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Effect of quenching and tempering on microstructure and mechanical

properties of 410 and 410 Ni martensitic stainless steels

Article in Journal of Materials Research · January 2017

DOI: 10.1557/jmr.2016.485

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 ARTICLES

Effect of quenching and tempering on microstructure and

mechanical properties of 410 and 410 Ni martensitic stainless steels
Masoud Mirzaeea)
Department of Materials, Mashhad Branch, Islamic Azad University, Mashhad 9187147578, Iran
Amir Momeni and Niloofar Aieni
Materials Science and Engineering Department, Hamedan University of Technology, Hamedan 6516913733, Iran
Hamid Keshmiri
Esfarayen Steel Complex, Esfarayen 1589673711, Iran

(Received 5 August 2016; accepted 28 November 2016)

In this research, the effect of austenitizing at 900–1100 °C and tempering at 250–650 °C on the
microstructure and mechanical properties of 410 and 410 Ni martensitic stainless steels was
investigated. The transformation of austenite to ferrite surrounded the austenitizing within the
temperature range of 900–1050 °C. The grain size and hardness measurements proved that
austenitizing at 1050 °C leads to the partial dissolution of carbides without a considerable growth
of austenite grains. The mechanical tests showed two peaks in strength and troughs in ductility by
tempering at 450 and 650 °C due to the formation of primary and secondary carbides. The better
ductility and fracture toughness in 410 Ni, comparing to 410, were attributed to the effect of Ni
on stacking fault energy. Fractured surfaces revealed ductile fracture of the samples tempered at
low temperatures, e.g., 250 °C. However, after tempering at 450 and 650 °C, 410 showed a brittle
fracture and 410 Ni exhibited a dual intergranular-brittle fracture mechanism.

I. INTRODUCTION austenitizing temperature should be high enough to

Heat treatment is a crucial step in the processing route
of different types of steels. The precise control of heat
treatment can improve the mechanical properties and
microstructure. Generally speaking, heat treatable steels
are those which have tendency for the martensitic trans-
formation through quenching of austenite. The martensitic
stainless steels (MSSs) are a major group of high-alloy
heat treatable steels which provide high strengths and good
corrosion resistance for some industrial applications such
as steam turbine blades, valves, shafts, screws, and plastic
molds.1,2 Their successful performance necessitates a good
combination of strength and ductility which is acquired by
a precise control of heat treatment. The heat treatment for
MSSs includes austenitization, quenching, and tempering.
While austenitization-quenching leads to a hard martens-
itic structure with low ductility, tempering restores ductil-
ity at the expense of hardness and provides a desired
combination of hardness and ductility. Therefore, a sort of
parameters in austenitization-quenching and tempering
steps affects the mechanical properties.3,4
The formation of a single-phase austenitic structure
and the dissolution of carbides and other phases are the
major aims of austenitizing. For this purpose, the
Contributing Editor: Jürgen Eckert
a)
Address all correspondence to this author.
e-mail: masoud.mirzaee98@gmail.com
DOI: 10.1557/jmr.2016.485
dissolve all carbides into austenite.5 On the other hand,
chromium carbides which are often present in MSSs
control the grain growth and participate in the formation
of finer austenite structure before quenching.6 The finer
austenite grain size which is obtained at lower austeni-
tization temperatures leads to the finer martensite units or
packets which provide higher strength and toughness.7,8
Such opposite effects of austenitization temperature has
been a challenge for the proper design of heat treatment
for MSSs.9 In addition, some other parameters such as
quenching rate have been found influential on the
structure and mechanical properties of as-quenched
martensite.2
As mentioned, tempering is the second step of heat
treatment in MMSs which is designed to provide a desired
combination of toughness and strength.10 The recovery of
dislocations and exit of supersaturated carbon leads to the
partial transformation of martensite into ferrite which
imparts lower strength and higher toughness to the
tempered MSS.11 However, there are several investiga-
tions showing that some tempering regimes increase
hardness and degrade fracture toughness.12,13 Such
anomalous behavior, termed as embrittlement or second-
ary hardening, has been attributed to the precipitation of
new carbides.13–15 It is manifest that the extent
of secondary hardening depends on the dissolution of
primary carbides through austenitization.16 The undesired
regimes of embrittlement should be determined and

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 M. Mirzaee et al.: Effect of quenching and tempering on microstructure and mechanical properties
avoided in the processing route of MSSs. This is because
the formation of secondary carbides not only decreases
the fracture toughness, but also degrades the corrosion
resistance of MSSs by depleting Cr from the matrix.17–20
In current research, the influence of austenitizing
treatment on the mechanical properties of as-quenched
martensite in AISI 410 and Ni-bearing 410 (often called
AISI 414) MSSs has been investigated and related to the
dissolution of carbides. In the next step, the effect of
tempering on the strength and toughness was investigated
and the regimes of secondary hardening were related to
the carbides precipitation in the steels.
II. MATERIALS AND METHODS
The chemical composition of AISI 410 and Ni-bearing
410 MSSs, which are called 410 and 410 Ni later on, are
given in Table I. The samples of both steels with nearly
identical grain size (Fig. 1) and hardness were austenitized
at 900, 980, 1010, 1050, and 1100 °C for 1 h and then
quenched in water to the ambient temperature. The as-
quenched specimens were then prepared by the standard
metallographic techniques and etched in the Villella’s
reagent (1 g picric acid, 5 mL HCl, 100 mL ethanol) to
reveal the prior austenite grain boundaries. The Clemex
software was used to determine the average grain size of
prior austenite in the heat treated samples. The micro-
structures were characterized by the optical microscopy and
the average grain size of the samples was determined based
on the ASTM E112. To follow the influence of austenitizing
on the dissolution of carbides, Rockwell C hardness testing
and X-ray diffraction (XRD) measurements were performed
on the as-quenched samples. Based on the grain size
measurements, hardness testing and XRD results the best
temperature for austenitizing was determined as 1050 °C.
TABLE I. Chemical composition of MSSs used in this investigation.
Element composition C Cr Ni Mo
410 0.11 12.50 0.08 0.27
410 Ni 0.12 12.48 1.01 0.25
FIG. 1. Starting microstructures of the studied alloys: (a) 410 and (b) 410 Ni.
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For the second step of heat treatment, the samples of
both steels were austenitized at 1050 °C and then
tempered for 2 h in temperature range of 250–650 °C
with the interval of 50 °C. Figure 2 exhibits the schematic
representation of the thermal cycles adopted for the first
and second steps of heat treatment in this investigation.
The mechanical properties of the tempered samples were
evaluated by tensile testing (according to ASTM E8M)
with the cross-head speed of 1 mm/min and impact tests
(according to ASTM E23) at
18 °C. Field emission
scanning electron microscope (FESEM; model TSCAN,
Carl Zeiss AG, Jena, Germany) was used to characterize
the microstructures and fracture surface of the tensile test
samples.
III. RESULTS AND DISCUSSION
A. Effect of austenitizing temperature on
as-quenched microstructure and hardness
Figures 3 and 4 show the prior austenite grain structure
in the samples after austenitization at various temperatures
and quench in water. Most of the micrographs show
a martensitic structure in which the prior austenite grain
boundaries have been partly revealed by the Vilella’s
reagent. However, the both steels show a light phase
network along the prior austenite grain boundaries after
austenitizing at 900 °C. Since d-ferrite is often observed as
discrete islands in MSSs,21,22 the light phase which has
decorated the prior austenite grain boundaries in Figs. 3(a)
and 4(a) seems to be the untransformed martensite which
has been tempered at the studied temperature. The plate-
like morphology of this phase supports this idea. The
microhardness values of 276 and 475 HV for the light and
dark phases confirmed that the lighter phase has been
tempered at the austenitization temperature.
Si Mn P S Nb Fe
0.05 0.47 0.025 0.007 0.015 Rem.
0.04 0.46 0.025 0.005 0.015 Rem.
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 M. Mirzaee et al.: Effect of quenching and tempering on microstructure and mechanical properties

FIG. 2. Schematic representation of the heat treatment steps applied on the samples: (a) austenitization and (b) tempering.

FIG. 3. Prior austenite grain structure in 410 MSS after austenitization at various temperatures of (a) 900 °C, (b) 980 °C, (c) 1010 °C, (d) 1050 °C,
and (e) 1100 °C and quenching in water.

The previous investigations have declared that dual- toughness of MSSs by facilitating the cracks formation
phase microstructures in DSSs such as the coexistence of and propagation along the matrix/d-ferrite interfaces.21,22
d-ferrite with austenite are deleterious for the fracture It has been understood that d-ferrite promotes the

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 M. Mirzaee et al.: Effect of quenching and tempering on microstructure and mechanical properties

FIG. 4. Prior austenite grain structure in 410 Ni MSS after austenitization at various temperatures of (a) 900 °C, (b) 980 °C, (c) 1010 °C,
(d) 1050 °C, and (e) 1100 °C and quenching in water.

nucleation and coalescence of microvoids and facilitates
fracture even at high temperatures.23,24 It seems that
austenitization at higher temperatures, i.e., over 900 °C,
should be preferred due to the formation of a uniform
martensitic structure in the as-quenched material. Figure 5
presents the phase diagrams of the steels calculated by the
Thermocalc software. It is observed that d-ferrite, aus-
tenite, M23C6, and M7C3 carbides are the constituent
phases of in the austenitization temperature range. It is
also worthy to note that the addition of 1 wt% Ni has no
considerable effect on the phase regions (Fig. 5) or the
microstructural evolutions through austenitization (Figs. 3
and 4). Figure 5 also shows that the maximum temper-
ature for austenitization is about 1100 °C; because at
temperatures beyond 1100 °C microstructure consisted of
d-ferrite and carbides. It is also worthy to note that the
complete dissolution of carbides in both the steels needs
heating up to temperatures well above 1100 °C where the
microstructure becomes fully ferritic. Therefore, the
austenitizing within the adopted temperature range would
reduce the amount of carbides by dissolving them into
austenite. On the other hand, although increasing the
austenitizing temperature leads to the better dissolution of
carbides in the matrix, it would also accelerate the growth
of austenite grains, which is undesirable. For this
purpose, the variations of austenite grain size and
hardness with the austenitization temperature were de-
termined as shown in Figs. 6 and 7. It is observed that
austenitization in range of 900–1050 °C does not
considerably change the prior austenite grain size. This
implies that the carbides could effectively inhibit the
austenite grain growth up to 1050 °C. According to the
phase diagrams in Fig. 5, by heating the steels above
1050 °C, austenite and M23C6 carbides transform to
d-ferrite and M7C3 and finally to d-ferrite, through the
following steps:

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 M. Mirzaee et al.: Effect of quenching and tempering on microstructure and mechanical properties
FIG. 5. Equilibrium phase diagram for the alloys 410 and 410 Ni
calculated by Thermocalc software.
FIG. 6. Prior austenite grain size with temperature.
1070 8C 1080; 8C
d þ c þ M23 C6
! d þ M23 C6
! d
1100; 8C
þ M7 C3
! d
By disintegrating austenite more Cr and C are dis-
solved into d-ferrite and diffuse toward the M23C6
carbide particles. This in turn accelerates the particles
coarsening at temperatures higher than 1050 °C and
decreases their pinning effect on the boundaries. As
a conclusion, there is an interrelation between trans-
formation of austenite to d-ferrite, average grain size and
carbides evolution. The hardness measurements in Fig. 7
show that by austenitizing at temperatures beyond
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FIG. 7. Hardness measurement of quenched specimens after
austenitization.
1050 °C hardness drops due to the fast coarsening of
grains and carbide particles. It is also worthy of attention
that the existence of 1 wt% Ni in 410 Ni cannot
compensate its lower hardness due to the lager grain size
comparing to 410.
XRD measurements of the samples austenitized at
1010, 1050, and 1100 °C in Fig. 8 shows that the amount
of carbides decrease with increasing temperature. It is
also observed that the peak intensities are relatively larger
for 410 Ni. This can be attributed to the effect of Ni on
decreasing the solubility of Cr in the matrix. In other
words, Ni forces Cr to more take part in the formation of
carbides instead of being soluble in the matrix. Therefore,
it is manifest that the amount of carbides in 410 Ni should
be slightly higher than 410. The increase in the intensity
of the peaks pertaining to Cr7C3 and the decrease in those
of Cr23C6 with increasing temperature are in agreement
with the previous results. However, the appearance of
Cr23C6 peaks in the spectrums of 410 Ni is referred to the
effect of Ni on postponing the transformation of austenite
to d-ferrite.
B. Effect of tempering temperature on
microstructure, mechanical properties, and
fracture behavior
ð1Þ
After austenitization and quenching, the steels possess
high strength and low ductility. Tempering is a comple-
mentary heat treatment which often aims at reaching
a desirable combination of hardness and ductility.25 To
study the tempering behavior of the steels 410 and 410
Ni, the samples were austenitized at 1050 °C and then
tempered in temperature range of 250–650 °C.
Figure 9 shows the variations of hardness and elonga-
tion of the specimens tempered at different temperatures.
The continual decrease in hardness and corresponding
increase in elongation imply that the ductility of both
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 M. Mirzaee et al.: Effect of quenching and tempering on microstructure and mechanical properties

FIG. 8. XRD patterns of carbides present in 410 Ni (a, c, and e) and 410 (b, d, and f) after austenitization at (a, b) 1010 °C, (c, d) 1050 °C and (e, f) 1100 °C.

FIG. 9. Variation of hardness and elongation with tempering temperature.

steels improves at the expense of strength. The same
results are inferred from the variations of ultimate tensile
strength (UTS) and Charpy impact energy in Fig. 10. By
tempering at low temperatures, dislocations formed
during the displacive transformation of austenite to
martensite are annihilated by recovery. This, in turn,
alleviates the internal residual stress in martensite and
FIG. 10. Variation of UTS and Charpy impact energy with tempering
temperature.
decreases hardness. At higher temperatures, the recovery
is accelerated and proceeds with diffusing carbon out of
the martensite layers.26 While the carbon atoms make
clusters of carbide particles inside or outside the layers,
martensite gradually turns into ferrite. Therefore, except

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 M. Mirzaee et al.: Effect of quenching and tempering on microstructure and mechanical properties

for the temperatures corresponding to the formation of

carbides, the continual decrease in the hardness continues
until a ferritic matrix is formed.26
It is evident that the existence of Ni has improved the
ductility and toughness of 410 Ni, comparing to 410.
Therefore, the assignment of 410 Ni can be helpful for
industrial parts which need high strength as well as
acceptable fracture toughness. The improvement of
ductility and toughness by adding Ni can be attributed
to increase in the stacking fault energy (SFE) of the steel.
As Ni is a high SFE metal,27 it increases the SFE value of
410 and therefore facilitates the dislocation glide. The
variation of mechanical properties with tempering tem-
perature in Figs. 9 and 10 introduce two critical temper-
atures at the inflection points of the curves. The results of
hardness measurement in Fig. 9 indicate that the strength
of both materials increase by tempering at 450 and
550 °C; Whereas, tempering at other temperatures leads
to the abrupt decrease in strength. Tempering at these
temperatures is accompanied by a similar increase in
UTS and decrease in ductility and fracture toughness.
These changes may be associated with the secondary
precipitation of chromium carbides as reported in the
literature.28–31 As mentioned in the previous section,
austenitizing at 1050 °C effectively decrease the volume
fraction of pre-existing carbides by dissolving them into
the austenitic matrix. Therefore, the austenite at high
temperatures is enriched in alloying elements and more
withstand against the displacive martensitic transforma-
tion. This in turn depresses the martensite start temper-
ature, Ms, leading to more remained austenite after
quenching. During tempering at low temperatures, the
remained austenite decomposes to a mixture of ferrite
and cementite.26 As this mixture is harder than austenite,
the hardness and UTS increase and ductility and
toughness adversely decrease. It has been observed that
the decomposition of retained austenite and the diffu-
sion of supersaturated carbon out of martensite simple
carbides propel the formation of some simple carbides
of types M2C or M3C which increase hardness and
degrade ductility.26 Therefore, the restoration of hard-
ness and UTS and degradation of ductility and tough-
ness in samples tempered at about 450 °C can be
attributed to the decomposition of austenite and forma-
FIG. 11. FESEM images of the samples of 410 (a, c, e, and g) and
tion of primary carbides in both steels. By tempering at 410 Ni (b, d, f, and h), tempered at (a, b) 450 °C, (c, d) 550 °C, (e, f)
higher temperatures the primary carbides are dissolved, 650 °C, and (g, h) magnified views of e and f.
leading to the amelioration of impact and elongation
properties32 and new more stable and more complex
carbides of M7C3 or M23C6 are formed and increase However, based on the discussion of Figs. 9 and 10 some
hardness to the second peak, which is observed around very small primary carbides (d , 50 nm) would be
550 °C. responsible for the increase in strength and decrease in
Figure 11 shows the FESEM images of the carbides ductility and toughness. Figures 11(c) and 11(d) show
formed during tempering at different temperatures. two sets of carbide particles with different sizes in both
Figures 11(a) and 11(b) show that tempering at 450 °C steels. The fine precipitates (d , 50 nm) which are
does not lead to the formation of large carbide particles. observed within the martensite layer are the primary

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 M. Mirzaee et al.: Effect of quenching and tempering on microstructure and mechanical properties

carbides and the larger ones which are observed between
the martensite layers are the secondary carbides. During
tempering at low temperatures, i.e., below 450 °C,
trapped carbon atoms take the opportunity to get out of
martensite structure and form some clusters of primary
carbides within the martensite layers.26 By tempering at
higher temperatures, i.e., 550 and 650 °C, such clusters
are dissolved and the more stable carbide particles pre-
cipitate at the interface of the martensitic layers. The
comparison of Figs. 11(e) and 11(f) reveals that the
secondary carbides have occupied the interfaces of
the martensitic layers. Chakraborty and his coworkers
showed that the small carbides particles which are formed
at low temperature tempering (around 450 °C) are of type
M2C (M is a participation of all carbide forming
elements).15 They also found that Fe has a greater role
than other alloying elements in such carbides. It was
found that by increasing the tempering temperature the
primary carbides are replaced with new carbides of
M23C6 which are richer in Cr.15

FIG. 12. SEM images from the fractured surfaces of 410 (a, c, and e) and 410 Ni (b, d, and f) tempered at (a, b) 250 °C, (c, d) 450 °C, and (e, f) 650 °C.

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 M. Mirzaee et al.: Effect of quenching and tempering on microstructure and mechanical properties
In agreement with the XRD results in Fig. 8, Fig. 11
also shows that 410 Ni has larger particles than 410. As
discussed, Ni reduces the dissolution of Cr in the matrix
and feed carbides with more Cr and C atoms. Figures 11
(g) and 11(h) show the magnified view of primary and
secondary carbides in the studied steels. More primary
carbides within the martensite layers in 410 [Fig. 11(g)],
comparing to 410 Ni [Fig. 11(h)] indicates that the rate of
tempering in 410 Ni is faster than 410.
The typical SEM images from the fractured surfaces of
the tensile samples are shown in Fig. 12. The micro-
graphs of Figs. 12(a) and 12(b) clearly show large
dimples on the fracture surfaces of samples tempered at
250 °C. In agreement with the results of Figs. 9 and 10,
these observations indicate that both steels bear ductile
fracture after tempering at low temperatures. For the
samples tempered at 450 °C, Figs. 12(c) and 12(d) show
that different mechanisms should be prevailing. While
Fig. 12(c) shows a brittle fracture with cleavage charac-
teristics for 410, Fig. 12(d) indicates that intergranular
fracture is the dominant fracture mechanism for 410 Ni.
Based on this observation, the better ductility and
toughness of 410 Ni, reported in Figs. 9 and 10, can be
attributed to the plastic deformation which occurs during
the intergranular fracture. It is clear that the intergranular
fracture in 410 Ni is related to the existence of Ni. The
previous investigations have shown that the intergranular
fracture occurs when the grain boundary is weakened by
the segregation of detrimental elements such as S or P.33
There are some reports that S tends to segregate to grain
boundaries in Ni-based or Ni-bearing alloys.34–36 In
addition, the presence of S has been found responsible
for grain boundary weakening in some Ni-containing
alloys.37,38 It is interesting to note that Ni has the highest
grain boundary energy (cgb) among FCC metals such as
Ag, Al, Au, and Cu.39 Besides, Najafabadi et al.40
suggested that the segregation of Ni atoms to the grain
boundaries increase cgb in Ni–Al alloys. Consequently, it
can be proposed that higher cgb in 410 Ni increases the
propensity for the segregation of S to the grain bound-
aries, giving rise to grain boundary weakening and
decohesion in tension.
Figures 12(d) and 12(e) represent the fracture surfaces
of the samples tempered at 650 °C. It is obvious that 410
has broken with a brittle mechanism which is attributed to
the existence of secondary carbides. However, the mi-
crograph of 410 Ni shows a dual mechanism of cleavage-
intergranular fracture as arrowed in Fig. 12(e). As shown
in Fig. 11, tempering at 650 °C leads to the formation of
secondary carbides which increase the tendency for
cleavage fracture. However, the segregation of S to the
prior austenite grain boundaries increases by increasing
the tempering temperature. This in turn leads to a com-
petition between the crystalline and grain boundary
routes of cracking in 410 Ni.
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IV. CONCLUSIONS
In this research, the effect of austenitization and
tempering on the microstructure and mechanical proper-
ties of 410 and 410 Ni MSSs was investigated. The major
results are summarized as follows:
(1) In both steels, austenitization at 900 °C leads to
remaining a tempered martensite network on the prior
austenite grain boundaries.
(2) At temperatures over 1050 °C, austenite gradually
transforms to d-ferrite.
(3) The grain size and hardness measurements showed
that austenitization at 1050 °C leads to the partial
dissolution of carbides without a considerable growth
of austenite grains. However, austenitization at temper-
atures beyond 1050 °C resulted in a dramatic drop in
hardness due to fast grain growth.
(4) The mechanical tests (tensile, hardness, and im-
pact) showed that tempering at 450 and 650 °C leads to
increase in strength and decrease in ductility and tough-
ness due to the formation of primary and secondary
carbides. The ductility and fracture toughness were better
for 410 Ni comparing to 410.
(5) The fractured surfaces showed that both steels tend
to ductile fracture after tempering at low temperatures. At
high tempering temperatures, however, 410 showed
a brittle fracture; 410 Ni exhibited a dual intergranular-
brittle fracture mechanism.
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