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Article history:
Received 2 June 2014
Received in revised form 7 August 2014
Accepted 14 August 2014
Available online 15 August 2014
Keywords:
RAFM steel weld
Transmission Electron Microscopy
INRAFM steel
PWHT of RAFM steel
Microstructural characterization
a b s t r a c t
This paper presents a detailed electron microscopy study on the microstructure of various regions of weldment
fabricated by three welding methods namely tungsten inert gas welding, electron beam welding and laser beam
welding in an indigenously developed 9Cr reduced activation ferritic/martensitic steel. Electron back scatter diffraction studies showed a random micro-texture in all the three welds. Microstructural changes during thermal
exposures were studied and corroborated with hardness and optimized conditions for the post weld heat
treatment have been identied for this steel. HollomonJaffe parameter has been used to estimate the extent
of tempering. The activation energy for the tempering process has been evaluated and found to be corresponding
to interstitial diffusion of carbon in ferrite matrix. The type and microchemistry of secondary phases in different
regions of the weldment have been identied by analytical transmission electron microscopy.
2014 Elsevier Inc. All rights reserved.
1. Introduction
The reduced activation ferritic/martensitic (RAFM) steels, which
were initially developed for special high active waste storage of radioactive structures of fusion reactors, has been considered as the primary
material for construction of rst wall and test blanket module in the fusion reactors [13]. The chemical composition of 9Cr RAFM steel has
been arrived at by modifying the conventional grade 91 steel (9Cr
1Mo0.06Nb0.2 V0.05 N) with the substitution of Mo and Nb, the
high induced radioactive elements by W and Ta [4,5]. Tungsten addition
increases not only the creep rupture strength but also the ductile to brittle transition temperature (DBTT). Tantalum plays an important role in
lowering the DBTT of the RAFM steel by way of rening the prioraustenite grain size. The physical metallurgy of ferritic/martensitic
steels with respect to stability of microstructure on thermal and irradiation exposures, inuence of chemical composition and heat treatments
has been extensively studied by several researchers [6,7]. The 9Cr RAFM
steels possess desirable properties such as good mechanical properties,
adequate creep resistance up to 873 K, good weldability and limited radiological activation in addition to better void swelling resistance
[812]. Ferritic/martensitic steels in general, bear a complex microstructure and the mechanical properties are inuenced by the prior austenite
grain size (PAGS), martensite lath size, dislocation density, chemistry
and size of the precipitates.
Corresponding author.
E-mail address: vtp@igcar.gov.in (E. Rajendra Kumar).
http://dx.doi.org/10.1016/j.matchar.2014.08.013
1044-5803/ 2014 Elsevier Inc. All rights reserved.
214
Table 1
Chemical composition of the two RAFM steels used in this study [22].
Steel
Cr
Mn
Ta
Ti
Ni
Mo
Nb
1W
IN-RAFM
9.04
9.03
0.08
0. 12
0.55
0.56
0.22
0.24
1.0
1.39
0.06
0.06
0.022
0.029
0.005
0.002
b0.002
b0.002
b0.002
b0.001
0.005
0.005
0.005
0.005
0.001
0.002
0.001
0.001
Table 2
Welding parameters.
Welding technique
TIG
EB
Laser
0.15
0.9
10
0.6
0.36
1
0.21
30
2. Experimental
9Cr RAFM steels with 1 and 1.4 mass% of tungsten procured from M/s
MIDHANI, Hyderabad in the form of 12 mm and 6 mm thick plates have
been used in the present study. The steel was used in the standard heat
treated condition namely normalizing at 1253 K/1 h followed by tempering at 1033 K/1 h. Chemical composition of the two steels is given in
Table 1. Based on an earlier work on structureproperty correlations the
1.4% W steel has been designated as an Indian RAFM or INRAFM steel
which possesses good creep resistance with adequate ductility for fabrication of the test blanket module [21,22]. Autogenous bead-on-plate welds
were fabricated with both steels using 200 mm 200 mm 12 mm steel
plates. EBW and LBW joints of INRAFM steel were fabricated using 6 mm
plate as per optimized conditions [23] to obtain high quality welds. Details
Fig. 1. Microstructure of the normalized and tempered 9Cr1W RAFM steel. a) SEM micrograph showing tempered martensite structure. b) Thin foil TEM micrograph showing triple point
(arrow marked) of prior austenite grains and martensitic laths. c) Lenticular inter & intralath precipitates. d) Course globular precipitates in a well recovered region.
of the welding processes are given in Table 2. Autogenous TIG weld process was specically chosen to avoid compositional changes if any in
the weld metal as well as to simulate conditions similar to EBW and
LBW where ller material is not used.
Classication of different regions of the weldment as a function of
distance from fusion zone has been made for study of microstructural
and microchemical features. Further TIG welded joints were heat treated at three different temperatures in the range of 8731033 K for durations of 15, 30, 60 and 120 min to optimize the PWHT condition for the
indigenous steel. EB and laser welded joints were subjected to the optimum PWHT at 1033 K for 60 min.
215
Fig. 2. TEM micrograph of carbon extraction replica of 1W RAFM steel showing. a) inter and intra lath boundary carbides (diffraction evidence from MX (left) and M23C6(right) in
inset). b & c) EDS spectrum from Cr rich M23C6 carbide and V rich MX carbide respectively. d) Histogram showing the size distribution of carbides in normalized and tempered steel.
216
were prepared from each region of the weld and were used extensively
to identify the type and chemistry of carbides. TEM studies were carried
out on thin foils as well as carbon extraction replicas using Philips CM
200 under an operating voltage of 120200 kV, with INCA energy
dispersive spectrometer (EDS). The EDS spectra were quantied by
Fig. 3. Hardness prole and micrographs from various regions of TIG weldment of RAFM steel. a) Hardness plot across weldment of 1 and 1.4W steel, b) weld showing columnar grains and
a typical martensitic structure (inset), c) coarse grained heat affected zone, d) ne grained heat affected zone showing ferrite grains (arrow marked) with lower defect density, e) crystal
orientation map (standard IPF Z coloring) from the weld region showing random texture and f) subset region of a prior austenite grain with coarse martensite substructure.
217
Fig. 4. Bright eld TEM micrographs of carbon extraction replicas from HAZ showing. a) Dissolution of carbides in the CGHAZ region except a few retained primary TaC precipitates. b) High
number density of carbides in FGHAZ.
218
microtexture, while Fig. 3f clearly conrms the large size of the prior
austenite grains in the weld region. The difference in prior austenite
grain size in the different regions of the weldment can be understood in
terms of the peak temperature attained by the region as a function of distance from the heat source. Immediate to FGHAZ a very narrow region
Fig. 5. Hardness proles and microstructures of EB weldment of 1.4W RAFM steel. a) Hardness prole across the weldment b) columnar microstructure in the weld. c & d) EBSD crystal
orientation map (standard IPF Z coloring) from weld region and a typical prior austenite grain. e) CGHAZ with typical martensitic structure but PAGS comparable to base metal and
f) FGHAZ with signatures of large number of precipitates.
219
beam welds was measured as ~ 0.7 mm, which is far lower than the
TIG (1.6 mm) bead on plate welds.
The microstructural parameters are compared in Table 3. The important differences observed in EBW and LBW as compared to TIG welding
are highlighted below:
a) LBW showed low width of the weld resulting in a narrow HAZ. EBW
also exhibited similar characteristics except the entry side of the
beam.
b) Smaller PAGS of the weld metal in EBW and LBW compared to TIG
welds could be due to lower residence time at peak temperature
and high cooling rates associated with the welding technique. The
lower residence time at peak temperature and high cooling rates
are also manifested in ner lath size in EBW and LBW as compared
to TIG weld.
3.3. Optimization of Post Weld Heat Treatment Conditions
It is well known that PWHTs are necessary in ferritic/martensitic
steels to remove the residual stresses, to improve toughness and to
Fig. 6. Extraction replica micrograph taken from heat affected zone of EB weldment of 1.4W RAFM steel showing, a & b) the presence of few ne carbides in CGHAZ and large number of
coarse carbides in FGHAZ. c & d) Size distribution of carbides in CGHAZ and FGHAZ.
220
Fig. 7. a) Microhardness prole across laser weld of 1.4W RAFM steel. b) Fully martensite structure in weld. c & d) EBSD crystal orientation map from weld region and a typical prior
austenite grain. e) Martensite with carbides in CGHAZ and f) FGHAZ showing martensite with ne PAGS.
from the weldments, heat treated at 873, 973 and 1033 K for 1 and 2 h
durations.
Fig. 8bd shows the SEM micrographs of weld region heat treated for
973 K/2 h, 1033 K/1 h and 1033 K/2 h respectively. The lath morphology
of martensite is evident in the specimen treated at lower temperatures,
TIG weld
(1.4W)
EB weld
(1.4W)
Laser weld
(1.4W)
6
1.6
490 10
515 10
10
41
26
10
~300500
4.0
1.4
474 10
484 10
18
19
21
10
~150350
1.2
0.7
497 10
520 10
19
20
19
7
~200400
221
P H TC log t
where
P
H
T
t
C
HollomonJaffe parameter
HARDNESS value (VHN)
Temperature (K)
time (h)
a constant which depends on the composition of the steel and
thermal history.
Fig. 8. Optimization of PWHT for 1W RAFM steel. a) Microhardness prole before and after various PWHTs. b, c & d) Micrographs of weld region after PWHT of 973 K/2 h, 1033 K/1 h and
1033 K/2 h.
222
Fig. 9. Effect of temperature and duration of tempering on hardness and recovery rate.
a) Variation of hardness of weld zone (RAFM 1W) with respect to time and temperature.
b) Hardness vs HollomonJaffe parameter: T temperature in K & t time in h.
c) Arrhenius plot of the rate of recovery of weld region.
223
Table 4
Comparison of microstructural/microchemical parameters of two ferritic steels [27].
Steel
Heat treatment
PAGS
(average)
(m)
Lath size
(nm)
Hardness
(VHN)
M23C6
MX
9Cr1WVTa
1253
1033
1333
1033
14
700800
230 5
1030 nm
40
5001000
205 5
30300 nm
Cr, W rich
40400 nm
Cr, Mo rich
9Cr1MoVNb
K/1
K/1
K/1
K/1
h (n)
h (t)
h (n)
h (t)
4080 nm
Acknowledgments
The authors would like to express their thanks to Dr. P.R. Vasudeva
Rao, Director, Indira Gandhi Centre for Atomic Research, for his constant
support.
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