Materials Engineering (ME 252)

Dr. Hany Ammar

Metallography: Specimen Preparation
for Microstructure Analysis
Metallography is the science and art of preparing a
metal surface for analysis by
Sectioning
Grinding
Polishing, and
Etching
to show microstructual features and constituents.
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.
Grain Boundaries

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
alloy strength is usually increases as the average
grain size decreases.

Grain size 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
Microstructure Analysis

Studying microstructure characteristics of

materials.

Studying structure-properties relationship.

Evaluate the effect of processing parameters

on microstructure/properties.
Sample Preparation

Sectioning is the first step in the overall process of specimen

preparation. Sectioning must be careful not to significantly
alter the microstructure during sectioning.

Sawing is perhaps the oldest method of sectioning that is still

used today. It can be accomplished with a hand-held hacksaw,
but it can alter the microstructure.

Abrasive Wheel Sectioning is the most popular method of

sectioning. Wheels made of silicon carbide, aluminum oxide,
and diamonds are used in the sectioning process. With this
type of sectioning, the metallographer has more control over
the conditions used for cutting the samples.

Wire Saws produces minimal damage, 3 modes – abrasive,

electrolytic, and chemical etching.
Sample Preparation

Precision Cutting Machine

Sample Preparation

Mounting
Typically used for small or irregularly shaped samples
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.
Cold mounting can be done using two components resins
and hardener. It takes few hours to complete.
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.
Sample Preparation

Mounting Machine
Sample Preparation

Grinding
It removes damage introduced by sectioning

Grinding occurs in sequences of finer and finer abrasives

Typical grit sequence: 120, 240, 320, 400, 600, 1200 mesh.

Subsequent finer abrasives might also be employed.

Wet grinding is typically used: better to minimize heat generated,

minimizes metal entrapment between particles.

Steps of grinding

1. Grinding sequence – 120, 240, 320, 400, 600 grit SiC rotating 45 or 90
degrees between steps (center to edge)

2. Rotate sample counter to the wheel rotation. Always use light pressure
applied at the center of the sample. 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.

3.Wash after each step under running water and rinse with alcohol
Sample Preparation

Grinding papers
Sample Preparation

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 µm).
Or diamond past with diamond particles ranged from 1-6 µm.
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.
Sample Preparation

Polishing Clothes
Sample Preparation
Etching
Process used to reveal the microstructure of a metal or alloy.
Because many microstructural details are not observable on an as-polished
specimen, the specimen surface must be treated to reveal such structural
features as grains, grain boundaries, twins, slip lines, and phase boundaries.
Etchants attack at different rates areas of different crystal orientation,
crystalline imperfections, or different composition.
The resulting surface irregularities differentially reflect the incident light,
producing contrast, coloration, etc.
Etchant 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 the figure in next slide.
Etching should always be done in stages, beginning with light attack, an
examination in the microscope and further etching only if required.
If you overetch a sample on the first step then the polishing procedure will
have to be repeated.
After each etching, the specimen should be thoroughly washed in running
water, followed by drying off with acetone or alcohol.
Sample Preparation
Etching
Sample Preparation

Etching
The table below gives the etchants for some alloys

Sample Etchant

Al alloys Keller’s (2 ml HF +3 ml HCL + 5 ml NO3+ 190 ml water)

Cu-Zn alloy 10 ml HNO3+90 ml water

(brass)

Steel and cast Nital (2% HNO3 + 98% ethanol)

irons
Start Lab Work

Experiment # 1
Questions