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Nuclear Engineering and Design 182 (1998) 181 – 192

A study on NDE method of thermal aging of cast duplex


stainless steels
Toru Goto a,*, Takeshi Naito b, Takasi Yamaoka c
a
Department of Mechanical Engineering, Fukui Uni6ersity of Technology, 3 -6 -1 Gakuen, Fukui, Japan
b
First Experimental Laboratory, Takasago R & D Center, Mitsubishi Hea6y Industries, Ltd, 2 -1 -1 Shinhama, Araicho,
Takasago, Japan
c
Nuclear Plant Department, Kobe Shipyard and Machinery Works, Mitsubishi Hea6y Industries, 1 -1 -1 Wadasaki-Cho, Hyogo,
Kobe, Japan

Abstract

To maintain the integrity of applications of the duplex stainless steels currently in service, a study was conducted
to develop a method to nondestructively estimate their Charpy-impact energy at room temperature. It was found that
hardness of the ferrite phase is a reliable indicator of the process of embrittlement during long-term heating of duplex
stainless steels. However, further information on the ferrite phase and the austenite phase is required for the
estimation of Charpy-impact energy. An equation composed of the hardness values of ferrite and austenite phases,
the ferrite content and the average spacing of ferrite phase islands was presented as a method applicable to the
nondestructive estimation of Charpy-impact energy at room temperature. © 1998 Elsevier Science S.A. All rights
reserved.

1. Introduction soud et al., 1993; Yi et al., 1993) have been


conducted to assess the state of in-service
Cast duplex stainless steels have been found to components.
be susceptible to thermal aging embrittlement at Although it has been reported that an increase
operating temperatures for their applications. Ex- in hardness of the ferrite phase is closely related
tensive studies have been conducted in order to to embrittlement for duplex stainless steels
elucidate the mechanisms of thermal aging (Cho- (Trautwein and Gysel, 1982; Massoud et al.,
pra, 1990) and to evaluate end-of-life aging 1993), there have been no reports of a method
(Chung, 1991). However, in spite the apparent that has been successful in the nondestructive
importance of maintaining the integrity of compo- estimation of fracture toughness of aging steels.
nents of cast duplex stainless steels, only a limited The authors believe that the theory of fracture
number of studies (Donaldson et al., 1990; Mas- mechanics should be used in the assessment of
in-service components. Therefore, this study was
initiated to develop a method to nondestructively
* Corresponding author. 2-4 Kamoike, Uozumi-cho, Akashi estimate the Charpy-impact energy at room
674, Japan. Tel.: + 81 078 9477610; e-mail: goto@sdia.or.jp temperature.

0029-5493/98/$19.00 © 1998 Elsevier Science S.A. All rights reserved.


PII S0029-5493(97)00360-9
182 T. Goto et al. / Nuclear Engineering and Design 182 (1998) 181–192

Table 1
Chemical compositions of materials tested

Material Grade C Si Mn P S Ni Cr Mo Ferrite content (%)a

A SCS14A 0.058 0.74 0.75 0.027 0.008 10.71 19.98 2.12 10.8
B SCS13A 0.052 1.19 0.55 0.024 0.001 8.05 20.56 0.24 17.2
C Weld 316 l 0.040 0.31 1.26 0.011 0.004 11.40 19.00 2.10 6.6

a
Calculated using ASTM A800/A800M or Schöefer diagram.

Fig. 1. Microstructures of materials tested.


T. Goto et al. / Nuclear Engineering and Design 182 (1998) 181–192 183

Fig. 2. Charpy-impact energy vs aging time. Fig. 3. Micro-Vickers hardness of ferrite phase vs aging time.
184 T. Goto et al. / Nuclear Engineering and Design 182 (1998) 181–192

2. Experimental procedures and results

2.1. Materials

Materials tested were obtained from a CF8M


pipe, a cast CF8 plate and a weld metal of 316
l. Their chemical compositions and micro-struc-
tures are shown in Table 1 and Fig. 1, respec-
tively.
The samples were subjected to thermal aging
at 350, 400 and 450°C, and age-induced changes
in hardness of the ferrite phase, hardness of the
austenite phase and Charpy-impact properties
were observed.

2.2. Property changes

Charpy-impact tests were conducted at room


temperature. After the impact test, an end of the
broken specimen was mechanically polished and
etched for measuring the micro hardness and
observing the microstructure. The micro hard-
ness measurements were made on the ferrite
phase with 1 g as load and on the austenite
phase with 25 g as load using the Akashi Micro
Hardness Tester (MVK-G3), a commercially
available micro hardness tester.
The changes in Charpy-impact energy (Cv) at
room temperature are plotted against aging time
(t) in Fig. 2. The figure clearly demonstrates
that the embrittlement occurs in materials A and
B at various stages after 10 h of aging at 350,
400 and 450°C. However, material C does not
show any evident embrittlement even after sev-
eral thousand hours of heating.
An increase in hardness of the ferrite phase
has been reported to be closely related to em-
brittlement in duplex stainless steels (Trautwein
and Gysel, 1982; Donaldson et al., 1990; Mas-
soud et al., 1993). Therefore, the micro-Vickers
hardness value Hv(0.001) of five ferrite phase
islands was measured and the average value was
plotted against aging time (t), as shown in Fig.
3. When the figure is examined together with
Fig. 2, it can be seen that the hardening of the
ferrite phase corresponds well with the embrittle-
Fig. 4. Micro-Vickers hardness of austenite phase vs aging ment in the materials tested, and that Material
time. C also shows an increase in hardness of the
T. Goto et al. / Nuclear Engineering and Design 182 (1998) 181–192 185

Fig. 5. Charpy-impact energy vs micro-Vickers hardness of ferrite phase.

ferrite phase. On the other hand, the hardness of 3. Discussion


the austenite phase shows little change with age,
as seen in Fig. 4. 3.1. Fracture process

2.3. Charpy-Impact energy 6ersus Micro-Vickers In order to make a proper model of Charpy-im-
hardness of Ferrite Phase pact energy, a fractographic study was conducted
using the fracture surfaces of the Charpy-impact
At first, the relation between Charpy-impact test specimens. Several examples of S.E.M. photo-
energy and micro-Vickers hardness of the ferrite graphs obtained from fracture surfaces are given
phase was investigated by plotting both values, as in Fig. 6. These photographs demonstrate that the
shown in Fig. 5. From the figure, it can be seen fracture surface is composed of ductile fracture
that the relation should be expressed by a wide surfaces, cleavage of ferrite and phase boundary
band due to its dependency on the material. separation. All of the Material C specimens
186 T. Goto et al. / Nuclear Engineering and Design 182 (1998) 181–192

Fig. 6. Fracture surfaces of Charpy-Impact specimens. Fracture mode B, phase boundary separation; CF, cleavage of ferrite; D,
ductile failure.

showed ductile fracture mode with dimples. The become dominant, the process shown in Fig. 7
numbers in parentheses for each specimen in Fig. could be proposed as the fracture process for
5 represent the area fraction of ductile fracture duplex stainless steels after aging. Thus, Eq. (1)
surface AA (%). may give the Charpy-impact energy, Cv of duplex
If the phase boundary separation does not stainless steels.
T. Goto et al. / Nuclear Engineering and Design 182 (1998) 181–192 187

Fig. 6. (Continued)

Cv=g × ((1−AA/100) ×CvF +(AA/100) lent Charpy-impact energy of the ferrite phase, and
CvA indicates the equivalent Charpy-impact energy
× CvA) (1) of the austenite phase.
Let us assume that the micro-Vickers hardness of
where g is a constant for correction, AA indicates the ferrite phase HvF has a direct relation to CvF
the area fraction (%) of the austenite phase on the rather than to Cv, and that the relation can be
Charpy fracture surface, CvF indicates the equiva- expressed as:
188 T. Goto et al. / Nuclear Engineering and Design 182 (1998) 181–192

Fig. 7. Illustration of fracture process of Charpy impact test for duplex stainless steel.

Fig. 8. Charpy-impact energy obtained experimentally vs that estimated using Eqs. (1) – (3).
T. Goto et al. / Nuclear Engineering and Design 182 (1998) 181–192 189

Fig. 9. Illustration of microstructural parameters of duplex stainless steel. FN, ferrite content; FS, spacing of ferrite phase islands.

CvF= aF+ bF ×HvF (2) and the Cv obtained experimentally. The result of
this investigation is shown in Fig. 8, which plots
where aF and bF are material constants. Let us
the Charpy-impact energy obtained experimen-
further assume that there is also a relation between
tally versus that estimated using Eqs. (1)–(3).
hardness and Charpy-impact energy for the
Fig. 8 demonstrates that there is a clear correla-
austenite phase. If so,
tion between both Cvs. It also shows that the
CvA=aA+ bA ×HvA (3) model of the fracture process and the assumptions
of Eqs. (2) and (3) are the most probable explana-
where aA and bA are material constants and HvA tions for the Charpy-impact energy demonstrated
is micro-Vickers hardness of the austenite phase. in the aged duplex stainless steels.
Eqs. (1)–(3) indicate that if an estimation of the
area fraction of the austenite or ferrite phase on
the Charpy fracture surface is possible, it may also 3.2. Model for the nondestructi6e estimation of
be possible to evaluate the Charpy-impact energy Charpy-Impact Energy
of aged duplex stainless steels using micro-Vickers
hardness measurement. As a next step, microstructural parameters were
We investigated whether the assumptions de- investigated for the alternate of the area fraction
scribed by Eqs. (1) – (3) are valid or not. Using of austenite phase AA or ferrite phase AF on the
Eqs. (1)–(3) and the experimental data sets of AA, Charpy fracture surface. It can easily be assumed
HvF, HvA and Cv, we determined the most prob- that the most probable alternate of AF is the
able values of constants g, aF, bF, aA and bA ferrite content FN.
based on the method of least squares. The Cv of The two parameters described in Fig. 9, FN and
each specimen was estimated using Eqs. (1)–(3), FS, were measured in all of the broken Charpy test
the experimental data sets of AA, HvF, and HvA, specimens. Based on the results of the measure-
and the most probable constants. Finally, we ment, it was assumed that AF could be expressed
conducted a comparison between the estimated Cv as:
190 T. Goto et al. / Nuclear Engineering and Design 182 (1998) 181–192

Fig. 10. Charpy-impact energy obtained experimentally vs that estimated using Eqs. (1) – (4).

AF/100 = 1−AA/100 =cF + dF × FN/100 (4) Cv=g ×{(1+ eF× FS+ hF × FS2)
×(cF+ dF × FN/100) × (aF+ bF× HvF)
where cF and dF are constants and FN indicates
+(1−cF− dF× FN/100)
the ferrite content (%).
By inserting Eq. (4) into Eq. (1), Cv was esti- ×(aA+ bA×HvA)} (5)
mated and plotted against the Cv value obtained
experimentally in Fig. 10. Although Fig. 10 shows Cv=g× (1+ eF× FS+ hF×FS2)
that there is no argument against the use of FN as
× {(cF+dF ×FN/100) ×(aF+bF× HvF)
the alternate of AF, the large scatter of plotted
points in the figure discourages us from using Eq. +(1−cF− dF×FN/100)
(1).
× (aA+bA× HvA)} (6)
The effect of the morphology of the ferrite
phase was further investigated using the spacing where eF and hF are material constants. Eq. (5)
of ferrite phase islands, FS, as explained in Fig. 9. indicates the case where the ferrite phase mor-
The following two equations were proposed and phology expressed by FS affects only impact en-
compared with each other. ergy of the ferrite phase. On the other hand, Eq.
T. Goto et al. / Nuclear Engineering and Design 182 (1998) 181–192 191

Fig. 11. Charpy-impact energy obtained experimentally vs that estimated using Eq. (6).

(6) indicates the case where FS affects the overall duplex stainless steels currently in service, a study
value of impact energy. was conducted to develop a method to nondestruc-
Fig. 11 shows the plotting of the Cv estimated tively estimate their Charpy-impact energy at room
using Eq. (6) against the Cv obtained experimen- temperature.
tally. A fairly high coefficient of correlation, i.e. It was found that the hardness of the ferrite phase
0.952 was recognized in the relation between the is a reliable indicator of the process of embrittle-
two Cvs in Fig. 11. Eq. (5) also yielded a high ment during long-term heating for duplex stainless
coefficient of 0.915. steels. However, further information on the ferrite
To conclude, we would like to propose that Eq. phase and the austenite phase is required for the
(6) is the best model for the nondestructive estima- estimation of Charpy-impact energy.
tion of Charpy-impact energy at room temperature. An equation composed of the hardness values of
ferrite and austenite phases, the ferrite content and
the average spacing of ferrite phase islands was
4. Conclusion presented as a method applicable to the nonde-
structive estimation of Charpy-impact energy at
To maintain the integrity of applications of the room temperature.
192 T. Goto et al. / Nuclear Engineering and Design 182 (1998) 181–192

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