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Metallographic study of stainless steel

V. Duque. S. Suarez. J. Villalobos. S. Barbosa. J. Pérez.
Universidad de la Sabana

Abstract III. HYPOTHESIS

The main objective of this practice was to identify the microscopic
changes in a sample of stainless steel; the process followed was The microscopic photography of stainless steel will show a
polishing until obtaining the mirror effect in the material; etching transformation after each of the different phases.
aiming to eliminate impurities in the sample and lastly annealing
and cooling. In conclusion etching with nitric acid as etchant
caused corrosion and cooling the sample with water resulted better IV. METHOD
since the structures became visually sharper.
In order to prepare the sample of stainless-steel the following
methodology was used:
I. INTRODUCTION
Metallography is the study of materials microstructures, PHASE I. POLISHING
specifically of metals. Metallography techniques are also
This procedure consists in preparing the sample in order to
commonly applied to prepare ceramics and polymers;
identify the characteristics and structure, before it undergoes
however, these processes receive different names,
chemical and temperature changes.
ceramography and plastography respectively. There are
multiple techniques in metallography such as sectioning and
cutting, tempering, mounting, grinding, polishing, etching, DIAGRAM I. POLISHING
annealing and many others. For this experiment stainless steel
was selected and only three different metallography techniques Cleaning the sample of stainless-steel with a
were used. Phase I: polishing, Phase II: etching and lastly tissue in order to get rid of any external particle.
Phase III: annealing.

The polishing technique consist on using a rotating disc for

smoothing the metal surface. In this procedure the metal 2.Start of the polishing process. Exchange the
sample is moved in a clockwise direction to ensure an even sandpapers of different references into the
removal from the whole surface, this is why it is of major rotating disc.
importance to avoid prolonged polishing in only one direction.
The etching technique has a main requirement which is that
3. Polish the sample, until a shining and smooth
the sample must be conductive. Etchants meaning the
surface is obtained, lastly add aluminum oxide to
substance used for the etching process are usually acids, water
the sample.
or alcohol. For this technique the sample is immersed in a
bowl filled with the etching reagent or the sample could be
wipe up with a piece of cotton that was previously saturated
with the etchant. After this the sample must be washed in
water or alcohol and dried to avoid corrosion. Lastly the 4. Visualize the stainless-steel sample through a
annealing technique consists in heating up the metal sample microscope and record the result with a picture.
and letting it cool down slowly in order to toughen the
material and remove internal stress.
PHASE II. ETCHING
As mentioned above the metal sample chosen for this After the polishing process the stainless-steel sample went
experiment was stainless-steel, most known for its corrosion through an etching process, in which the etchant was picric
resistance. Stainless steel is used in the heavy industry and in acid. The purpose of this phase was to highlight the structures
construction because of its properties. Also, this type of present in the sample.
material doesn't have electromagnetic interactions with other
dipoles, this characteristic is very important in manufacturing DIAGRAM II. ETCHING
since it helps in process optimization.

II. OBJECTIVE
The objective of this experiment is to observe how the
microscopic structure of stainless-steel changes after different
types of metallographic techniques are applied.
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Phase I. Polishing
Clean the polished surface of the sample with
distilled water and cotton. Both samples showed a uniform and shinning surface after
exposed to aluminum oxide.

2.Apply picric acid or nitric acid to the

polished surface, wait five minutes.

3. Add ethanol to the polished surface, dry with

a compressor.

4. Visualize sample with a microscope and

record results with a picture
Image 1. Sample A
PHASE III. ANNEALING
To finalize the preparation of stainless-steel it is necessary to
complete the heating test in order to identify the effect of
temperature in the sample.

DIAGRAM III. ANNEALING

1.Put both samples inside

of a muffle type furnance.

2.Heat the samples to a

temperature of 300°C
during 30 minutes
Image 2.
Sample B
3. Take the samples out and
let them cool, one in each of
the two different methods

Let the sample cool for 45 Cool the sample by

minutes at room introducing it in a bowl
temperature with water.

4. Observe through a 4. Observe through a Image 3. Microscopic view of the samples after polishing
microscope and record the microscope and record the
result with a picture result with a picture

V. RESULTS
Once the three phases mentioned above were completed, the
following images were recorded.

It is important to specify the measures of the two samples of

stainless steel, which were:
 Sample A: 2 inches diameter and a height of 3.2 cm
 Sample B: 2 inches diameter and a height of 3.8 cm Image 4. Microscopic view of the samples after adding
aluminum oxide

Phase II. Etching
Sample A was tested with picric acid, while the sample B was
tested with nitric acid.
Image 5. Microscopic view of sample A (etchant: picric acid)
Image 6. Microscopic view of sample B (etchant: nitric acid)
Phase III. Annealing
Sample A was cooled at room temperature for 45 minutes and
sample B was dipped into a bowl of cold water in order to
reduce the temperature of the sample.
Image 7. Microscopic view of sample A (Room temperature)
Image 8. Microscopic view of sample B (Cold water)
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VI. ANALYSIS
Our stainless-steel sample was type 18/8 meaning the 8% of
nickel provides it with a corrosive resistance. This property
makes the material ideal for the heavy industry. Taking into
account the information recorded in the previous section an
analysis was made. Four different items were identified in the
images, being them forged lines of flow, grains, machining
prints and fractures orientations.
Initially the 18/8 stainless-steel had a rigid behavior since it
took a considerably large amount of time to expose a mirror
like surface. After a microscopical analysis three different
items were identified in the views of the samples after
polishing and are highlight in image 9. The items identified
where grains, dislocation limits and structural shapes.
Image 9. Items identified in the microscopic view after
polishing
Grains are contained inside the black circle; the structure
direction is inside the red oval and lastly the marks due to the
sandpaper are pointed by the blue arrow.
Image 9. Items identified in the microscopic view after adding
aluminum oxide
In image 10 grains are inside the black circle and the red
arrow makes explicit the direction of the structure. After the
aluminum oxide was added no foreign traits from the
sandpaper were visible.
The stainless-steel type 18/8 did not showed significant
changes in its surface after applying the different types of
etchants. However, sample A did show a higher resistance

when being exposed to the picric acid. This is shown in image
10.
Image 10. No major changes in sample A after etching
However, sample B which was treated with nitric acid did had
some significant changes after the etching process. A print due
to corrosion was notably visible, the reason for this is because
of the reaction between steel and oxygen present in the acid.
This is shown in image 11 where oxidation prints are circled
in red.
Image 11. Oxidation of sample B after etching
In the annealing phase sample A was the one cooled down at
room temperature while sample B was forced to cool faster as
dipped in cold water.
In this phase the imaging showed a larger difference since the
samples were previously involved in an etching process with
different etchant agents. Also, a different cooling process was
applied to each sample producing a larger difference. Imaging
from sample B shows a sharper and better well-defined
structure. Theoretically sample B should possess a bigger
toughness and resistance in comparison to sample A. The
accelerated cooling of stainless-steel in this case sample B
produces a decrease in the size of the grains, generating a
more uniform material.
VII. CONCLUSION
Taking into account the information and images gathered
through our research we concluded the following.
 Our hypothesis was wrong not all the images showed
a transformation after each of phases. Some of them
showed minimal changes other did showed significant
transformations.
 It can be said that the cooling process using water is
more effective than the room temperature method since
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the sudden change in temperature from hot to cold tend
to creates sharper and more fine microstructures.
RECOGNITIONS
The authors thank Professor A. Amadeus for the direction
and teaching given for the realization of the metallography
project. They thank J. Rodríguez for the accompaniment in the
metallography laboratory. They also thank the Duque,
Villalobos, Perez, Barbosa and Suarez families for the
financial support for the realization of this project.
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