Effect of Heat Treatment on Mechanical and Corrosion Properties of

Stainless Steel

V.Mounika1,a* ,K.Priyanka1,b, Ch.Nagarjun1,c, G.Anil Kumar1,d,A.D.S.Arjun1,e

1 Department of Metallurgical and Material Science Engineering

Rajiv Gandhi University of Knowledge Technologies, Nuzvid APIIIT Krishna (D),

Email:amounikareddy2229@gmail.com,bkotapriyanka634@gmail.com,

ccherukurinagarjun.iiitn@gmail.com,danil.guduturi@gmail.com,earjun.rgukt@gmail.com

*corresponding author: raja.anna@gmail.com

ABSTRACT

Stainless Steel used in a wide range of applications including plane, mechanical equipment
and railways. Stainless steel is only uses in major industry but can also be used in non-major industry
such as watch manufacturing that consists of micro size of elements. Stainless is an iron alloy
containing 0.02 to 2.14% of C, Cr content greater than 12% and other alloying elements. Engineering
materials, mostly steel, are heat treated under controlled sequence of heating and cooling to alter their
physical and mechanical properties to meet desired engineering application. In this study, the effect
of heat treatment (annealing, normalising, hardening, and tempering) on the microstructure and some
selected mechanical properties of stainless steel were studied. Solutionisation is the process of heating
to 10500c temperature and air cooled to get single phase homogeneous austenite phase. The steel
samples were heat treated in an electric tubular furnace at different temperature levels and holding
times and then cooled in different media. The microstructure of the sample was examined using
metallographic microscope. The mechanical properties (Rockwell Hardness & Brinell hardness) of
the treated and untreated samples were determined using standard methods. Corrosion Studies were
conducted for Heat treated and untreated samples by using Potentiostatic machine.

Key Words: Stainless Steel, Heat Treatment (Solutionisation), Microstructures, Hardness,

Corrosion, Potentiodynamic Curve.
Introduction:

Stainless steel:

The stainless steels are branch of the family of ferrous alloys designed for extremely high
levels of corrosion resistance. This effect is achieved by alloying primarily with chromium but may
also enhanced by the addition of elements such as molybdenum and nickel. Moreover, these alloy
elements may significantly alter the phase relationships in the steel and procedure a wide spectrum
of possible microstructures [1]. The range of microstructures serves to qualify some stainless steels
for special types of service beyond their use in corrosion service. 12wt% of chromium concentration
give the stainless character to the steel. To ensure a robust material, the higher chromium
concentration and other solute such as molybdenum, nickel and nitrogen is needed. Purpose of Heat
Treatment is to improve the microstructure and the properties for specific applications by the
application of different heat treatment processes like Annealing, Normalizing, Quenching &
tempering, Solutionisation and Austempering. Hardness is a vital property for the biomaterial to
withstand heavy loads. To improve wear and friction properties, generally, the hardness of the surface
should be increased. The results of the studies indicated that there was a significant improvement in
both corrosion and hardness in the case of implanted samples [2].

Solutionisation Heat Treatment:

This softening mechanism is used to bring solute additions trapped in second phases back into
solid solution. Prior to age- or precipitation hardening, the microstructure of the (heat treatable) alloy
is required to be super-saturated with the hardening elements and excess vacancies. This type of micro
structural state can only be obtained by solution heat treatment. Solution heat treatment affects the
mechanical properties of age or precipitation hardenable alloys [11]. The stainless steels are quite
often given the solution-annealing or quench-annealing treatment to obtain a single phase
homogenous austenite. In this treatment, steels are heated to 1050-11200c. Any chromium carbide, if
present, gets dissolve in austenite, which has high solubility of carbon at this temperature. After
solutionising, i.e., homogenizing, the steel is cooled rapidly through the critical range of 9000c to
4000c by quenching in water, oil, or air to avoid the reprecipitation of carbides. The choice of the
cooling medium depends on the section-thickness, as the small thin sections may be even air cooled.
Furnace cooling is never done [7].
Effecting Factors:

Heating Rate:

The faster the metal is heated to solution heat treatment temperature, the lesser is the chance
for new phases to form during heat treatment which have to be subsequently dissolved during solution
heating.

Soaking Time:

After heating the material above the solvus temperature, sufficient time must be given to
completely redissolve the second phase. The duration of soaking at the solution heat treatment
temperature is determined by the rate of dissolution of strengthening elements, the nature of the
alloys, and heating conditions (heating rate, soaking temperature).

Soaking Temperature:

The choice of soaking temperature (also referred to as peak metal temperature PMT) depends
on the alloy and rate at which the soluble particles dissolve. Different alloys have different solvus
temperatures and therefore the choice of PMT depends on the solvus temperature. PMT is usually
higher than the solvus temperature to ensure complete dissolution of second phases during solution
heat treatment. Higher temperatures accelerate dissolution and are useful to dissolve large second
phase particles.

Effects of Under-Solutionising

Solution heat treatment is only applicable to age- or precipitation hardenable alloys and these
alloys gain strength due to the presence of fine second phases. SHT is carried out before the final
ageing or precipitation heat treatment to re-introduce solute into the matrix so that it can be utilised
to form a fine dispersion of phases on subsequent processing [4]. Therefore, if the alloys are not fully
solutioned prior to ageing then the final properties of these alloys are affected as explained below.
Under solutionising results in less solute available to form clusters and precipitates during natural
ageing (ageing at room temperature). This in turn lowers strength. Under solutionising results in less
solute available to form clusters and precipitates during ageing at elevated temperature. This in turn
lowers strength. Incomplete dissolution of pre-existing particles prior to SHT can affect formability
of the aged material. Undissolved coarse particles might act as sites for strain localisation, leading to
premature failure during forming or in service [16].
Hardness:

It is the degree of resistance to indentation or scratching, abrasion and wear. It also the ease
with which atoms move or slip in a metal is an indication of hardness [18].

Brinell Hardness: In the Brinell hardness test, a hard spherical indenter is pressed under a fixed
normal load onto the smooth surface of a material. When the equilibrium is reached, the load and the
indenter are withdrawn, and the diameter of the indentation formed on the surface is measured using
a microscope with a built-in millimetre scale. The Brinell hardness is expressed as the ratio of the
indenter load W to the area of the concave (i.e., contact) surface of the spherical indentation that is
assumed to support the load and is given as Brinell hardness number (BHN).

Brinell hardness Measurements: =

( )

Where, P – Applied Load in kg, D – Diameter of indenter in mm. d – Diameter of indentation in mm

[18].
Rockwell Hardness: The Rockwell hardness test is defined in ASTM E 18 and several other
standards. Rockwell hardness testing differs from Brinell testing in that the Rockwell hardness
number is based on the difference of indenter depth from two load applications. Initially a minor load
is applied, and a zero datum is established. A major load is then applied for a specified period of time,
causing an additional penetration depth beyond the zero datum point previously established by the
minor load. After the specified dwell time for the major load, it is removed while still keeping the
minor load applied. The resulting Rockwell number represents the difference in depth from the zero
datum position as a result of the application of the major load. The entire procedure requires only 5
to 10 s [18].

Corrosion:

Corrosion is the destructive attack of materials when they react with environment by
chemically or electrochemically. This stainless steel alloys are mainly meant for corrosion resistance
applications [17].
Electrochemical Reaction:
Electrochemical reactions or Electrode reactions are that occur with charge transfer between
neutral or ionic reactants and a conductions material called electrode ,acting as an electron source.
Electrochemical reaction involves change in valence that is oxidation or reduction of the reacting
elements [17]. Stainless Steels having higher corrosion resistance compare to other ferrous alloys.
Because these alloys form passivation layer when react with the atmosphere. A major characteristic
of passive system is existence of a polarization curve (I, current density or rate, versus E, potential,
or driving force). A metal become passive when upon increasing its potential in the positive or anodic
direction, a potential is reached where the current (rate of anodic dissolution) sharply decreased to a
value less than that observed at a less anodic potential. This decrease in anodic dissolution rate, in
spite of the fact that driving force for dissolution is brought to a higher value, is the result of the
formation of a passive film. Employting Passivity to Control corrosion. Passivity can be used to
control corrosion by using methods that bring the potential of the surface to be protected to a value
in the passive region. This can be accomplished by using a device called a potentiostat, a current can
be applied to the metal to be protected that will set and control the potential at a value greater that the
passivating potential, Ep. This method of producing passivity is called anodic protection[17].

Experimental Procedure:

Heat Treatment

The steel samples which are in cylindrical shape with diameter of 25 mm and a thickness of
20 mm.The five stainless steel samples were given a common solutionising treatment to obtain a
single phase austenitic region by heating them to 10500 C and soaking for an hour followed by air
cooling to room temperature. The each solution treated stainless steel sample was subjected to ageing
treatments at particular temperatures those are at 5500 C, 5800 C, 6200 C and 6800 C and a common
soaking of 4 hours followed by air cooling to room temperature. After that the samples are polished
by using metallographic techniques to observe the microstructure.

Table 1: Heat Treatment

Solution treated Temperature(0c) Soaking time Type of cooling

10500c and air cool 550 4hr Air
below (condition A) 580 4hr Air
620 4hr Air
680 4hr Air

Metallography:

Metallography is the scientific discipline of examining and determining the constitution and
the underlying structure of (or spatial relationships between) the constituents in metals, alloys and
materials (sometimes called materialography).The most familiar tool of metallography is the light
microscope. Optical (light) characterization of the microstructures of metals and alloys involves the
identification and measurement of phases, precipitates, and constituents, and the determination of the
size and shape of the grains. [13]

Brinell Hardness:

The Brinell hardness tests were carried out for each specimen using a 3000 kg load Brinell
hardness tester and diameters of the indentations were found by using microscope. The Brinell
hardness values of all specimens were calculated using the formula given below.

2P
=
πD D − √D − d

Where, BHN is the Brinell hardness number, P is the applied load, D is the diameter of the
indenter and d is the diameter of the indentation.

Rockwell Hardness:

In Rockwell testing, the minor load is 10 kgf, and the major load is 60, 100, or 150 kgf. In
superficial Rockwell testing, the minor load is 3 kgf, and major loads are 15, 30, or 45 kgf.
In this process a minor load of 10 kgf is applied to eliminate the backlashes in measuring system and
causes the indenter to break through slight surface roughness. After that a major load of 150kgf is
applied. By using C scale the hardness values are noted.

Corrosion Studies:
Corrosion resistance of Austenitic Stainless Steels were studied by two techniques.
1. Weight loss method
2. Electrochemical method

Weight Loss Method

The samples were weighed by using electronic balance and subjected to 1N HCl for 30
minutes (0.5hr) time period. The samples were removed from the solution, dried in hot air oven and
weighed in electrical balance to obtain loss in weight. Corrosion rates were calculated using the
formula below:

534
( )=
Where, w is the weight loss of the sample (mg), is the density (gcm-3), A is the surface area of the
sample (in2) and T is the time (hour). [8]

Electrochemical Method

To study the electrochemical behaviour of stainless steel, all samples were polished with 120
grit SiC papers for obtained a smooth surface and exposed area of the sample was 1 square centimetre.
A typical three-electrode electrochemical corrosion cell was used in all the experiments. A saturated
calomel electrode (SCE) was used as reference. All measured potentials were referred to this
electrode. A platinum foil was used as the counter electrode. The Manganese bronze samples were
used as working electrodes. [17] A potentiostat (IVIUM), controlled by a personal computer, and the
commercial software was employed to obtain the potentiodynamic polarization curves. Before each
experiment, the open circuits potential (OCP) was recorded for 60 min. Polarization curves were
obtained potentiodinamically. Potentiodynamic polarization tests were carried out from 0.9250 V
versus OCP to +1.800 V versus reference electrode at a scan rate of 1 mV/s. The corrosion potential
(Ecorr) and corrosion current (Icorr) corrosion rate were determined from the polarization curves. The
corrosion rate can be determined using the formula expressed as follows.

( )=

Where, K1 = 0.1288 (mpy), EW is the equivalent weight, ρ is the density of the material (gcm3), Icorr
is the corrosion current (µA/cm2).

Results & Discussion:

Figure 1 Shows the optical micrograph of solution treated sample at 10500C. It reveals that
the homogenized austenite with fine grains containing some small amounts of carbides along the
grain boundaries.After solution treatment process a low temperature age hardening stage is employed
to achieve the required properties, as this treatment carried out at low temperatures no distortion
occurs and during the hardening process a slight decrease in size takes place. Figure 2 Micrograph of
solution treated and aged at 5500C reveals that the formation of carbides along the grain boundaries
without Affecting the grain size.
Figure 1: SS Solutionised at 10500C at 500X Figure 2: SS Solutionised and aged 5500C at 500X

Figure 3: SS Solutionised and aged 5800C at 500X Figure 4: SS Solutionised and aged 6200C at 500X

Figure 5: SS Solutionised and aged 6800C at 500X

Figure 3 shows that microstructure of austenitic stainless steel which was solution treated and
aged at5800C and soaking for 4 hours followed by air cooling to room temperature It can be seen that
the ageing treatment at 5800C results in slightly coarsened the size of the carbides while grain size is
remains unchanged. The volume fraction of carbides also increases. Figure 4 shows the
microstructure of austenitic stainless steel which was solution treated and aged at 620 0C and soaking
for 4 hours followed by air cooling to room temperature. It can be seen that the ageing treatment at
6200C results in significant change in volume fraction and size of the carbides. It reveals that the
volume fraction of carbides decreases by dissolving the fine carbides and also it is observed that the
increasing the grain size of the austenite takes place. Figure 5 shows the microstructure of austenitic
stainless steel which was solution treated and aged at 6800C and soaking for 4 hours followed by air
cooling to room temperature. It can be seen that the ageing treatment at 6800C results in optimum
grain size of Austenite and it is also observed that the increasing of volume fraction of carbides with
Optimum size of carbides along the grain boundaries takes place.

Hardness Values
The mechanical properties of stainless steels mainly depends on the microstructure and heat
treatment. Therefore the hardness values are mainly dependent on the heat treatment. Both Hardness
values Rockwell hardness and Brinell hardness values taken at various aged temperatures are
mentioned in the below table 2. From this values we conclude that hardness values increasing when
increasing the aging temperatures except at 6200C because of the dissolution of chromium. But at
again increasing the temperatures re appearance of carbides takes place so that at again when aging
at 6800C.

Table 2: Hardness Values at various processing temperatures

Processing conditions Rockwell hardness Brinell hardness

Solution treated at 10500 C 76.9 477.7
ST + aged at 5500 C 80.6 477.7
ST + aged at 5800 C 82 555.6
ST + aged at 6200 C 79.1 363.4
ST + aged at 6800 C 95.9 653.8

Corrosion rate Value

Weight loss method:

The results which are in the below table shown that weight loss and corrosion rate is high for
solution treated aged 5800C sample followed by just solutionised sample at 10500C.weight loss and
corrosion rate is very less for solution treated aged 5200C sample. The results shows that we can get
less weight loss and corrosion rate only at some optimum aged temperatures.
Table 3: Solutionised Heat Treatment of Stainless Steel Corrosion rate Values (weight loss
Method)

Initial Final Corrosion

Sample Weight loss
weight(grms) weight(grms) rate(mpy)

Cond A 34.9671 34.9641 0.0030 165.56

ST+ aged 5500C 37.1328 37.1309 0.0019 99.43
ST+aged 5800C 37.3055 37.3020 0.0035 183.5
ST+aged 6200C 36.4397 36.4378 0.0019 100.69
ST+aged 6800C 37.3975 37.3954 0.0021 110.41

Electrochemical Method

The corrosion rate values from the electro chemical studies are in this below table. From this
values we observed that corrosion rate is high for solution treated and aged at 5500C and low for
solution treated + aged 6200c. From table it is clearly indicating that from aged temperatures 5500C
to 6200C the corrosion rate values are decreasing. The results shows that at some optimum aged
temperature we got less corrosion rate values. At Temperature 5500C chromium carbides are formed
because of this chromium

Content decreases hence corrosion rate is increased whereas at 6200C all chromium carbides
are dissolved. This will give us high chromium content which will form passive layers. By Comparing
these weight loss method and electrochemical method. Both these values are not comparable. The
corrosion rate calculations at various aged temperatures are below
Table 4: Solutionised Heat Treatment of Stainless Steel Corrosion rate Values
(potentiodynamic studies)

CR=Corrosion Rate
Sample(0c) icorr in A
S.NO In 10-3 mm/yr
1 550 2.23146 23.3463
2 580 2.16380 22.6384
3 620 1.69279 17.7105
4 680 1.841740 19.2689
5 Condition A 2.187732 22.8888
Conclusions:

From the above results and graphs. We Can conclude that the mechanical properties and
corrosion rate values are mainly depends on the heat treatment and at solutionised temperatures. But
in order to get the optimum mechanical properties and corrosion resistance properties have to choose
the optimum temperatures.
From the above results and graphs. Can conclude that the mechanical properties and corrosion rate
values are mainly depends on the heat treatment and at solutionised temperatures. But to get the
optimum mechanical properties and corrosion resistance properties have to choose the optimum
temperatures.

1. The solutionised heat treatment of austenitic stainless steels shows microstructure containing
homogenized austenite with fine grains containing some small amounts of carbides along the
grain boundaries.
2. The temperature of ageing treatment affects the volume fraction, grain size of carbides as well
as grain size of austenite.
3. Ageing treatment at 6800 C gives the best microstructure with optimum grain size and volume
fraction of carbides along the grain boundaries.
4. At this temperature uniform distribution of carbides takes place and gives the maximum
Rockwell hardness value as 95.9 and maximum Brinell hardness value as 653.8.
5. In weight loss method at ageing temperatures 5500C gives the less corrosion rate.
This temperature is optimum for corrosion rate.
6. In potentiodynamic studies at ageing temperature 6200C gives the less corrosion rate. This
temperature is optimum for corrosion rate because at that temperature the chromium carbides
gets dissolved in the matrix so that it forms a passive layer on the surface hence corrosion rate
is decreased.

References:

1. Beaune, France, October 13, 2010.Environmental Engineering, Georgia Institute of

Technology, Atlanta, GA, 2011.
2. A. J. Sedriks, Corrosion of stainless steels, 2nd ed. New York: Wiley, 1996.
3. Maloney, "Case Carburized Stainless Steel Alloy for High Temperature
Applications," USA Patent, 1995.
4. R. D. Moser, "High-Strength Stainless Steels for Corrosion Mitigation in Prestressed
Concrete: Development and Evaluation," Ph.D. dissertation, School of Civil and Material
Science
5. M. Genet, Orban, C., "Steel, Alloys and Stainless: Part II," in Stainless Steel World,
6. ASM INTERNATIONAL, Electronic Materials Handbook, Volume 4
7. ASM INTERNATIONAL, Heat Treating, Volume 4
8. ZAKI AHMAD, Principles of Corrosion Engineering and Corrosion Control
9. S.L.Kakani, Amit Kakani, Material Science
10. CALLISTER (WILEY, 2007), Materials Science and Engineering an Introduction (7 Ed.)
11. Effect of Heat Treatment of Stainless Steels orthodontic wieres, OsmarAparecido
Cuoghi,Geraldo Francisco Kasbergen,Paulo Henrique dos Santos
12. MARS G.FONTANA, Corrosion Engineering Third Edition
13. H.K.D.H Bhadeshia Steels microstructure and properties by 3rd edition
14. Glyn Meyrick, Professor Emeritus Physical metallurgy of steel
15. Vijayendra Singh Heat treatment of steels, Heat Treatment of Steels(pg no 450-459)
16. Thomos G.Digges, Samuel Rosenberg, and Glenn W.Geil Heat treatment and properties of
Iron and Steel
17. ASM HAND BOOK 13A,Corrosion Fundamentals, Testing and protection
18. ASM HAND BOOK 8,Mechanical Testing And Evolution
19. American Society for Metals, Metals handbook (1948) and Vol. 1 and 2), Am. Soc.
Metals, Metals Park, Ohio.