Experiment 3

Experiment 3 – Metallographic Observations
1. 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.
2. Procedures
Metallography is essentially the study of the structural characteristics or constitution of a metal or an
alloy in relation to its physical and mechanical properties. The most important part of metallography
deals with the microscopic examination of a prepared metal specimen. The metallographic microscope
is described in Appendix D, which should be read carefully at this point. Correct preparation begins with
the selection of a suitable specimen and continues to the etching stage where the structure of the
specimen is revealed. The microscopic examination then defines clearly such structural characteristics
as grain size, the size, shape and distribution of secondary phases and non-metallic inclusions; and
segregation and other heterogeneous conditions.

These characteristics profoundly influence the mechanical properties and physical behavior of the metal.
Metallographic examination can provide quantitative information about specimen grain sizes, amount of
interfacial area per unit volume, and the amount and distribution of phases. When these and other
constitutional features are determined by microscopic examination and the extent to which they exist in
the microstructure is known, it is then possible to predict with considerable accuracy the expected
behavior of the metal when used for a specific purpose. Of equal importance is the fact that, within
limits, the microstructure can provide an accurate picture of the mechanical and thermal treatments
that a metal has received.
3. Preparation of Specimens
The technique for preparing metal sections can be divided into two groups, those processes involving
the use of emery papers and coarse abrasives (grinding) and the subsequent operations using fine
abrasives (polishing treatments). Grinding must be carried out carefully in such a way that all
microscopic constituents in the surface are preserved and that the grinding medium is not embedded in
the sample. To achieve this, the specimen is ground on successively finer grades of emery (sand) paper.
During grinding, the specimen is held with the newly formed scratches at right angles to the scratches
introduced on the preceding paper. Undue pressure should be avoided since the disturbed layer this
produces on the surface can extend to considerable depth. For some heat treated alloys and in
particular for many of the soft metals, it is an advantage to use paper thoroughly wetted. Grinding also
removes surface deformations. After grinding, the specimen is washed thoroughly in water and then
polished. Mechanical polishing can best be carried out by holding the specimen against a rotating disc
covered with a suitable pad that is impregnated with either a suspension of polishing alumina in water
or diamond dust oil.
4. Mounting of Specimens
It is frequently convenient to mount small specimens in bakelite or acrylic to aid specimen preparation,
grinding, polishing and etching. You will be given instructions on the use of the apparatus for mounting
specimens. The basic idea is that bakelite powder is thermosetting. Therefore the specimen is placed in
a tube 2/3 filled with powder. The tube is heated while the powder is compressed. The pressure and
heat are removed when the powder has completely melted and the bakelite has set. To maintain
orientation small shot are sometimes placed next to the specimen in some identifying arrangement.
5. Grinding and Polishing Procedure
The following instructions indicate the general method to be used in specimen preparation. The edges
of cylindrical metal specimens must first be beveled off to avoid damaging the polishing cloths. For Mg
and Al and their alloys, use the aluminum polishing wheels.
6. Etching
Etching is done to bring out the structure of the polished specimen. It is usually performed by subjecting
the polished surface to the chemical action of an appropriate reagent. However, the polished specimen
should first be examined unetched. Inclusions, flaws, scratches and

other defects can be observed in this way, and if they are identified before etching, subsequent
confusion and misinterpretation can be largely avoided. The specimen to be etched is treated by
immersion in, or by swabbing with, the appropriate reagent. It is impossible to lay down general rules
for the time of etching. Usually the desired effect will be produced between ten seconds and two
minutes. The specimen after etching should be washed in a stream of running water. The surface
should be dried untouched by holding in air current. When selecting etching times, it is more desirable
to under-etch than to over-etch. If a specimen, after a first attempt is found to be insufficiently etched,
the etching process can usually be repeated without further preparation of the surface. A specimen that
is over-etched can only be corrected by repolishing and then reetching for a shorter time.
7. The Metallurgical Microscope
Having already described in some detail the methods by which a metallographic specimen is best
prepared and subsequently etched for microscopic examination, it is now appropriate to discuss the
principles of the metallurgical microscope. A metallurgical microscope differs from a biological
microscope in the manner by which the specimen is illuminated. Because of the inability of visible
radiation to propagate through a metal specimen, observations are made using light reflected from the
polished surface. A horizontal beam of light is deflected by a plane glass reflector, upward and through a
microscope objective onto the surface of the specimen. A certain amount of incident light will be
reflected from the specimen surface back through the objective lens system and then through a second
lens system, the microscope eyepiece.
8. Photomicrographic Techniques
Materials engineers frequently need to photograph the metallographic work. The image desired is
projected into the binocular lens. Once proper focus is obtained, the computer software (Buehler
Omnimet Imaging system) is used to further analyze the microstructure.

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Experiment 3 – Metallographic Observations

Metallography is essentially the study of the structural characteristics or constitution of a metal or an

segregation and other heterogeneous conditions.

that a metal has received.

or diamond dust oil.

5. Grinding and Polishing Procedure

and Al and their alloys, use the aluminum polishing wheels.

should first be examined unetched. Inclusions, flaws, scratches and

7. The Metallurgical Microscope

principles of the metallurgical microscope. A metallurgical microscope differs from a biological

lens system, the microscope eyepiece.

Omnimet Imaging system) is used to further analyze the microstructure.

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