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J. Mater. Sci. Technol., 2010, 26(9), 810-816.

Effect of Aging on the Toughness of Austenitic


and Duplex Stainless Steel Weldments
Omyma Hassan Ibrahim1) , Ibrahim Soliman Ibrahim2) and Tarek Ahmed Fouad Khalifa3)
1) Metallurgy Dept., Nuclear Research Centre, Atomic Energy Authority, Egypt
2) Nuclear Safety Centre, Atomic Energy Authority, Egypt
3) Shoubra Faculty of Engineering, Benha University, Egypt
[Manuscript received August 31, 2009, in revised form February 26, 2010]

In the present study, the effect of aging heat treatment at 650, 750, and 850 C on the impact toughness of
316L austenitic stainless steel, 2205 duplex stainless steel and their weldments has been investigated. Welding
process was conducted using the TIG (tungsten inert gas) welding technique. Instrumented impact testing,
at room temperature, was employed to determine the effect of aging treatment on the impact properties of
investigated materials. Aging treatment resulted in degradation in the impact toughness as demonstrated by
the reduction in the impact fracture energy and deformation parameters (strain hardening capacity, fracture
deflection, and crack initiation and propagation energy). The degree of embrittlement was more noticeable
in duplex stainless steel parent and weld-metal than in 316L stainless steel and became greater with the
increase of aging temperature. The degradation in impact toughness was discussed in relation to the observed
precipitation of the intermetallic sigma phase in the microstructure of the stainless steel weldments and the
corresponding fracture surface morphology.
KEY WORDS: Austenitic and duplex stainless steels; Aging; Instrumented impact; Toughness

1. Introduction
Austenitic and austenitic-ferritic (duplex) stainless steels are widely used in many engineering applications. These steels present excellent combination
of corrosion resistance, ductility, toughness and weldability. They are used as structural materials and
components of heat transfer equipment in the chemical and petrochemical industries. In the nuclear industry, theses steels are employed as cladding materials in reactor pressure vessels and control rod assemblies as well as cooling system piping.
A serious drawback to using such steels and their
weldments is the degradation of corrosion and mechanical properties within certain high temperature
due to the microstructural changes.
Austenitic stainless steels may be susceptible to intergranular corrosion (sensitization)
caused by chromium depletion next to grain
Corresponding author.
Ph.D.;
E-mail
omyma essam@yahoo.com (O.H. Ibrahim)

address:

boundaries due to precipitation of M23 C6 carbides


during usage in the temperature range 540 to
860 C[1] . In the case of molybdenum-containing
austenitic stainless steels, such as AISI 316 and 316L
types, long exposure time in 650 to 900 C can lead
to the precipitation of the intermetallic sigma ((Fe,
Ni)x (Cr, Mo)y ) phase. During solidification or welding, delta ferrite phase formation might occur, which
renders the steel even more prone to precipitation of
sigma phase[2] .
In comparison to austenitic stainless steels, precipitation of sigma phase in duplex stainless steels
(DSS) occurs, within the ferrite phase at shorter
time, at higher temperatures and with larger volume
fractions[2] . For example, an aging treatment for 3 h
in the temperature range 800 to 850 C is sufficient
for the formation of 15% to 20% of sigma phase[2] . In
contrast to the carbides that form an almost continuous network in the austenite regions, sigma phase
is finely distributed within the ferrite. The emergence of carbide precipitates and sigma phase in the
austenitic and duplex stainless steels can render

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O.H. Ibrahim et al.: J. Mater. Sci. Technol., 2010, 26(9), 810816

Table 1 Chemical composition of base metals


316L
Duplex (2205)

C
0.020
0.020

Mn
1.50
1.50

Si
0.40
0.40

Ni
10.0
6.0

Cr
17.0
23.0

Mo
2.10
3.00

Fe
Bal.
Bal.

Table 2 Chemical composition of weld metal fillers


AWS E 316L
ER 2209 Duplex

C
0.020
0.030

Mn
1.80
1.50

them susceptible to embrittlement since such phases


suffer brittle fracture and offer a path for brittle crack
propagation, thus reducing ductility and toughness.
It should be mentioned that the weld metal behavior
of these steels is not as good as the base metal by
virtue of the relatively higher ferrite content[2] .
The present investigation is concerned with an
evaluation of the effect of aging heat treatment at
650, 750, and 850 C on the impact toughness of 316L
austenitic stainless steel, 2205 duplex stainless steel
and their weldments conducted through TIG (tungsten inert gas) welding technique. The correlation between the changes in the microstructure during aging
treatment, and impact toughness of the investigated
materials was assessed by instrumented impact testing.
2. Experimental
The chemical composition of the investigated materials is presented in Tables 1 and 2.
The 316L austenitic and 2205 duplex stainless
steel base were subjected to solution heat treatment at
1050 and 1150 C, respectively for one hour and then
water quenched. Isothermal aging treatment was applied to the above base and weld metals at 650, 750,
and 850 C for 3 h followed by furnace cooling.
Instrumented impact tests were conducted on unaged and aged specimens of the investigated material with dimensions of 55 mm10 mm4.5 mm at
room temperature the total capacity of the impact
machine (Amsler RKP-300, Switzerland) was 300 J
with a hammer velocity of 5.1 m/s.
3. Results and Discussion
3.1 Microstructure
The microstructure of the investigated austenitic
and duplex stainless steel (DSS) weldments is presented in Fig. 1. The 316L base metal (Fig. 1(a1))
is characterized by equiaxed austenite grains with an
average grain size of 50 m. As can be seen that the
structure is free from annealing twins. Aging of the
316L base metal, at 850 C, developed grain boundary precipitation of M23 C6 carbides (Fig. 1(a2)) indicating the occurrence of sensitization in this type of
stainless steel.
Figure 1(b1) shows an optical micrograph of 316L
TIG weld metal which displays a mixture of austenite

Si
0.07
0.90

Ni
11.7
9.50

Cr
18.70
23.0

Mo
2.70
3.00

Fe
Bal.
Bal.

phase and vermicular ferrite morphology that developed during the welding process. Aging of this 316L
TIG weld metal at 850 C results in the formation of
small amounts of sigma phase which precipitate in
the ferrite regions (Fig. 1(b2)). The precipitation in
sigma phase resulted from the transformation of delta
ferrite presented in the weld metal[1] .
Figure 1(c1) shows a micrograph of 2205 duplex
stainless steel base metal and it presents very fine
grained structure of 5 m of austenite within ferrite
matrix. This structure changed after aging at 850 C
into austenite phase and ferrite masses with apparent
white areas resembling sigma phase precipitates, as
shown by scanning electron microscopy (SEM) examination (Fig. 1(c2)). The 2205 duplex stainless steel
weld metal microstructure is shown in (Fig. 1(d1))
and it comprises acicular austenite structure within a
matrix of ferrite. Aging at 850 C of this weld metal
leads to the precipitation of sigma phase as white areas shown in (Fig. 1(d2)) through examination by
SEM. In this figure, sigma phase is seen as massive
morphology of particles larger in size than that in the
aged duplex stainless steel base metal.
3.2 Impact properties
Table 3 and Fig. 2 show the effect of aging temperature on the impact fracture energy of the austenitic
and duplex stainless steels base metal and weld metals tested at room temperature. In the un-aged condition, the impact fracture energy of the base metal
is higher than that of the weld metal by 13% (63 vs
55 J) and 30% (107 vs 75 J) for the austenitic and
duplex stainless steels, respectively. This can be ascribed to the relatively higher content of delta ferrite
in the weld metal than that in the base metals. In addition, the internal residual stresses produced during
the welding process could give rise to the weld metal
yield strength, leading to a reduction in the impact
energy[3] .
It also can be seen that, the impact fracture energy values of the duplex stainless steel, base and weld
metals, are higher than those of the austenitic stainless steel by 41% (107 vs 63 J) and 27% (75 vs 55 J),
respectively. This can be attributed to the much finer
grain size of the duplex stainless steel base metal compared to that of the austenitic stainless steel (5 vs
50 m), which leads to a higher resistance to the propagation of brittle cracks and consequently a higher

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O.H. Ibrahim et al.: J. Mater. Sci. Technol., 2010, 26(9), 810816

Fig. 1 Microstructure of 316L and duplex stainless steels base and weld metals: (a1) 316L BM, (a2) 316L BM 850 C,
(b1) 316L WM, (b2) 316L WM 850 C, (c1) DSS BM, (c2) DSS BM 850 C, (d1) DSS WM, (d2) DSS WM 850 C

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O.H. Ibrahim et al.: J. Mater. Sci. Technol., 2010, 26(9), 810816

Table 3 Impact fracture energy of tested materials at room temperature


Base metals impact fracture energy/J Weld metals impact fracture energy/J
AR
650 C
750 C
850 C
AW
650 C
750 C
850 C
316L
63
63
55
36
55
47
22
21
Duplex
107
38
16
7
75
7
3
3
Notes: ARas-received condition, AWas-welded condition
80

120

(a)

(b)

100

Duplex base metal

60

Duplex weld metal

Impact Energy / J

Impact energy / J

70

50
40
30
20

316L base metal


316L weld metal

10
0

200

400

80
60
40
20

600

Aging temperature /

800
o

1000

200

400

600

Aging temperature /

800
o

1000

Fig. 2 Variation of impact fracture energy with ageing temperature: (a) austenitic stainless steel, (b) duplex
stainless steel

impact toughness[2] .
Table 3 shows that aging heat treatment leads to
a gradual decrease in the impact fracture energy for
both the austenitic and duplex stainless steels. A reduction of 43% (63 vs 36 J) and 62% (55 vs 21 J) is
observed for the impact energy of the base and weld
metal of the austenitic stainless steel, respectively after aging at 850 C for 3 h. The corresponding reduction in impact energy values of the duplex stainless
steel base and weld metal is 93% (107 vs 7 J) and
96% (75 vs 3 J), respectively. This shows that the degree of reduction in impact energy is much higher in
the duplex stainless steel than that in the austenitic
stainless steels.
3.3 Load time traces
Figure 3 presents load-time traces of the investigated materials produced from instrumented impact
testing before and after aging treatment at 850 C.
These traces are a manifestation of the embrittlement
features produced by the aging process. These features are summarized in Table 4 and they comprise
the following: (1) an increase in both yield (Py ) and
maximum (Pmax ) loads after aging at 850 C; (2) a
reduction in the strain hardening capacity, as indicated by the increase in the ratio between the yield
and the maximum loads (Py /Pmax ); (3) a reduction in
the initiation (Ei ) and propagation (Ep ) energy values due to the aging process; (4) a reduction in the
total dynamic deflection (TDD) which represents the
total amount of strain exerted at each test condition.
These observations could be associated with the
microstructural (Fig. 1) and fractural (Fig. 4) features
as defined by optical microscopy and SEM, in addi-

tion to the measured ferrite content of the investigated


materials before and after aging processes.
3.4 Austenitic stainless steel weldments
The decrease in the impact fracture energy of
316L austenitic stainless steel base metal from 63 to
36 J (Table 3) is accompanied by appearance of grain
boundary precipitation (Fig. 1(a2)), which is shown
by EDX analysis to contain increased content of Cr
element indicating presence of M23 C6 carbides. The
fracture surface (Fig. 4(b)) reveals mixed mode of
ductillity (dimples) and brittlement (cleavage facets).
Grain boundary carbide precipitation has long been
known to initiate cleavage fracture[1] , which leads to a
reduction in the impact energy of austenitic stainless
steels. Measurement of the ferrite content of the 316L
base metal showed a value of about 1.65% which decreased down to 0.25% after aging at 850 C for 3 h.
This indicates very little formation of sigma phase
which might be transformed from delta ferrite and
contributed to the embrittlement processes[4] .
On the other hand, the amount of reduction in
the impact fracture energy of the 316L weld metal,
after aging at 850 C, was much greater than that
of 316L base metal (62% vs 43%). The ferrite content of the 316L TIG weld metal decreased, due to
aging, from 6% to 0.75% which indicates the transformation of delta ferrite to sigma phase at this aging temperature[4] . The corresponding fractograph
of this condition (Fig. 4(d)) reveals the mixture of
very fine shallow dimples and very small cleavage
facets which accounts for the observed embrittlement.
Sigma phase is susceptible to brittle fracture and thus
offers a path for brittle crack propagation and hence

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O.H. Ibrahim et al.: J. Mater. Sci. Technol., 2010, 26(9), 810816

Fig. 3 Instrumented impact test traces for 316L and duplex stainless steels base and weld metals: (a) 316L BM
(63 J), (b) 316L BM 850 C (36 J), (c) 316L WM (55 J), (d) 316L WM 850 C (21 J), (e) DSS BM (107
J), (f) DSS BM 850 C (7 J), (g) DSS WM (75 J), (h) DSS WM 850 C (3 J)

O.H. Ibrahim et al.: J. Mater. Sci. Technol., 2010, 26(9), 810816

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Fig. 4 Fracture surface of 316L and duplex stainless steels base and weld metals as revealed by SEM: (a) 316L
BM (63 J), (b) 316L BM 850 C (36 J), (c) 316L WM (55 J), (d) 316L WM 850 C (21 J), (e) DSS BM
(107 J), (f) DSS BM 850 C (7 J), (g) DSS WM (75 J), (h) DSS WM 850 C (3 J)

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O.H. Ibrahim et al.: J. Mater. Sci. Technol., 2010, 26(9), 810816

Table 4 Instrumented impact test parameters for the tested materials at room temperature
Py
Pmax
Py /Pmax
Ei
Ep
Et
TDD
/kN
/kN
/%
/J
/J
/J
/mm
316L BM
3.7
7.3
52
32
31
63
17.5
316L BM-850 C
21
35
60
13.5
22.5
36
1.5
316L WM
4.2
6.5
51
29
26
55
20
316L WM-850 C
4.8
6.5
65
13.5
7.5
21
7.5
Duplex BM
7
11
64
40
67
107
20
Duplex BM-850 C
13
15.5
84
5.7
1.3
7
0.75
Duplex WM
6
10.3
58
22
53
75
15
Duplex WM-850 C
13
13
100
3
0.2
3
0.35
Notes: Py yield load, Pmax maximum load, Py /Pmax strain hardening capacity, Ei crack initiation energy,
Ep crack propagation energy, Et total fracture energy, TDDtotal dynamic deflection

reducing toughness[5] .
3.5 Duplex stainless steel weldments
The embrittlement behavior of the duplex stainless steel weldments due to aging treatment was more
evident than that of 316L austenitic stainless steel
weldments. The reduction in the impact fracture energy of the duplex stainless steel base and weld metal
was 93% and 96%, respectively after aging at 850 C.
Load-time traces of both duplex stainless steel base
and weld metals display complete brittle behavior
(Fig. 3(f) and (h)) with evidence of load drop. This
brittle aspect is represented by the change in the fracture surface features (Fig. 4(f) and (h)). Figure (4)
shows variation from the well defined deep dimples
of the un-aged duplex stainless base and weld metals (Fig. 4(e) and (g)) to cleavage facets that appear
larger in the weld metal (Fig. 4(f) and (h)). The microstructures of the aged duplex stainless steel base
and weld metals (Fig. 1(c2) and (d2)) display heavy
precipitation of sigma phase at the boundaries of the
ferrite phase[6] . This was supported by the EDX
analysis which gave high percent of molybdenum element essential for the formation of sigma phase[7] .
The dense precipitation of sigma phase was also indicated by the large drop in the ferrite content, from
49.5% to 7.5% for the base metal and from 45.5% to
11.5% for the weld metal which is in agreement with
other comparative data[8,9] .
4. Conclusions
In the present study, an evaluation of the effect of
aging heat treatment at 650, 750, and 850 C on the
impact toughness of 316L austenitic stainless steel,
2205 duplex stainless steel and their weldments using
TIG (tungsten inert gas) welding technique has been
given. The main conclusions are:
(1) In the un-aged condition, the duplex stainless steel parent and weld metal specimens exhibit
higher impact energy level than the corresponding
316L austenitic stainless steel specimens.
(2) Aging treatment results in gradual embrittle-

ment as demonstrated by the reduction in the impact


fracture energy and deformation parameters.
(3) The degree of embrittlement is more noticeable in duplex stainless steel parent and welds metals
than in 316L stainless steel, becoming greater with
the increase of the aging temperature.
(4) The degradation in impact toughness is discussed in relation to the observed precipitation of the
intermetallic sigma phase which appears more intense
in the microstructure of duplex stainless steel weldments.
(5) SEM examination reveals that the reduction in
impact energy due to aging is associated with the formation of shallow ductile dimples and cleavage facets
on the fracture surface of 316L and duplex stainless
steels, respectively.

Acknowledgement
The authors gratefully acknowledge the technical assistance and provision of the welding facilities by Prof. Dr.
A.A. Sadek, Central Metallurgical Research and Development Institute (CMRDI).
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[4 ] S. Kozuh, M. Gojic and L. Kosec: Mater. Geoenvironment, 2007, 54(3), 331.
[5 ] R. Badji, M. Bouabdallah, B. Bacroix, C. Kahloun, B.
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[6 ] J. Michalska and M. Sozanska: Mater. Charact., 2006,
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[7 ] J.D. Kordatos, G. Fourlaris and G. Papadimitriou:
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[8 ] M. Martins and L.C. Casteletti: Mater. Charact.,
2009, 60, 792.
[9 ] M. Pohl, O. Storz and T. Glogowsldt: Mater. Charact., 2007, 58, 65.

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