Lab I - Metallography-Revised
Lab I - Metallography-Revised
Lab I - Metallography-Revised
ADVANCED PROGRAM
Materials Science and Engineering
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Hanoi, 2023
MSE: 3317
(Materials Science and Engineering Laboratory-I)
I. Introduction
The objectives of this laboratory are to introduce the basic steps of
metallographic sample preparation, photography (using metallurgical) and
microstructural analysis. In this experiment, the student will learn the most
common form of metallography by imaging the microstructure of metal alloys
using optical microscopy.
Metallography is used to produce images of the materials. (Even though the
word “metallography” begin with “metal”, the method is applicable in a number
of different areas of materials science and engineering.) Sample preparation is
the first and often the most critical step in metallography. Specimen surfaces
must be prepared to reveal the microstructure without introducing undesired
artifacts.
A major use of metallography is in quality control of materials processing.
Materials processing steps are often designed to produce a specific
microstructure –e.g. smaller grains tend to increase hardness while large grain
provide enhanced ductility. Metallography is used to characterize the
microstructure and therefore, provide the feedback needed for optimizing
processing conditions. Metallography is also an important tool in characterizing
manufacturing defects and in failure analysis.
II. Experimental Procedure
A. Sample preparation
Sample preparation can be the most critical part of the whole procedure. It
will determine the quality of sample you will have to examine and analyze.
Although sample preparation tends to be an art rather than a strict science, there
are a few commonalties which will make the preparation process simple: 1) do
not rush through the procedure - there is adequate time for everyone to
complete the experiment and those with the best samples are usually those who
take their time, 2) do not skip any of the grinding or polishing steps – each step
must be completed in order to remove the deformation and defects left by the
previous coarser grit, 3) rinse your samples thoroughly before moving to the
next grinding or polishing step, and 4) feel free to ask your TA for advice help.
1. Equipment
Grinding and polishing machines
Etching solution for steels and cast irons
Metallurgical microscopes
2. Demonstration
i) Sectioning
Sectioning is the removal of a representative sample, with the desired
orientation, from a parent piece. A low speed abrasive saw is typically
used for this operation to avoid unintentional heat treatment of the sample.
But in this lab, a high-speed cut-off saw is used to section the sample as
the heat generated during sectioning will not alter the features that will be
observed in the sample.
ii) Mounting
Samples are typically mounted in epoxy to facilitate handling during
subsequent preparation steps. In this lab, we will use fast cure acrylic
mounting compound.
iii) Grinding
Grinding with abrasive powders removes the severe surface damage
produced by sectioning. The sample surface is ground with a series of
progressively finer grits. We will begin with rough grinding using 120 grit
paper to remove excessive acrylic from the sample surface, followed by
grinding the surface with 240, 800 and 1200 grit papers in succession. The
surface should be inspected frequently to evaluate the progress. Even and
randomly oriented scratches on the sample surface indicate the
completion to a grinding step.
iv) Polishing
Polishing produces a flat and scratch free surface. Samples are
polished using a suspension of fine abrasive particles (5 m and less in
diameter) applied to a polishing cloth. In this lab, we will use 0.3 m
abrasive particle suspensions to obtain the desired polish. A well-polished
sample will display a flat, smooth and mirror-like surface.
Note: Samples should be thoroughly cleaned with water after each grinding
or polishing step to prevent coarse abrasive particles from contaminating the
subsequent finer grinding or polishing stage.
v) Etching
Examination of a polished specimen before etching may reveal gross features
such as porosity, cracks, and nonmetallic inclusions. Chemical or
electrochemical etching, however, is often required to reveal the desired contrast
in subtler aspects of the microstructure. Etching causes most metals to lose their
bright, mirror – like appearance. Following etching, the specimen is rinsed in
running water, then in isopropyl alcohol. And finally dried in a stream of warm
air.
3. Preparation of steel specimen
Each student will prepare a steel specimen for metallographic examination.
a) Using a grinding machine to grind the specimen surfaces in 5 steps
using wet SiC papers (120, 240, 400, 800 and 1200 grit).
b) Then polish the surfaces on cloth wheels using 0.3 m Al2O3
suspensions (H2O based). In succession.
c) Thoroughly clean the sample surfaces with running water following by
rinsing with ethanol and dry.
d) Swab the polished surfaces with a freshly made etchant solution (nital
solution 4%HNO3 in Ethanol): rinse in water and alcohol, and dry.
Note: Etching, typically takes a second or two. Over – etching can burn
the sample surface.
B. Optical Microscopy and Photography
Metallurgical microscopes use reflected light. The classroom instructor will
explain the operation of an optical microscope. Fig. 1 illustrates the image
formation in a metallurgical microscope with the aid of a schematic ray diagram.
Fig.2 shows a photo of the Zeiss inverted metallurgical microspore (Model
Axiovert 25CA).
1. Equipment:
Metallurgical microscopes with CCD cameras, video monitor and a
printer.
Polished and etched steel samples
Polished and etched cast iron samples.
Fig. 1. Image formation in a metallurgical microscope using bright-field illumination
Fig 2. Photo of the Zeiss inverted metallurgical microscope (Model Axiovert 25CA)
2. Microstructural Examination of Steel Samples
Each student will examine and sketch the microstructures of all the steel
and iron samples given. Correlate the microstructures with the composition of
the samples with the aid of the Fe-C binary phase diagram (Fig.3).
IV. References:
1. ASM Metals Handbook, 9th Ed., Vol.9 , Metallography and
Microstructures, American Society of Metals, Metals Park , Ohio. 1985.
2. ASM Metals Handbook, 9th Ed., Vol .10, Materials
Characterization, American Society of Metals, Metals Park, Ohio, 1985.
3. ASM Metals Handbook, 10th Ed., Vol. 2, Alloy Phase Diagrams,
ASM International, Metals Park, Ohio, 1994.
4. W.D. Callister, 5th Ed.; Fundamental of materials science and
engineering; John Wiley & Son Inc.; 2000.
Fe-0.2%C (Mag. 100) Fe-0.2%C (Mag. 200) Fe-0.2%C (Mag. 500)