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Effect of thermomechanical treatment and tempering temperature on


microstructure and tensile properties of India specific reduced
activation ferritic martensitic steel

P. Anil Kumar , J. Vanaja , G.V. Prasad Reddy ,


G.V.S. Nageswara Rao

PII: S0022-3115(22)00665-1
DOI: https://doi.org/10.1016/j.jnucmat.2022.154186
Reference: NUMA 154186

To appear in: Journal of Nuclear Materials

Received date: 29 September 2022


Revised date: 1 December 2022
Accepted date: 2 December 2022

Please cite this article as: P. Anil Kumar , J. Vanaja , G.V. Prasad Reddy , G.V.S. Nageswara Rao ,
Effect of thermomechanical treatment and tempering temperature on microstructure and tensile prop-
erties of India specific reduced activation ferritic martensitic steel, Journal of Nuclear Materials (2022),
doi: https://doi.org/10.1016/j.jnucmat.2022.154186

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© 2022 Published by Elsevier B.V.


Highlights

• Thermomechanical treatment (TMT) refines the lath width, M23C6 and MX precipitates
• Microstructural stability of the INRAFM steel enhances upon TMT
• TMT at 973 K followed by tempering at 1033 K exhibits better tensile properties
• Enhanced ductility is an added benefit of the steel upon TMT

1
Effect of thermomechanical treatment and tempering temperature on microstructure and
tensile properties of India specific reduced activation ferritic martensitic steel

P. Anil Kumar1, J. Vanaja2, G. V. Prasad Reddy2, 3 and G. V. S. Nageswara Rao1,*


1
Department of Metallurgical and Materials Engineering,
National Institute of Technology Warangal, Warangal-506004, Telangana, India
2
Indira Gandhi Centre for Atomic Research, Kalpakkam-603102, Tamil Nadu, India
3
Homi Bhabha National Institute, Training School Complex, Anushakti Nagar,
Mumbai-400094, India
*Corresponding author: gvsnr@nitw.ac.in

Abstract
In the present work, India specific reduced activation ferritic martensitic (INRAFM) steel was
subjected to thermomechanical treatment (TMT) consisting of warm rolling at 973 K, followed
by tempering for 90 min at two temperatures 1033 K and 1063 K, named as TMT1 and TMT2
conditions. Microstructural characteristics, hardness and tensile properties (at 300-873 K) of the
INRAFM steel in TMT1 and TMT2 conditions are presented. INRAFM steel has shown
significant improvement in hardness, tensile strength properties in TMT1 condition (i.e.,
tempered at 1033 K) compared to conventional normalizing and tempering due to
microstructural refinement. However, tempering at higher temperature (1063 K) diminished the
beneficial effects of TMT. The refinement in M23C6 and MX precipitates and ample
improvement in their number density complemented by relatively high dislocation density
(produced upon thermomechanical treatment) mainly contribute to the enhancement of elevated
temperature strength of the steel tempered at 1033 K. On the other hand, the drop in strength of
the steel tempered at 1063 K is attributed to the coarsening of M23C6 precipitates, annihilation
and recovery of dislocation structure, with less number density of MX precipitates. Moreover,
apart from enhancing the strength, the ductility of the steel has immensely improved in TMT1
condition. These promising results make TMT processed INRAFM steel a potential candidate
material for nuclear fusion reactor applications.

Keywords: Thermomechanical treatment; Tempering; M23C6 and MX precipitates; Tensile


properties

2
1. Introduction

Nuclear fusion energy is a potential energy source for addressing the future demands. It is
advantageous in terms of safety, minimal radioactive emission, and sustainability. In the recent
past, extensive efforts are in progress for the design and development of advanced materials for
the structural components in next generation nuclear fusion reactors. During service, these
materials are exposed to environments like high neutron irradiation, mechanical and thermal
loadings [1, 2]. The selection of materials for structural components is of importance to maintain
the structural integrity in extreme conditions. Reduced activation ferritic martensitic (RAFM)
steels are the candidate materials being considered for the structural components in nuclear
fusion reactor. Low/reduced activation is the main attractive characteristic feature in RAFM
steels, which was developed by replacing radioactive elements (molybdenum/niobium) with low
activation elements (tungsten/tantalum) in modified 9Cr-1Mo steel. In addition to low activation,
RAFM steels also possess exceptional thermo-physical characteristics and better resistance
towards void swelling caused by radiation compared to austenitic stainless steels [3-5]. The
plasma facing test blanket module in International Thermonuclear Experimental Reactor (ITER)
and divertor cassette in demonstration fusion power plant (DEMO) are the closest applications of
RAFM steels in fusion power reactors [6-8]. Intense research is in progress from many countries
on the development of different variants of RAFM steels. India has developed four heats of
RAFM steels by varying tungsten content (1, 1.4, 2.0 wt. %) and tantalum content (0.06, 0.14 wt.
%). Based on the extensive research, it is observed that the steel with tungsten content of 1.4 wt.
% and tantalum of 0.06 wt. % shows better physical and mechanical properties and is specified
as India specific reduced activation ferritic martensitic (INRAFM) steel [9, 10]. The evolution of
tempered martensitic structure and precipitation of secondary phases during operation will
determine the strength in 9Cr steels [11]. Nevertheless, at temperatures exceeding 823 K, this
steel experiences a significant change in microstructural features such as coarsening of M23C6
precipitates (where "M" denotes Cr, W and Fe), laves phase precipitation, widening of lath
structure, recovery of dislocation sub-structure etc. These changes in microstructure during
service impair its mechanical properties [12, 13]. The elevated temperature mechanical
characteristics of RAFM steels can be enhanced by increasing their microstructural stability.
This can be obtained by decreasing the size of M23C6 and MX (where "M" denotes Ta/V, while

3
"X" denotes N/C) precipitates with concomitant increase in density and refinement of the lath
structure [14]. Some studies [15-17] have reported that thermomechanical processing is a
potential approach for enhancing the number density of precipitates (M23C6 and MX) along with
their refinement. In addition, the thermomechanical treatment also refines the lath width along
with an increment in dislocation density. The dislocations induced during deformation acts as
potential sites for the precipitation of nano sized MX carbonitrides [18]. The presence of large
density of MX precipitates within the martensitic lath structure obstructs the dislocations motion
and contributes to precipitation strengthening [19]; whereas the M23C6 primarily nucleate at the
boundaries of prior austenite grain/packet/lath substructure. The finer M23C6 precipitates restrict
the coarsening of lath structure and increase the stability of the structure at elevated
temperatures. Prakash et al. [16] reported an improvement in mechanical properties of RAFM
steel through refinement of these precipitates and lath structure by thermomechanical treatment.
Vivas et al. [17] found an increment in density of dislocations and refinement in size and amount
of MX carbonitrides by ausforming 9Cr ferritic/martensitic steel. The authors also reported an
improvement in creep rupture strength of the alloy due to refinement in microstructural features.

Furthermore, the tempering temperature and time plays a vital role in improving toughness and
ductility of ferritic martensitic steels. Segregation of carbon into lattice defects, evolution of
carbide precipitates, recovery of martensitic lath structure and reduction in dislocation density
during tempering treatment significantly changes the characteristics of microstructure [20]. An
immense knowledge on microstructural features such as precipitates size, orientation and their
distribution are required to tailor the mechanical properties. Yan et al. [21] reported an
improvement in toughness of the 9Cr-3W-3Co steel with raise in tempering temperature from
1013 K to 1053 K at 3 h tempering. This is attributed to the decrease in the dislocation density
and super saturation of the interstitial atoms. However, the information on tempering effect after
thermomechanical treatment is very limited in the open literature. In the present work, the effect
of thermomechanical treatment and subsequent tempering at two different temperatures on
microstructural features and resultant tensile properties of INRAFM steel are presented. The
tensile and hardness properties are correlated to the size and amount of M23C6/MX precipitates
and texture of the material upon thermomechanical processing.

4
2. Material and experimental details

The India specific reduced activation ferritic martensitic (INRAFM) steel plate with dimensions
of 250 mm 125 mm 25 mm was received from Indira Gandhi Centre for Atomic Research
(IGCAR), Kalpakkam in normalized and tempered condition. The composition (in wt. %) of the
steel is Fe-9.03Cr-1.38W-0.24V-0.06Ta-0.126C. The steel plate was subjected to austenitization
at 1423 K for10 min to homogenize the structure. Subsequently, the plate was transferred into
another furnace maintained at 973 K, i.e. warm rolling temperature. Then the thermomechanical
treatment was performed on the steel by warm rolling. A reduction in thickness of 25% was
imparted to the steel during warm rolling. Subsequent to the thermomechanical treatment, the
steel was tempered at two temperatures, 1033 K and 1063 K, for 90 min with the aim of studying
the influence of tempering on microstructural features and mechanical characteristics. Hereafter,
the steel in the normalized and tempered condition is denoted as N+T, and that subjected to
warm rolling at 973 K followed by tempering at 1033 K and 1063 K for 90 min are referred to as
TMT1 and TMT2 respectively. Microstructural characteristics of INRAFM steel in N+T, TMT1
and TMT2 conditions were assessed by using a field-emission scanning electron microscope
(FESEM) (Make: Carl Zeiss and Model: SUPRA 55VP) equipped with electron backscatter
diffraction (EBSD) (Oxford integrated instrument). The samples for microscopic examination
were polished on different grits of silicon carbide emery papers. Final mirror finish was obtained
by polishing on velvet cloth using 1μm diamond paste. Villella’s reagent (picric acid-1g, HCl-5
ml, ethyl alcohol-100 ml) was used as an etching agent to reveal the microstructural features. For
EBSD studies, the samples were manually prepared by using abrasive silicon carbide papers up
to grit size of 2500 followed by electro-polishing with 4 vol. % perchloric acid (HClO4) and 96
vol. % methanol (CH3OH) solution at 20 V. EBSD mapping was carried out by using a step size
of 0.4 μm. For data processing, the HKL software was used. Microstructural analysis by
transmission electron microscope (TEM) was performed by using Technai G2 F20 TWIN TMP
instrument. Initially, the samples for TEM analysis were mechanically thinned up to a thickness
of 60 microns. Later, 3 mm diameter disc samples were snipped from these samples by using
indigenously developed grid punch equipment. After that electro polishing was carried out on the
disc samples by using 20% HClO4 and 80% CH3OH solution at 238 ± 2 K and 20 V. The
hardness and tensile tests were performed on the INRAFM steel in N+T, TMT1 and TMT2

5
conditions. The hardness was determined by making use of Vickers hardness tester (make:
Matsuzawa, model: VMT-X7) for a dwell time of 15 s under a load of 10 kg. Tensile tests were
carried out in the temperature range of 300K to 873K at a strain rate of 310−4 s−1.

3. Results
3.1. Microstructural features

The field-emission scanning electron microscope (FESEM) images of the steel in N+T, TMT1
and TMT2 conditions are depicted in Figs. 1a, c and e respectively. The images portray the
distribution of M23C6 precipitates of varying sizes along the prior austenite
grain/packet/block/lath boundaries. While the steel in N+T condition (Fig. 1a) reveals relatively
low dense and large sized M23C6 precipitates, the steel in TMT1 and TMT2 conditions (Figs. 1c
and e) portray relatively finer precipitates with large number density. This might be due to
possession of more potential sites such as packet/block/lath boundaries upon thermomechanical
treatment which enhances the precipitation of M23C6 [22]. To illustrate the extent of refinement
on structural features, the transmission electron microscope (TEM) images of the INRAFM steel
in all three conditions are presented in Figs. 1b, d and f. These images reveal the presence of
tempered martensitic lath structure with the distribution of M23C6 precipitates along the sub
grain/lath boundaries and MX carbonitrides within the lath regions. Energy dispersive
spectroscopy (EDS) analysis of the precipitates present along the boundaries suggests that these
precipitates were abundant in chromium (Cr), iron (Fe) with the presence of the small amount of
tungsten (W) and identified as M23C6 (Fig. 1g), whereas the intra lath precipitates are rich in
tantalum (Ta), vanadium (Va) and found as MX (Fig. 1h) precipitates. The warm rolling of the
INRAFM steel in the metastable austenitic condition is thought to minimize the segregation of
elements such as vanadium and tantalum to grain boundaries by providing preferential sites such
as dislocations for the precipitation of MX carbonitrides within the lath regions. It must also be
emphasized that thermomechanical treatment refines the martensitic lath width, 150-335 nm and
225-350 nm in TMT1 and TMT2 conditions respectively, compared to 300-430 nm in N+T
condition. The studies on 9Cr steels reveal that the coarser the prior austenite grain (PAG) size,
the coarser will be packet/block size [17] and finer the lath size in thermomechanical treated
condition [22]. Table 1 shows the literature data of prior austenite grain (PAG) size and
corresponding lath width reported for distinct materials in different conditions. The extensive

6
data presented in Table 1 confirms clearly the refinement in lath width despite higher prior
austenite grain after thermomechanical treatment, which eventually results in improvement of
mechanical properties.

(a) (b)

MX
M23C6 Sub grain boundaries

M23C6
M23C6 Lath boundaries

(c) (d)
M23C6

Lath boundaries M23C6

M23C6
M23C6
MX

(e) (f)

M23C6

M23C6 M23C6

Lath boundaries

MX

7
(g) Fe, Cr, W rich M23C6

(h) Ta, V rich MX

Fig. 1. Left (a, c, e): FESEM images of INRAFM steel in (a) N+T, (c) TMT1 and (e) TMT2
conditions. Right (b, d, f): TEM images of the steel in the corresponding conditions, (g) EDS
analysis of M23C6 precipitate and (h) EDS analysis of MX precipitate with corresponding site of
interest in the respective images.

8
Table 1. Literature data on prior austenite grain (PAG) size and lath widths obtained in different materials in different conditions

Condition
Thermomechanical treatment cycle PAG size, Lath width,
Material Ref.
Normalizing Tempering Re- m nm
Warm rolling Aging Tempering
austenitization
At 1253 K for At 1038 K for
- - - - 102 272
30 min 90 min
RAFM steel
(9Cr-1W-0.06Ta)
At 1423 K for
At 973 K with
At 973 K for
At 1038 K for [16]
- - 10 min - AC to 30 min - AC 17513 179
25%  90 min
973 K to RT
At 1313 K for At 1033 K for
- - - - 25 55850
P 91 steel 30 min 150 min
(Modified 9Cr–1Mo At 1423 K for
At 973 K with
At 973 K for
At 1033 K for [23, 24]
steel) - - 10 min - AC to 30 min -AC 75 490100
25%  150 min
973 K to RT
At 1423 K for At 1043 K for
- - - - 250–300 330 ± 40
1h 4h
9Cr3W3CoVNb steel
with balanced B and N
At 1423 K for At 923 K with
At 973 K for [25]
- - 30 min - AC to 25%  then - 350 215 ± 25
60 min
923 K WQ
At 1323 K for At 1053 K for
- - - - 20–25 250-500
30 min 90 min
Modified 9Cr–1Mo steel
(Grade 91)
At 1423 K for At 873K with
At 973 K for [26]
- - 30 min-AC to 25%  then - 40 210
90 min
823 K WQ
At 1313 K for At 1003 K for
- - - - 43±4 36035
30 min 60 min
At 1498 K for 5 At 1013 K for
- - - - 250±7 35020
min 45 min
G91 steel - -
At 1173 K with
- 128±17 31832
[17, 22,
40%  27]
At 1498 K for 5 At 1173 K with At 1013 K for
- - - 141±19 28526
min 20%  45 min
At 873 K with
- - - 259 ± 13 21259
20% 
At 1253 K for At 1038 K for
- - - - 12 ± 2 300-430
30 min 90 min
At 1423 K for Present
At 973 K with At 1033 K for
INRAFM steel - - 10 min - AC to - 180 ± 4 150-335
25%  90 min study
(9Cr-1.4W-0.06Ta) 973 K
At 1423 K for
At 973 K with At 1063 K for
- - 10 min - AC to - 182 ± 6 225-350
25%  90 min
973 K
: Reduction in thickness (deformation); AC: Air cooling; WQ: Water quenching; RT: Room temperature
9
The average size (𝑑̅ v) and number density (𝑁𝑉 ) (number of particles per unit volume) of the
M23C6 and MX particles were determined by using the mean diameter method proposed by
Fullman [28] for spherical particles and is given by the relationships shown in equations (1) and
(2) respectively.
𝜋 𝑛
𝑑̅ v = 2 1 (1)
∑𝑛
𝑖=1𝑑
𝐴𝑖

𝑁𝐴
𝑁𝑉 = (2)
𝑑̅ v

where 𝑑𝐴𝑖 represents the size of the ith precipitate particle, which was measured by using the
Image J application and n denotes the number of the particles, NA denotes the number of particles
per unit area which is given by n/Aobs, where Aobs denotes the observed area.
The size and number density of M23C6 precipitates were estimated from FESEM images, whereas
that of MX precipitates were determined from TEM images. More than 250 M23C6 and 100 MX
particles size was measured from three images to obtain the precipitates average size in the
respective conditions. The estimated average size and number density of the precipitates in
INRAFM steel in different conditions are shown in Table 2. While the size of the M23C6 and MX
precipitates are observed to be around 110 nm and 40 nm in N+T condition, they are refined to
45 nm and 22 nm in TMT1 and 57 nm and 29 nm in TMT2 conditions respectively. In addition,
the thermomechanical treated steel shows a large number density of finer precipitates
(M23C6/MX) (Fig. 1) compared to those in N+T condition. It may be noted that the
thermomechanical treatment also refines the martensitic lath structure and this lath refinement
increases the nucleation sites for precipitation of M23C6 precipitates [22]. The density of
dislocations also increases upon thermomechanical treatment [29], which acts as potential sites
for the precipitation of MX carbonitrides. Thereby, increasing the amount of M23C6 and MX
precipitates (𝑁𝑉 ) from 0.46  1019 m−3 and 4.8  1019 m−3 in N+T condition to 1.42  1019 m−3 and
20.4  1019 m−3 in TMT1 condition and 1.66  1019 m−3 and 9.2  1019 m−3 in TMT2 condition.
The high number densities of fine precipitates in thermomechanical treatment condition enhance
the microstructural stability of the steel and improve its mechanical characteristics. The M23C6
precipitates present at the boundaries of lath/packet/block restrict their motion and thus
enhances/imparts structural stability. Several researches [14, 16, 30, 31] have reported that the
MX precipitates are exceptionally more effective in improvement of elevated temperature

10
properties than M23C6 carbides and lath substructures, as the former enhances the strength by
dislocation-precipitate interactions.

Table 2. Average M23C6 and MX particle size and number density of INRAFM steel in different
condtions.
Average M23C6 Number density of Average MX Number density of
Condition
particle size, nm M23C6 particle, m−3 particle size, nm MX particle, m−3
N+T 110 0.46 1019 40 4.8  1019
TMT1 45 1.42 1019 22 20.4  1019
TMT2 57 1.66 1019 29 9.2 1019

Furthermore, in detail energy dispersive spectroscopy (EDS) analysis has been carried out on
M23C6 precipitates (Fig. 2) in INRAFM steel in N+T, TMT1 and TMT2 conditions. The size of
the precipitates is directly related to the rate at which Ostwald ripening process occurs in it [22].
In martensitic steels, the carbon atoms tend to segregate around dislocations and grain
boundaries (active nucleation sites) [32]. Chromium diffuses into these active nucleation sites
and form respective carbides (M23C6) along PAG/packet/block/lath boundaries. The steel in N+T
condition possesses relatively low dislocation density and small grain boundary regions/less
potential sites. The precipitation of these carbides first occurs along the PAG boundaries due to
possession of higher energy and also as more carbon is readily available. As a result, the
precipitates are larger in N+T condition. Hot working of the steel induces higher dislocation
density and brings out refinement in lath structure. The latter being important as lath boundaries
increase density of nucleation sites. As a result, the potential sites for nucleation of M23C6
precipitate increases in thermomechanical treated condition. This in turn leads to the distribution
of chromium at numerous sites, thereby resulting in the precipitation of high number density of
fine carbide precipitates. The FESEM-EDS composition plot shown in Fig. 2 indicates only
qualitative information, as Cr content in such precipitates usually range from 22-46% as per
TEM-EDS analysis [16, 33]. The steel in TMT1 and TMT2 conditions shows depletion in Cr and
W contents as compared to N+T condition. Increasing tempering temperature (in TMT2
condition) would usually increase the diffusivity of the elements that result in formation of high

11
amount of coarser carbide precipitates, in comparison to TMT1 condition as evinced from Figs.
1c and e.

120
Cr C W Fe

100
Element Wt. %

80

60

40

20

0
N+T TMT1 TMT2
Material Condition
Fig. 2. Variation of elemental weight % in M23C6 precipitates for INRAFM steel in (a) N+T, (b)
TMT1 and (c) TMT2 conditions.

Electron backscatter diffraction (EBSD) investigations were performed on INRAFM steel in


N+T, TMT1 and TMT2 conditions to examine the effect of thermomechanical processing and
tempering temperature on microstructural features. The obtained EBSD micrographs of the
INRAFM steel in all three conditions are shown in Figs. 3a, c and e. The different colours in
Figs. 3a, c and e correspond to different crystallographic orientations observed normal to the
plane. These images show distinct prior austenite grains with lath martensitic structure. The prior
austenite grains (PAG) are subdivided into packets that are further partitioned into blocks. The
distribution of the martensitic blocks/packets can be seen clearly in Figs. 3c and e with different
orientations. It is worth noting that the EBSD maps step size (0.4μm) is too large to accurately

12
define lath size or dislocation density. The PAG size of the steel in N+T condition is observed to
be 12 2 m whereas it enlarges to 180 4 m and 1826 m in TMT1 and TMT2 conditions.
Studies on 9Cr steels have reported the coarsening of prior austenite grains upon
thermomechanical treatment [16, 22]. This grain coarsening is due to complete dissolution of
M23C6 precipitates during re-austenitization [23]. The impeding action offered by the M23C6
precipitates on the boundaries gets reduced due to their dissolution, which in turn results in the
coarsening of the prior austenite grains. No appreciable change in prior austenite grain size can
be seen with raise in tempering temperature from 1033 K (TMT1) to 1063 K (TMT2). This is in
agreement with Zhao et al. [20] who reported that tempering temperature doesn’t have
significant effect on prior austenite grain size.
The amount of carbon content in INRAFM steel is 0.126 wt. %. Since it belongs to low carbon
steel, the packet/block size of the present steel in all three conditions is considered to be obeying
the linear relation with the PAG size [32]. The linear relation described below is applied to
determine the packet and block size.
𝑑𝑝𝑎𝑐𝑘𝑒𝑡 = 0.4 𝐷𝑔 (3)
𝑑𝑏𝑙𝑜𝑐𝑘 = 0.067 𝐷𝑔 (4)
where 𝑑𝑝𝑎𝑐𝑘𝑒𝑡 , 𝑑𝑏𝑙𝑜𝑐𝑘 and 𝐷𝑔 represent the respective size packet, block and prior austenite
grain. Earlier research [34-36] shows that this block/packet size is the key microstructural
features that control the strength of martensitic steels and follows Hall-Petch relationship. The
calculated size of the packet and width of the block are listed in Table 3. It can be also seen from
Table 3 that the steel in TMT1 and TMT2 conditions exhibits larger block/packet size as
compared to N+T condition. Increase in tempering temperature (in TMT2 condition) has no
appreciable effect on packet/block size of the studied steel. It is noteworthy from the equations
(3) and (4) that the microstructural characteristics of packet/block size is strongly dependent on
the PAG size, which in turn relay on the obstructing effect caused by the M23C6 precipitates on
the boundaries. As the steel was subjected to the same austenitization condition (1423K for 10
min), prior to TMT1 and TMT2, the prior austenite grain coarsening behaviour will be similar
(Figs. 3c and e) and attributes to no considerable change in packet/block size. However, the
increase in tempering temperature has significant influence on the precipitation kinetics in the
steel by the diffusion of atoms.

13
Table 3. Microstructural features of INRAFM steel in different conditions.
Prior austenite grain
Condition Packet size (𝑑𝑝𝑎𝑐𝑘𝑒𝑡 ), μm Block size (𝑑𝑏𝑙𝑜𝑐𝑘 ), μm
size (𝐷𝑔 ), μm
N+T 12 ± 2 ~4.8 ~0.8
TMT1 180 ± 4 ~72 ~12
TMT2 182 ± 6 ~73 ~12.4

The Kernel Average Misorientation (KAM) map shows the misorientation of one data point from
its neighbouring data point within a given area and they provide a good measure of dislocation
density in the material [37]. Higher KAM value indicates the presence of high dislocations
density in the material. The KAM maps recorded on the studied steel in N+T, TMT1, and TMT2
conditions are depicted in Figs. 3b, d and f and the corresponding KAM distribution values (Fig.
4) are observed to be 0.65, 0.85 and 0.75 respectively. While the low KAM value in N+T
condition is due to its unstrained condition (exclusive of transformation induced strains), the
thermomechanical treatment induces deformation induced strains that increases the KAM values.
This in turn indicates the presence of high dislocation density in TMT processed condition.
While the KAM value in TMT1 condition is 0.85 (highest), it is decreased to 0.75˚ in TMT2
condition. The reduction in KAM value in TMT2 condition can be ascribed to the lowering in
density of dislocations due to their annihilation with raise in tempering temperature. The
appearance of more blue colour (low misorientation) in KAM map in TMT2 condition (Fig. 3e)
as compared to TMT1 condition (Fig. 3d) clearly indicate the reduction in dislocation density.

14
(a) (b)

(c) (d)

(e) (f)

Fig. 3. Electron backscatter diffraction images (left side) and Kernel Average Misorientation
maps (right side) of INRAFM steel in (a & b) N+T, (c & d) TMT1 and (e & f) TMT2
conditions.

15
1.2
INRAFM (9Cr-1.4W-0.06Ta) N+T
1.0 TMT1
TMT2

0.8
Number fraction

0.6

0.4

0.2

0.0

0 1 2 3 4 5
Kernel Average Misorientation, degree

Fig. 4 Kernel Average Misorientation (KAM) distribution profiles of INRAFM steel in different
conditions.

3.2. Texture evolution


A pole figure is a projection of the grains with certain crystallographic orientation aligned along
each real space direction onto a sphere and it represent the micro texture in materials. In order to
compare pole figures, it is required to normalize them. The normalization ensures that the
random intensity in the pole figure is equivalent to an intensity of one. In EBSD, the statistical
description of the intensity of a fibre is known as the multiple of uniform density (MUD) and is
quantified using the maximum intensity of the contoured pole figures. The {100}, {110} and
{111} pole figures of INRAFM steel in N+T, TMT1 and TMT2 conditions are shown in Fig. 5.
The pole figures are normalized, and the corresponding figure densities are represented as
multiples of the uniform density. The texture developed in the steel in all three conditions
predominantly resembles the texture components of BCC which consists of α-fiber and γ-fiber
intensities [38]. The alpha fibre texture component is in rolling direction (RD) having a fibre axis
{110}, whereas gamma fibre component is in normal direction with the fibre axis {111}. The
evolved texture in the thermomechanical treatment samples (Fig. 5b and c) represents the rolling
16
texture. The steel subjected to thermomechanical treatment exhibits a strong fibre texture with
higher intensity as compared to N+T condition. This is due to higher deformation induced strains
during warm rolling. Texture has weakened slightly upon tempering at elevated temperature. The
pole figure density increases from 1.73 in N+T condition to 5.94 in TMT1 and 5.55 in TMT2
conditions due to change in grain orientation during deformation. The slight decrease in pole
figure density, i.e. decrease in texture with increase in tempering temperature (in TMT2
condition) is due to recovery process.

(a)

(b)

(c)

Fig. 5. The pole figure densities of INRAFM steel in (a) N+T, (b) TMT1 and (c) TMT2
conditions.

17
3.3. Hardness
In general, the hardness and strength of the steel increases with rise in carbon content,
dislocation density and number density of fine precipitate present in it. Further, for a given
carbon content, the strength will be higher for fine carbide spacing than with a coarse inter-
particle spacing. The hardness values measured on INRAFM steel in N+T, TMT1 and TMT2
conditions are depicted in Fig. 6. The hardness of INRAFM steel in N+T condition is found to be
203  2 HV10 and that in TMT1 and TMT2 conditions are 222  3 HV10 and 208  3 HV10
respectively. The hardness increased drastically to 413  3 HV10 upon thermomechanical
treatment (without tempering). The high density of dislocations induced during deformation of
the steel by warm rolling, the formation of hard martensite and transformation induced strains
reflects in this extensive increase in hardness. The tempering of the steel brings down the
dislocation density owing to processes of recovery/annihilation, and coarsening of precipitates
[39, 40]. Furthermore, tempering also replaces the hard martensitic structure of high dislocation
density with tempered martensite of low dislocation density thereby lowering the hardness. For
the aforementioned reasons, the hardness value decreases with raise in tempering temperature.
The steel in TMT1 condition manifests higher hardness than TMT2 and N+T conditions, in par
with the microstructural features explained earlier, i.e., high number density of fine MX
precipitates with high dislocation density in the steel in TMT1 condition. The steel in TMT2
condition possesses larger density of M23C6 precipitates than those in TMT1 condition as
discussed earlier. M23C6 precipitates mainly restrict the moment of boundaries and stabilize the
structure.

18
500
INRAFM (9Cr-1.4W-0.06Ta)
413
Macro Vickers hardness, Hv10

400

300

222
203 208
200

100

0
N+T TMT TMT1 TMT2
without tempering

Material condition
Fig. 6. Hardness of INRAFM steel in different conditions.

Fig 7 depicts the influence of tempering time on hardness of the INRAFM steel in normalized
and tempered (N+T) and thermomechanical treated conditions with tempering at 1033 K (TMT1)
and 1063 K (TMT2). In all the three cases, the hardness is found to decrease rapidly during the
initial period, followed by a gradual decline with increase in tempering time. The initial rapid
decrease in hardness is due to the annihilation of dislocations and faster recovery of lath
martensitic structure [41]. The thermomechanical processed steel tempered at 1033 K (TMT1)
and 1063 K (TMT2) exhibits higher hardness as compared to the normalized steel (tempered at
1033 K) at all tempering times. This could be due to slower recovery of martensitic structure.
Furthermore, the high dense dislocation networks induced during warm rolling enhance the
precipitation of MX carbonitrides during tempering [16] which in turn slows down the recovery
process through dislocation–precipitate interactions. In addition, the processed steels also possess
high density of fine M23C6 precipitates which offer resistance of recovery and migration of

19
boundaries [42]. It implies that the studied steel in thermomechanical treated condition is more
structurally stable than the steel in normalized and tempered condition. The increase in
tempering temperature from 1033 K (TMT1 condition) to 1063 K (TMT2 condition) enhances
the recovery process and hence results in lower hardness values.

450
INRAFM (9Cr-1.4W-0.06Ta)
Normalized (Tempered at 1033K)
Macro Vickers hardness, Hv10

400 TMT1 (Tempered at 1033K)


TMT2 (Tempered at 1063K)

350

300

250

200

150
0 20 40 60 80 100 120
Tempering time, min
Fig. 7. Effect of tempering time on hardness of INRAFM steel in different conditions.

3.4. Tensile properties


Figs 8a, b and c depicts the engineering stress versus engineering strain plots of INRAFM steel
in N+T, TMT1 and TMT2 conditions, which are obtained by carrying out tensile tests in the
temperature regime 300-873 K at a strain rate of 310-4 s-1. The tensile curves display the
characteristic stress strain behaviour, i.e., the steel exhibits yield strength (YS) followed by
limited work hardening until the ultimate tensile strength (UTS). Beyond UTS the material
displays a gradual decrease in strength with pronounced post necking elongation till failure. The
post necking elongation is much higher than the uniform elongation (i.e., elongation up to UTS)
at all the temperatures. The strain to failure (𝑒𝑓 ) values shows a decreasing trend with raise in
temperature from 300 to 673K and later on it increases. The decreasing/increasing trend in
failure strains between the temperature regions 473-773 K can be attributed to the dynamic strain

20
ageing (DSA) affect. The indetailed explanation on the ductility parameters will be described
below. Few researchers [16, 43, 44] have reported a similar type of behaviour for RAFM steels
and Fe-Cr-Mo FM steels. The reduction in strength values with increase in temperature is
attributed to the precipitates coarsening and the dynamic recovery processes. The engineering
stress versus engineering strain plot of the steel in all three conditions at selected temperatures is
shown in Fig. 8d. It is apparent from the Fig. 8d that the steel in TMT1 condition exhibits a
higher stress response as compared to N+T and TMT2 conditions. The same is observed in the
variation of the YS and UTS properties presented in Figs. 9a and b. Microstructural features
elucidated in the previous sections substantiate this enhancement in tensile properties of TMT1
condition.

900

800
(a) INRAFM (9Cr - 1.4W - 0.06Ta)
Strain Rate : 3x10-4s-1
N+T
300K
Engineering stress, MPa

473K
700 573K
673K
600
773K
823K
500
873K
400

300

200

100

0
0 5 10 15 20 25
Engineering strain, %

21
900
INRAFM (9Cr - 1.4W - 0.06Ta)
800
(b) Strain Rate : 3x10-4s-1
TMT1
300K
473K
Engineering stress, MPa

700
573K
600 673K
773K
500 823K
873K
400

300

200

100

0
0 5 10 15 20 25
Engineering strain, %

800 (c) INRAFM (9Cr - 1.4W - 0.06Ta)


Strain Rate : 3x10-4s-1
TMT2
300K
700 473K
Engineering stress, MPa

573K
600 673K
773K
500 823K
873K
400

300

200

100

0
0 5 10 15 20 25
Engineering strain, %

22
900
N+T - 300K
800
(d) INRAFM (9Cr - 1.4W - 0.06Ta)
Strain Rate : 3x10-4s-1 TMT1 - 300K
TMT2 - 300K
700 N+T - 673K
Engineering stress, MPa

TMT1 - 673K
600 TMT2 - 673K
N+T - 873K
500 TMT1 - 873K
TMT2 - 873K
400

300

200

100

0
0 5 10 15 20 25
Engineering strain, %

Fig. 8. Engineering stress versus engineering strain plots of INRAFM steel tested at different test
temperatures in (a) N+T condition, (b) TMT1 condition, (c) TMT2 condition and (d) Combined
plots at selected temperatures.

Figs 9a and b shows the variation of 0.2 percent normalized yield strength (YS) and normalized
ultimate tensile strength (UTS) of the steel as a function of temperature. The strength properties
(YS & UTS) in respective conditions are normalized with N+T condition. It is evident from the
figure that, the YS and UTS are strongly influenced by the thermomechanical treatment and
tempering temperature at different test temperatures. The YS and UTS follow the order in
TMT1>TMT2>N+T. While the steel in N+T condition exhibits lower strength values due to its
lower structural stability, that in TMT1 condition shows higher YS and UTS. The higher YS and
UTS are attributed to the presence of finer lath size, numerous M23C6 and MX carbonitrides with
finer size in TMT1 condition. On the other hand, the steel in TMT2 condition displays the
strength values lower than TMT1 condition at all test temperatures due to low volume fraction of
MX carbonitrides with reduction in number density of dislocations by annihilation/
rearrangement [11]. In addition, the pinning effect of M23C6 precipitates on lath boundary and
MX carbonitrides on dislocations gets reduced due to their coarser size and hence lowers the
strength values. Vivas et al. [22] reported the coarsening of block size upon thermomechanical

23
treatment in G91 steel. Despite of having coarser block size, the authors [22] have reported an
increment in the creep rupture strength of the steel in thermomechanical treated condition. In the
present study also, the increment in strength values (YS and UTS) was observed with increase in
packet size/block size due to the changes in microstructural features upon thermomechanical
treatment. The material strength is influenced by various strengthening mechanisms such as solid
solution strengthening, precipitation hardening, dislocation strengthening, and boundary
hardening. The solid solution strengthening depends on the alloy content in the steel. In the
present study, the steel in all conditions possesses same amount of elements such as carbon,
tungsten, tantalum and nitrogen, thereby it can be considered that the strengthening affect caused
by solid solution in same in all cases. The precipitation hardening, dislocation-dislocation
strengthening and boundary strengthening are the major strengthening mechanisms in
thermomechanical treated INRAFM steel, thereby resulting in higher YS and UTS.

Figs 9c and d depict the ductility characteristics of INRAFM steel in N+T, TMT1 and TMT2
conditions, in the temperature range of 300 to 823 K. In comparison to N+T condition, the
thermomechanical treated steel exhibits a higher percent elongation and a lower percent
reduction in area. This suggests that apart from increasing the strength values, thermomechanical
treatment also increase the elevated temperature ductility of the INRAFM steel. The increase in
percent elongation of the steel is significantly higher in TMT1 condition than in TMT2
condition. This improvement in ductility of the steel in the TMT1 condition is primarily due to
the presence of fine and numerous M23C6 precipitates along the PAG and lath boundaries that
provide structural stability at high temperatures. This corroborates with the results of Prakash et
al. [16]. Increase in tempering temperature (in TMT2 condition) weakens the ductility of the
steel due to recovery processes and coarsening of carbide precipitates. However, the ductility of
the steel in TMT2 condition is relatively better than that in N+T condition. The steel in all
conditions exhibits a trough region in the temperature regime 473K-773K, beyond which the
percent elongation increases. The observation of the trough in ductility curve at intermediate
temperatures is usually attributed to the occurrence of dynamic strain aging (DSA) [45].

24
1.4
INRAFM (9Cr - 1.4W - 0.06Ta) N+T
(a)
Strain Rate : 3x10-4 s-1 TMT1
Normalized Yield Strength

1.3 TMT2

1.2

1.1

1.0

0.9
300 400 500 600 700 800 900
Temperature, K

1.4
INRAFM (9Cr - 1.4W - 0.06Ta) N+T
(b)
Normalised Ultimate Tensile Strength

Strain Rate : 3x10-4 s-1 TMT1


TMT2
1.3

1.2

1.1

1.0

0.9
300 400 500 600 700 800 900
Temperature, K

25
28

26
(c) INRAFM (9Cr - 1.4W - 0.06Ta)
Strain Rate : 3x10-4 s-1
N+T
24 TMT1
TMT2
Elongation, %

22

20

18

16

14

12
200 300 400 500 600 700 800 900
Temperaure, K
95
INRAFM (9Cr - 1.4W - 0.06Ta)
(d) Strain Rate : 3x10- s- 4 1

90
N+T
TMT1
Reduction in Area, %

85 TMT2

80

75

70

65
300 400 500 600 700 800 900
Temperature, K
Fig. 9. Variation of (a) yield strength, (b) ultimate tensile strength, (c) percentage elongation and
(d) percentage reduction in area with temperature for INRAFM steel in all the three conditions.

26
4. Discussion

4.1. Microstructural refinement upon thermomechanical treatment and tempering

The structural stability of 9Cr steels during service is greatly influenced by the
thermomechanical treatment. In the present work, the studied steel possesses tempered
martensitic lath structure with distribution of laths/sub-grains/blocks/packets in a prior austenite
grain. Mainly two precipitates M23C6 and MX are present in the INRAFM steel. M23C6
precipitates were abundant in Cr, W and Fe elements and which are decorated along the
boundaries, whereas Ta and V enhanced MX precipitates were present in the intra-lath regions.
From the sequence of observations made from EBSD/FESEM/TEM, the evolution of structural
features upon thermomechanical treatment is represented schematically (Fig. 10). The sample
during austenitization composed of austenite (γ) phase and MX carbonitrides, austenitization
(1423 K for 10 min) prior to warm rolling dissolve the M23C6 carbides (dissolution temperature,
Td = 1342K), while MX precipitates (Td = 1563K) remain in the material [46]. The warm rolling
and tempered steel shows an increment in boundary regions (Fig. 3c & e). This results in the
availability of more nucleation sites for the precipitation of M23C6 precipitates upon tempering.
In addition to this, the density of dislocations in martensitic lath structure is also increased by
warm-rolling. Furthermore, the abundance of dislocations acts as a nucleation sites for the
precipitation of MX carbonitrides. Thus the steel in TMT1 (tempered at 1033 K) and TMT2
(tempered at 1036 K) conditions displays numerous M23C6 carbides with finer size along the
boundaries with an increment in the volume fraction of MX precipitates in the structure. The lath
boundaries may predominantly grow into sub grain boundaries depending on the tempering
conditions. The M23C6 exerts the Zener pinning pressure on the lath/block/packet boundaries and
stabilize the structure, whereas MX precipitates retards the motion of dislocations. Many
investigators [14, 16, 19, 24] have reported that the finer size precipitates with high number
density have greater impact on the stability of the structure. As compared M23C6 precipitates,
MX carbonitrides play a vital role in stabilizing the structure by retarding the dislocations motion
and recovery of lath martensitic structure at elevated temperatures. However, the precipitates
characteristics vary upon tempering at different temperatures even though the TMT treated
samples imparted with same amount of deformation. The number density of M23C6 precipitates

27
increased with increase in tempering temperature. The precipitation reaction is diffusion-
controlled process. As the diffusivity of atoms is high at elevated temperature, copious number
of precipitates nucleate, and their growth occurs at higher tempering temperature. As a result, the
size of the precipitates nucleated is smaller at low tempering temperature whereas with increase
in tempering temperature the coarsening of precipitates occurs by Oswald ripening [47]. Because
of this, the size and number density of M23C6 precipitates are larger in TMT2 condition (Fig. 1e)
than those in TMT1 condition (Fig. 1c). The number density of MX precipitates reduced with
raise in tempering temperature. This could be due to availability of less potential sites
(dislocations) for the precipitation of MX precipitates. It must be emphasized that the present
steel in TMT1 and TMT2 conditions possesses numerous precipitates with smaller size as
compared to as-received conditions (Table 2). Thereby, these finer precipitates help in improving
the structural integrity of INRAFM steel at high temperatures.

Fig. 10. Schematic illustration of the structural features evolution upon thermomechanical
treatment and tempering.

4.2. Influence of thermomechanical treatment and tempering on mechanical properties

As mentioned earlier, the INRAFM steel subjected to thermomechanical treatment and tempered
at different temperatures exhibits an improvement in the tensile properties as compared to N+T
condition. Tan et al. [48] reported that the lath structure, dislocations and precipitates M23C6/MX

28
are the major structural features that assist in enhancing the strength values in 9Cr steels by
stabilizing the structure. The authors also mentioned that the strength contribution from
boundaries such as PAG/packet/block is negligible. In the present work, the steel in N+T
condition exhibit lower strength values due to the presence of coarse M23C6/MX precipitates, low
dislocation density and coarser lath width. Whereas, the steel in TMT1 and TMT2 conditions
possessed high tensile strength values, compared to N+T condition. This can be attributed to the
refinement in precipitates size and increment in their population, finer lath width and an
improvement in dislocation density. The presence of greater population of finer precipitates
enhances the pinning effect on the movement of boundaries by M23C6 precipitates and on the
movement of dislocations by MX carbonitrides. In addition, the movement of dislocations will
also be prevented by their interaction and significantly increases the strength. These findings
support that the precipitate-dislocation or dislocation-dislocation interactions are the main
reasons behind enhancement in the tensile strength values. Furthermore, the strength properties
(YS and UTS) decrease with raise in tempering temperature. The decline in strength is attributed
to the weak strengthening affect caused by precipitates, lath width and dislocations. As the
tempering temperature increase, the precipitates gets coarsen and their capacity to pin the motion
of boundaries and dislocations is diminished. This leads to migration of boundaries and
dislocations, thus in turn decreases the strength values. Moreover, the annihilation/recovery of
dislocations with raise in tempering temperature is found to reduce the strengthening effect.
Nevertheless, it was observed that the strength values decrease with raise in test temperature for
the steel in all conditions. At lower temperature the ability of dislocations to migrate in the lattice
is lower and results in higher strength. Further, the increase in test temperature activates the
diffusion process which aids the dislocations to move easily and lower the strength values. It is
clearly evident form YS and UTS plots, that the steel displays humps/plateaus in the intermediate
temperature regime 473-773 K. Many investigators [16, 43, 45] have found the presence of
plateau region in 9Cr steels, which has been associated with the occurrence of dynamic strain
aging (DSA). Extensive jagged flow behaviour is one of the several manifestations of DSA and it
occurs due to pinning of dislocations with the interstitials atoms [49]. At temperature above 773
K the strength values reduces rapidly, this is due recovery/annihilation of martensitic
structure/dislocations, coarsening of lath structure and precipitates. In precipitation strengthen
alloys, the precipitates function as a sink for the carbon/chromium atoms and significantly delay

29
the onset of DSA [45]. In the present study, the obtained fine precipitates with high number
density by thermomechanical treatment acts as sink and swallow the interstitial
carbon/chromium atoms. This in turn reduces the interactions between interstitial atoms and
dislocations. As a result of this, the steel in thermomechanical treated and tempered at two
different temperatures exhibits a less pronounced DSA effect than N+T condition.

4.3 Strengthening mechanisms

Detailed investigations on the strength contribution from different strengthening mechanisms for
the steel in N+T, TMT1 and TMT2 conditions has been carried out. Solid solution strengthening,
grain boundary strengthening, precipitation strengthening, and dislocation strengthening are the
major strengthening mechanisms that contribute to the strength of the steel. The martensitic lath
width facilitates the grain boundary strengthening in 9Cr RAFM steels. The following equation
was used to evaluate the grain boundary strengthening [2]

𝑀𝐺𝑏
∆𝜎𝑔𝑏 = (5)
𝑚𝑙

where M is the Taylor factor with a value of 3, G is the shear modulus (87 GPa for INRAFM
steel [50]), b is the Burgers vector (2.4810-10 m [51],) and 𝑚𝑙 is the average martensitic lath
width (N+T = 378 nm, TMT1 = 247 nm and TMT2 = 294 nm).

The primary precipitates present in 9Cr steels are M23C6 and MX carbonitrides. According to the
dispersed barrier hardening (DBH) model [52], and the Orowan strengthening mechanism [53],
the strengthening effect caused by M23C6 carbides and MX carbonitrides, respectively, may be
explained by
∆𝜎𝑀23 𝐶6 = MαGb √𝑁𝑑 (6)
0.7𝑀𝐺𝑏√𝑓𝑣
∆𝜎𝑀𝑋 = (7)
𝑑

where α is the barrier strength factor with a value of 1, N is the number density of the
precipitates, d is the respective average particle size (as indicated in Table 2) and fv is the
volume fraction .

30
The above empirical equations have been used for the evaluation of strengthening effect caused
by each parameter and the obtained results are depicted in Fig. 11. The calculated strengthening
effect caused by martensitic lath width, M23C6 and MX precipitates for the steel in N+T
condition are found to be 171MPa, 46.04 MPa and 45.67 MPa respectively; in TMT1 condition,
these values are 262 MPa, 51.74 MPa and 70.41 MPa; and in TMT2 condition, these values are
220 MPa, 62.96 MPa and 53.24 MPa respectively. It is also evident from the plot, that the steel
in TMT1 shows more pronounced overall strengthening effect; this was followed by the steel in
TMT2 condition compared to that in N+T condition. This can be attributed to the refinement of
structural features upon TMT. In addition, the strength contribution by dislocations and solid
solution strengthening are extra, which are also to be considered to arrive at final strength. It may
be noted that the strength contribution from the martensitic lath width is more than the
precipitate strengthening for the steel in all three conditions. However, the increase in tempering
temperature (TMT2) lowers the strengthening value due to coarsening of precipitates and lath
width structure.

500
INRAFM (9Cr-1.4W-0.06Ta) ∆σMX
∆σM23C6
400 ∆σgb
Strength value, MPa

300

200

100

0
N+T TMT1 TMT2
Material condition
Fig. 11. Strength contribution from grain boundary (∆𝜎𝑔𝑏 ), M23C6 and MX precipitates
(∆𝜎𝑀23 𝐶6 𝑎𝑛𝑑 ∆𝜎𝑀𝑋 ) in the INRAFM steel in different conditions.

31
5. Conclusions

The effect of thermomechanical treatment and subsequent tempering temperature on


microstructural features and tensile properties of INRAFM steel were investigated. The results
are compared with the same steel used in conventional normalized and tempered (N+T)
condition. The conclusions drawn from the results are as follows:
(i) Microstructural characterization using electron microscopy (FESEM and TEM) suggests
that the thermomechanical treated steel shows larger prior austenite grains/blocks/ packets
that are decorated with numerous finer M23C6 precipitates and refinement in lath structure
embedded with MX precipitates.
(ii) Higher Kernel Average Misorientation value of the steel in TMT1 condition observed by
electron backscatter diffraction suggests that the steel possesses high dislocation density
and a strong fibre texture due to change in grain orientation upon deformation.
(iii) The steel in TMT1 condition shows higher microstructural stability compared to N+T and
TMT2 conditions and resulted in higher hardness and tensile properties.
(iv) As compared to N+T condition, the steel in TMT1 condition provides considerable increase
in yield strength (22.8% at 300 K, 22.64% at 673 K and 17.42% at 873 K) and ultimate
tensile strength (10.24% at 300 K, 14.0% at 673 K and 22.12% at 873 K); whereas the steel
in TMT2 condition evinces a marginal increase in yield strength (5.14%, 5.72% and
5.85%) and ultimate tensile strength (2.22%, 1.65% and 7.21%) at respective test
temperatures due to its high temperature tempering effect.
(v) Apart from exhibiting higher yield and tensile strengths, the steel in TMT1 condition
display additional benefit of higher ductility. The percentage increase in elongation are
found to be 9 at 300 K, 26 at 673 K and 12.35 at 873 K, whereas the percentage
decrement in reduction in area are found to be 9.0, 2.6 and 5.4 at the respective test
temperatures with respect to N+T condition.
(vi) The improved strength together with enhanced ductility, upon TMT, make the INRAFM
steel a candidate material for the components of nuclear fusion reactors.

32
Data availability

The data supporting the findings of this study are available from the corresponding author upon
request.

CRediT authorship contribution statement


P. Anil Kumar: Investigation, Analysis, Visualization, Writing - original draft. J. Vanaja:
Investigation & Review & Editing. G. V. Prasad Reddy: Conceptualization, Supervision,
Writing - Review & Editing. G. V. S. Nageswara Rao: Conceptualization, methodology,
Funding acquisition, Supervision, Project administration, Writing - Review & Editing.

Declaration of competing interest


The authors declare that they have no known competing financial interests or personal
relationships that could have appeared to influence the work reported in this paper.

Acknowledgements
This work was supported by University Grants Commission (UGC)-Department of Atomic
Energy (DAE) Consortium for Scientific Research (Sanction No. CSR-KN/CRS-93/2016-
17/1134). The authors profoundly thank Nuclear Fuel Complex, Hyderabad for providing TEM
facility. The authors also acknowledge the Director, National Institute of Technology Warangal
for constant support.

Data availability

The data supporting the findings of this study are available from the corresponding author upon
request.

CRediT authorship contribution statement


P. Anil Kumar: Investigation, Analysis, Visualization, Writing - original draft. J. Vanaja:
Investigation & Review & Editing. G. V. Prasad Reddy: Conceptualization, Supervision,
Writing - Review & Editing. G. V. S. Nageswara Rao: Conceptualization, methodology,
Funding acquisition, Supervision, Project administration, Writing - Review & Editing.

33
Declaration of competing interest
The authors declare that they have no known competing financial interests or personal
relationships that could have appeared to influence the work reported in this paper.

Acknowledgements
This work was supported by University Grants Commission (UGC)-Department of Atomic
Energy (DAE) Consortium for Scientific Research (Sanction No. CSR-KN/CRS-93/2016-
17/1134). The authors profoundly thank Nuclear Fuel Complex, Hyderabad for providing TEM
facility. The authors also acknowledge the Director, National Institute of Technology Warangal
for constant support.

Declaration of Competing Interest

☐ The authors declare that they have no known competing financial interests or personal
relationships that could have appeared to influence the work reported in this paper.

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