Experiment 2

Sample Preparation methods for Metallography

In the study of metallic materials it is often to analyze the phases exist and grain size in the
structure. Details of the structure of metals are not readily visible through naked eyes, but
grain structures in metals may be seen with the aid of the microscope. Metals characteristics
such as grains sizes, effect of heat treatment and carbon content of steels may be determined.
The metals used for metallurgical examination must be prepared and polished carefully
before a good micrograph can be observed under microscope.

The main steps of specimen preparation for light microscopy include the following:

• sectioning;
• mounting;
• grinding;
• polishing; and
• etching.

Sectioning:

Sectioning serves two purposes: generating a cross section of the specimen to be examined;
and reducing the size of a specimen to be placed on a stage of a light microscope, or reducing
the size of a specimen to be embedded in mounting media for further preparation processes.
The main methods of sectioning are abrasive cutting, electric discharge machining, and
microtomy that is mainly for polymer specimens.

Cutting
Abrasive cutting is the most commonly used method for sectioning materials. Specimens are
sectioned by a thin rotating disc in which abrasive particles are supported by suitable media.
The abrasive cutoff machine is commonly used for sectioning a large sample. The machine
sections the sample with a rapidly rotating wheel made of an abrasive material, such as
silicon carbide, and bonding materials such as resin and rubber. The wheels are consumed in
the sectioning process. Abrasive cutting requires cooling media in order to reduce friction
heat. Friction heat can damage specimens and generate artifacts in the microstructure.
Commonly used cooling media consist of water-soluble oil and rust-inhibiting chemicals. The
abrasive cutoff machine can section large specimens quickly but with poor precision.

More precise cutting can be achieved by a diamond saw or electric discharge machine
(EDM). The diamond saw is a precision abrasive cutting machine. It sections specimens with
a cutting wheel made of tiny diamond particles bonded to a metallic substrate. A cooling
medium is also necessary for diamond saw cutting. Electrically conductive materials can be
sectioned by an EDM. Cutting is accomplished by an electric discharge between an electrode
and the specimen submerged in a dielectric fluid. EDM is particularly useful for materials
that are difficult to section by abrasive cutting. EDM may produce significant changes at the
machined surface because the electric discharge melts the solid in the cutting path. The
solidified material along a machining path must be carefully removed during further
preparation processes.
Microtomy
Microtomy refers to sectioning materials with a knife. It is a common technique in biological
specimen preparation. It is also used to prepare soft materials such as polymers and soft
metals. Tool steel, tungsten carbide, glass, and diamond are used as knife materials. A similar
technique, ultramicrotomy, is widely used for the preparation of biological and polymer
specimens in transmission electron microscopy.

Mounting
Mounting refers to embedding specimens in mounting materials (commonly thermosetting
polymers) to give them a regular shape for further processing. Mounting is not necessary for
bulky specimens, but it is required for specimens that are too small or oddly shaped to be
handled or when the edge of a specimen needs to be examined in transverse section. There
are two main types of mounting techniques: hot mounting and cold mounting. There are two
main types of mounting techniques: hot mounting and cold mounting.

Hot mounting
A specimen is placed in the cylinder of a press and embedded in polymeric powder. The
surface to be examined faces the bottom of the cylinder. Then, the specimen and powder are
heated at about 150 ◦C under constant pressure for tens of minutes. Heat and pressure enable
the powder to bond with the specimen to form a cylinder.
Phenolic (bakelite) is the most widely used polymeric powder for hot mounting. Hot
mounting is suitable for most metal specimens. However, if the microstructure of the material
changes at the mounting temperature, cold mounting should be used.

Cold mounting
a polymer resin, commonly epoxy, is used to cast a mold with the specimen at ambient
temperature. A cold mounting medium has two constituents: a fluid resin and a powder
hardener.The resin and hardener should be carefully mixed in proportion following the
instructions provided. Curing times for mounting materials vary from tens of minutes to
several hours, depending on the resin type.

(a) (b)

(c)

Figure 1 Cold mounted specimens: (a) mounted with polyester; (b) mounted with acrylic;
and (c) mounted with acrylic and mineral fillers.

Grinding and Polishing

Grinding refers to flattening the surface to be examined and removing any damage caused by
sectioning. The specimen surface to be examined is abraded using a graded sequence of
abrasives, starting with a coarse grit. Commonly, abrasives (such as silicon carbide) are
bonded to abrasive paper. Abrasive paper is graded according to particle size of abrasives
such as 120-, 240-, 320-, 400-, and 600-grit paper. The starting grit size depends on the
surface roughness and depth of damage from sectioning. Usually, the starting grade is 240 or
320 grit after sectioning with a diamond saw or EDM. Both hand grinding and machine
grinding are commonly
used.
Grinding
First, specimens are rinsed with running water to remove surface debris before switching
grinding belts; and secondly, specimens are rotated 90◦ from the previous orientation.
Rotation ensures that grinding damage generated by a coarse grit is completely removed by a
subsequent f iner grit. Thus, at the end of any grinding step, the only grinding damage present
must be from that grinding step. Damage from the final grinding step is removed by
polishing.

Polishing
Polishing is the last step in producing a flat, scratch-free surface. After being ground to a 600-
grit finish, the specimen should be further polished to remove all visible scratches from
grinding. Polishing generates a mirror-like finish on the specimen.

Fig 2. Sample of specimen surfaces after grinding and polishing with abrasives of different grits and
size.

Etching
Chemical etching is a method to generate contrast between microstructural features in
specimen surfaces. Etching is a controlled corrosion process by electrolytic action between
surface areas with differences in electrochemical potential. During etching, chemicals
(etchants) selectively dissolve certain areas of the specimen surface because such areas
exhibit different electrochemical potentials and will serve as the anode in an electrochemical
reaction on the specimen surface. For example, grain boundaries in polycrystalline materials
are more severely attacked by etchant, and thus are revealed by light microscopy because
they reflect light differently, and appear as the dark lines. Also, grains are etched at different
rates because of differences in grain orientation (certain crystallographic planes are more
subject to etching), resulting in crystal faceting. Thus, the grains show different brightness.
Etching a specimen that has a multiphase microstructure will result in selective dissolution of
the phases. Etching can simply be performed by immersion or swabbing. For immersion
etching, the specimen is immersed in a suitable etchant solution for several seconds to several
minutes, and then rinsed with running water. The specimen should be gently agitated to
eliminate adherent air bubbles during immersion. For swab etching, the polished surface of a
specimen is wiped with a soft cotton swab saturated with etchant. Reagents used for Fe and
steels are Nital, 1–10 ml HNO3 in 90–99ml methanol Picral. The specimens under
examination are dried after etching is completed.