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Iran J Sci Technol Trans Sci
https://doi.org/10.1007/s40995-018-0604-y (0123456789().,-volV)(0123456789().,-volV)

RESEARCH PAPER

Microhardness Characterization of Fe- and Co-Based Superalloys

Ibrahim Karaca1 • Selva Büyükakkas1

Received: 4 August 2017 / Accepted: 27 June 2018

Ó Shiraz University 2018

Abstract
The reverse indentation load-size effects of Fe–Mn–Si and Co–Mn–Si superalloy have been investigated by measuring
Vickers hardness. The characterized superalloy samples are presented in the reverse indentation load-size effects, which is
known as the microhardness increases with increasing applied load behavior. The theoretical model is rearranged and
investigated according to the reverse indentation load-size effects using reconstituted Meyer law, proportional specimen
resistance model, and modified proportional specimen resistance model. The reconstituted modified proportional specimen
resistance model is highly suitable for describing the data of the Fe–Mn–Si and Co–Mn–Si alloys. SEM micrographs show
that Co-based alloys exhibited a dendritic microstructure and Fe-based alloys were presented austenitic microstructure. In
this study, the load range from 0.49 to 9.8 N was applied to the materials, but no crack is observed on the surface of the
material. This can only be attributed to the occurrence of the elastic deformation which yields reverse indentation size
effect in these samples.

Keywords Superalloy  SEM  Microhardness  Reverse indentation size effects (RISE)  Fe–Mn–Si  Co–Mn–Si

1 Introduction metals react to the external load and other properties

The iron, cobalt, or nickel-based alloys, which have been
used in the industrial applications, are called superalloy
(Jovanovich et al. 2007). Their applications compose the
backbone of various materials ranging from space vehicles
to power generation and furnace industries (Emam Islam
et al. 2015; Levitin 2006). Mechanical properties play an
important role for their practical applications and are inti-
mately connected with their structure and other physical
and chemical properties (Kavetskyy et al. 2010). A design
engineer is interested in the behavior of materials under
load, which is mechanical in nature to design of the
engines. The determination of the behavior of the materials
is vitally important to the technological and industrial
applications regarding strength, hardness, toughness, elas-
ticity, plasticity, brittleness, and ductility mechanical
properties. They are used as the measurements of how
& Ibrahim Karaca
i.karaca@ohu.edu.tr
1
Department of Physic, Faculty of Arts and Science, Niğde
Ömer Halisdemir University, 51240 Nigde, Turkey
(Callister and Rethwisch 2009).
In this paper, the reverse indentation load-size effects
(RISE) of Fe–Mn–Si and Co–Mn–Si superalloys have been
investigated by SEM micrographs and through some
reconstituted theoretical hardness models as Meyers, PSR,
and MPSR according to RISE behavior using Vickers
hardness numbers.
2 Theoretical Background
Among the several experimental methods, indentation
hardness testing is commonly used for the investigation of
mechanical properties of materials. The indentation size
effect (ISE) is well known as to be the dependency of the
microhardness H with the applied indentation test load P.
There are two types of ISE: (1) normal ISE and (2) reverse
ISE. In the former case, the measured hardness decreases
with increasing test load, while in the latter case, the
measured hardness increases with an increase in the
applied load (Kavetskyy et al. 2010).

123

2.1 Normal Indentation Size Effect (ISE)
Resistance to permanent deformation, especially deforma-
tion by indentation, is described as hardness. Indentation
hardness is defined as pressure, simply proportional to the
ratio of the indenter size area (Atkinson 1995). The Vickers
microhardness, H, is defined as the ratio of the peak
indentation load, Pmax, for the project area, Ac, of the
hardness impression (Toplu et al. 2015). The Vickers
hardness (HV) may be determined by the following
equation:
 modified proportional specimen resistance (MPSR) model:
Pmax  .   
HV ¼ ¼ 2F sin 136 2 d2 ¼ 1:8544 Pmax d 2 ;
Ac
ð1Þ
where d is the diagonal length of indent. The microhard-
ness definition of solids is proportional to applied inden-
tation test load (P). This is known as the indentation size
effect (ISE) and usually involves a decrease in the apparent
microhardness with increasing applied test load, i.e., with
increasing indentation size (Toplu et al. 2015; Kölemen
et al. 2004). This is usually called ‘normal ISE’. The
occurrence of the different number of phenomena is
attributed to the work hardening during indentation, and
plastic deformation occurs. The indentation elastic recov-
ery, mixed elastic/plastic deformation response to the
material regarding the size of dislocation loops formed
during indentation, strain gradients associated with dislo-
cations, indentation edges acting as plastic hinges, and
indenter friction resistance coupled with the elastic resis-
tance of the specimen (Sangwal 2000).
It was summarized as follows for normal indentation
size effect used in microhardness analyses in some
approaches. A detailed study of microhardness analysis
was given in early works (Toplu et al. 2015; Yilmaz et al.
2013; Dogruer et al. 2013; Kiliçaslan et al. 2013).
According to ISE Meyer’s law defined as
P ¼ adn ; ð2Þ
where a and n are constants. The unitless exponent, n,
Meyer’s number (or index) is the slope of the straight line
that can be obtained when lnP is plotted against lnd and a
(Toplu et al. 2015). The existence of a reverse ISE trend is
that the measured microhardness increases with applied
load. According to ISE, the proportional specimen resis-
tance (PSR) model is an alternative analysis of the behavior
of materials which is based on the following equation:
P ¼ a1 d þ a2 d 2 ; ð3Þ
where a1 and a2 are the experimental constants. Equation 2
can be transformed into
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Iran J Sci Technol Trans Sci
P=d ¼ a1 þ a2 d: ð4Þ
Equation 3 means that according to the proportional
specimen resistance (PSR) model, a1 and a2 are experi-
mental constants and can be evaluated through the linear
regression of P/d versus d. According to the analysis by Li
and Bradt (1996), the parameters a1 and a2 can relate to the
elastic and plastic properties of the test material, respec-
tively. According to ISE, considering the effect of the
machining-induced plastically deformed surface on the
hardness measurement Gong et al. (1999) suggested the
P ¼ a0 þ a1 d þ a2 d 2 ; ð5Þ
where a0, a1, and a2 are experimental constants. Equation 5
is a modified form of the PSR model with the same
physical meaning of the parameters a1 and a2, as the ones
in Eq. 3. The values of a0, a1, and a2 can be evaluated by
plotting the P data against d.
2.2 Reconstituted Hardness Models According
to RISE
An opposite or reverse form of the indentation size effect,
RISE, has also been observed in many studies, called
reverse indentation size effect (RISE) (Güder et al. 2011).
As depicted in Fig. 1, the apparent microhardness increases
with an increase in applied indentation test load. The RISE
phenomenon occurs only in materials in which plastic
deformation is predominant. For metallic materials, it may
originate from the work hardening of the test specimen
during the indentation loading. RISE effect shows that the
material undergoes a relaxation which involves a release of
the indentation stress when it is away from the surface of
the indentation site. This may be because of the crack
formation, dislocation, and/or elastic deformation of the tip
of the indenter.
Fig. 1 Normal and reverse indentation size effect (ISE) forms
Iran J Sci Technol Trans Sci

2.2.1 Reconstituted of Meyer’s Law
The existence of a reverse ISE trend is the observation of
the measured microhardness increasing with applied load.
The exponent, n, in Meyer’s number (or index) has nega-
tive values. Namely, according to the RISE, Meyer’s law in
Eq. 2 can be rewritten as
P ¼ adn ¼ að1=dn Þ; ð6Þ
where a and n are constants. Equation 6 is a modified form
of Meyer’s law with the same physical meaning of the
parameters an as the ones in Eq. 2. It implies that micro-
hardness increases with the increase in the applied inden-
tation test load, because the applied load is balanced by the
total specimen resistance (Li and Bradt 1996). According
to the RISE, a and n experimental constants can be eval-
uated through the linear regression of ln P versus ln(d).
This is obtained from the above-mentioned Eq. 6:
ln P ¼ ln a  n ln d: ð7Þ
The difference of Eq. 7 from Meyer’s law of ISE
behavior is that the n values in each curve have a negative
sign.
2.2.2 Reconstituted Proportional Specimen Resistance
(RPSR) Model
PSR model which is based on Eq. 2 is reconstituted and an
alternative analysis of behavior of materials is observed
and this can be written as follows:
P ¼ a1 =d þ a2 =d2 ; ð8Þ
where a1 and a2 are experimental constants. Equation 8 can
be transformed into
Pd ¼ a1 þ a2 d: ð9Þ
Equation 9 means that according to the proportional
specimen resistance (PSR) model, a1 and a2 are experi-
mental constants. They can be evaluated through the linear
regression of Pd versus 1/d. As stated by Li and Bradt
(1996), the parameter a1 and a2 can relate to the elastic and
plastic properties of the test material, respectively. The
parameter a1 is a measure of the surface effects during
microhardness indentation, which is directly related to the
ISE contribution, while a2 directly related to the load-in-
dependent microhardness value (Machaka et al. 2011).
2.2.3 Reconstituted Modified Proportional Specimen
Resistance (RMPSR) Model
by Gong et al. (1999), we can modify it as RMPSR model
as follows:
P ¼ a0 þ a1 =d þ a2 =d2 ; ð10Þ
where a0, a1, and a2 are experimental constants. The
parameter a0 is a constant related to the residual surface
stresses associated with the surface grinding and polishing
processes during sample preparation (Machaka et al. 2011).
Equation 10 is a modified form of the PSR model with the
same physical meaning of the parameters a1 and a2, as the
ones in Eq. 9. Therefore, a2 denotes the resistance to crack-
free plastic deformation and can be used to estimate the
load-independent hardness when no 1SE is present (when
a1= 0) and based on the indenter profile (Wade et al. 2014).
The values of a0, a1, and a2 can be evaluated by plotting
the P data against 1/d.
3 Materials and Methods
In this study, to prepare superalloy, the high-purity-pow-
dered Fe, Co, Mn, and Si (%99, 99) elements were used.
The percentage of four selected alloys is Fe–40%Mn–
2%Si, Fe–40%Mn–5%Si, Co–40%Mn–2%Si, and Co–
40%Mn–5%Si and their chemical composition is given in
Table 1. These alloys were prepared in high-temperature
induction furnace (25 kVA and 400 kHz AC power
TRUMPF Hüttinger induction generator included vacuum
induction melting furnace) under an argon atmosphere in
quartz tubes. Heat treatment is applied to homogenize the
materials at 1200 °C for 16 h and then quenched thrown
into the water at room temperature (this is well known as
melt quench method). Quenched samples are mechanically
cut exactly the same as the disc shape, 10 mm diameter,
and 3 mm thickness, with a diamond cutter. All samples
are polished to take clear images of scanning and taking
photos through electron microscope optical microscope,
respectively.
Table 1 Chemical composition
Alloy Fe% Mn% Si%
of alloys
Fe–Mn–Si 58 40 2
55 40 5
Co% Mn% Si%

Considering the effect of the machining-induced plastically Co–Mn– 58 40 2

Si 55 40 5
deformed surface on the hardness measurement suggested

123

4 Materials Characterization
The SEM micrograph was taken with using LEO 440
computer-controlled digital model SEM (scanning electron
microscope) at room temperature. One can see in Fig. 2, a
typical SEM micrograph of (a) Co–40%Mn–2%Si, (b) Co–
40%Mn–5%Si. (c) Fe–40%Mn–2%Si, and (d) Fe–
40%Mn–5%Si alloys. Figure 2a exhibits a dendritic
microstructure. With increasing of the Si percentage, so as
to suppressed dendritic growth, the dendritic microstruc-
ture is not clearly observed in Fig. 2b. Notice that the
dominant solidified is made up of columnar dendrites. The
austenite structure is clearly observed in Fig. 2c, d for Fe-
based alloys.
5 Results and Discussion of Microhardness
According to Reverse ISE
5.1 Reconstituted Meyer’s Law
Because of the reconstitute Meyer’s law, as in the ISE
(Toplu et al. 2015), the constants a and n are taken from the
slope of the straight line that can be obtained when lnP is
plotted against lnd, and lna. The existence of a reverse ISE
trend is the measuring of the microhardness increasing as a
result of applied load, as shown in Fig. 3.
The reconstituted Meyer law analysis of samples shows
that sample Co–%40Mn–%2Si has a strongly different
Fig. 2 Typical SEM micrograph of a Co–40%Mn–2%Si, b Co–40%Mn–5%Si, c Fe–40%Mn–2%Si, and d Fe–40%Mn–5%Si alloys
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Iran J Sci Technol Trans Sci
positive value of Meyer constant (n) from the others and
this value is 3.0606. This is to say that the sample obeys to
Meyer law according to Normal ISE, but the others show
the reverse ISE, as shown in Table 2. Therefore, the sam-
ples need to be analyzed through other models.
5.2 Reconstituted Proportional Specimen
Resistance (RPSR) Model
As in the PSR model, according to the reconstituted pro-
portional specimen resistance (RPSR) model, a1 and a2 are
the experimental constants. They can be evaluated through
the linear regression of Pd versus 1/d. According to
reconstituted proportional specimen resistance (RPSR)
model, the difference between samples of Pd and 1/d can
be seen in a) Co–40%Mn–2%Si and b) Co–40%Mn–5%Si,
as shown in Fig. 4. From the results of the analysis pre-
sented in Fig. 4, it may be noted that, as expected for the
reverse ISE, the values of the correction factors of a2 in the
reconstituted proportional specimen resistance (RPSR)
models are negative for the experimental Pd versus 1/
d data. This means that in the case of the reverse ISE, a
specimen undergone a plastic recovery. Besides, the values
of the correction factors of a1 in the RPSR model are
positive. This means that in the case of the reverse ISE, a
specimen is not undergone a plastic recovery, but it depicts
an elastic deformation. Nevertheless, these are not suffi-
cient to thoroughly understand and explain the properties
of samples and we need another model to investigate and
Iran J Sci Technol Trans Sci

Fig. 3 Best-fit analysis (red line) and the difference between lnP and lnd according to the reconstituted Meyer law samples (black dot) a Co–
40%Mn–2%Si, b Co–40%Mn–5%Si, c Fe–40%Mn–2%Si, and d Fe–40%Mn–5%Si

Table 2 Reconstituted Meyer law’s constants of best-fit correlation meaning of the parameters a0, a1, and a2 should be eval-
uated by plotting the linear regression of P versus 1/
Sample ln a n Correlation factor, r2
d. According to the reconstituted modified proportional
Co–40%Mn–2%Si 208.3261 60.4605 0.9967 specimen resistance (RMPSR) model, the P versus 1/
Co–40%Mn–5%Si 95.8516 46.5969 0.9999 d changes of a–d for the samples of Co–40%Mn–2%Si,
Fe–40%Mn–2%Si 244.8260 62.2080 0.9971 Co–40%Mn–5%Si, Fe–40%Mn–2%Si, and Fe–40%Mn–
Fe–40%Mn–5%Si 107.5504 39.9371 0.9844 5%Si are plotted in Fig. 5. According to the RMPSR model
given in Eq. 10, the experimental data are in the fitted
regression line. Constants in Eq. 10 are determined as
understand the sample properties. All of these support the expected for the RMPSR model, but the sample of Fe–
higher negative value of a2 as - 14,251.7320 N/lm2, as 40%Mn–5%Si has a slightly different value of the a0 and
shown in Table 3. The results for the overall best-fit a1 and has an opposite sign than other samples, as shown in
analysis samples showed that the lower R2 0.6222 is a Table 4. However, it does not pose a problem to select the
statistical measure of how close the data are in the fitted best suitable model for the analyses of the samples.
regression line. That is why we cannot use this model to Besides, best-fit samples analysis presents that the higher
choose as a model. R2 of 0.9999 is a statistical measure of how close the data
are in the fitted regression line. As a result, the reconsti-
5.3 Reconstituted Modified Proportional tuted MPSR model can be used for the investigation of
Specimen Resistance (RMPSR) Model these superalloy properties.

PSR model, suggested by Gong et al. (1999), should be

reconstituted according to RISE and the same physical

123
 Iran J Sci Technol Trans Sci

Fig. 4 Best-fit analysis (red line) and the difference between Pd and 1/d according to reconstituted proportional specimen resistance (RPSR)
model (black dot) a Co–40%Mn–2%Si, b Co–40%Mn–5%Si, c Fe–40%Mn–2%Si, and d Fe–40%Mn–5%Si

Table 3 Reconstituted proportional specimen resistance (RPSR) test load shows that the microhardness increases with the
model constants from best-fit correlation for samples Co–%40Mn– increase in applied load, which can be regarded as the
%2Si, Co–%40Mn–%5Si, Fe–%40Mn–%2Si, and Fe–%40Mn–%5Si behavior of the reverse indentation size effect (Sangwal
Samples Constants in equation, P ¼ a1 =d þ a2 =d2 2000). Similar results have been obtained in some works,
where the apparent microhardness increases with the
a1 (N/lm) a2 (N/lm2) r2
increase in applied load, and this is well known as reverse
Co–40%Mn–2%Si 592.6404 - 12,508.5293 ISE observed in b-SiAlON Ceramic (Güder et al. 2011),
Co–40%Mn–5%Si 321.3910 - 3617.4447 0.6222 glasses (Sebastian and Khadar 2005), and single crystals
Fe–40%Mn–2%Si 632.5142 - 14,251.7320 0.6825 (Sangwal and Surowska 2003; Sangwal et al. 2003). The
Fe–40%Mn–5%Si 565.9843 - 10,854.2010 0.7256 reverse ISE can occur not only in the case of plastic
deformation but also energy loss owing to the cracking of
the specimens during indentation. When the same load is
applied to the samples, no cracking is observed even the
5.4 Microhardness Results higher load is applied. However, the only sample of Co–
40%Mn–5%Si has cracks, and the beginning of it is
It can be seen in Fig. 6 that the differences of the Vickers observed in the optical micrograph, as shown in Fig. 6b.
microhardness with the applied indentation test load vary Hardness is the measurement of the indenter influence
from 0.49 to 9.8 N and shown in a) Co–40%Mn–2%Si, b) into the material by different shapes. When the load
Co–40%Mn–5%Si, c) Fe–40%Mn–2%Si, and d) Fe– applied, the resistance of a material occurs to prevent
40%Mn–5%Si. The inset in Fig. 6 depicts an optical indenter deformation. This makes up four components due
micrograph of a typical Vickers indentation which is to: (1) friction at the indenter; (2) elastic deformation; (3)
obtained through maximum test load impression (9.8 N). plastic deformation; and (4) specimen cracking. According
The change of microhardness versus applied indentation to Li and Bradt (1996), referenced the reverse ISE,

123
Iran J Sci Technol Trans Sci

Fig. 5 Best-fit analysis (red line) and the difference between P and 1/d according to reconstituted modified proportional specimen resistance
(RMPSR) model (black dot) a Co–40%Mn–2%Si, b Co–40%Mn–5%Si, c Fe–40%Mn–2%Si, and d Fe–40%Mn–5%Si

Table 4 Reconstituted modified proportional specimen resistance Only the sample of Co–40%Mn–5%Si shows the beginning
(RMPSR) model constants of best-fit correlation for samples of Co– of cracks in higher test load application.
%40Mn–%2Si, Co–%40Mn–%5Si, Fe–%40Mn–%2Si, and Fe– The ISE and reverse ISE behavior are investigated and
%40Mn–%5Si
modeled with different materials and models. Sangwal
Samples Constants in equation, P ¼ a0 þ a1 =d þ a2 =d 2 et al. (2002) were reported the experimental data on the
a0 (N) a1 (N/lm) a2 (N/lm2) r2 microhardness of some cobalt-based alloys determined by
Vickers pyramidal indenters fitted to a Neophot-2 micro-
Co–40%Mn–2%Si 0.6516 - 0.1229 0.0059 scope and a PMT-3 hardness tester, and to critically
Co–40%Mn–5%Si 0.6771 - 0.1300 0.0116 0.9999 examine the ISE phenomenon from the standpoint of var-
Fe–40%Mn–2%Si 1.2542 - 0.1359 0.0050 0.9998 ious approaches and models proposed in the literature. In
Fe–40%Mn–5%Si - 1.5042 0.0457 0.0038 0.9999 the case of Co-based alloys, Hanemann tests give normal
ISE, while PMT-3 hardness tester shows reverse ISE. A
survey of the conclusion derived from these works shows
that none of the models can be accepted as the best to
frictional and elastic effects lead to the normal ISE, while describe the ISE in different crystals. They were reported
indentation cracking contributes to the reverse ISE. In the in the next year that in the range of high indentation loads,
case of indentation cracking, the apparent hardness is the microhardness of cobalt-based alloys, as determined
measured by a Vickers diamond indenter (Li and Bradt using the proportional specimen resistance model, is
1996; Sebastian and Khadar 2005). In this study, although practically independent of the applied load. The
the test load ranges from 0.49 to 9.8 N, no crack on the microstructures and mechanical properties CoCrMo alloys
surface of the material is observed. This is because the only consisting of 1.68–4.33%Pd were studied via Knoop
elastic deformation yields to reverse ISE in these samples. indentation hardness tests, by Sahin et al. (2015). They

123

Fig. 6 Variation of the Vickers microhardness with the applied indentation test load a Co–40%Mn–2%Si, b Co–40%Mn–5%Si, c Fe–40%Mn–
2%Si, and d Fe–40%Mn–5%Si. The inset in Fig. 5 depicts an optical micrograph of a typical Vickers indentation image, 9.8 N load
were observed load dependence behavior and it was
rationalized using the Hays–Kendall model. Load-inde-
pendent Knoop hardness values are 5.153, 4.882, and 4.637
GPa for 1.68Pd, 2.70Pd, and 4.33Pd, respectively. As a
result, they have reported that the resultant load-indepen-
dent hardness decreases with the increase of palladium
ratios. Bekteş et al. (2004) were investigated that the
microhardness of Fe–Mn binary alloys with different
compositions using a Vickers microhardness tester and
their results were used to analyze by the classical Meyer’s
law and proportional specimen resistance model the
microhardness behavior. They were determined that the
ISE behavior is best described by Meyer’ law and the PSR
model of Li and Bradt. It was found that the Fe–Mn binary
alloys become harder with increasing Mn composition and
this can be attributed to solid-solution hardening. Budiarsa
(2013) was used in the ISE study where carbon steel with
carbon content 0.10%C, 0.54%C, and 0.85%C. The ISE
data were analyzed by fitting data following the Meyer
power law and the proportional specimen resistance (PSR)
models. The results show that the ISE data correlated well
with Meyer’s power law and the PSR models.
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Iran J Sci Technol Trans Sci
As a result of the above-mentioned applications, reverse
ISE may be observed in the same material, depending on
the material composition, producing methods and proper-
ties. However, this phenomenon remains to be poorly
understood and seen in superalloy. Therefore, various
materials need to be investigated.
6 Conclusion
The Fe–40%Mn–2%Si, Fe–40%Mn–5%Si, Co–40%Mn–
2%Si, and Co–40%Mn–5%Si superalloys were made up by
melting quench method. Their reverse ISE behavior is
investigated with the reconstituted Meyer law, PSR, and
modified PSR models. The most suitable model was
determined as the reconstituted MPSR model concerning
the experiment results and regression analyses. The results
showed that the occurrence of the elastic deformation
yields to reverse ISE in these samples. Only the sample of
Co–40%Mn–5%Si shows the beginning of cracks in the
case of higher test load. However, this phenomenon
remains poorly understood and seen in superalloy.
Iran J Sci Technol Trans Sci
As a result, the presented work results as given above
have been obtained to useful data for technological appli-
cation with Fe- and Co-based superalloys. Beside of this
work, indeed, Fe and Co-based superalloys are needed to
investigate another property of these alloys in the next.
Therefore, various materials need to be investigated using
the theoretical models.
The presented work results are good agreement of the
using a Vickers microhardness tester with Sangwal et al.
(2002), Sahin et al. (2015) and Bekteş et al. (2004).
Because they were investigated the ISE and analyzed with
the Meyer power law, the proportional specimen resistance
(PSR) models and the modified proportional specimen
resistance (PSR), and others model, as we done.
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