Journal of Metals, Materials and Minerals, Vol.20 No.3 pp.

25-29, 2010

Stress Corrosion Cracking Behavior of Austenitic Stainless Steel AISI 304

with Cold Work Severities of 60 and 90 Percent Reduction in Thickness

Kitikhun SUTTHIPRAPA, Nathapon JUMAO, Weerawat SRICHANCHAENG,

Jirawat CHATDUMRONGSAKUL and Pornwasa WONGPANYA*

School of Metallurgical Engineering, Suranaree University of Technology

Nakhon Ratchasima, 30000, Thailand

Abstract

The effect of cold work intensity on the stress corrosion cracking (SCC) behavior of AISI 304
austenitic stainless steel was studied in accordance with the ASTM G36-94. The samples were unidirectional
cold-rolled up to 60 and 90 percent reduction in thickness, prepared to be U-bend specimens and tested in
boiling 42 wt% magnesium chloride solution at 1551C. The result indicated that the cold work intensity
significantly impacted on the cracking appearance. The result indicated that the cold work intensity
significantly impacted on cracking appearance. By considering the microstructure from scanning electron
microscope (SEM) after SCC testing, transgranular cracking appeared in the sample with 60 percent
reduction in thickness while the sample with 90 percent reduction in thickness showed intergranular
cracking. The corrosion severity associated with stress significantly depends on the percent reduction in
thickness. Corrosion rate in terms of millimeter per year increased with the level of cold work intensity.

Key words: Austenitic stainless steel, Cold work, Stress corrosion cracking, Magnesium chloride solution

Introduction
Austenitic stainless steels have been
extensively used in many engineering applications
because their corrosion resistance and mechanical
property.(1) It is necessary to use manufacturing
processes, i.e. cold rolling, forging and deep
drawing, in order to reach high strength and
hardness for engineering applications. An extra
high cold work level has been used normally in
manufacturing processes in order to get the near
net shape. And, it is also known that after plastic
deformation of austenitic stainless steels, there are
two important phenomena, i.e. work hardening and
partial transformation of austenitic phase to be an
alpha and epsilon martensite.(1) Moreover, strain
hardening is increased significantly with the cold
work level during fabrication; subsequently
stainless steel is susceptible to stress corrosion
cracking (SCC) in service time.(1-4) In order to
evaluate effect of high cold work intensity on stress
corrosion cracking of austenitic stainless steel,
this study has been performed. Firstly, the
commercial AISI 304 stainless steels were cold-
rolled of up to 60 and 90 percent reduction
in thickness after that they were prepared to be
U-bend specimens and boiled in magnesium
chloride solution. Weight loss then was determined
before the corrosion rate in terms of millimeter per
year has been calculated. Finally, fracture surface
was investigated by Scanning Electron Microscope.
Materials and Experimental Procedures
The material used in this work is a commercial
austenitic stainless steel AISI 304 having 12.5 mm
in thickness. The chemical compositions measured
by an emission spectroscopy are composed of
0.06wt%C, 18.60wt%Cr, 8.52wt%Ni, 0.55wt%Si,
2.00wt%Mn, 0.03wt%P, 0.03wt%S and Fe balanced.
Firstly, the plate of AISI 304 stainless steel,
12.5 mm thickness, was solution annealed at
1050C for 45 minutes and water-quenched. Then
the plate was stress relief at 150C for 1 hour to
remove residual stress from the manufacturing
processes. Nitrogen gas was flow into the tube
furnace to prevent the element oxidation during
heat treatment process. After that the plate was
unidirectional cold-rolled of up to 60 and 90
percent reduction in thickness at room temperature.
Then the plates were polished by silicon carbide
paper up to 1200-grit for removing all coarse
scratches and contaminations. The samples were
rinsed by distilled water, acetone and were air-
dried before preparing a U-bend specimen in

*Corresponding author Tel: +66 4422 4486; Fax: +66 4422 4482; E-mail: pornwasa@sut.ac.th
26
SUTTHIPRAPA, K. et al.

accordance with ASTM G30-97.(5) Finally, the

samples were tested according to ASTM G36-94 (6)
in a boiling 42wt% MgCl2 at 1551C. All of
experimental procedures were summarized in
Figure 1.

(a) An example of U-bend specimen according to

ASTM G30-97

Figure 1. Experimental procedures for stress corrosion

cracking evaluation of austenitic stainless
steel AISI 304 with cold work severities of
60 and 90 percent reduction in thickness.
An example of shape and dimension of U-
bend specimen was shown in Figure 2 (a). There
are many sizes of the U-bend specimen in
accordance with ASTM G30-97.(5)The tested size
is dependent on an original size of law material and
the level of applied cold work. The real sample
used for testing was shown in Figure 2 (b). After
the SCC test has been done, the corrosion products
were removed by mechanical procedure as following
ASTM G1-03.(7) Weight loss measurement has
been done in order to determine corrosion rate in
the next step. The degree of corrosion was
evaluated in terms of corrosion rate by using a
formulae given below(7)
(1)
KW
Corrosion rate =
DAT
where K , W , D , A and T are a constant value
(in this case it is set to be 8.76 10 4 for corrosion
rate in terms of millimeters per year), weight loss
in grams, density in g/cm3 (7.94 for AISI 304),
tested area in cm2 and time of exposure in hours,
respectively.
(b) Real specimen used for SCC test
Figure 2. U-bend specimen.
Results and Discussion
Effect of Cold Work Level on Microstructure of
Austenitic Stainless Steel AISI 304
Microstructures of austenitic stainless steel
AISI 304 in the as solution-annealed condition are
austenite as shown in Figure 3 (a). After the
austenitic stainless steel AISI 304 was cold-rolled
of up to 60 and 90 percent reduction in thickness;
the microstructures have been altered. The
microstructures of AISI 304 were dependent on
cold work level. The presence of austenite with
twinning band and acicular martensite has been
found in the sample with 60 percent reduction
thickness as shown in Figure 3 (b). While in the
sample cold-rolled of up to 90 percent reduction in
thickness, the interlocking between austenite and
martensite has been found and they showed small
grains in the direction of cold rolling as shown in
Figure 3 (c). These results showed good agreement
with the observation of the other authors.(2-3)
 27
Stress Corrosion Cracking Behavior of Austenitic Stainless Steel AISI 304 with Cold Work
Severities of 60 and 90 Percent Reduction in Thickness

Crack Behaviour of Cold-Rolled Austenitic Stainless

Steel in Boiling 42wt% Magnesium Chloride
Solution at 1551C

Stress Corrosion Cracking (SCC) test of

the cold-rolled austenitic stainless steel has been
done in boiling 42wt% magnesium chloride
solution at 1551C. After the U-bend specimen
had been boiled in the certain solution; the failure
time was observed by considering the first time of
crack initiation. It was found that failure time of U-
bend specimen decreased significantly with cold
work level as shown in Table 1. For the sample
(a) At as solution-annealed with cold-rolled of up to 60 percent reduction in
thickness, the first time of crack initiation is 257
minutes or 4.28 hours while the sample with cold-
rolled of up to 90 percent reduction in thickness
cracked in 42 minutes or 0.70 hours.

(b) At 60 percent reduction in thickness

(a) Crack appearance

(c) At 90 percent reduction in thickness

Figure 3. Microstructure of samples after cold rolled.

Table 1. Failure time of samples in 42wt% MgCl2 boiling

solution.
(b) Transgranular cracking in sample with 60 percent
Failure time (minutes) reduction in thickness
60 percent reduction in 90 percent reduction in
thickness thickness Figure 4. Photograph and SEM micrograph of sample
257 42 with 60 percent reduction in thickness after
SCC test.
28
SUTTHIPRAPA, K. et al.
The examination of microstructure was
carried out after the SCC test to evaluate the type of
crack. From the results, it indicated that appearance
of crack was different and dependent on the level
of cold work as shown in Figures 4 and 5. At 60
percent reduction in thickness, the brittle fracture
and transgranular cracking appeared as shown in
Figure 4 (a) and (b) because most of microstructures
were the acicular martensite. Therefore, the
specimen having the acicular martensite was
exposed to boiling magnesium chloride solution; it
was easily broken and the main mode of crack was
transgranular cracking.
(a) Crack appearance
(b) Intergranular cracking in sample with 90 percent
reduction in thickness.
Figure 5. Photograph and SEM micrograph of sample
with 90 percent reduction in thickness after
SCC test.
Figure 5 shows the intergranular cracking
associated with dimple for the sample cold-rolled
of up to 90 percent reduction in thickness. At 90
percent reduction in thickness, the intergranular
cracking behavior appeared. From the results, this
could be explained that the high cold work level
induced chromium carbide precipitation along
grain boundary; subsequently the sample was
prone to be sensitization. Thus the certain sample
was placed in the aggressive media; it was easily
susceptible to intergranular corrosion cracking. (1, 8)
Corrosion Rate of Cold-Rolled Austenitic Stainless
Steel after SCC Test
In order to understand the effect of cold
work level on corrosion behaviour of AISI 304, the
corrosion rate in terms of millimeters per year has
been calculated by using equation 1. Firstly, the
weight loss in grams of each specimen was
determined and summarized in Table 2.
Table 2. Weight loss of each specimen after SCC test.
Weight loss (grams)
60 percent reduction in 90 percent reduction in
thickness thickness
0.0473 0.0154
From failure time and weight loss of each
specimen in Tables 1 and 2, the corrosion rate can
be calculated as following:
For the specimen with 60 percent reduction
in thickness:
8.76 10 4 0.0473
Corrosion rate =
7.94 (12 1.5 2) 4.28
= 3.39 millimeters per year
For the specimen with 90 percent reduction
in thickness:
8.76 10 4 0.0154
Corrosion rate =
7.94 (12 1.5 2) 0.70
= 6.80 millimeters per year
The corrosion rate of each specimen is
shown in Figure 6. It is seen that the corrosion rate
strongly depends on the cold work levels. From
previous SEM micrographs, cracking appearance
may not be a good indicator for corrosion severity.
 29
Stress Corrosion Cracking Behavior of Austenitic Stainless Steel AISI 304 with Cold Work
Severities of 60 and 90 Percent Reduction in Thickness

2. Zandrahimi, M., Bateni, M.R., Poladi, A. & Szpunar, J.A.

8.00
(2007). The formation of martensite during
7.00 wear of AISI 304 stainless steel. Wear. 263
C o rro sio n ra te in m m /y r

: 674-678.
6.00

5.00 3. Milad, M., Zreiba, N., Elhalouani, F. & Baradai, C.

4.00
3.00
2.00
1.00
0.00
60
percent reduction in thickness
Figure 6. Corrosion rate of samples after SCC test.
Conclusions
The stress corrosion cracking behavior of
AISI 304 austenitic stainless steel with different
cold work intensities was studied in a boiling 42wt %
magnesium chloride solution at 1551C. The
following conclusions can be drawn:
1. Microstructures of AISI 304 austenitic
stainless steel depend on the cold work level, i.e.
austenite with twinning band and acicular
martensite after cold-rolled of 60 percent reduction
in thickness and the interlocking between austenite
and martensite after cold-rolled of 90 percent
reduction in thickness.
2. Failure time is strongly decreased with
the high level of cold work.
3. Transgranular and intergranular cracking
can be found in AISI 304 stainless and its
appearance depends on the level of cold work.
Corrosion rate is increased, if the high level of cold
work is applied in manufacturing process.
(2008). The effect of cold work on structure
and properties of AISI 304 stainless steel.
J. Mater. Process. Tech. 203(1-3) : 80-85.
4. Garca, C., Martn, F., De Tiedra, P., Heredero, J.A.
& Aparicio, M.L. (2001). Effects of prior
cold work and sensitization heat treatment
on chloride stress corrosion cracking in type
90
304 stainless steels. Corros. Sci. 43(8) :
1519-1539.
5. ASTM Standard G 30-97. (2003). Standard
practice for making and using U-bend
stress corrosion test specimens. American
Society for Testing and Materials.
6. ASTM Standard G 36-94. (2000). Standard
practice for evaluating stress corrosion
cracking resistance of metals and alloys in
a boiling magnesium chloride solution.
American Society for Testing and Materials.
7. ASTM Standard G 1-03. (2003). Standard practice
for preparing, cleaning, and evaluating
corrosion test specimens. American Society
for Testing and Materials.
8. Jones, D.A. (1996). Principles and prevention of
corrosion (2nd ed.) London : Prentice Hall :
pp.292-304.

Acknowledgement

The authors would like to express sincere

thank for supporting sample (U-bend) preparation
from Failure Analysis and Materials Degradation
(FAMD) Centre.

References

1. Sedriks, A.J. (1996). Composition, structure,

and mechanical properties: corrosion of
stainless steels (2nd ed). New York : John
Wiley & Sons Inc.: pp.267-300.