See

discussions, stats, and author profiles for this publication at: https://www.researchgate.net/publication/269577237

Study on tempering behaviour of AISI 410

stainless steel
Article in Materials Characterization February 2015
DOI: 10.1016/j.matchar.2014.12.015

CITATIONS

READS

495

7 authors, including:
Gopa Chakraborty

Shaju K Albert

Indira Gandhi Centre for Atomic Research

Indira Gandhi Centre for Atomic Research

12 PUBLICATIONS 35 CITATIONS

186 PUBLICATIONS 993 CITATIONS

SEE PROFILE

SEE PROFILE

Thomas Paul

Arup Dasgupta

Indira Gandhi Centre for Atomic Research

Indira Gandhi Centre for Atomic Research

45 PUBLICATIONS 243 CITATIONS

93 PUBLICATIONS 653 CITATIONS

SEE PROFILE

All in-text references underlined in blue are linked to publications on ResearchGate,

letting you access and read them immediately.

SEE PROFILE

Available from: Thomas Paul

Retrieved on: 30 August 2016

Materials Characterization 100 (2015) 8187

Contents lists available at ScienceDirect

Materials Characterization
journal homepage: www.elsevier.com/locate/matchar

Study on tempering behaviour of AISI 410 stainless steel

Gopa Chakraborty a,, C.R. Das a, S.K. Albert a, A.K. Bhaduri a, V. Thomas Paul a,
G. Panneerselvam b, Arup Dasgupta a
a
b

Metallurgy & Materials Group, Indira Gandhi Center for Atomic Research, Kalpakkam 603102, India
Chemistry Group, Indira Gandhi Center for Atomic Research, Kalpakkam 603102, India

a r t i c l e

i n f o

Article history:
Received 4 June 2014
Received in revised form 12 December 2014
Accepted 13 December 2014
Available online 15 December 2014
Keywords:
Martensite
Tempering
Embrittlement
Carbide
XRD
TEM

a b s t r a c t
Martensitic stainless steels nd extensive applications due to their optimum combination of strength, hardness
and wear-resistance in tempered condition. However, this class of steels is susceptible to embrittlement during
tempering if it is carried out in a specic temperature range resulting in signicant reduction in toughness. Embrittlement of as-normalised AISI 410 martensitic stainless steel, subjected to tempering treatment in the temperature range of 673923 K was studied using Charpy impact tests followed by metallurgical investigations
using eld emission scanning electron and transmission electron microscopes. Carbides precipitated during tempering were extracted by electrochemical dissolution of the matrix and identied by X-ray diffraction. Studies indicated that temper embrittlement is highest when the steel is tempered at 823 K. Mostly iron rich carbides are
present in the steel subjected to tempering at low temperatures of around 723 K, whereas chromium rich carbides (M23C6) dominate precipitation at high temperature tempering. The range 773823 K is the transition temperature range for the precipitates, with both Fe2C and M23C6 types of carbides coexisting in the material. The
nucleation of Fe2C within the martensite lath, during low temperature tempering, has a denite role in the embrittlement of this steel. Embrittlement is not observed at high temperature tempering because of precipitation of
M23C6 carbides, instead of Fe2C, preferentially along the lath and prior austenite boundaries. Segregation of S and
P, which is widely reported as one of the causes for temper embrittlement, could not be detected in the material
even through Auger electron spectroscopy studies.
2014 Elsevier Inc. All rights reserved.

1. Introduction
Martensitic stainless steels (SS) nd extensive application in steam
turbine blades, marine turbine blades, compressor blades etc. due to optimum combination of strength, hardness, and wear and corrosion resistance [1,2]. To achieve the desired microstructure and mechanical
properties, martensitic SS in the as normalised condition is subjected
to an appropriate tempering heat treatment. However, for a given duration of tempering, a continuous decrease in hardness with increase in
tempering temperature often does not take place due to the complex
nature of the tempering behaviour. Instead, in certain alloy steels secondary hardening is observed during the tempering heat treatment. Signicant reduction in impact toughness with fracture mode changing
from ductile to intergranular is also observed, which is referred as temper embrittlement.
There is a difference in opinion in the published literature on the
cause of temper embrittlement in this class of steels. Some researchers
have identied the main cause for this embrittlement as secondary
hardening due to heterogeneous carbide precipitation [3,4] whereas
others have pointed out that segregation of impurities like P and Sb at
Corresponding author.
E-mail address: gopa_mjs@igcar.gov.in (G. Chakraborty).

http://dx.doi.org/10.1016/j.matchar.2014.12.015
1044-5803/ 2014 Elsevier Inc. All rights reserved.

prior austenite grain boundaries during tempering heat treatment is

mainly responsible [5,6]. It is reported that for 16Cr2Ni martensitic
SS that temper embrittlement is caused by secondary hardening due
to precipitation of Cr7C3 and Cr2C carbides which takes place at temperature range close to 973 K [7]. No impurity segregation could be detected for this material although the steel contains more than 0.01 wt.% P.
Lim et al. [2] indicated secondary hardening to be the sole cause for temper embrittlement of AISI 403 martensitic SS with 0.01 wt.% P. For 410
SS, it is reported that tempering in the range of 623923 K produces a
change from M3C type carbide to M7C3 and M23C6 type carbides accompanied by a secondary hardening and notable loss of notch impact
toughness [8].
However, many other studies on temper embrittlement have identied impurity segregation at grain boundary during tempering heat
treatment as major cause of temper embrittlement. P segregation
could be successfully detected by Auger electron spectroscopy (AES)
in freshly fractured samples of steels that have undergone temper embrittlement [1,6,9]. Tsay [1] indicated P as the primary residual impurity
responsible for temper embrittlement of 403 SS with 0.01 wt.% P. Similarly, P segregation was found to be the primary cause for embrittlement of 12%Cr martensitic SS containing 0.016 wt.% P [6]. Studies
also indicated that P can co-segregate with Cr at the grain boundaries
[10,11]. It has been documented that Mn and Si promotes P segregation,

82

G. Chakraborty et al. / Materials Characterization 100 (2015) 8187

whereas Mo, if not bound as carbide is benecial in scavenging P and

other embrittling impurities [12,13].
For prototype fast breeder reactor (PFBR), in advanced stage of construction in India, AISI 410 SS is chosen as the material for sprocket used
in the fuel handling machine in which a chain and pulley mechanism is
used to transfer the fuel into as well as from the reactor core. Sprocket is
machined from a bar of 950 mm and 200 mm thick and in order to
achieve the specied hardness of 29 RC for this material, it is subjected
to a normalising and tempering treatment in the semi-nished condition. The tempering temperature chosen for this heat treatment by the
fabricator was 838 K and cracks developed in the sprocket material
after this heat treatment. This incident was the reason for undertaking
a systematic study on the tempering behaviour and embrittlement issues of AISI 410 SS with an objective of identifying a suitable heat treatment for the sprocket material in order to achieve desired properties
without the risk of cracking during heat treatment and subsequent service. This paper presents the results of this study and also brings out the
role of different carbides formed during tempering in embrittlement of
this steel.

In order to identify the various precipitates formed during tempering at 723, 823 and 923 K, X-ray diffraction (XRD) analysis was carried
out with Cu K-alpha radiation source at 2/min scan speed on precipitates extracted by dissolving the matrix from the corresponding
specimens. The dissolution of the matrix and extraction of the precipitates were carried out electrochemically using a solution containing
10 vol.% of hydrochloric acid in methanol with specimen as anode and
platinum electrode as cathode maintained at a potential difference of
1.5 V. Specimens were polished up to 600 grit emery paper and dissolution was carried out for 24 h before extracting the precipitates. Filter
paper of pore size 0.1 m was used for vacuum ltration of the solution
and the precipitates collected over lter paper was transferred on glass
slide for XRD analysis.
An attempt was also made to identify possible segregation of the impurity elements like S and P by measuring their concentration at the
grain boundaries of specimens tempered at 723, 823 and 923 K using
Auger Electron Spectroscopy (AES). These studies were performed at
the freshly fractured surfaces of the impact tested specimens as well
as after sputtering the surface with Ar+ for 3 min and Differential
Auger spectra were recorded.

2. Materials & methodology

3. Results
In the present study, AISI 410 SS (chemical composition as determined by optical emission spectrometer is listed in Table 1) plate of
dimensions 500 250 12 mm3 was normalised at 1253 K. For normalising heat treatment, the base plate was heated inside a mufe furnace
from room temperature to the normalising temperature at a heating
rate of 10 K/min, held at that temperature for 30 min followed by air
cooling. Specimen blanks of dimensions 60 12 12 mm3 were sectioned from the base plate and were subjected to tempering treatment
for 1 h at different temperatures in the range 673 to 923 K at intervals of
25 K.
Charpy impact test specimens (55 10 10 mm3 with a 45 V notch
at the centre) were machined out from these heat treated specimen
blanks and tested at room temperature. Three tests per specimen
were performed and the average of the recorded values was considered
as the impact toughness. Fracture surface of the impact tested samples
were examined in detail under scanning electron microscope (SEM).
For microstructural observations, specimens of dimensions 25 10
10 mm3 were prepared by standard metallography techniques and
etched with Villella's reagent. These specimens were examined under
eld emission scanning electron microscope (FESEM) to nd out variation in microstructure with tempering treatment. Hardness measurements were carried out using Vickers hardness tester at 10 kg load and
the average of three hardness readings is reported as the hardness value.
Based on impact toughness values of the specimens and microstructural observations, samples subjected to tempering treatment at 723,
823 and 923 K were selected for detailed examination using transmission electron microscopy (TEM) to understand the change in the microstructure with tempering temperature. Extraction replicas were
prepared from polished and etched specimens by carbon deposition
and subsequent extraction of various precipitates using freshly prepared Villella's reagent into the deposited carbon lm. The extracted
lms were then rinsed with methanol and nally with distilled water.
Samples thus prepared were collected over copper grid and was observed under Analytical transmission electron microscopy (ATEM).
Using ATEM and extraction replica, it was possible to identify the type
and chemistry of the carbide by Selected Area Diffraction (SAD) and Energy Dispersive X-Ray Spectra (EDS) analysis, respectively, without any
matrix interference.
Table 1
Chemical composition (in wt.%) of the AISI 410 stainless steel investigated.

AISI 410

Cr

Mn

Si

Fe

0.14

11.2

0.9

0.46

0.01

0.003

Balance

Impact toughness for 410 SS in normalised condition is around 59 J

and there is a marginal improvement (69 J, 65 J, 62 J) while tempering
at low temperature range i.e., 673723 K (Fig. 1a). However, impact
toughness decreased with the increase in tempering temperature for
the specimens tempered in the range of 748823 K. Maximum reduction in impact toughness is observed in the tempering temperature
range of 723773 K and for 773823 K range the reduction in toughness
with change in tempering temperature is only marginal. Minimum
value of impact toughness (18 J) was recorded for specimens tempered
at 823 K. A gradual increase in impact toughness with temperature was
observed for specimens tempered at temperatures above this up to
923 K, the maximum temperature of tempering employed in the present study. Fig. 1b shows variation in hardness with tempering temperature. Both in Fig. 1a & b error bars are shown along with the average data
for impact toughness and hardness, respectively, and the scatter in the
data for hardness is negligible. Hardness of the steel in normalised condition is ~522 VHN, which decreases during tempering treatment. With
increasing tempering temperature from 673 to 923 K there is a continuous decrease in the hardness from about 450 to 250 VHN. Though, no
secondary hardening is observed; the decrease in hardness in the temperature range 723773 K (the range for which maximum reduction in
toughness with tempering temperature is observed) is only marginal
compared to that observed in the temperature range 773923 K (Fig. 1).
Fractographs of the impact tested specimens in the as-normalised
condition and tempered at 723, 773, 798, 823 and 923 K for 1 h after
normalising are given in Fig. 2(af). Fracture surface of the normalised
specimen is brous indicating ductile mode of failure (Fig. 2a). Fracture
mode of specimen tempered at 723 K is also ductile and the dimple size
is much smaller than the normalised sample (Fig. 2b) indicating a
higher degree of ductility. However for specimens tempered at 773
and 798 K (Fig. 2cd), the fracture mode is predominantly brittle with
cleavage mode of fracture. Specimen tempered at 823 K is also fractured
in a brittle manner; but the mode of fracture is fully intergranular with a
lot of ne grain boundary cracks. This observation is in agreement with
minimum toughness observed for specimens tempered at this temperature. For specimens tempered at 923 K the fracture mode is a mixture
of both intergranular and ductile (dimples can be noticed at the facture
surface (Fig. 2f)). This is also in agreement with the improvement in
toughness observed by tempering at 923 K. From the impact toughness
values and fractographs of the specimens, temperature range of
maximum embrittlement is identied as 773848 K for 410 SS with
maximum severity of embrittlement at 823 K. Based on this, three representative specimens corresponding to tempering treatment at 723 K

G. Chakraborty et al. / Materials Characterization 100 (2015) 8187

500

80

(a)

(b)

60

Hardness (VHN)

Impact toughness (J)

83

40

20

Normalized steel: 59J

0
600
700

800

900

1000

400

300

Normalized hardness: 522 VHN

200
600
700
800

900

1000

Temperature (K)

Temperature (K)

Fig. 1. Variation in (a) impact toughness, (b) hardness with tempering temperature of 410 SS.

(below this temperature range), 823 K (within this temperature range)

and 923 K (above this temperature range) were selected for detailed
metallographic investigations to identify possible reasons for this
embrittlement.

Microstructure of the 410 SS in normalised condition revealed lath

martensite with very less or almost no carbide precipitation at lath
boundaries (not shown here). FESEM images of samples tempered at
723, 823 and 923 K are shown in Fig. 3ac. The micrograph of 723 K

(a)

(b)

(c)

(d)

(e)

(f)

Fig. 2. Fractographs of 410 SS samples in different heat treated conditions: (a) normalised and tempered at (b) 723 K, (c) 773 K, (d) 798 K, (e) 823 K and (f) 923 K.

84

G. Chakraborty et al. / Materials Characterization 100 (2015) 8187

tempered sample reveals lath martensite structure with very ne precipitates within the laths. Images of samples tempered at 823 and
923 K clearly show tempered martensite structure with precipitates
decorating the lath boundaries (Fig. 3bc). For specimens tempered at
823 K, precipitates are present within the lath as well as along the lath
boundaries (Fig. 3b). However, after tempering at 923 K, precipitates
are found predominantly along the lath and prior austenite boundaries.
Further, ne precipitates are seen in specimen tempered at 723 and
823 K, whereas, precipitates are relatively large in size in specimen tempered at 923 K.
Fig. 4 shows TEM micrographs taken from carbon extraction replica
of the steel tempered at various temperatures. The steel specimen
tempered at 723 K contains predominantly elongated needle like
(length width) carbide precipitates (Fig. 4a), which is rich in iron
(Fig. 5a). The average iron to chromium ratio of the carbides as determined by energy dispersive X-ray spectroscopy (EDS) is 4.7. The specimen subjected to tempering at 823 K contains precipitates with three
different morphologies elongated, nearly globular and globular (indicated as 1, 2 and 3 in Fig. 4b). EDS analysis (Fig. 5bd) of the precipitates
indicates that elongated precipitates are iron rich carbides (similar to
those observed after 723 K/1 h tempering) and globular precipitates
are chromium rich carbides (un-labelled EDS peeks are from copper
grid). In the case of nearly globular carbide, there is substantial presence
of both Fe and Cr. For 923 K tempered specimen only globular precipitates can be detected, which are chromium rich carbides. The size of
the precipitates is also considerably large in this specimen. A qualitative
comparison of the volume fraction and morphology of the precipitates
extracted from specimens subjected to these three tempering
heat treatment indicates that volume fraction of the precipitates after
723 K heat treatment is considerably lower than those obtained after
the other two heat treatments.
In order to identify crystal structure, selected area diffraction (SAD)
of few chosen precipitates were taken. Fig. 6(a) and (b) shows micro
diffraction patterns obtained from the iron rich lenticular precipitates
observed in the steel tempered at 723 and 823 K, respectively. Analysis
of the pattern revealed that they are belonging to Fe2C type (HCP).
Fig. 6(c) shows a SAD pattern taken from the chromium rich globular
precipitates observed in steel tempered at 923 K. These precipitates
were identied as M23C6 (M = Cr, Fe) (fcc) type.

(a)

XRD analyses of the precipitates extracted by electrochemical dissolution of the matrix of the specimens tempered at 823 K and 923 K are
shown in Fig. 7(a) and (b). The quantity of precipitates collected by dissolution of 723 K tempered sample was too less to carry out XRD studies
using them. The results of XRD analysis also support TEM observations.
In 823 K tempered specimen different types of carbides are present. The
presence of eta-carbide (Fe2C) can be detected along with M23C6 carbides (Fig. 7a). For 923 K tempered specimen only M23C6 type carbides
are found. Further, for 823 K tempered specimen, highest intensity is recorded for Cr15.58Fe7.42C6, whereas for 923 K tempered specimen
highest intensity is recorded for Cr22.23Fe0.77C6 carbide indicating
change in chemistry of the M23C6 carbide with the increase in tempering temperature (Fig. 7). This decrease in the Fe content in M23C6 carbides is an indication of progress of tempering.
AES studies carried out on fracture surfaces could not detect any evidence of P and S segregation at the grain boundaries in specimens tempered at 723 K, 823 K and 923 K. It should be noted that as the beam size
is in micron levels, the resolution of the AES used in the present study is
limited and it may not be able to detect segregation in sub-micron
levels. Further, specimens examined were those fractured using impact
testing machine; not those fractured in situ in a mechanical stage of AES.
4. Discussion
AISI 410 SS in normalised condition comprises of lath martensitic
structure, which is hard (522 VHN) and of low toughness (impact
toughness = 59 J). It is already mentioned that during tempering heat
treatment at 838 K cracks had developed on a component (the sprocket
of the fuel handling machine) made of this steel. Results of the present
study indicate that this martensitic class of steel shows drastic fall in impact toughness when subjected to tempering in the temperature range
of 748 K923 K. Hence, it is reasonable to attribute the cause of cracking
observed in the sprocket material to the embrittlement observed in this
steel. In search of causes for this embrittlement, two probable metallurgical effects were investigated, rst is segregation of impurities like P, S
at grain boundaries and the second one is the precipitation sequence
and morphology of carbides during tempering. The former could not
be detected even by AES; but signicant changes in the precipitation behaviour of the steel with tempering temperature could be identied.

(b)

(c)

Fig. 3. FESEM micrographs of 410 SS samples tempered at (a) 723 K, (b) 823 K and (c) 923 K.

G. Chakraborty et al. / Materials Characterization 100 (2015) 8187

(a)

(b)

85

(c)
(3)
(1)
(2)

Fig. 4. TEM micrographs of 410 SS samples tempered at (a) 723 K, (b) 823 K and (c) 923 K.

Hence, it is reasonable to assume that precipitation of carbides has a

major role in the embrittlement observed in the steel in this temperature range.
Tempering behaviour of an as quenched alloy steel is inuenced signicantly by the tempering temperature. In the low temperature range
of tempering, there will be some reduction in the dislocation density of
the martensitic structure and rejection of the carbon by the martensite
which result in the reduction in hardness and improvement in toughness. Impact toughness values of the steel after tempering at 673 K,
698 K and 723 K (69, 65 and 62 J, respectively) are higher than that of
the normalised steel (59 J). In the case of hardness the corresponding
values are 456, 446 and 443 VHN which are lower than the hardness
of 522VHN obtained for normalised steel. The carbon rejected from
the martensite during tempering forms carbides. At low temperatures
of tempering, the carbides formed are rich in Fe, even though these carbides are not the equilibrium carbides [14]. This is because of the slow
diffusion of alloying atoms (Cr) at these temperatures and availability
of Fe atoms in the neighbourhoods of carbon atoms to form carbides.
These carbides nucleate uniformly throughout the matrix; but do not
grow much due to low diffusion rates at these temperatures. Hence,
400

400

(b)
Normalized Intensity (counts)

Fe

300

200

100

Cr
Fe

Cr

(c)

Fe

Normalized Intensity (counts)

(a)

300

200

100

Fe

Cr

Cr
300

10

100

Cr

Energy (KeV)

10

Energy (Kev)

400

Cr

(e)

300

200

100

Cr Fe

Cr
300

200

Fe
100

Cr

Fe

0
1

Energy (KeV)

10

Energy (KeV)

400

(d)

Fe

0
1

Normalized Intensity (counts)

Fe

200

0
1

Normalized Intensity (counts)

Normalized intensity (counts)

400

these carbides offer increased precipitationdislocation interactions

thereby imparting a strengthening effect on the steel which partially
or fully nullify the softening expected due to carbon rejection from the
martensite lattice and decrease in dislocation density. In many steels,
secondary hardening, i.e. increase in hardness with increase in tempering time and temperature, in the temperature range of 623 K to 923 K
has been reported [2,8]. In the present study secondary hardening is
not observed during tempering; but the plateau observed in the plot
of tempering temperature vs. hardness (Fig. 1b) in the temperature
range of 723773 K and very ne carbides seen in steels tempered at
723 K (Fig. 3a) are clear indications of the contribution of the carbides
in strengthening the matrix. This strengthening effect of the matrix
has an adverse effect on the impact toughness of the steel. Thus, for
lower tempering temperature range i.e. 673 K723 K, although impact
toughness of the tempered steel is higher than that of normalised
steel, a gradual decrease in impact toughness with increasing tempering
temperature can be noticed. One may also notice that there is a shift
from ductile to cleavage type of fracture with increase in tempering
temperature from 723 to 798 K (Fig. 2bd). However, steel tempered
at 823 K responds differently during impact test; mode of fracture is

Energy (KeV)

Fig. 5. TEM-EDS spectra of AISI 410 SS samples tempered at (a) 723 K, (bd) 823 K and (e) 923 K.

10

10

86

G. Chakraborty et al. / Materials Characterization 100 (2015) 8187

(a)

(b)

(c)

Fig. 6. Diffraction pattern taken from (a) Fe2C precipitate (sample tempered at 723 K) along b1546N zone axis, (b) Fe2C precipitate (sample tempered at 823 K) along b1213N zone axis, and
(c) M23C6 precipitate (sample tempered at 923 K) along b132N zone axis.

predominantly intergranular (Fig. 2e) and toughness is lowest. Both

grain boundary carbides and matrix carbides are present after tempering at this temperature and apparently, the grain boundary carbides
weaken the boundaries while the matrix precipitates have a strengthening effect on the matrix and hence, after tempering at this temperature, specimen subjected to impact test fracture intergranularly with
minimum toughness. At still higher tempering temperatures, Fe2C carbides are not formed and hence there is no strengthening effect of the
matrix from these carbides; matrix experience only softening due to decrease in dislocation density coming from higher tempering kinetics of
the martensite at higher tempering temperatures. Hence, for specimens
tempered at temperatures above 823 K, though the mode of fracture is
predominantly intergranular due to precipitation that occur along the
prior austenite grain boundaries, deformation of the matrix also takes
place making the mode of fracture more ductile than in the case of specimens subjected to tempering at 823 K (Fig. 2f) with corresponding improvement in the toughness (Fig. 1a) and reduction in hardness
(Fig. 1b). Hence, the effect of tempering temperature on impact toughness of AISI 410 steel is quite complex. For steel tempered at low temperatures (673723 K), mode of fracture is predominantly ductile
with some cleavage and impact toughness is higher than that of the normalised steel. With increase in tempering temperature from 723 K to
798 K there is a drastic reduction in toughness and the mode of fracture
changes to predominantly cleavage type. Fe2C is the main carbide
formed during tempering in this temperature range. However, with further increase in tempering temperature to 823 K, grain boundary carbide M23C6 starts forming resulting in a change in fracture mode from
cleavage to predominantly intergranular (Fig. 2e) and minimum values
for impact toughness (18 J). At still higher tempering temperatures only
grain boundary carbides, no matrix carbides form, and matrix softens

3.Cr15.58Fe7.42C6

150

6.Fe2C, Cr21.34Fe1.66C6

100
1

1.Cr22.23Fe0.77C6

4.Cr15.58Fe7.42C6
5.Fe2C, Cr18.93Fe4.07C6

50

(b)

2.Cr22.23Fe0.77C6

200

Intensity (counts)

150

1.Fe2C

(a)

Intensity (counts)

250

making the steel again ductile and the fracture mode changes to
mixed; a combination of intergranular and ductile (Fig. 2f) with a corresponding increase in toughness.
The temperature range of 773848 K appears to be the zone of
transition for the different tempering behaviours described above. Accordingly, both the types of carbides observed in the specimens are tempered at 823 K. Further there is almost a bottom plateau for variation of
toughness with tempering temperature in this range; with toughness
value being higher both above and below this range of tempering
temperatures. It is also interesting to note that the chemistry of
the alloy carbides observed in specimens tempered 823 K is different
from those tempered at 923 K. Although the alloy carbides identied at high temperature tempering are of M23C6 type; the volume
fraction of these carbides with substantial Fe content (Cr15.58Fe7.48C6)
is more after tempering at 823 K than that of 923 K (Fig. 7a). After
923 K tempering, most of the carbides present are Cr22.23Fe0.77C6
(Fig. 7b).
From the above discussion, it is clear that though alloy carbides of
the type M23C6 are the equilibrium carbides for this class of steels, the
carbides formed during low temperature tempering are of Fe2C type.
The size, morphology and distribution of these carbides are signicantly
different from those of the M23C6 type carbides. It can be noted that the
temperature range 773848 K is the regime when Fe2C type carbides
start dissolving and M23C6 type carbides start forming. Hence, both
types of carbides are present, one strengthening the matrix and the
other weakening the prior austenitic boundaries. Hence, toughness is
the lowest when both types carbides are present. After high temperature tempering, only alloy carbides, not Fe2C carbides are present at
the end of tempering treatment and accordingly impact toughness improves. It is quite possible that impurity segregation along the prior

2.Cr15.58Fe7.42C6

100

2
50

5 6
0

0
25

50

Two theta

75

25

50

75

Two theta

Fig. 7. XRD patterns of precipitates obtained from electrochemical dissolution of AISI 410 SS samples tempered at (a) 823 K and (b) 923 K.

G. Chakraborty et al. / Materials Characterization 100 (2015) 8187

austenite grain boundaries can accelerate this embrittlement; but no

evidence of such segregation is observed in the present study.
As already mentioned, this study was originally undertaken because
of the cracking observed during heat treatment of the sprocket material
carried out to achieve the desired hardness. Now, based on these results,
it was recommended to choose a tempering temperature for the sprocket outside the embrittling range for the steel and then carry out nitriding
of the sprocket material to achieve the minimum specied hardness on
the surface. The option of using the sprocket of AISI 410 SS in the as-normalised condition was not considered because of the high residual
stresses in the as-normalised condition and hardness level far above
the minimum specied which can increase the risk of fracture during
sudden loading that the sprocket may experience during fuel handling.
Nitriding of the sprocket would ensure a tough sprocket material with
high hardness for the teeth of the sprocket, over which the chain will
move. High surface hardness of the sprocket teeth would prevent its deformation caused by the high stresses that the moving chain will impart
on the sprocket teeth.
5. Conclusions
The present research work indicates that AISI 410 SS, which has
moderate toughness and high hardness in normalised condition, suffers
embrittlement, with 773848 K being the tempering temperature range
of maximum embrittlement. Results showed that types of carbides precipitated during different temperatures of tempering vary and iron rich
Fe2C type of carbides are present in the temperature range where susceptibility to embrittlement is maximum. Embrittlement is not observed when the carbides present are only M23C6 type and this occurs
at high temperatures of tempering (N 823 K).

87

References
[1] L.W. Tsay, Y.M. Chang, S. Torng, H.C. Wu, Improved impact toughness of 13Cr martensitic stainless steel hardened by laser, J. Mater. Eng. Perform. 11 (4) (2002)
422427.
[2] L.C. Lim, M.O. Lai, J. Ma, Tempering of AISI 403 stainless steel, Mater. Sci. Eng. A 171
(1993) 1319.
[3] G.V. Prabhu Gaunkar, A.M. Huntz, P. Lacombe, Role of carbon in embrittlement phenomena of tempered martensitic 12Cr0.15%C steel, Mater. Sci. 14 (1980) 241252.
[4] S.K. Bhambri, Intergranular fracture in 13 wt.% chromium martensitic stainless steel,
J. Mater. Sci. 21 (1986) 17411746.
[5] Yang Gang, Wang Chang, Liu Xin-quan, Liu Zheng-dong, Embrittlement mechanism
due to slow cooling during quenching for M152 martensitic heat resistant steel, J.
Iron Steel Res. Int. 17 (6) (2010) 6066.
[6] R. Guiliou, M. Guttmann, Ph. Dumoulin, Role of molybdenum in phosphorousinduced temper embrittlement of 12% Cr martensitic stainless steel, Mater. Sci. 15
(1981) 6372.
[7] K.P. Balan, A. Venugopal Reddy, D.S. Sarma, Austenite precipitation during tempering in 16Cr2Ni martensitic stainless steels, Scr. Mater. 39 (7) (1998) 901905.
[8] H. Tanczyn, Advances in the Technology of Stainless Steels and Related Alloys,
ASTM, 1965 (Chapter 12).
[9] Liu Ning, Deng Zhonggang, Huang Menggen, Effect of heat treatment on microstructure and mechanical properties of martensiticferritic steel containing 17%Cr and
2%Ni, Mater. Sci. Technol. 7 (1991) 10571062.
[10] J.C. Murza, C.J. McMahon Jr., The effects of composition and microstructure on temper embrittlement in 2 Cr1Mo steel, Eng. Mater. Technol. 102 (1980) 369375.
[11] T. Angeliu, E.L. Hall, M. Earsen, et al., The long term aging embrittlement of Fe12Cr
steels below 773 K, Metall. Mater. Trans. A 34 (4) (2003) 927934.
[12] Z. Qu, C.J. McMohan Jr., The effects of tempering reactions on temper embrittlement
of alloy steels, Metall. Trans. 14A (1983) 11011108.
[13] J.H. Bulloch, J.J. Hickey, Reverse temper embrittlement of turbine bolts during an
outage, Theor. Appl. Fract. Mech. 20 (1994) 141147.
[14] C.M. Fang, M.A. Van Huis, H.W. Zandbergen, Structure and stability of Fe2C phases
from density-functional theory calculations, Scr. Mater. 63 (2010) 418421.