Metallography Specimen Preparation and Examination

Metallography is the study of a materials microstructure. Analysis of a materials microstructure aids in

Background:

Materials engineers can predict the general behavior of materials by observing their
microstructure. Besides the crystallographic nature of a material, imperfections inside a
material have an even greater influence on the mechanical properties, i.e. tensile, fatigue,
creep, fracture toughness, impact properties. Some defects such as missing planes of atoms, called
dislocations, are responsible for plastic deformation of crystalline solids. Others such as grain
boundaries, precipitates, twins and cracks alter stress distribution in a material and the accompanying
motion of dislocations. Some defects such as missing atoms and dislocations cannot be observed
optically except by their effects, i.e. strain, etch pits, slip lines. Other defects such as grain boundaries,
twins, precipitates, can be observed readily in the microscope.Metallography consists of the study of
the constitution and structure of metals and alloys. Much can be learned through specimen
examination with the naked eye, but more refined techniques require magnification and preparation of
the material's surface. Optical microscopy is sufficient for general purpose examination; advanced
examination and research laboratories often contain electron microscopes (SEM and TEM), x-ray and
electron diffractometers and possibly other scanning devices. Incorrect techniques in preparing a
sample may result in altering the true microstructure and will most likely lead to erroneous
conclusions. It necessarily follows that the microstructure should not be altered. Hot or cold working
can occur during the specimen preparation process if the metallurgist is not careful. Expertise at the
methods employed to produce high-quality metallographic samples requires training and practice. The
basic techniques can be learned through patient persistence in a matter of hours. This module takes the
student through the metallographic sample preparation process step-by-step with demonstrations and
explanations of sectioning, mounting, course & fine grinding, polishing, etching and microscopic
examination.

1) Sectioning:

SECTIONING, the removal of a conveniently sized, representative specimen from larger sample, is
one of five major operations in the preparation of metallographic specimens. The methods that can be
used in sectioning possibly are Fracturing , Sawing , Shearing , Abrasive Cutting , Use of wire
saws or by Electric Discharge Machining.
However the method we used in our laboratory for sectioning the specimen is by the use of Hand
Saw. Sawing, perhaps the oldest sectioning method, can be performed using a hand-held hacksaw, a
band saw, or an oscillating
power hacksaw. Hand-held hacksaws or band saws, either vertical or horizontal, generally do not
generate enough frictional heat to alter the microstructure; However, frictional heat can temper the
blades enough to eliminate their cutting ability. Although coolants should be used in any type of
sectioning, band saw cutting can be performed without a coolant; the speed is slow enough that
frictional heat is not detrimental to the material. In the case of power hacksaws, with their thicker and
coarser blades, a coolant must be used, because the depth of deformation introduced by this severe
method of sectioning can be quite deep.

2) Mounting:

Small samples are generally mounted in plastic for convenience in handling and to protect the edges of
the specimen being prepared. Compression-type molding is commonly applied to encase specimens in
1 to 1.5 inch diameter plugs of a hard polymer. Compression molding materials are classified as either
thermosetting or thermoplastic:

1. Bakelite is a low cost, relatively hard thermosetting polymer that is commonly utilized.
2. Expensive Transoptic Thermoplastics are utilized when transparency is required.
Mounting involves placing the specimen in a mold and surrounding it with the appropriate powders.
The mold and its contents are then heated under pressure to the thermal setting or the softening
temperature. Once the powder sets, thermosetting mounts can be removed from the mold without
lowering the temperature; thermoplastic mounts must be cooled to ambient temperature before
removal. Mounting pressure or temperature may alter the structure of low melting temperature or soft
and/or fragile specimens; therefore, castable (cold-mounting) techniques have been developed.
Plastics that set at room temperature are referred to as castable (cold-mounting) materials. The most
widely used materials are epoxy resins. Epoxies resist acids and strong solvents effectively, a desirable
characteristic in any mounting material. Epoxies and thermoplastic materials are relatively soft
mounting materials, and the specimen in such a mount must often be surrounded by a hard material,
for example, hardened steel balls . This material helps retain the edges of the sample by maintaining a
flat surface during grinding and polishing.

3) Grinding:

Grinding is generally considered the most important step in specimen preparation. Care must be taken
to minimize mechanical surface damage. Grinding is generally performed by the abrasion of the
specimen surface against water lubricated abrasive wheels (assuming water does not adversely affect
the metal). Grinding develops a flat surface with a minimum depth of deformed metal and usually is
accomplished by using progressively finer abrasive grits on the grinding wheels. A typical sequence
might begin with 120- or 180-grit papers and proceed to 240, 320, 400, and 600 grits. Scratches and
damage to the specimen surface from each grit must be removed by the next finer grinding step. The
surface damage remaining on the specimen after grinding must be removed by polishing. If this
disturbed or deformed metal at the surface is not removed, microstructural observations may be
obscured. Because structure and properties are so closely related, conclusions based on the structure in
would lead to incorrect interpretation of the anticipated behavior of the metal.

Generally there are two steps involved in grinding which are termed as follows :
Coarse Grinding.
Medium and Fine Grinding.

3.1) Coarse Grinding:

In view of the perfection required in an ideally prepared metallographic sample, it is essential that
each preparation stage be carefully performed. The specimen must:
1. Be free from scratches, stains and others imperfections which tend to mark the surface.
2. Retain non-metallic inclusions.
3. Reveal no evidence of chipping due to brittle intermetallic compounds and phases.
4. Be free from all traces of disturbed metal.
The purpose of the coarse grinding stage is to generate the initial flat surface necessary for the
subsequent grinding and polishing steps. As a result of sectioning and grinding, the material may get
cold worked to a considerable depth with a resultant transition zone of deformed material between the
surface and the undistorted metal. Course grinding can be accomplished either wet or dry using 80 to
180 grit electrically powered disks or belts, but care must be taken to avoid significant heating of the
sample. The final objective is to obtain a flat surface free from all previous tool marks and cold
working due to specimen cutting. An important factor throughout the Coarse Grinding and Fine
Grinding Stages is that the scratches be uniform in size and parallel to each other in any one grinding
stage. Proper grinding involves rotation of the sample by 90o between stages while the grinding angle
must be held constant during the grinding at any one stage.

3.2) Medium and Fine Grinding:

Medium and Fine Grinding of metallurgical samples are closely allied with the Coarse Grinding which
precedes them. Each stage of metallographic sample preparation must be carefully performed; the
entire process is designed to produce a scratch free surface by employing a series of successively finer
abrasives. Failure to be careful in any stage will result in an unsatisfactory sample.
The idea is to carefully move from one stage to the next where the abrasives become finer at each
successive stage. Movement from one stage to the next should only proceed when all of the scratches
from the preceding stage are completely removed. In general, successive steps are 320, 400 and 600 or
1000 grit SiC and the grinding rate should steadily decrease from one stage to the next. Proper
grinding involves the rotation of the sample between stages while the grinding angle must be held
constant during the grinding at any on stage.

4) Polishing:
Polishing involves the use of abrasives, suspended in a water solution, on a cloth-covered electrically
powered wheel. Diamond abrasives provide the best, and most expensive, compounds utilized in
polishing; standard sized aluminum oxide powders are applied for general use purposes. Following the
final 600 grit fine-grinding stage, the sample MUST be washed and carefully dried before proceeding
to the first polishing stage! At the polishing stages, even hard dust particles in the air which settles on
the polishing cloth can cause unwanted scratching of the specimen! Careful washing of the specimen
and the operator's hands must be carried out prior to each stage of polishing!
The specimen is initially held at one position on the wheel, without rotation, until most of the previous
grinding marks are removed. It can be rotated slowly, counter to the wheel rotation, During the initial
polishing stage, moderate pressure can be applied to the specimen and the entire stage should
generally take 1 or 2 minutes!
For precision work, extremely fine grades of diamond abrasives may often be used for the final
polishing sequence. Cerium Oxide is especially excellent for the final polishing of aluminum and
other soft metals and alloys. The best abrasive types and sizes for various metals and alloys are listed
in the literature. The most commonly used polishing or buffing wheels are sisal buffing wheel ,
cushion buffing wheel and loose cotton wheel.
Generally, polishing can also be accomplished electrochemically, using an electrolytic cell which is
similar to the ones used for electroplating, except that the polishing cell operates in reverse. The metal
atoms are thus stripped from the specimen surface. Careful control is required for electropolishing; it
is best suited to finishing a large number of identical specimens.

5) Etching:

Microscopic examination of a properly polished, unetched specimen will reveal only a few structural
features such as inclusions and cracks or other physical imperfections. Etching is used to highlight,
and sometimes identify, microstructural features or phases present. Even in a carefully prepared
sample, a surface layer of disturbed metal, resulting from the final polishing stage, is always present
and must be removed. Etchants are usually dilute acid or dilute alkalis in a water, alcohol or some
other solvent. Etching occurs when the acid or base is placed on the specimen surface because of the
difference in rate of attack of the various phases present and their orientation. The etching process is
usually accomplished by merely applying the appropriate solution to the specimen surface for several
seconds to several minutes. During the electrochemical etching of metallic specimens, reduction
(cathodic reactions) and oxidation (anodic reactions) take place. All metals contacting the etching
solutions tend to become ionized by releasing electrons. The extent of this reaction can be recorded by
measuring the electrochemical potential. This is performed by comparing the potential of metal versus
the standard potential of a reference electrode. The tabulation of various metals results in the
electromotive series of elements: Li+, Na +1, K+1, Ca+2, Ba+2, Be+2, Mg+2, Al+3, Mn+2, Zn+2, Cr+3, Cd+2,
Ti+1, Co+2, Ni+2, Pb+2, Fe+3, H+1, Sn+4, Sb+3, Bi+3, As+3, Cu+2, Ag+1, Mg+2, Au+3, Pt+3
Procedure
First of all take the required material which is to be observed under microscope or whose
 metallography is to be required. ( circular cross section brass in our case).
Then to carry out its sectioning, use hand held saw. Clamp the brass rod in bench vice jaws and
cut the suitable length of circular cross section brass almost 2.5cm.
After sectioning, take the specimen i.e the sample which is to be observed and cool it in
atmosphere. The specimen will be very hot after sawing due to friction.
After cooling, the next step is to do grinding to make the cross section (anyone of the two)
smooth, free from imperfections and free from all traces of disturbed metal.
For coarse grinding, use Silicon Carbide (SiC) paper or simply sand paper of grit 180. The
technique is to make a water film or 1-2mm thickness on sand paper and slide the cross section of
specimen on this water film to and fro for about 7 minutes.
After coarse grinding, there comes the step of medium grinding, for medium grinding use silicon
carbide paper of grit 400 and do the same process as for coarse grinding.
After medium grinding, there comes the step of fine grinding, for this purpose repeat the same
process as used for coarse and fine grinding but with silicon carbide paper of grit 1000.
After successive grinding steps, there is a need of polishing step to improve its appearance.
Polishing also improves the visibility of microstructure of specimen under microscope.
To carry out polishing, a buffing wheel is used on which a diamond abrasive is pasted and buffing
wheel is rotated at about 200-300 rpm and specimen is held against the wheel while it is rotating.
The polishing is stopped when you see the glossy appearance on cross sectional side of brass
specimen.
After that, etching of specimen is done to reveal the microstructure and phases present in the
specimen. The reagent used for etching of brass is (HNO 3 + H2O) in 1:1 proportion. Hold the
specimen in tongs dip the cross section to be examined in said reagent for about 8-10 seconds and
after that dip it in the water to avoid any damage to the specimen.
After etching , the specimen is then observed under metallurgical microscope and photograph of
revealed structure is taken.
Snaps of specimen after different steps are shown at the end of the report.
Precautions:
After sawing hold the specimen in glove to avoid any damage to skin because of high heat
generated during sawing.
While shifting from coarse to medium and medium to fine grinding, wash the specimen
thoroughly with water to avoid abrasive particles to accumulate on the specimen.
Extra care should be taken while polishing because if the quantity of diamond abrasive is more
than adequate, blackish layer will start to appear on the edges on specimen.
Etching is done for very small time just for about 8-10 seconds otherwise etchant will damage the
specimen.
 After Sectioning. After Coarse Grinding.

After Fine Grinding. After Polishing.

After Etching.
References:
Metals Handbook - Ninth Edition (Volume 9 - Metallography and Microstructures).

http://imechanica.org/files/handout9.pdf
http://www.metallographic.com/Technical/Basics.pdf