopic techniques Optical
microscopy used to obtain an enlarged image of a small object. In
general, a compound microscope consists of a light source, a
condenser, an objective, and an ocular or eyepiece, which can be
replaced by a recording device such as a photoelectric tube or a
photographic plate. The optical microscope is limited by the
wavelengths of the light used and by the materials available for
manufacturing the lenses.

Grain Size Determination:- Grain Size Determination How to

report an average grain size? Draw few random straight lines
through the micrograph. The grain boundaries intersecting each
line are counted. The average grain size is obtained by dividing
the total length of the lines by the number of intersections taking
into account the magnification used to produce the micrograph.

1.3 What is Micro structural Analysis used for?

Micro structural and micro structural examination techniques are employed in areas
such as routine quality control, failure analysis and research studies. In quality
control, micro structural analysis is u s e d t o d e t e r m i n e i f t h e s t r u c t u r a l
p a r a m e t e r s a r e w i t h i n c e r t a i n s p e c i f i c a t i o n s . I t i s u s e d a s a criterion for
acceptance or rejection. The micro structural features sometimes considered are grain
size, amount of impurities, second phases, porosity, segregation or defects present. The
amount or size of these features can be measured and quantified, and compared to the
acceptance criterion. Various techniques for quantifying micro structural features, such
as grain size, particle or pore size, volume fraction of a constituent, and inclusion rating,
are available for comparative analysis. Micro structural analysis is used in failure
analysis to determine the cause of failure. Failures can occur due to improper
material selection and poor quality control. Micro structural examination of a failed
component is used to identify the material and the condition of the material of the
component. Through micro structural examination one can determine if the component
was made from specified material and if the material received the proper processing
treatments. Failure analysis, examining the fracture surface of the failed component,
provides information about the cause of failure. Failure s u r f a c e s h a v e b e e n w e l l
documented over the years and certain features are associated with
certain types of failures. Using failure analysis it is possible to determine the
type of stress that caused the component to fail and often times determine the origin
of the fracture. analysis is used in research studies to determine the micro structural
changes that occur as a result of varying parameters such as composition, heat
treatment or processing steps. Typical research studies include micro structural
analysis and materials property testing. Through these research programs the
processing - structure - property relationships are developed.
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2.2 Why is the microstructure of a material

important?
The most important aspect of any engineering material is its structure. The structure of
a material is related to its composition, properties, processing history and performance.
And therefore, studying the microstructure of a material provides information

linking its composition and processing to its properties and performanc e.

Interp retation of microstructures requires an understanding of the p r o c e s s e s
by which various structures are formed. Physical Metallurgy is the
s c i e n c e w h i c h provides meaningful explanations of the microstructures, through
understanding what is happening is inside a metal during the various processing
steps. Metallographic is the science of preparing specimens, examining the
structures with a microscope and interpreting the microstructures. T h e s t r u c t u r a l
features present in a material are a function of the composition and
f o r m o f t h e starting material, and any subsequent heat treatments and or
processing treatments the material receives. Micro structural analysis is used to
gain information on how the material was produced and t h e q u a l i t y o f t h e
resulting material. Micro structural features, such as grain size,
i n c l u s i o n s , impurities, second phases, porosity, segregation or surface
effects, are a function of the starting material and subsequent processing
treatments. The micro structural features of metals are well- d e f i n e d a n d
documented, and understood to be the result of specific
t r e a t m e n t s . T h e s e micro structural features affect the properties of a material,
and certain micro structural features are associated with superior properties.

1.Microstructure
Microstructure is defined as the structure of a prepared surface or thin foil of material as
revealed by a micr oscope above 25 magnification. The microstructure of a
material (which can be broadly classified into metallic, polymeric, ceramic and
composite) can strongly influence physical properties s u c h a s s t r e n g t h ,
toughness, ductility, hardness, corrosion resistance, high/low
t e m p e r a t u r e behavior, wear resistance, and so on, which in turn govern the
application of these materials in industrial practice.
1.1 What is microstructure?
When describing the structure of a material, we make a clear
distinction between its crystal structure and its microstructure. The
term crystal structure is used to describe the average positions of
atoms within the unit cell, and is completely specified by the lattice
t yp e a n d t h e fractional coordinates of the atoms (as determined, for
example, by X-ray diffraction). In other words, the crystal structure describes the
appearance of the material on an
Atomic (or ) length scale
. The term microstructure is used to describe the appearance of the material on the
nm-cm length scale
. A reasonable working definition of microstructure is: Microstructure can be
observed using a range of microscop y techniques . The micro structural
features of a given material may vary greatly when observed at different
length scales. For this reason, it is crucial to consider the length scale of the
observations you are making when describing the microstructure of a material.

The arrangement of phases and defects within a material.

2.Metallography
Metallography is the science and art of preparing a metal surface for
a n a l y s i s b y g r i n d i n g , polishing, and etching to reveal the structure of the
specimen. Ceramic, sintered carbide or any other solid material may also be
prepared using metallographic techniques, hence the collective term, materialography.
Metallographic and materialographic specimen preparation seeks to find the true
structure of the m a t e r i a l . M e c h a n i c a l p r e p a r a t i o n i s t h e m o s t c o m m o n
m e t h o d o f p r e p a r i n g t h e s p e c i m e n s f o r examination. Abrasive particles are
used in successively finer steps to remove material from the specimen surface until
the needed metallographic surface quality is achieved. A large number of material
graphic preparation machines for grinding and polishing are available, meeting
different demands on preparation quality, capacity, and reproducibility. A systematic preparation method
is the easiest way to achieve the true materialographic structure.

Introduction
The examination of microstructure is one of the principal means of evaluating alloys and
products to determine the effects of various fabrication and thermal treatments and
to analyze the cause of failur e. Main micro structural changes occur during
freezing, homogenization, hot or cold working, a n n e a l i n g , e t c . G o o d
interpretation of the structure relies on having a complete history of the
specimen. I n g e n e r a l , t h e m e t a l l o g r a p h i c o f m e t a l s a n d m e t a l l i c a l l o y s i s a
h a r d j o b i n t h e m e a n i n g t h a t materials represent a great variety of chemical
compositions and thus a wide range of hardness and different mechanical properties. Therefore
the techniques required for metallographic examination may vary considerably between
soft and hard alloys. Moreover, one specific alloy can contain several micro
structural features, like matrix, second phases, dispersions, grains, sub grains and
thus grain boundaries or sub boundaries according to the type of the alloy and its thermal or
thermo mechanical history . Howe ver , som e methods of samp le prepa ration and
observatio n are quite general and apply to all such materials. A s a g e n e r a l r u l e ,
examination should start at normal eye vision level and proceed to
h i g h e r magnification. Simplicity and cost make optical examination (macro and
micro) the most useful. When the magn ification and the depth of focus becom e too
low, the elect ron microscopes are required.
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