STAINLESS STEEL

METALLOGRAPHY
Camila Ureña, Marlon Bello, Gina Ramírez, Luisa Cárdenas, Laura Trejos, Valentina Castiblanco
Universidad de La Sabana
Chía, Cundinamarca

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I. ABSTRACT examination of specimens with a

One of the disciplines responsible for the metallurgical microscope. The structures
study of the structure of the different observed in the microscope are often
materials corresponds to the metallography. recorded photographically [1]. This method is
The present report shows the theoretical and probably the most effective diagnostic tool
used in the evaluation of metals and the
experimental collection obtained through the
products made from them. It is particularly
metallographic analysis of a stainless-steel effective in failure analysis, helping explain
rod, in order to study the microstructure of material behavior, and as a monitor for
the metal, by means of the microscope, control and improvement of products and
observing the structures that are formed after processes [2].
the treatments made. These tests to which the
stainless steel was subjected correspond to a Stainless steel is defined as a ferrous alloy
sanding and polishing, where it can be seen with a minimum of 10% chromium content.
This name comes from the fact that stainless
that it lacked more precision and more time to
steel does not strain, rust or corrode as easily
do this part, of annealing and tempering, it
as ordinary steel [3]. Furthermore, the
was not possible to achieve a homogeneous chromium content of the steel allows the
structure of the steel and in the etching could formation of a rough, adherent, invisible,
see that the piece that best resisted the attack corrosion-resisting chromium oxide film on
was the piece three. the steel surface. If damaged mechanically or
chemically, this film is self-healing,
providing that oxygen, even in very small
II. INTRODUCTION amounts, is present. The corrosion resistance
and other useful properties of the steel are
The present practice is about how the enhanced by increased chromium content and
metallography uses in the stainless steel and the addition of other elements such as
determine the behave of this one and its molybdenum, nickel and nitrogen. [4]
properties according to the phases that it will
be given along the article. The principle Finally, in order to determine the properties
material were three sticks of stainless steel and do the respect analysis, the phases of this
that were bought in a specialized store. procedure were polishing with sandpaper,
etching with HCl and the process of
Metallography is the study of the structure of annealing and tempering.
metals and of metal alloys through the
 III. THEORETICAL troostite, sorbitol, ledeburite, steadite and
FRAMEWORK graphite [5], which will be describe
briefly in the next point.
a. Metallography.
Metallography is the discipline that b. Stainless steel
microscopically studies the structural Stainless steels are iron base alloys that
characteristics of a metal or an alloy, looking contain generally 11% of chromium. Other
for microstructure, inclusions, thermal elements are added to this kind of steel
treatments to which it has been subjected, in because there are some specific demands of
order to determine if said material meets the the environment that need to be cover, these
requirements for which it has been designed; elements are: Nickel, copper, titanium and
we can also find the presence of molten, more are the commonly used elements that
forged and laminated material. We can know used to get the specific steel grade [6]. They
the distribution of phases that make up the are used for corrosion and high-temperature
alloy and non-metallic inclusions, as well as resistance applications, the first one is
the presence of segregations and other obtained by the presence of a thin and stable
irregularities. [5] Chromium oxide or Nicker oxide film that
protects the steel. It should have at least 10%
of Cr to develop the tenaciously adhering.
Stainless steels are classified into five
families, the first four are based on their
crystallographic structures; martensitic,
Fig. 1 Some examples of microstructures [5]. ferritic, austenitic, and austenitic plus ferritic
(called duplex); and the last one is based on
Within the metallography we can distinguish two the type of heat treatment, these are called
classes: precipitation-hardenable alloys, often also
 Quantitative metallography: This called PH steels.
determines the size of the grains, the  The martensitic are essentially FeCrC
percentage that contains the material, the alloy that have boy centered
shape and type of non-metallic tetragonal (bct) crystalline structure
inclusions, the shape and type of the which can be hardened by heat
graphite, in the case of cast irons and treatment and have a good resistance
other data specific to each component. to corrosion.
With these data, it is possible to identify  The ferritic are straight iron-
each component, predict the mechanical chromium allows that has body
behavior and the method with which the center cubic (bcc), this type has good
material was processed. [5] ductility and are easy to work with.
 The austenitic contain Chromium,
 Qualitative metallography: consists only nickel, carbon and other alloying
in observing the microstructure, elements. They have low temperature
determining which are the ductility, that’s why they don’t have
microconstituents that composes it. The hardened by heat treatment.
microconstituents vary according to the  The duplex contains 50% of ferritic
type of gang analyzed and according to phase and 50% of austenitic phase.
the thermal treatments, mechanical  The PH steels is defined as caused by
treatments, manufacturing processes and the precipitation of a constituent from
other processes to which the material has a supersaturated solid solution, PH
been subjected. For steels, the main alloys can achieve high strength [6].
constituents are: ferrite, cementite,
austenite, perlite, martensite, bainite, c. Sanding and
polishing.
 temperature throughout the cross-section of
In the preparation of metals to perform the the component and complete austenization.
metallographic analysis should start with the It's one of the heat treatment processes of
roughing which prepares the surface for steel and other ferrous alloys where these
polishing, eliminating the distorted layers, materials are heated above their critical
and thus obtain a flat surface, since the temperatures long enough for transformations
microscope has only a small local depth, then to take place. If an austenitized material is
it is passed to the sanding and finally to the followed by a quenching process, then this
polishing, which has the purpose of material becomes hardened. Quenching is
eliminating the scratches of the roughing and performed at a rate that is fast enough to
the zone of metal deformed by plasticity, this transform the austenite into martensite [9]
can be done using a damp cloth with a Finally, it is cool the hot steel component to
suspension of alumina in water or diamond room temperature slowly.[8]
powder in alcohols . Under normal
conditions, a thin film of oxide is present on
the surface, and if you insist on polishing,
you can deform the structure of the surface
layers. But it is not enough to get a very
specular surface properly smooth, free of
scratches; In addition, the non-metallic
inclusions must be preserved intact in order to
correctly judge the cleanliness of the metal,
and more importantly, that the polished
surface is free of any tiny amount of metal Fig 3. A typical heat treatment cycle to produce spheroidised
structure.[9]
that has flowed or altered that prevents its
true structure from being seen.[7]
The tempering is another way of heat
d. Heat treatment. treatment that follows the quenching, which
The heat treatment includes heating and is a process that consist to put the material
cooling operations or the sequence of two or into water after the whole heat process. The
more such operations applied to any material quenching is important because it eliminates
in order to modify its metallurgical structure most of the drawbacks produces by correcting
and alter its physical, mechanical and excessive hardness and brittleness of the
chemical properties. The two principal hat material and increase the ductility and the
treatment is the annealing and tempering. [8] resistance impact like the Fig 2 shows [10]-

The annealing refers to a wide group of heat

treatment processes and is performed
primarily for homogenization,
recrystallization or relief of residual stress in
typical cold worked or welded components.
Depending upon the temperature conditions
under which it is performed, annealing
eliminates chemical or physical non-
homogeneity produced of phase Fig 2. Effect of tempering in the hardness and toughness of a
transformations. In this process the first step carbon steel [10]
is heating the steel component, after is
holding the steel component at this e. Chemical Attack
temperature for a definite holding (soaking) The chemical attack is a process where the
period of at least 20 minutes per cm of the corrosion of the sample can be controlled,
thick section to assure equalization of this process can be done if the surface is
submerged in any type of suitable solution, eliminate internal tensions and change the
this chemical solution depends on the mechanical resistance. For this, two cylinders
material and its composition, the temperature were introduced in the microwave at 396 ° C
and time of the attack. In the case of stainless for thirty minutes, immediately, one of these
steel, there are few options for the chemical cylinders was submerged in water until its
solution such as Hydrochloric acid, sulfuric temperature adjusted to the environment and
Acid, Titanium tetrachloride and water [11], the other cylinder was cooled outside the
in this experiment we used Hydrochloric microwave until the temperature reached that
Acid. of the environment. Finally, the surfaces of
the two cylinders were seen in the microscope
IV. METHODOLOGY and the final structure of the steel was
observed after the accomplished procedures.
Initially the materials used were: three sticks
of stainless steels type 316, sandpapers, HCL V. RESULTS:
6.3% M, microwave, polishing
metallographic, water, microscope and In the first part, after doing the polishing with
stainless steel. 60, 300, 1000, 1200, 2000 and 2500
To begin with, were 3-cylinder type 316 sandpaper, we obtained this image of the
stainless steel (which were named from one three pieces respectively that were taken with
to three), which were subjected to a process a normal camera:
of acclimation in the polishing
metallographic. First, we used the sandpaper
type 60, which removed peaks that had steel
on its surface, material with the sandpaper,
type 300, is then polished to remove any deep
scratches in the area to study, later sandpaper
type 1000 and 1200 were used to clean the
surface in such a way that the scratches were
minimal to observe the change in the surface.
Finally, we used sandpaper type 2000 and
Fig. 4 Piece one after sanding.
2500 buffing the area to study and observe, in
the microscope, the surface of the material. It
was found that cylinders one and two, the
surface of the material could be more correct,
so these were used to perform the following
procedure.

In the second instance, was a process of

etching unprotected for cutting parts of the
surface of the material, this operation was
carried out with 6.3% m hydrochloric acid. Fig. 5 Piece two and three after sanding.
The surface of the cylinder was submerged in
the reagent for two minutes and immediately In the second part, the images of the pieces
they were washed with distilled water, and after the polishing but taken with a
they were at rest until their total drying. Then microscope at different visions:
were the surfaces observed of cylinders under
the microscope.

Finally, annealing and tempering techniques

were carried out to identify, recover and
 Fig. 6 Piece one after sanding at 100x. Fig. 10 Piece two after the chemical attack with HCl at 100x.

Fig. 7 Piece two after sanding at 100x Fig. 11 Piece two after the chemical attack with HCl at 100x
from another angle.
.

Fig. 8 Piece three after sanding at 100x.

Fig. 12 Piece three after the chemical attack with HCl at 100x.

Then after the etching with Hydrochloric

Acid for all the three pieces we obtained
these photos with the microscope, also a
different vision:

Fig. 13 Piece three after the chemical attack with HCl at 100x
from another angle.

Finally, after selecting the stick one and two,

the process of heat treatment was made, for
Fig. 9 Piece one after the chemical attack with HCl at 100x the number one the tempering and for number
two the annealing and we got to these photos
that also were taken with microscope at keeping in mind their mechanical and
different vision: chemical properties and doing some tests that
improve these properties [11]. For this
reason, in this procedure firstly the sanding
process was done using different kind of
sandpapers caliber (grain sizes), where if the
number of conventions was bigger, the
sandpaper will have a fine and soft texture.
The figure 4 y 5 shows that the stick steels
produce reflects at the end of the sanding,
because some scratches were eliminated in
Fig. 14 Piece one after tempering process at 10x. the final roughing and it obtained a surface
with some specular characteristics (soften,
brightness, etc.). When the microscopic
analysis is done (Fig 5,6 y 7) at 100x, we can
realized some scratches in all of the stainless
steel samples, but it is important to highlight
that the best treatment of sanding was the
sample number 3. There were some problems
in the sanding process, that’s why some
hypothesis can be mentioned. In the first
Fig. 15 Piece one after tempering at 100x. place, the sandpaper that were used had a
grain surface of Silicium carbide, specials for
solids and tenacious solids like marble,
titanium, glass fibers and more, but for
materials with plastered and long chips walls
like metals and alloys (in this case stainless
steel), it is better to use sandpaper with grain
surface of Aluminum oxide to get a total
polished and brightness mirror [1]. On the
other hand, like the results said, we used
sandpaper with several conventions of 60,
Fig. 16 Piece two after annealing at 10x.
300, 600, 1000, 1200, 2000 and 2500
respectively. The change of sandpaper from
1200 to 2000 is considerable and could affect
in the sanding moment, as it should have been
used a sandpaper with a number of
conventions in the range previously
mentioned, because the 2000 don’t eliminate
the whole scratches that still stands after the
polishing with the 1200; that’s why a
sandpaper of 1500 would have given better
Fig. 17 Piece two after annealing at 100x. results. In addition, the material could have
been treated with the sandpaper for a more
VI. ANALYSIS considerable time, since for each one it was
A metallographic analysis is based on the polished for 6 minutes, and although the
study of the micro structure properties that human eye saw a very considerable
identified the metals and some alloys,
brightness, the microscopic analysis shows rapidly attacks chromium alloys and nickel
that it was not at all like that [7]. (like stainless steel) and that could also
generate a better visualization of its structure.
One of the most common characteristics of all
types of stainless steel, is the great resistance In addition to this, another factor that can
to atmospheric corrosion, the attack of cold or infer the metallographic analysis, is the
hot acids and oxidation with formation of resolution of the image, since it is in 100x
crusts at high temperatures [4]. and should be used generally with an image
resolution of 500x if you want to take a good
These acid attacks are carried out with the
microstructure reveal of the material.
objective that the material's atoms can be
visualized, since they dissolve easily and Tempering is frequently used to improve the
besides that in the process, they have much tenacity of different types of steels so that
more reactive grain limits, it makes them they resist much more during industrial
change their reflexivity and increase their processes in which they may be involved. In
visibility [4]. short, it is a process in which the material is
heated to temperatures very close to the
As we can see in figures 9 to 13, the side
melting point in a given time, then let it cool
effects are obtained because of the polishing
to room temperature and observes certain
process was not carried out correctly,
results. For this case, we use part 1, to which
however, certain types of particles are
this thermal process was carried out. If we
observed (especially in Figures 12 and 13).
analyze the results obtained, we can see
from which it can be inferred, that some of
certain types of spots in both the 100x and
that behave or the form of those particles are
10x resolution, from which it can be deduced
referred to some of the structures that form
that they are due to the slow cooling with the
the stainless steel and that in this way would
ambient temperature, and led to the formation
mean that in that part would present a better
of a very known, which is the "tempered
resistance to corrosion [5].
steel"[10].
In addition, the acid attacks generate a color
The annealing is used to recrystallize the
contrast as a result of a series of
hardened stainless steels and extract
electrochemical reactions in H + medium
chromium carbides. In addition, this
with a metal. in the same order, in that case, it
treatment homogenizes the welds of the steel,
is easily to see a change in color to a tone
and consists in bringing the material to
almost like coffee, which means a formation
considerably high temperatures and
in the film of the sample and therefore a
immediately cooling it in a medium that for
remarkable micro structural reveal.
this case was water, in order to overcome the
However, this may change with respect to sensitization [8]. In our experimental case, we
which acid is to be used. To sum up, in our use what we called from the beginning piece
case we made use of a strong acid, which is 2 to apply such treatment. The results are
hydrochloric acid (HCl); this acid is a observed in Fig 16 and 17, in which at a
compound that in all its concentrations, it resolution of 100x, the material presents a
attacks stainless steel because is easily to fairly uniform behavior, and this can be
destroys its passivity [9]. Nonetheless, this is explained by the possible recrystallization of
not the only acid that can generate a change steel, in which phenomena such as the
in the steel, there are a variety of acids that carburation and the incrustation on the
can obtain better results such as sulfuric acid, surface of the metal, which in the end
which at concentrations higher than 20% p / v
improves properties in the steel, such as [5] Capote, V. (2011). Metallography. Digital magazine for
teaching professionals, 89 (17)
hardness and electrical conductivity [8].
[6] Ramesh Singh (2016). Applied Welding Engineering
(Second Edition). Pages 83-90. Available:
VII. CONCLUSIONS https://doi.org/10.1016/B978-0-12-804176-5.00008-6
[Accessed 12 Mar. 2019]
The first treatment that was made to the
pieces of stainless-steel was the sanding and [7] Morral, F.R., Jimeno, E. & Molero, P. (1985). General
polishing, although a completely accurate Metallurgy, Barcelona, Spain: Reverte.
result was not obtained, the piece that had the
[8] IIT Bombay. (2013). Lección 7 Diseño para tratamiento
best results was piece three according to the térmico. Available:
images observed at x100, since it was the one https://nptel.ac.in/courses/112101005/downloads/Module_4_L
ecture_7_final.pdf [Accessed 13 Mar. 2019]
that it presented less scratches due to
roughing, less presence of impurities and [9] S. H. Avner. (2010). “Introduction to physical metallurgy”,
more space between the lines. TATA McGraw hill, 2nd 8. J. B. Bralla, “Design for
manufacturability handbook”, McGraw hill handbooks, 2nd
In the case of etching, hydrochloric acid for edition. edition.

this case, it was observed that piece one and

[10] Mesquita, RA, Barbosa, CA, y Machado, AR (2017).
the second suffered severe damage, but the Tratamiento térmico de aceros para herramientas. Acabado
piece three was the one that best resisted this integral de materiales, 214–245. Available doi: 10.1016 /
b978-0-12-803581-8.09191-8 [Accessed 13 Mar. 2019]
process, since there was no evidence of
corrosion as in the first two cases. [11] Escuela colombiana de ingeniería Julio Garavito (2011).
Metalografía protocolo. Available:
In the same way, when anneling was done in https://www.escuelaing.edu.co/uploads/laboratorios/7643_met
alografia.pdf [Accessed 12 Mar. 2019]
piece two, the images captured by the
microscope show us a better visualization of ANNEXES:
the stainless steel structure than when the
tempering was done in piece three.

VIII. REFERENCES

[1] MIT (2003). THE METALLOGRAPHIC EXAMINATION

OF ARCHAEOLOGICAL ARTIFACTS. [ebook] Available
at: https://ocw.mit.edu/courses/materials-science-and-
engineering/3-094-materials-in-human-experience-spring-
2004/laboratories/manual_suppl.pdf [Accessed 14 Mar. 2019].

[2] T. Murphy, "THE USE OF METALLOGRAPHY TO

IDENTIFY COMMON PROBLEMS IN PM STEELS",
PowderMet, 2009. [Online]. Available: She was borned on April 20, 1999.
https://pdfs.semanticscholar.org/f3ed/b30aa7f2410ab17bdaf52 Cúcuta-Colombia. She graduates from
cbc9a540ebfbab1.pdf. [Accessed: 14- Mar- 2019]. Calasanz School, right now she’s
studying chemical engineering at the
[3] BerkeleyPoint (n.d.). What is Stainless Steel?. [online] “Universidad de La Sabana” located in
Berkeley Point. Available at:
Chía, Cundinamarca. She loves dancing.
https://www.berkeleypoint.com/learning/stainless.html
[Accessed 14 Mar. 2019].

[4] SSINA (n.d.). STAINLESS STEEL OVERVIEW:

FEATURES & BENEFITS. [online] The Stainlesss Steel
Information Center. Available at:
http://www.ssina.com/engineer/overview/features.html
[Accessed 14 Mar. 2019].
 graduated from the Liceo General Serviez, in
Villavicencio-Meta, he is currently a student
of chemical engineering at the "University of
La Sabana" located in Chia, Cundinamarca.

Gina Alejandra Ramírez. He was born on

January 19, 2000 in Villavicencio. She
graduated from the Gimnasio Campestre La
Fontana, in the same city. She is currently a
student of chemical engineering at the
"University of La Sabana" located in Chia,
Cundinamarca. Luisa Fernanda Cárdenas Flórez, was born on
June 15, 1999 in Bucaramanga, Colombia.
She was graduated from Colegio la Merced.
She is currently studiying chemical
engineering at the university of La Sabana.
Ubicated in Chia, Colombia.

María Valentina Castiblanco Jiménez. She

was born on October 22, 1999. Bogotá-
Colombia. Colegio Nelson Mandela, she is
currently studying chemical engineering at
the “Universidad de la Sabana” ubicated in
Chia, Cundinamarca.

Marlon Elian Bello Sepúlveda. He was born

on August 17, 2000. Cáchira, Norte de
Santander, Colombia. He was graduated from
Colegio Nuestra Señora del Rosario. He is
currently studying chemical engineering at
the university of La Sabana located in Chia,
Cundinamarca.

Laura Marcela Trejos Vence. He was born on

April 3, 2000. Bogotá-Colombia. She