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Welding International
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To cite this article: Hiroyuki Hirata, Tomohiko Omura, Kana Jotoku, Jun Nakamura & Takahiro Osuki (2015) Effects of
chemical compositions and microstructure on hydrogen embrittlement of austenitic stainless steel weld metal in high-
pressure gaseous hydrogen environment, Welding International, 29:12, 922-927, DOI: 10.1080/09507116.2014.921084
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Welding International, 2015
Vol. 29, No. 12, 922–927, http://dx.doi.org/10.1080/09507116.2014.921084
Selected from Quarterly Journal of the Japan Welding Society 2013 31(4) 246– 251
The effect of chemical compositions and microstructures on hydrogen embrittlement of austenitic stainless steel weld metals
in high-pressure hydrogen gas was surveyed by using the slow strain rate test (SSRT). As a result, hydrogen embrittlement of
the weld metal was hardly influenced by d ferrite in the weld metal, but by stability of austenite phase, which was estimated
by Md30 value or Ni equivalent. In the weld metal with poor stability of austenite, a0 -martensite was formed near a crack
induced by SSRT. In addition, although the crystal structure of a0 -martensite is as same as d ferrite, susceptibility of
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hydrogen embrittlement became higher with the increase in a0 -martensite. The mechanism to explain the difference between
d ferrite and a0 -martensite was considered as following. The hardness, which increases the hydrogen embrittlement
susceptibility in bcc structure, is higher in a0 -martensite than in d ferrite. In addition, a0 -martensite might be formed
continuously with propagation of a crack. Therefore, the effect of a0 -martensite on hydrogen embrittlement could be larger
compared with d ferrite.
Keywords: weld metal; hydrogen embrittlement; austenitic stainless steel; d ferrite; martensite
Note: Nicq ¼ Ni þ 0:65Cr þ 0:98Mo þ 1:05Mn þ 0:35Si þ 12:6C; Md30 ¼ 413 2 462ðC þ NÞ 2 9:2Si 2 8:1Mn 2 13:7Cr 2 9:5Ni 2 18:5Mo.
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2. Test specimens and experimental methods with a bcc structure in the weld metal was measured
2.1 Test specimens by X-ray diffraction. Furthermore, the fracture surface
was inspected using a scanning electron microscope
Ten-millimetre thick steel sheets based on SUS308L and
(SEM).
SUS316L, with varied contents of Cr and Ni, as shown in
Table 1, were used as test specimens. In the laboratory,
these were prepared by the metal being melted in vacuo on 3. Experimental results
a 17-kg scale, forged and rolled before being solid-solution 3.1 Microstructure of the weld metal
heat-treated at 1323 K £ 1.8 ks. Table 1 shows the Ni
An example of the microstructure of the weld metal is
equivalence [11], expressing the effect of alloy elements
shown in Figure 2. Regardless of their chemical
on their respective austenite phase stability found by
compositions, in all weld metals there is a phase other
Equation (1), and the Md30 value, expressing the
than the matrix found at the dendrite boundaries.
temperature (8C) at which 50% of martensite from
Differences in the quantity of this produced due to their
austenite by 30% working found from Equation (2) [12].
chemical composition are also observed. Table 2 shows
Nicq ¼ Ni þ 0:65Cr þ 0:98Mo þ 1:05Mn þ 0:35Si
þ 12:6C; ð1Þ
Phase observed at dendrite boundary 8.71 22.23 3.4 Figure 4. SEM images of fractured surface of test specimens
316E Matrix 11.86 18.59 2.53 after SSRT in high-pressure H2 gas.
Phase observed at dendrite boundary 10.55 20.62 3.09
results of inspection of fractured surfaces after SSRTs in a
high-pressure hydrogen gas environment of SUS308L
the results of a quantitative analysis made using an weld metal and SUS316L weld metal, with the same d
electron-probe micro-analyser (EPMA) of the quantities of ferrite ratio of approximately 10%. Figure 5 shows the
Cr, Ni and Mo in the matrix and at the dendrite boundaries. results of a microscopic examination of fracture surfaces
Cr and Mo were at a higher density and Ni at a lower in the SSRT test fracture surfaces of SUS308L weld metal
density, in the phases observed at the dendrite boundaries and SUS316L weld metal with the same d ferrite ratio of
than in the matrix. It was judged from these findings that approximately 7%. Inspection of the fracture surfaces
this was d ferrite produced during solidification [13]. showed that SUS316L weld metal, in which almost no
relative reduction of area was noted, underwent full
deformation before fracture and showed a dimpled
appearance over the entire fracture surface. Fracture
3.2 Hydrogen embrittlement susceptibility of weld surface inspection also showed that the principal cracks
metals did not selectively propagate in ferrite but also penetrated
The relationship between the ratio of reduction of area in austenite and no secondary cracking propagation was
atmosphere to the reduction of area in a high-pressure observed. By contrast, although the d ferrite content was
hydrogen gas environment (hereafter relative reduction of the same, SUS308L weld metal, in which there was
area) found by SSRT and the d ferrite ratio in the weld marked relative reduction of area, quasi-cleavage-type
metal is shown in Figure 3. When the d ferrite ratio fracture surface, unaccompanied by deformation, was
increases, almost no decrease in relative reduction of area observed. However, although inspection of the fracture
was noted in SUS316L weld metal whereas a decrease, surface showed initiation of many secondary cracks, and
albeit very slight, in relative reduction of area was noted in the propagated cracks penetrated into both d ferrite and
SUS308L. Also when the content of d ferrite ratio is the austenite, and no clear difference with SUS316L weld
same, the relative reduction of area in SUS308 weld metal metal was noted. Figure 6 shows Ni equivalence and Md30
was smaller than that in SUS316. Figure 4 shows the values, as found in Equations (1) and (2), plotted against
relative reduction of area. A good correlation was
observed between these parameters, which show the
stability of austenite, and relative reduction of area. When
Ni equivalence exceeded 28% or the Md30 value was
lower than 2 308C, there was almost no reduction in the
fracture area reduction value in the high-pressure
hydrogen gas environment.
These results indicate that, within the scope of this
study, hydrogen embrittlement susceptibility is more
strongly affected by the stability of austenite during
working than by the d ferrite content in weld metal during
solidification and the basic composition may also be
thought to affect this.
Figure 7 shows the results of hardness values obtained
Figure 3. Effect of d ferrite fraction in weld metal on relative by microVickers tests of the fracture surface region for the
reduction of area evaluated by SSRT. fracture of a test specimen during SSRTs of SUS308L
Welding International 925
(b)
Figure 6. Effects of Ni equivalent and Md30 value of weld Figure 8. Effect of Md30 value on fraction of bcc/d ferrite phase
metal on relative reduction of area evaluated by SSRT. before and after SSRT.
926 H. Hirata et al.
5. Conclusion
4. Discussion of the effect of microstructure on the
hydrogen embrittlement susceptibility of weld metal (1) Within the range of chemical compositions in this
As stated above, within the scope of this study, the effect study, d ferrite in weld metal has a slight effect on
of d ferrite produced during solidification on the hydrogen hydrogen embrittlement susceptibility.
embrittlement susceptibility of weld metal is small. (2) In the case of weld metal with high hydrogen
By contrast, when an a0 -martensite phase is produced, embrittlement susceptibility, a0 -martensite is pro-
despite the fact that, like d ferrite, it has a bcc structure, the duced due to strain being induced by SSRT. There is a
hydrogen embrittlement susceptibility is increased. The correlation between the a0 -martensite ratio and the
reasons are considered as described below. hydrogen embrittlement susceptibility of weld metal,
It is known that hydrogen embrittlement susceptibility with hydrogen embrittlement susceptibility increas-
in ferrite steel with a bcc structure is dependent on its ing with increase in the quantity produced.
hardness, and the hydrogen embrittlement susceptibility is (3) The reason that the effect of a0 -martensite on
higher in materials with a greater hardness [16,17]. hydrogen embrittlement susceptibility is more
As shown in Figure 7, the results of hardness measurement marked than that of d ferrite is that a0 -martensite is
and examination of the microstructure of the region of the metallurgically more hydrogen embrittlement sus-
fracture in the specimen fractured during a SSRT showed ceptible than d ferrite and also that it is thought to be
that a structure thought to be a0 -martensite produced by produced continuously due to strain concentration at
working was harder than d ferrite. Furthermore, although the crack tip.
experimental proof for this remain a matter for the future,
because hydrogen which causes embrittlement is present
in solid solution in greater quantities in austenite than in Acknowledgement
ferrite [7], it is thought probable that the a0 -martensite This study contains a part carried out as a Hydrogen Society-
produced by the working transformation of austenite, building Joint Basic Development Project of the New Energy and
which contains hydrogen in solid solution, contains a Industrial Technology Development Organisation (NEDO).
Welding International 927
type 316 series austenitic stainless steels at low tempera- 15. Nishiyama Z. Transformable martensite, the basic collec-
tures. J Jpn Inst Met. 2003;67(9):456– 459 (in Japanese). tion. 16. Maruzen; 1971 (in Japanese).
7. Fukuyama S, Zhang L, Yokogawa K. Development of 16. Hinotani S, Terasaki F, Takahashi K. Hydrogen embrittle-
materials testing equipment in high pressure hydrogen and ment of high strength steels in high pressure hydrogen gas at
hydrogen environment embrittlement of austenitic stainless ambient temperature. Tetsu-to-Hagane.
steels. J Jpn Inst Met. 2004;68(2):62 – 65 (in Japanese). 1978;64(7):899– 905 (in Japanese).
8. Ando S, Kikuta Y, Kimura Y. Modern welding technology, 17. Kushida T. Tokyo University graduation dissertation. (in
Series 5. Sanpo Syuppan; 1980 (in Japanese). Japanese).