Experiment 1: MICROSTRUCTURE OBSERVATION

1.0 Objectives

a. To develop skills on grinding, polishing, and etching samples (ceramic and

polymer) and observe samples microstructures using optical metallurgy
microscope.
b. To understand basic principle of optical microscope and its utilities.
c. To develop skills using Inverted Trinocular Microscope (VBT-2T).

2.0 Introduction

Materials microstructure consists of grain, grain boundaries, sediment, porosity,

impurities, and infinitesimal solution phase that can only be viewed using metallurgy
microscope. Microstructure analysis is structure characterization research of
materials which correlate with mechanical properties and material physics.
Microstructure is a characteristic that can be observes using optical metallurgy
microscope after the precise sample preparation had taken place. Microstructure
failures such voids and cleavage could be observed after the polishing process.
However, for materials such metals and alloys, microstructures such as grain
boundaries, alloy phases and surface layers can be seen after the etching process.
Microstructure’s observation techniques are useful and can be applied in:

-Industrial; in metallurgy, alloy, and ceramic quality assurance.

-Advance materials research laboratory; in searching for new materials.

2.1 Sample holder

Sample holder is made in order to hold the sample while doing other processes such
as grinding and polishing. There are two ways of preparing the sample holder:

-Cold method the mixture of epoxy and hardener is. poured into a mold that contains
the sample until the mixture become hard.

-Heat method sample is position in a hot - compressor mold and being poured with
fenolic substance. Then it is heated to certain temperature and compressed. Finally,
the sample will stick to the pallet caused by compression given.
2.2 Sample cutting

High-speed diamond cutter machine is used for cutting the sample surface. In cutting
process, sample's surface must be assured is free from any big scar. While cutting,
the sample must be kept in moderate temperature using. cooling liquid to:

-Prevent deformation as the temperature arises while cutting

-Remove impurities at surface while cutting

2.3 Grinding and Polishing

2.3.1 Grinding

This process is done in order remove the to deformation and being used together
with water to control the temperature of samples besides removing the balance of
impurities. The grinding process is normally started with rough grinding using silicon
carbide paper, size 80 or 120 mesh, which means that the roughness of the paper is
about 500-10 micron. Then, it is followed by soft grinding using silicon carbide paper
of 240, 320, 400 and 600 that give the surface's roughness of 10-0.1 micron.

2.3.2 Polishing

After grinding, the sample is being washed and dried. Then, the sample needs to be
polished using polishing machine to remove the deformation effect of grinding.
Polishing machine contains soft fabric (silk, nylon, and cotton). A diamond polisher
material must be put onto the polisher board and the normal size of diamond
polisher’s grains used are 6, 3, 1 micron.

2.4 Etching

Etching is done to get the surface structure of the sample. Normally, there are two
ways of etching:

-Chemical etching - etching process that use chemical liquid with the sample.

-Thermal etching etching process which heating up sample to a certain temperature.

2.5 Metallurgy microscope

This microscope is using optical light reflection that contains:

-Torching system.

-Objective system.

-Eye lenses microscope system.

3.0 Instrumentation

-Diamond cutter machine

-Hand grinder machine.

-Polishing machine Silicone carbide paper (600, 800 and 1200 mesh)

-Diamond polisher (6 and 1 micron)

-Metallurgy microscope

-Sample (metal, alloy, and ceramic)

4.0 Experimental procedure

4.1 Sample holder preparation

a) Released agent being swept to the Inner surface of mould and left dried.

b) Placed sample into the mould.

4.2 Sample cutting

a) Dry samples were being sliced using machine with diamond blades.

b) Coolants liquids used in the cutting machine in under to prevent the deformation
caused by the temperature, which increased while cutting process held.

c) Samples that have been cut are washed with distilled water and left dried.
d) The surface structures of samples after the cutting process were analyzed using
the metallurgy microscope.

4.3 Grinding and polishing

a) Grinding process has been done using silicon carbide paper in order to remove
the cutting deformation marks.

b) The grinding process started using low mesh value of silicone carbide paper
(rough grinding) around 80 to 120 mesh and followed with fine grinding using silicon
carbide paper (240, 320, 400 and 600 mesh). While grinding, a little amount of water
was used in order to lower the temperature and to flow off grinding leftover.

c) The samples were rubbed onto the silicon carbide in vertical direction with
rotations about 45° to 90° for about 2 minutes, as to get flat surface of samples.

d) Samples washed using distilled water and acetone after the grinding process and
left dried.

e) Polishing process has been done using polishing machine in order to vanish the
deformation marks occur during grinding processes.

f) Diamond polisher with size of 6 micron was sprayed onto the polishing cloth (silk,
nylon, and wools) on the polishing plate and let it rotate for a while.

g) Samples placed onto polishing plate while push it firmly in the anti-clockwise
direction. These steps have to be done for about 2 minutes.

h) Steps g) repeated using diamond polisher with size of 1 micron.

i) Samples washed using acetone and left dried.

j) The samples analyzed using metallurgy microscope after polishing processes.

This has been done with cautious as to get the accurate surface image of the
samples.
4.4 Etching

a) Etching process depends on type of samples used.

i. Ceramic

Thermal etching was performed to ceramics samples at temperature less than 100°C
(from samples sintering temperature) for about 1 hour.

ii. Metal or alloy

Chemical etching was performed. The samples were dipped into 2% nitric acid
solution for about 2-3 seconds. Nitric acid is an etching reagent. Then the samples
rinsed using distilled water and acetone and left dried.

iii. Sample's microstructure was observed after etching.

iv If the microstructure observation is not clear, the etching process need to be

repeated.

5.0 Result

Microscope observation under X10 magnification

Microscope observation under X20 magnification

Microscope observation under X50 magnification

Microscope observation under X100 magnification

6.0 Discussion

In this experiment, we mixed epoxy and hardener to make a sample holder to hold
the sample. The mixture need to be done carefully to make sure no bubble come out
and need to hold the mold carefully because the reaction produce heat made the
mold really hot. The sample was observed under microscope after etching with
different magnification. The roughness of the sample can be seen clearly under the
microscope. As the magnification increased, we can see the texture of the surface
clearer.

7.0 Conclusion

In conclusion, we manage to develop skills on grinding, polishing, and etching

samples (ceramic and polymer) and observe samples microstructures using optical
metallurgy microscope. Furthermore, we also manage to understand basic principle
of optical microscope and its utilities. Finally, we manage to develop skills using
Inverted Trinocular Microscope (VBT-2T).

8.0 References

-https://thefutureofthings.com/15208-who-invented-the-metallurgical-microscope/

-https://www.azom.com/article.aspx?ArticleID=3504