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International Conference on Recent Advances in Mechanical Engineering and Interdisciplinary Developments [ICRAMID - 2014]

Improvement of stress corrosion cracking (SCC)


resistance of a 7150 Al-Zn-Mg-Cu alloy by
retrogression and reageing (RRA) treatment
Prasanta Kumar Rout*

M M Ghosh

K S Ghosh

Department of Metallurgical and Materials Engineering, National Institute of Technology (NIT)


Durgapur, India,
E-mail:prasantonnet55@yahoo.com
ksghosh2001@yahoo.co.uk
Abstract A 7150 Al-Zn-Mg-Cu alloy is artificially aged at 120 oC
for varying time. The peak hardness (T6 temper) is obtained at about
24 h at that temperature. Further, the T6 temper is subjected to
retrogression and reageing (RRA) treatment. Slow strain rate test
(SSRT) has been carried out on the T6 and RRA tempers. SSRT
results indicated that the RRA temper have higher resistance to SCC
compared to that of T6 temper. SCC behaviour of the alloy tempers
have been explained with the help of microstructural features studied
by transmission electron microscope (TEM). The large, discrete and
discontinuous grain boundary precipitates observed in the
microstructure of the RRA temper are believed to be the responsible
factor for achieving higher SCC resistance. Further, SEM
fractographs and crack morphology have also been analyzed to
evaluate the SCC behaviour of the alloy tempers.
Keywords 7150 Al-Zn-Mg-Cu alloy, RRA treatment, Stress
corrosion cracking, Transmission electron microscopy, Scanning
electron microscopy.

I. INTRODUCTION
7xxx series Al-Zn-Mg-Cu alloys undergo precipitation
hardening and widely used in the aircraft industries as
structural components because of their high specific strength
[1], [2]. However, this series of aluminium alloys are very
much susceptible to stress corrosion cracking (SCC) in the
peak aged (T6) temper. Over aged temper (T7) has higher
resistance to SCC, but it has 10-15% lower strength compared
to that of T6 temper [3], [4]. For the past several years, efforts
have been made to optimize the strength and SCC resistance
of the alloys by adapting proper ageing schedules. Cina [5]
proposed a new ageing technique termed as retrogression and
reaging (RRA) to improve the SCC resistance without
significant loss of peak aged strength. A number of literature
is available dealing with the effect of RRA treatment on SCC
behaviour of 7xxx series (7050, 7075, 7020 etc.) alloys [6],
[7]. Since, the microstructural features (principle responsible
for SCC process) of the 7xxx series alloys are very complex
and the alterations of microstructural features (governing
factor of the SCC mechanisms) depend on many variables
such as alloy chemistry, the solute content, Zn/Mg and Cu/Mg
ratio, artificial ageing schedules, retrogression temperature
and time etc., the research on this field is still very active and
vibrant. The present investigation is aimed to study the effect
of RRA treatments on SCC behaviour of a high strength 7150
Al-Zn-Mg-Cu alloy.

II. EXPERIMENTAL DETAILS


The chemical composition (wt. %) of the 7150 Al-Zn-MgCu alloy (2 mm thick sheet) is Zn6.30, Mg2.40, Cu2.30,
Zr0.12, Fe0.10, Si0.05 and Albalance. The
microstructure of the alloy was observed by an optical
microscope (Leica DM 2500 M). For assessing the isothermal
ageing behaviour, specimens (i.e. coupons of dimensions 10
mm X 10 mm X 2 mm) were cut from the alloy sheet. The
specimens were solution treated at 475 oC for 45 minutes,
water quenched, followed by artificial ageing at 120 oC for
varying time. To produce RRA temper, the T6 temper
specimen was heated at 200 oC for different short time, then
water quench (retrogression process), and finally the
retrogressed specimens were reaged at 120 oC for 24 h similar
to the T6 temper. Hardness of the aged specimen was
measured using a Vickers micro-hardness tester (Model
MMT-X78, Matsuzawa Co Ltd.) with an applied 200 gf load.
A JEOL JEM-2100 high resolution transmission electron
microscope (HRTEM) is used to observe the microstructural
features of these tempers. TEM samples were prepared by
twin jet electrolytic polishing in a solution containing 30 vol.
% nitric acid and 70 vol. % methanol.
Tensile testing was carried out in a universal testing
(INSTRON 8516) machine at a cross-head speed of 2 mm
min1. To evaluate the SCC behaviour of the T6 and RRA
tempers, slow strain rate tests (SSRT) were carried out by
using a constant extension rate test (CERT) unit (M/s Cortest
Inc., Ohio, USA). In SSRT, specimens were tested in air and
in 3.5 wt. % NaCl solution at an initial strain rate of 3.3 X
106 s1. Specimen with gauge dimensions of 15 mm length, 6
mm width and 2 mm thickness were prepared from the long
transverse (LT) direction of the alloy sheet as per the ASTM
E8-1983 standard. Tensile tests at nominal strain rate and
SSRT were repeated to check the reproducibility of the
results. A scanning electron microscope (S300N, Hitachi,
JSM-5800, JEOL) and optical microscope are used to observe
the fracture surfaces and stress corrosion (SC) crack
morphology of failed specimens, respectively.

ISBN 978-93-80609-17-1
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III. RESULTS AND DISCUSSION

International Conference on Recent Advances in Mechanical Engineering and Interdisciplinary Developments [ICRAMID - 2014]

A. Isothermal Ageing and Retrogression and Reaging (RRA)


Behaviour
Fig. 1a shows the age hardening behaviour of the 7150
alloy, artificially aged at 120 oC for varying time. The
variation of hardness with ageing time displays the
characteristic age hardening behaviour of aluminium alloys,
i.e. progressive increase of hardness with ageing time, there,
reaching to maximum value (peak aged condition) and them
decrease of hardness value. The ageing curve displays that the
peak hardness (HV10 202) is attained at about 24 h, and this is
attributed to the precipitation of primarily large numbers of
fine disc shaped '(MgZn2) precipitates.

B. Tensile Testing

200

Fig. 2 shows representative stressstrain curves of the


7150 alloy of T6 and RRA tempers tested in air at a crosshead
speed of 2 mm min-1. The T6 temper exhibits the highest yield
strength (YS) (546 MPa) and ultimate tensile strength (UTS)
(589 MPa). The RRA temper has also achieved a YS (530
MPa) and UTS (579 MPa). The retrogressed (5 min) state has
lower YS (403 MPa) and UTS (503 MPa) values with respect
to T6 and RRA tempers, but the ductility is higher. The lower
strength value of retrogressed state is due to the dissolution of
' precipitates which is not longer stable at the retrogression
temperature (200 oC). Regaining of strength upon reageing the
retrogressed state is because of reprecipitation of '
precipitates within the matrix.

Vicker Hardness, (HV10)

220

180
160
140
120
100
80

Ageing Temp:120 C
0

20

40

60 80
Time, h

100

120

(a)
Fig. 1a Variation of hardness of the 7150 alloy during isothermal ageing.

205
200
Vicker Hardness, (HV10)

Fig. 1b exhibits the variation of hardness with


retrogression time at a retrogression temperature of 200 C
and the change in hardness on subsequent reaging the
retrogressed state at 120 oC. During retrogression (Fig. 1b),
there is a sharp decrease of hardness, attainment of a
minimum hardness, then slight increase in hardness and
thereafter there is slight decrease of hardness values for the
retrogression time studied. The lowest hardness value is
attained at about 5 min of retrogression, and this is attributed
to the dissolution of metastable ' precipitates into -solid
solution. Further, Fig. 1b indicates that reaging of 5 minutes
retrogressed state resulted in attaining the hardness close to
the peak hardness value.

195
190
185
180
175
170

Retrogression at 200 C
Retrogression and re-aging at
o
120 C for 24 h
160
0 2 4 6 8 10 12 14 16 18 20 22
Retrogression Time, min
165

(b)
Fig. 1b Variation of hardness during retrogression and subsequent reaging.

C. Microstructure
Fig. 3 shows the optical microstructure of the as-rolled
sheet of the 7150 aluminum alloy in three principal directions.
The microstructure of the alloy in all direction reveals the
presence of recrystallized and unrecrystallized grains as well.
The grains in the longitudinal (L) direction are flattened, but
in the long transverse (LT) and short transverse (ST)
directions the grains are highly elongated and appeared as
pancake shape. The microstructure also exhibits numerous
second phase intermetallic particles (marked with arrow) such
as Al7Cu2Fe and Al2CuMg phases [8].
Fig. 4a shows the TEM micrograph of T6 temper, consist
of a large numbers of fine ' precipitates (~5 nm) within the
grains and the distribution of continuous precipitates (~20
nm) along the grain boundary. These microstructural features
consisting numerous fine ' precipitates is considered to be the
cause of peak hardness. Fig. 4b, the TEM micrograph of the
RRA temper, exhibits also fine ' precipitates (~5 nm) within
the grains and the precipitates along the grain boundary.
But, these precipitates are larger in size (~75 nm), discrete
in nature and discontinuously distributed along the grain
boundary compared to that observed in T6 temper.
The alteration in microstructure of the RRA temper is
mainly associated with the retrogression process. During
retrogression process only ' precipitates dissolved, but
precipitates remain undissolved. Reageing the retrogressed

ISBN 978-93-80609-17-1
322

International Conference on Recent Advances in Mechanical Engineering and Interdisciplinary Developments [ICRAMID - 2014]

state promoted the reprecipitation of ' phase whilst the preexisted precipitates at grain boundary have grown in size
and in consequence became discrete and discontinuous. Thus,
the microstructure of RRA temper contains a very fine and
numerous ' precipitates inside the grains similar to T6
temper, but the grain boundary precipitates are larger and
discontinuously distributed.

Fine ' precipitates

600

Continuous precipitates

Stress, MPa

500
400
300

(a)

200
Peak aged (T6)
Retrogress state
Retrogress & re-aged (RRA)

100
0
0

10

Strain, %

15

Discontinuous precipitates

20

Fig. 2 Stress-strain curves of the 7150 alloy of various tempers tested at


a crosshead speed of 2mm min1.

Intermetallic
(b)
Fig. 4 TEM micrographs of the 7150 alloy of various tempers (a) T6
and (b) RRA.

D. Stress Corrosion Cracking (SCC) Behaviour

Fig. 3 Triplanar optical micrographs of the rolled 7150 aluminium


alloy.

Fig. 5(a-b) and Table I show a few representative


stressstrain curves and data of the 7150 alloy of T6 and RRA
tempers tested in the SSRT unit, respectively. The SCC
susceptibility index (ISCC) is reported by ductility ratio (DR)
i.e. the ratio of % strain to fracture in the environment to that
in air (i.e. env air ) [4], [9]. The higher the value of DR the
greater is the resistance to SCC.
Fig. 5 and Table I indicate that the DR values of T6 and
RRA tempers in the 3.5 wt. % NaCl solution are 0.70 and
0.92, respectively. This indicates that the RRA temper has
enhanced the SCC resistance of the alloy. The improvement of
SCC resistance is attributed to the changes in the grain
boundary microstructure (Fig. 4b) upon RRA treatment.

ISBN 978-93-80609-17-1
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International Conference on Recent Advances in Mechanical Engineering and Interdisciplinary Developments [ICRAMID - 2014]

during slow strain rate testing (SSRT) acted as crack initiation


sites and crack propagation path as well leading to
intergranular stress corrosion cracking (IGSCC). However, the
coarse and widely spaced precipitates distributed
discontinuously along the grain boundary of the RRA temper
did not act as continuous network of corrosion path/channel
and thereby decreases the susceptibility to intergranular
corrosion with an associated concomitant enhancement of
resistance to stress corrosion cracking.
Fig. 6a, the fractograph of the T6 temper failed sample
tested in 3.5 wt. % NaCl solution exhibits prominent
intergranular cracking, a few secondary cracks and very fine
numerous dimples in some of the grains (lower and left
portion of the fractograph). The overall fracture surface looks
like a rock candy type brittle intergranular appearance. In this
fractograph, elongated pancake shape grains separated by
intergranular cracking are clearly visible. However, when the
RRA treated specimen tested in solution, the fractograph (Fig.
6b) displays mix mode of fracture surface. Short intergranular
cracking and various sizes of dimples are observed. The
proportion of intergranular cracks and their sizes, however,
are lesser than those seen in the fractograph of T6 temper.
Thus, from the observations of the fractographic evidences
and features, it can be inferred that the RRA temper has
higher resistance to SCC compared to that of T6 temper,
which is in good agreement with the observed SSRT results
and the characteristic TEM microstructural features.

600

Stress, MPa

500
400
300
200

Air
3.5 wt.% NaCl solution

100
0

4
6
Strain,%

10

(a)

600

Stress, MPa

500
400
300
200

Air
3.5 wt.% NaCl solution

100
0

6
8
Strain,%

10

12

(b)
Fig. 5 A few representative stressstrain curves of the 7150 aluminium
alloy of various tempers tested in air and in 3.5 wt. % NaCl solution
(a) (T6) and (b) (RRA).

TABLE I
SSRT RESULTS OF THE 7150 ALUMINUM ALLOY OF T6 AND RRA
TEMPERS.

Alloy
temper
T6
RRA

Environment
Air
3.5 wt.% NaCl
solution
Air
3.5 wt.% NaCl
solution

YS,
MPa

UTS,
Mpa

530
530

577
569

%
Strain
to
fracture
9.35
6.58

514
512

567
560

12.46
11.48

Intergranular cracking

Ductility
ratio
(DR)
-0.70

(a)

-0.92

The (MgZn2) precipitates located along the grain


boundaries of the 7150 alloy are more electrochemically
active than the -matrix [6], [10], [11]. When the T6 temper
was exposed to corrosive environment, the precipitates
preferentially dissolved due to the galvanic reaction between
the precipitates and adjacent alloy matrix, and resulted in an
active corrosion path. The galvanically corroded regions (i.e.
dissolved continuous precipitates) under applied loading

ISBN 978-93-80609-17-1
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(b)
Fig. 6 SEM fractographs of SSRT specimens of 7150 aluminium alloy of
various tempers tested in 3.5 wt.% NaCl solution (a) T6 and (b) RRA.

International Conference on Recent Advances in Mechanical Engineering and Interdisciplinary Developments [ICRAMID - 2014]

Fig. 7(a-c) shows the evidences of secondary stress


corrosion (SC) cracks remained at near-by region of the gauge
portion of the failed specimen of T6 temper tested in 3.5 wt.%
NaCl solution. Fig. 7a shows a number of pits (acted as stress
concentration), cracks as well that have been initiated from
the base of the pits and the propagation of cracks. Figs. 7b
displays the cracks originated from the edge of the specimen.
These cracks initiation sites are not from the pits base but
probable from the intergranularly denuded regions i.e. from
the preferential dissolved of anodic grain boundary
precipitates/regions. Further, Fig. 7c (sample is lightly
polished and etched) reveals numerous fine corrosion pits and
cracks. The cracks path is zig-zag in nature and propagated
along the grain boundaries.

Pit base

micrographs of the T6 and RRA tempers exhibited very fine


' precipitates within the matrix. Further the micrographs
showed that the precipitates are very closer to each other
and continuously distributed along the grain boundary of the
T6 temper. However, in the RRA temper the precipitates
were larger in size, discrete in nature and distributed
discontinuously along the grain boundary. The intergranular
cracking observed in the T6 temper suggested that the grain
boundaries acted as a most preferential and active corrosion
path for stress corrosion cracking (SCC). The RRA treatment
applied to the 7150 alloy has a beneficial effect with enhanced
resistance to SCC, without any significant loss in the strength
value. The improved SCC resistance of the RRA temper is
attributed to the presence of larger, discrete and discontinuous
precipitates along the grain boundary, which did not act and
make an active intergranular corrosion path for SCC.
ACKNOWLEDGEMENTS
The authors acknowledge to Prof. M. J. Starink and Dr.
Nong Gao, faculty of Engineering and the environment,
University of Southampton, Southampton, UK for providing
the 7150 alloy. The authors also very much thankful to the
staff members of Central Research Facility (CRF), IIT
Kharagpur, India for allowing us to avail the facilities of
SEM, TEM, and hot and cold rolling.

(a)

REFERENCES

(b)

(c)
Fig. 7 Optical photomicrographs showing secondary stress corrosion
(SC) cracks in the 7150 aluminium alloy of T6 temper tested in 3.5
wt. % NaCl solution.
V. CONCLUSIONS

Variation of hardness with ageing time of the 7150 alloy


exhibited the characteristic precipitation hardening
phenomena. SSRT results indicated that RRA tempers have
higher resistance to SCC compared to that of T6 temper. TEM

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[8] D.K. Xu, N. Birbilis and P.A. Rometsch, Effect of S- phase dissolution
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[9] A.Venugopal, K. Sreekumar and V.S. Raja, Stress corrosion cracking
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