Experiment 2

Showing the Structure of Metallic Materials by Microscopical Examination.

Structural constitution can be made visible by microscopical examination. Microscopical

examination of metallic materials calls for prior treatment of the specimens by which the structure
becomes visible.

The structural constitution permits a conclusion to be drawn as to the properties and

possible use of the materials such examination is also used for production control purposes.

This experiment shall serve to give an insight into the structure of the metallic materials by
microscopical examination and the metallic materials by microscopical examination and to
compare different alloys as well as to get to know the structure prior to and after the treatment.

Materials and Equipment.

a) A reflected light microscope type `Olympus’ with 10 to 100 times magnification.

b) A wet grinding equipment type `Pace Technologies’ round SiC abrasive paper with 8 and
10-inch diameter waterproof and grain sizes:

Standard Grit Nomial Micron Size

240 : 58.5 𝜇𝑚
320 : 40.5 𝜇𝑚
400 : 21.8 𝜇𝑚
600 : 15.3 𝜇𝑚

c) Polishing equipment type `Pace Technologies’, diamond polishing abrasives –

polycrystalline diamond suspensions.

d) A graduated cylinder 300 ml.

e) Steel specimens of unhardened, harden and annealed (size of the specimen approx 25 mm
diameter and 20 mm long).

f) A hair drier.
 1. Etchants.
- 3 ml concentrated nitric acid
- 97 ml ethyl alcohol
- Cleaning Rag
- 300 ml ethyl alcohol, cotton wool, instruction manual for necessary equipment.
- 500 ml distilled water.

Note :

For this experiment, three types of specimen are required (hardened, unhardened, and
annealed). The specimen must have a smooth surface. To carry out the experiment the
specimens must be ground and polished first.

Method/Procedure:

a) Study the instruction manual for the wet grinding equipment.

b) Put on the abrasive papers for the 1st. and 2nd. grinding pass.

The specified round abrasive papers and used in the following sequences:

1st. grinding pass : grain size 240 = 58.5 𝜇𝑚

2nd. grinding pass : grain size 320 = 40.5 𝜇𝑚
3rd. grinding pass : grain size 400 = 21.8 𝜇𝑚
4th. grinding pass : grain size 600 = 15.3 𝜇𝑚

c) Turn on the water feed.

d) Put the specimen into the operation.

e) Take a specimen and put it carefully (gripping it firmly with the fingers) with slight
pressure onto the rotating abrasive paper for the 1st. grinding pass (see Figure 1).

Note :

Make sure that the specimen is not forced out of your hand. Continue grinding until the
grinding marks, which were visible before, cannot be seen any longer.
 Figure 1

f) Turn the ground face of the specimen by 90° after the 1st. grinding marks have been
ground off and grind on the abrasive paper for the 2nd. Pass until the grinding marks of
the 1st. grinding pass has vanished.

g) Switch off the wet grinding equipment and turn off the water feed.

h) Remove the abrasive paper.

i) Put on the abrasive paper for the 3rd. and 4th. grinding pass.

j) Continue grinding up to 4th. grinding pass following the same procedure as for the 1st.
and 2nd. pass.

k) Remove the grinding residues from the specimen by rinsing it with running water.

l) Put the specimen under the hot hair drier for drying.

m) Grind the other two specimens in the same manner.

2. Polishing of the Specimen.

a) Study the instruction manual for the polishing equipment.

b) Put on the polishing cloth on the disc of the machine.

 c) Prepare the machine for the operation and apply several beads of diamonds and/or for
initial pad wetting on the polishing cloth. Drip onto the surface at a rate of 1-2 drops
every 10-15 seconds depending upon the polishing speed and surface area of the
samples.

d) When polishing the specimen, hold it with both hands, apply a moderate amount of
pressure, and don't let it go. (The rough polishing stages should take between 1 and 2
minutes each).

e) Before proceeding to the next polishing stage, wash and dry the specimen and hands
thoroughly then rinse the specimen.

f) Repeat steps c and d for the 1-micron stage (final polishing stage).

g) Before proceeding to Etching, wash and dry the specimen and hands thoroughly then
rinse the specimen with distilled water. Do not touch the specimen surface.

3. Etching of the Polished Specimen Surface.

a) Pour the etchant into the plastic bowl (approx. 5 mm high level of etchant).

b) Rub the hardened and unhardened specimens with an alcohol-soaked wad of the
cotton wool.

c) Put the specimen with the ground face into the etchant.

d) After a few seconds of etchant look at the surface of the specimen and, if it is not
shining anymore but matt, stop the etchant process by running water. Then flush away
the water by ethyl alcohol and dry the specimen under a hot air drier.

Note :

The etchant has caused changes on the polished surface affecting the unhardened
specimen in the form of contrast etching or etchant bringing out grain boundaries relief.

1- Contrast etching
2- Grain-boundary
3- Light incidence
 4. Carrying Out of the Microscopical Examination of the Structure.

The microscopical examination starts with the lowest magnification. For illumination,
incident light bright-field illumination is applied.

a) Study the instruction manual of the light microscope.

b) Turn the eyepiece up to the stop by means of the knurled screws of the microscope.

c) Put the unhardened specimen on the center of the table of the microscope with the
etched face showing to the objective.

d) Look at the specimen from the side and turn the eyepiece by means of the knurled
screws of the microscope towards the specimen until the distance between the
objective and specimen is approximately 2 mm.

e) Prepare the microscope for the incident-light bright-field illumination.

f) Switch on the illumination device of the microscope, look at the metal surface of the
specimen and slowly turning the eyepiece upwards by means of the knurled screws of
the microscope until a clear image of the specimen surface can be seen in the eyepiece.

g) Try to thoroughly examine the structure of the unhardened specimen and to find out
special features.

h) Sketch the structure and note down all data of the microscope. If the equipment is
complete, a microphoto of the structure may also be taken.

i) Repeat the whole procedure with the hardened specimen and then with the annealed
specimen.

j) Compare the structure pattern of the three types of the specimen.

Evaluation.

a) State the difference in the structure of :

- Unhardened steel
- Hardened steel
- Annealed steel
 What is your conclusion from that relating to practice

b) Describe and sketch the differences in the structure of the specimens.

c) What effects can the different structure have on the properties of the materials?

d) The student should record in a `table’ under the following headlines:

- Specimen’s Number/Group
- Magnification (X)
- Structural Constituents
- Comments.