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Abstract
Effects of nitrogen and high temperature aging on phase precipitation of duplex stainless steels have been investigated. The precipitation
of phase increases with the increase of aging time. The precipitation rate at 900 C aging is the fastest and that at 700 C aging is the lowest.
The higher the aging temperature, the larger the size of phase precipitates. At the same condition, the more the nitrogen content, the lower
the content of phase in duplex stainless steel.
2005 Elsevier B.V. All rights reserved.
Keywords: Aging; Phase; Precipitation; Intermetallic phase
1. Introduction
The reason why duplex stainless steel (DSS) can possess
excellent properties is principally because it is influenced by
a phase balance between austenitic phase ( phase) and ferritic phase ( phase). It is generally considered that any of
the two phases which is lower in percentage must not be less
than 30% [1]. Although ferritic phase has better partial corrosion resistance and mechanical strength [2,3], it is liable to
produce phase and has lower ductility, among other disadvantages [4]. On the other hand, austenitic phase has better
ductility, toughness and reducing acid resistance [5,6].
Nitrogen, an austenitic stabilizing element, if added, can
help to stabilize austenitic phase in DSS [7,8]. Addition of
nitrogen will not only increase the mechanical properties of
DSS but also enhance resistance against pitting and crevice
corrosion [8,9].
After aging at high temperature 6001000 C, DSS will
precipitate a number of intermetallic phases, such as phase,
phase, , M7 C3 , M23 C6 , Cr2 N, etc. [1013], in which
damage of phase is most severe. Not only will phase
0921-5093/$ see front matter 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2005.03.111
C.-S. Huang, C.-C. Shih / Materials Science and Engineering A 402 (2005) 6675
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Table 1
Chemical composition of duplex stainless steels used (wt.%)
Sample
Si
Mn
Ni
Cr
Mo
A
B
C
0.02
0.022
0.021
0.41
0.47
0.48
2.04
2.00
2.07
0.021
0.026
0.027
0.0061
0.006
0.006
5.507
5.51
5.51
22.6
22.6
22.6
3.251
3.254
3.25
0.14
0.18
0.22
2. Experimental procedure
2.1. Material
The specimens used in this research are made using
high-frequency vacuum refinement to deploy 2205 duplex
stainless steel with different nitrogen contents, 0.14, 0.18
and 0.22%, respectively. To begin with, DSS is cut into
small pieces (which must not be powder), which are in turn
immersed in acetone solvent for ultrasonic vibration cleaning to remove grease on the stainless steel. After that, alloy
elements that have been calculated are deployed, including pure iron powder, ferromanganese, ferromolybdenum,
ferrochromium, manganese nitride and pure nickel. After
the alloy composition is calculated and weighed, all alloy
elements are then placed in a crucible pending smelting.
The DSS alloy composition of this research is shown in
Table 1.
For specimens containing different percentages of nitrogen after smelting, parts near the riser and not smooth are
cut, burrs removed and a grinder is used to make their
surface smoother. Then, they are heated in a furnace to
1250 C, and 1.5 h after being kept at constant temperature,
undergo hot forging to forge them to about 3 mm in thickness.
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C.-S. Huang, C.-C. Shih / Materials Science and Engineering A 402 (2005) 6675
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Mo and depleted in Ni and as result favours phase precipitation [12,13]. This results in the co-precipitation of
and austenite. Therefore, with the increase of phase,
phase will also increase. And at this moment, ferritic phase
will decrease. From this experiment, it can be observed in
Fig. 4 that the phase indeed will increase with aging time,
in particular in the period from 0 to 10 h, when its precipitation increment is the most. But from 10 to 24 h, the phase
increment tends to slow down. This phenomenon, regardless of nitrogen content, tends to always come to this result,
which does not run counter to the research of predecessors
[17,21].
Fig. 3(ac) accounts for 0.14, 0.18 and 0.22% nitrogen
contents, respectively. Under 800 C aging, comparing these
figures, if given the same aging time, it can be found that the
more the nitrogen content, the less is the phase content. This
is because nitrogen is an austenitic stabilizing element. It will
directly increase the austenitic phase content and decrease
the percentage of ferritic phase in DSS, thereby indirectly
leaving less room for phase after precipitation to develop.
Consequently, the addition of nitrogen content does help slow
down the precipitation rate of phase.
The above can be verified with numerical comparisons by
means of image analysis. As shown in Fig. 4, the phase
indeed will increase with aging time, in particular in the
period 010 h, during which it grows most drastically, but
fortunately, after 1024 h, it tends to slow down. The amount
of the phase precipitating 1 h after aging is not much, which
is because the aging time is too short, making the phase fail
to continue growing. But here, the nitrogen amount has no
great influence on the phase precipitation, the maximum
difference less than 3%. After the aging time increases to 10
and 24 h, nitrogen content has greater effect on slowing down
the phase. As a result, after 800 C aging, the increase of
nitrogen does have a positive effect on retarding the precipitation of phase.
Fig. 5 is an XRD analytical illustration of different nitrogen contents of DSS after being heated to 800 C and kept at
constant temperature for 24 h. From this figure, it is obvious that as the aging time increases to 24 h, the peak of
ferritic phase is led to become lower conspicuously, gradually
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under the same aging time, the more the nitrogen content,
the less its phase content, which is the same with 800 C
aging but which is more obvious than after 800 C aging.
Furthermore, through numerical comparisons by means of
image analysis, as shown in Fig. 4, under 800 C aging, nitrogen content rises from 0.14 to 0.22%, and under aging time
10 h, the maximum difference is about 7%, and under 24 h,
about 10%. However, under 700 C aging, as shown in Fig. 7,
although the maximum difference is only about 3% under
aging time 10 h, by 24 h the maximum difference has already
reached about 16%, and as the distance is increasingly bigger, by 48 h the maximum difference reaches as high as 23%.
As a result, under 700 C aging, the effect of phase slowing down is better than under 800 C aging. But under XRD
analysis (Fig. 8), after 0.18% N and 0.22% N DSS undergoes 700 C 48 h aging, no obvious phase peak is found.
In contrast, 0.14% N DSS has obvious phase emerging,
and its ferritic phase peak also drops remarkably. Therefore,
for high nitrogen content DSS and lower nitrogen content
DSS after 700 C aging, the difference in phase precipitation is considerably huge. The cause might be that for
DSS under the same alloy composition, the higher the temperature, the more the ferritic phase; by contrast, the lower
the temperature, the more stable is the percentage of both
phases.
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Fig. 10. X-ray diffraction pattern of duplex stainless steel after 900 C
24 h aging: (a) 0.14%, (b) 0.18% and (c) 0.22%.
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Fig. 13. X-ray diffraction pattern of duplex stainless steel after 950 C 24 h
aging: (a) 0.14%, (b) 0.18% and (c) 0.22%.
Fig. 14. Effect of nitrogen content and aging time at 950 C on content in
duplex stainless steel.
C.-S. Huang, C.-C. Shih / Materials Science and Engineering A 402 (2005) 6675
[3]
[4]
[5]
[6]
[7]
[8]
[9]
4. Conclusions
(1) phase is a phase rich in chromium and molybdenum.
Its quantity will increase with aging time. In the process,
under 800 and 900 C aging, after 10 h, saturation will
be reached, and under 700 C aging, no saturation status
is found within the period of time when this experiment
was conducted.
(2) phase precipitates most rapidly in precipitation rate
under 900 C aging, and most slowly under 700 C aging,
which needs to take as much as 10 h before any trace of
phase is observed.
(3) The higher the aging temperature, the bigger the phase
grains precipitating.
(4) Under the same aging conditions, the higher the nitrogen
content, the lower the phase content in DSS, which is
most obvious under 700 C aging, followed by 800 C,
and under 900 and 950 C aging, this phenomenon is
least obvious. Therefore, slowing down phase precipitation by adding nitrogen is most effective under 700 C,
whereas the effect is not obvious under 900 and 950 C.
(5) Although DSS will have phase precipitating after hightemperature aging and then cause an uneven distribution
of chromium and molybdenum, there still will be a selfrecovery. The self-recovery of 800 C aging specimens
occurs 1024 h, that of 900 C aging specimens 110 h
and that of 700 C aging specimens needs as long as
2448 h to take place.
[10]
[11]
[12]
[13]
[14]
[15]
[16]
[17]
[18]
[19]
[20]
[21]
[22]
[23]
[24]
[25]
References
[1] M. Barteri, F. Mancia, Corrosion 43 (1987) 518525.
[2] S. Jana, J. Mater. Process. Technol. 33 (1992) 247261.
[26]
[27]
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