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Effect of heat treatment on an AISI 304 austenitic stainless steel evaluated by

the ultrasonic attenuation coefficient

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DOI: 10.3139/120.110878

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 448 MECHANICAL TESTING/MATERIALOGRAPHY

Effect of heat treatment on an

AISI 304 austenitic stainless steel
evaluated by the ultrasonic
attenuation coefficient
Materials Testing downloaded from www.hanser-elibrary.com by Hanser Verlag (Office) on May 3, 2016

Abbas Moghanizadeh and The properties of metals can be substantially changed by various meth-
Abolfazl Farzi, Esfarayen, Iran ods, one of them is using heat treatment processes. Moreover, ultrasonic
testing is the most preferred and effective, nondestructive testing tech-
nique for characterization of mechanical material properties. Austenitic
stainless steel AISI 304 serves in many applications due to high strength
and corrosion resistance. In certain applications, it is important to evalu-
Article Information ate the mechanical properties of AISI 304 stainless steel. In this study,
Correspondence Address the ultrasonic method (attenuation measurement technique) is used to
For personal use only.

Abbas Moghanizadeh evaluate the hardness of AISI 304 stainless steel samples which were
Department of Civil Engineering,
Esfarayen Branch,
heat treated at different levels. Due to the heat treatment process, each
Islamic Azad University, sample has its specific microstructure and hardness which attenuate ul-
Esfarayen, Iran trasonic waves appropriately. The ultrasonic and hardness test show that
E-mail: abbas.moghanizadeh@gmail.com
it is possible to evaluate the hardness of AISI 304 stainless steel by ultra-
Keywords
Ultrasonic attenuation coefficient, hardness, sonic attenuation coefficient. In addition, the relationship between ultra-
heat treatment, austenitic stainless steel sonic attenuation coefficients and time of heat treatment is investigated.

The properties of metals can be substan-
tially changed by various methods, one of
them is using heat treatment processes; in
addition, evaluation of the physical proper-
ties is significant in a number of applica-
tions [1]. Characterization of material prop-
erties by nondestructive testing takes on
an increasingly important role, especially
in the industry, as it can be used to monitor
components during the manufacturing pro-
cess as well as in operation [2].
Ultrasonic testing is the most preferred
NDT technique for characterization of mate-
rial properties due to the fact that ultra-
sonic waves are significantly affected by
changes in microstructural or mechanical
properties of materials [3]. Although ultra-
sonic techniques have a unique ability to
detect discontinuities such as voids, cracks,
and inclusions, they have a potential to eval-
uate such material characteristics as micro-
structure, grain size, yield strength, frac-
ture toughness, volume fraction of second
phase and residual stress [4]. The study of
ultrasonic wave propagation in metals and
composites can provide information on the
microstructure as well as the mechanical
and physical properties of the material [5].
Ultrasonic velocity and attenuation
measurements are two conventional meth-
ods to determine the properties of materi-
als [1]. The ultrasonic velocity technique in
longitudinal and shear modes can be cor-
related to various material properties [2].
The ultrasonic wave velocity depends on
elastic constants and density of the metals.
The ultrasonic velocity can be used to de-
termine the mechanical properties of steel
[6]. The influence of hardening, tempering
and annealing on the velocity of ultrasonic
vibrations was studied by Muravev [7].
Prasad and Kumar have correlated sound
velocity and ultrasonic attenuation with
the heat treatment conditions of steel cast-
ings [8]. Bouda et al. measured sound ve-
locity and attenuation by both longitudinal
and transverse wave at the half cylindrical
shape Jominy specimens of steel [9].
Attenuation refers to the loss of sound
energy of the ultrasonic beam which passes
through the material [3]. The attenuation
coefficient is determined by measuring the
reduction in amplitude of an ultrasonic
wave which has traveled a known distance
through a material. Attenuation is a fre-
quency-dependent coefficient and can be
written as:
1 AX
a(f) = − 20log (1)
x A0
with A0: initial amplitude of the ultrasonic
wave (x = 0) and Ax: amplitude after trave-
ling a distance × [1].
It is shown that the microstructure and
crystalline defects affect the ultrasonic at-

© Carl Hanser Verlag, München  Materials Testing  58 (2016) 5


tenuation [10]. The ultrasonic attenuation
measurement technique is widely used in
material property characterization to deter-
mine grain size [9], fracture toughness [11]
and recrystallization [12].
According to Vasconcelos et al. [17], each
grain within an attenuating material con-
tributes to attenuation depending on the
ratio of the acoustic wavelength of the prop-
agating pulse (λ) to the mean grain diame-
ter (D) of the material structure [13]. The
attenuation coefficient of the ultrasonic
wave is affected by absorption and scatter-
ing [1]. Absorption occurs because of the
dislocation damping, magnetic resistance
or thermal elasticity, and scattering can ap-
Materials Testing downloaded from www.hanser-elibrary.com by Hanser Verlag (Office) on May 3, 2016
pear due to grain boundaries, voids, inclu-
sions, second-phase particles and cracks
[14]. Several studies have been done to in-
vestigate the ultrasonic attenuation in ex-
tensive range of different materials includ-
ing: vanadium, niobium and tantalum at
low temperatures [15], plain carbon steel
consisting of considered ferrite, pearlite,
ferrite–pearlite and martensite microstruc-
tures [16] and even granites [17].
One of the most important properties of
For personal use only.
materials is hardness which is dependent
on ductility, elastic stiffness, plasticity,
strain, strength, toughness, viscoelasticity
and viscosity [18]. Hardness refers to the
resistance of material to plastic deforma-
tion. It is measured in terms of resistance to
indentation by using Brinell, Vickers and
Rockwell hardness testers [19]. It has been
observed that the velocity varies paraboli-
cally and attenuation varies linearly and in-
versely with the hardness [2]. In addition, a
touch sensor based on piezoelectric ceramic
transducers for detection of thickness and
hardness has been developed [20]. The ul-
trasonic technique is also used to measure
the depth of surface hardening [21].
Heat treatment is a usual method to im-
prove the mechanical properties of steel
such as hardness for different applications
in many industries [9]. During heat treat-
ment, the microstructure of materials
changed to acquire the desirable mechani-
cal properties; however, measuring these
changes by destructive methods is not only
expensive, but also impossible in some ap-
plications. The ultrasonic testing technique
based on velocity and attenuation measure-
ment was developed in authors’ laboratory
to qualify the heat treatment of these steels.
The results reveal that there is also an in-
crease in ultrasonic attenuation after heat
treatment of 17-4 PH stainless steel [3]. The
wave velocity and attenuation of SAE 52100
samples quenched at different tempera-
58 (2016) 5
MECHANICAL TESTING/MATERIALOGRAPHY
tures have also been studied by Papadakis
[22]. In addition, the ultrasonic attenuation
is used to evaluate the heat treatment of
materials assessment in environmental
degradation of materials [23]. The AISI 304
austenitic stainless steel is the most versa-
tile used stainless steel available in a wider
range of products (from chemical contain-
ers to heat exchangers). This type is the
most widely used alloy of austenite group
which has a nominal composition of 18 %
chromium and 8 % nickel [24].
The aim of this study is to assess the po-
tential of the ultrasonic nondestructive eval-
uation technique in order to measure the
hardness of AISI 304 austenitic stainless
steel samples which were hardened at dif-
ferent levels during heat treatment. The ul-
trasonic attenuation as a common technique
is used to measure the changes in hardness
of this alloy during the heat treatment.
Experimental procedure
Material. The chemical composition of
AISI 304 austenitic stainless steel (UNS
S30400) used in the present study is given
in Table 1. To prepare samples, AISI 304
stainless steel in form of hot rolled bars
were cut to create 48 cylindrical samples
20 mm in diameter and 100 mm in height.
Subsequently, the samples were ground to
obtain appropriate roughness and surface.
Heat treatment. The heat treatment pro-
cesses are designed according to advice
proposed by industrial experts. Due to
some differences in grain size and banding
in the initial microstructures, all samples
are austenitizing at 1150 °C for 1 h before
quenched in water. As a result, the initial
microstructures of all samples are austen-
ite with a homogeneous composition of car-
bon and other alloying elements.
The two main factors, which affect the
austenitization of AISI 304 stainless steel,
are temperature and time [25]. Hence, all
prepared samples were processed by differ-
ent heat treatment levels including 2 levels
N Ni Mo Cr S P
0.10 10.5 - 20.0 0.030 0.045
Table 1: Chemical composition of the AISI 304 grade stainless steel
Time (min) Time (min) Time (min)
120 60 30
120 60 30
Table 2: Heat treatment parameters
449
in temperature (1000 °C and 1050 °C) and
6 levels in time. All heat treatment details
are shown in Tables 2. The samples were
cooled in water.
Hardness measurement. Hardness lev-
els of the samples were obtained by a Rock-
well A hardness tester, using a 60 kg load
in 10 seconds. For each sample, at least five
indentations were made under similar con-
ditions and the averages of the diagonal
lengths of the indentations were used to
compute the Rockwell A hardness.
Ultrasonic attenuation measurements.
The ultrasonic attenuation in the samples
was measured by contact pulse echo ultra-
sonic method according to ASTM C1332−01
that suggests a useful test method for meas-
uring and comparing microstructural varia-
tions among different samples of the same
material of monolithic ceramics and also
polycrystalline metals. Transducers with
150 mm diameter and frequencies of 4 MHz
normal beam longitudinal wave probe were
employed for the attenuation evaluation. In
order to achieve standard coupling condi-
tions during the ultrasonic assessment of
all specimens, a 250 g load was applied,
and also glycerine was used as couplant.
Signal acquisition was carried out accord-
ing to the drawing shown in Figure 1. The
attenuation was measured at least three
times under the same conditions and the
average of them are used.
Metallography. Microstructures were ob-
served using an optical microscope (BX61,
Olympus). Samples were ground with SiC
paper, polished and etched at room tempera-
ture. Etchant solution was a mixture of
100 ml water, 100 ml hydrochloric acid and
10 ml nitric acid. The grain sizes were
measured by linear intercept method. The
intercept method involves an actual count of
the number of grains intercepted by a test
line or the number of grain boundary inter-
sections with a test line, per unit length of
test line, used to calculate the mean lineal
intercept length, ℓ. ℓ is used to determine
the ASTM grain size number, G.
Si Mn C Grade Fe
0.75 2.0 0.08 304 66.495
Time (min) Time (min) Temperature
10 5 1000 °C
10 5 1050 °C
 450 MECHANICAL TESTING/MATERIALOGRAPHY
Results and discussion
Relationship between ultrasonic attenua-
tion coefficient and hardness. Ultrasonic
attenuation coefficient of the samples was
found by using the equations above. After
heat treatment at different levels, the ultra-
sonic attenuation coefficient and the hard-
ness of all samples were measured.
Figures 2 and 3 show the relationship be-
tween hardness of samples and ultrasonic
attenuation in heat treatment temperature
at 1000 °C and 1050 °C, respectively. Two
important parameters affect ultrasonic at-
tenuation coefficients by scattering: grain
boundaries and second-phase particles
Materials Testing downloaded from www.hanser-elibrary.com by Hanser Verlag (Office) on May 3, 2016
[14]. In this study, the selected AISI 304
stainless steel has a single-phase austenitic
microstructure; thus phase changing does
not attenuate ultrasonic waves. Therefore,
Figure 1: Schematic
illustration of the
For personal use only.
experimental set up
Figure 2: Variation in ultrasonic attenuation
with hardness at 1000 °C with error bars show-
ing the standard error of the measured value
Figure 4: Microstructure and grain size of samples heat treated for 5 and
10 minutes
the changing grain size occurring during
heat treatment has a great influence on the
ultrasonic attenuation coefficients.
Relationship between heat treatment
parameters and microstructure of sam-
ples. Grain size has a significant effect on
the physical properties of metals, so micro-
structure of the samples is observed by an
optical microscope. The microstructure of
samples for different times of heat treat-
ment (5 and 10 minutes) is shown in the
Figure 4. Also Figure 5 shows the micro-
structure of samples with a heat treatment
of 60 and 120 minutes. It is clear that grain
size rises by increasing the time of heat
treatment, with the exception of 5 minutes,
this heat treatment dose has no strong ef-
fect on the grain size.
Relationship between heat treatment
parameters and ultrasonic attenuation
Figure 3: Variation in ultrasonic attenuation
with hardness at 1050 °C with error bars show-
ing the standard error of the measured value
Figure 5: Microstructure and grain size of samples heat treated for 60 and
120 minutes
coefficients. Time and temperature play an
important role in changing physical prop-
erties such as hardness by heat treatment.
The relationship between time of heat
treatment and hardness of samples at
1000 °C is presented in Figure 6. As ex-
pected, increasing the time of heat treat-
ment leads to a rise in hardness of sam-
ples in initial time periods (lower than 30
minutes) but after extending the time of
heat treatment, the hardness of samples
declines. And there is a slight increase in
hardness for samples which are heat
treated for 120 minutes as illustrated in
Figure 6.
As shown in Figure 7, the ultrasonic at-
tenuation coefficient increases remarkably
by increasing the time of heat treatment
during the first 30 minutes. However, for a
time greater than 30 minutes, the ultra-
sonic attenuation coefficient remains
steady before showing a slight increase for
samples which are heat treated for more
than 60 minutes. Meanwhile, as shown in
the Figures 8 and 9, the samples heat
treated at a temperature of 1000 °C follow
a similar pattern.
Totally, for the time period lower than
30 minutes, hardness value of annealed
samples heat treated at 1000  °C and
1050 °C increases with a slight increase in
the time of heat treatment. This increase in
hardness can be attributed to precipitation
of chromium carbides in the grain bounda-
ries of the sensitized sample [25].
The precipitated chromium carbides im-
pede dislocation movement and reduce
the defects within the crystal lattice of
sensitized sample. Therefore, the hard-
ness of samples increases. Beyond 30 min-
utes of heat treatment, a reduction of
hardness is observed which can be associ-
ated to grain growth phenomenon. In-
creasing the time of heat treatment leads
to size increase of grain in metals. Hall
58 (2016) 5

Figure 6: Effect of tempering time on the
hardness at 1000 °C with error bars showing
the standard error of the measured value
Materials Testing downloaded from www.hanser-elibrary.com by Hanser Verlag (Office) on May 3, 2016
Figure 8: Effect of tempering time on the
hardness at 1050 °C with error bars showing
the standard error of the measured value
For personal use only.
showed the variation of hardness of met-
als with grain size, whereas a plot of the
hardness number against 1/d1/2, where d
stands for the grain diameter, generates a
straight line [26]. Thus, increasing the
size of grains leads to a decrease of sam-
ples hardness.
The main reason for ultrasonic attenua-
tion increase at a temperature of 1000 °C
and 1050  °C is grain size increase.
Whereas grain growth occurs during heat
treatment when recovery and recrystalli-
zation stages are completed, a reduction in
the internal energy can only be achieved
by reducing the total area of grain bound-
ary. Hence, the hardness of samples be-
gins to decrease with increasing the size of
grains at high temperatures (1000 and
1050 °C); in addition, increasing grain
size affects the ultrasonic coefficients di-
rectly. Moreover, according to the research
done by Nowacki [13], each grain within
an attenuating material contributes to at-
tenuation depending on the mean grain
diameter (D) of the material structure.
Thus by increasing the grain size, the ul-
trasonic attenuation will be raised. Mean-
while, some experimental errors can be
obtained due to differences in grain size
caused by heterogeneity in chemical com-
position or chromium carbide precipita-
58 (2016) 5
MECHANICAL TESTING/MATERIALOGRAPHY
Figure 7: Effect of tempering time on the
ultrasonic attenuation at 1000 °C
Figure 9: Effect of tempering time on the
ultrasonic attenuation at 1050 °C
tion band and also by nonuniformity in
heat treatment or heat transfer.
Conclusions
The purpose of this research is to derive
relationships between the ultrasonic tech-
nique and hardness at different tempering
temperatures for AISI 304 alloy steel. The
results reveal that the ultrasonic attenua-
tion coefficients can identify any hardness
changes in the microstructure of AISI 304
austenitic stainless steel at different tem-
peratures as listed below.
1. 
At the temperatures of 1000 °C and
1050 °C, the grain sizes of the micro-
structure rise by increasing the time of
heat treatment.
2. 
At the temperature of 1000  °C and
1050 °C, the hardness of samples de-
clines with increasing the time of heat
treatment; furthermore, the ultrasonic
attenuation increases in initial time of
heat treatment.
Totally, the investigation reveals that there
is an inverse relationship between hard-
ness and ultrasonic attenuation coeffi-
cients in AISI 304 austenitic stainless steel.
Accordingly, it is possible to use ultrasonic
attenuation for evaluating the hardness of
this alloy.
451
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25 R. Wendel, J. Dual: Application of neural net- evaluation of materials properties by using ultra-
works to quantitative nondestructive evalua- sonic testing. He graduated from K. N. Toosi Uni-
tion, Ultrasonic 34 (1996), pp. 461-465 versity of Technology, Tehran, Iran, in Mechanical
DOI:10.1016/S0963-8695(97)82084-1 Engineering (manufacturing and production).
26 E. O. Hall: Variation of hardness of metals with Currently, he is a PhD student in biomedical engi-
grain size, Nature 173 (1954), pp. 948-949 neering (biomaterial) at the Isfahan University of
Technology, Isfahan, Iran. His further research in-
Bibliography terests cover biomedical engineering, especially
3D bio printing, using ultrasonic in drug delivery
DOI 10.3139/120.110878 and improving surface in biomaterials.
Materials Testing Abolfazl Farzi is a lecturer at Islamic Azad
58 (2016) 5, pages 448-452 University, Esfarayen, Iran. He graduated from
© Carl Hanser Verlag GmbH & Co. KG K. N. Toosi University of Technology, Tehran, Iran,
ISSN 0025-5300 in Civil Engineering using nondestructive tests in
materials. He is a specialist in water engineering
The authors of this contribution and published several papers about water quality
control. Besides that, he is extending his research
Abbas Moghanizadeh, born in 1980, is a re- to environmental issues with the aim of finding
searcher in NDT, modern machinery and biomedi- green solutions for challenging problems in engi-
cal engineering. He has a special interest in the neering.
Abstract
Evaluierung der Auswirkung der Wärmebehandlung auf einen hochle-
gierten austenitischen Stahl AISI 304 mittels Ultraschallschwächungs-
koeffizient. Die Eigenschaften von Metallen können durch verschiedene
Verfahren beträchtlich verändert werden, eines von ihnen stellen Wärme-
behandlungsprozesse dar. Darüber hinaus ist die Ultraschallprüfung ein
bevorzugtes und effektives, zerstörungsfreies Prüfverfahren zur Charakte-
risierung der mechanischen Eigenschaften. Hochlegierte austenitische
Stähle des Typs AISI 304 werden aufgrund ihrer hohen Festigkeit und Kor-
rosionswiderstandes vielfach angewandt. Daher ist es wichtig, die mecha-
nischen Eigenschaften des Stahls AISI 304 zu bestimmen. In der diesem
Beitrag zugrunde liegenden Studie wurde daher das Ultraschallverfahren
(Technik der Schwächungsmessung) angewandt, um die Härte des hochle-
gierten austenitischen Stahls AISI 304, der unterschiedlich wärmebehan-
delt wurde, zu evaluieren. Aufgrund der Wärmebehandlung hat jede Probe
ihre spezifische Mikrostruktur und Härte, die die Ultraschallwellen ent-
sprechend abschwächen. Die Ultraschallversuche und Härtemessungen
zeigen, dass es möglich ist, die Härte des hochlegierten austenitischen
Stahls AISI 304 mittels des Schwächungskoeffizienten zu bestimmen. Zu-
sätzlich wurde das Verhältnis der Ultraschallschwächungskoeffizienten
und der Wärmebehandlungszeit untersucht.
58 (2016) 5