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Effects of heat treatment parameters on microstructural changes and

corrosion behavior of Al 7075 Alclad alloy

Article  in  Anti-Corrosion Methods and Materials · September 2012

DOI: 10.1108/00035591211265523

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Anti-Corrosion Methods and Materials
Emerald Article: Effects of heat treatment parameters on microstructural
changes and corrosion behavior of Al 7075 Alclad alloy
M. Askari-paykani, M. Meratian, M. Shayan, K. Raeissi

Article information:
To cite this document: M. Askari-paykani, M. Meratian, M. Shayan, K. Raeissi, (2012),"Effects of heat treatment parameters on
microstructural changes and corrosion behavior of Al 7075 Alclad alloy", Anti-Corrosion Methods and Materials, Vol. 59 Iss: 5 pp.
231 - 238
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 Effects of heat treatment parameters on
microstructural changes and corrosion behavior
of Al 7075 Alclad alloy
M. Askari-paykani, M. Meratian, M. Shayan and K. Raeissi
Department of Materials Engineering, Isfahan University of Technology, Isfahan, Islamic Republic of Iran

Abstract
Purpose – The purpose of this paper is to investigate the microstructural changes and stress corrosion cracking behavior via two-stage stressing
u-bent tests for T6 and T73 tempers of Al 7075 Alclad alloy.
Design/methodology/approach – Study was made of the effects of heat treatment; two-stage stressing u-bent, metallography, scanning electron
microscopy, energy dispersive spectroscopy were employed.
Findings – The results showed that the T6 heat treatment formed some very fine transgranular and coarse intergranular precipitates containing two
compositions of (Fe/Cu/Si-rich) and (Mg/Si-rich) phases. The T73 treatment also precipitated some fine transgranular precipitates and coarse
intermetallics with a (Fe/Cu-rich) composition. In T6-treated samples, stress corrosion cracking (SCC) occurred after 155 days due to the high
susceptibility of the grain boundaries. In T73-treated samples, the SCC did not occur even after 210 days. The dissolution of the Alclad layer in the
corrosive media increased pH values and left the sample in the passivation region, protecting the sample from further corrosion attack.
Originality/value – Based on microstructural and SCC resistance properties obtained by heat treatments, the T73 heat treatment with a tempering
temperature of 1078C for seven hours as the first step and 1708C for 19 hours as the second step can be recommended for Al 7075 Alclad sheets.

Keywords Alloys, Stress (materials), Physical properties of materials, Al 7075 Alclad, Heat treatment, Stress corrosion cracking,
Scanning electron microscopy

Paper type Research paper

1. Introduction that the microstructure of T73 tempered samples exhibited

The Al 7075 alloy is classed amongst the heat treatable
(precipitation hardening) aluminium alloys, with wide
applications in the automotive and aerospace industries, owing
to their low density, high strength, ductility, suitable toughness,
and fatigue resistance. However, the alloy is susceptible to
different forms of corrosion attack, such as pitting, intergranular,
exfoliation, and stress corrosion cracking (SCC).
In Al 7075 alloy, a relatively large variety of intermetallics
exist that resist heat treatment, while certain strengthening
particles in the structure, such as MgZn2 (h-phase), can be
influenced in terms of their size, stoichiometry ratios, and
distribution, by heat treatment.
These intermetallics can play a critical role as initiation sites
for pitting attack on Al 7075 alloys. They contain copper and
iron, which are cathodic with respect to the matrix, and hence
they promote dissolution of the aluminum, whereas
magnesium-rich intermetallics are anodic and these will
dissolve preferentially.
Viana et al. (1999) showed that the microstructure of T6
tempered Al 7075 samples exhibited a high density of very
fine precipitates, mostly h́ phase, as well as small amounts of
Guinier-Preston (GP) zones and h phase. They also showed
The current issue and full text archive of this journal is available at
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Anti-Corrosion Methods and Materials
59/5 (2012) 231– 238
q Emerald Group Publishing Limited [ISSN 0003-5599]
[DOI 10.1108/00035591211265523]
rather coarse and uniformly distributed h-phase precipitations
within the grains. The increased concentration of
strengthening precipitates at the grain boundaries degrades
the resistance of the alloy to the intergranular stress corrosion
cracking (IGSCC).
In essence, the propagation of stress corrosion cracks in
aluminum alloys proceeds along grain boundaries and forms a
kind of corrosion that sometimes is considered to be a
particular type of intergranular corrosion where mechanical
stresses accelerate crack propagation along the grain
boundaries.
The aim of the present work was to investigate the
mechanism involved in microstructural changes in the Al
7075 Alclad alloy under different heat treatment cycles. An
optimum heat treatment cycle was introduced in order to
improve resistance to SCC for some sensitive aerospace
applications.
2. Materials and methods
2.1 Materials and heat treatment cycles
The chemical composition of the Al 7075-T6 Alclad in the as-
received form of rolled plates with a thickness of 1.6 mm is
shown in Table I. Samples with dimensions of 120 £ 20
(mm) were solution annealed and then aged to the peak
strength of T6 and over-aged according to T73. In Al 7075
alloy, MgZn2 and Al2CuMg precipitates should be in the
molten state at temperatures higher than 4808C. This may
cause local melting during the annealing process. Thus,
a solution annealing temperature of 4708C was selected.
The solution annealed samples then were quenched in water
at 508C in order to avoid stress localizations and subsequently

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 Effects of heat treatment on corrosion of Al 7075 Alclad alloy Anti-Corrosion Methods and Materials
M. Askari-paykani, M. Meratian, M. Shayan and K. Raeissi Volume 59 · Number 5 · 2012 · 231 –238

Table I Chemical composition of Al 7075 Alclad used Figure 2 Specifications of the two-stage U-bent sample according to
ASTM G30-94
Elements Zn Mg Cu Cr Fe Si Mn Ti Al
Wt% 5.4 2.28 1.46 0.209 0.29 0.108 0.079 0.022 Bal

were kept in ice-brine to avoid natural ageing. The first and

second steps for ageing treatments are shown in Figure 1. The
heat treatment processes were undertaken in a tube furnace
under a controlled argon atmosphere.

2.2 Microstructural characterizations

Both optical (OM) and scanning electron microscopes (SEM –
Philips XL30 and VEGA\\TESCAN equipped with an ESD
probe) were utilized for the microstructural observations. The
surfaces of the specimens were ground down to 4,000 grit with
abrasive SiC papers followed by polishing with 1/4 mm alumina
powder. The specimens were washed with water and alcohol
and etched using Kellers etchant and subsequently washed and
dried quickly to be transferred to the microscope holder for
microstructural observations.
Figure 3(c) shows the cross section of the Alclad sheet of a
2.3 U-bent stress corrosion tests
T6-treated sample, indicating the thickness of the aluminum
Two-stage U-bend stress corrosion tests were carried out
layer, which was approximately 50 mm. The microstructures
according to the ASTM G30-94 standard. This standard
of the T73-treated samples at an ageing time of 7 h for the
describes the procedures for making and using
first step and at 19 h for the second step are shown in Figure 4.
U-bend specimens for evaluation of SCC in metals. The
As can be observed, the fine transgranular precipitates
heat treated samples with dimensions of 120 £ 20 (mm)
(Figure 4(a)) and the coarse intermetallics can be
were degreased in acetone and washed with distilled water
distinguished in a similar manner to that for the T6-treated
and then dried quickly. Figure 2 shows the scheme for the
sample (Figure 4(b)). The coarse intermetallics with light
two-stage U-bend sample. The bent region of the specimens
grey color were identified to be an Fe/Cu-rich phase using
was completely immersed in an aqueous 3.5 percent NaCl
EDS analysis (Figure 5).
solution acidified with HCl to pH 2. The solution pH was
Figure 6 shows the microstructure and the chemical
maintained constant during the experiments. The strains on
composition of the Alclad layer on the T6-treated sample
the outer surface of the bent samples consisted of a plastic
after two days of immersion during the U-bend test. It is clear
strain resulting from the two-stage U-form and an elastic
in Figure 6(a) that the grains of the Alclad layer had been
strain due to fastening of the nut.
attacked significantly. After two days of immersion, the pH
rose surprisingly to 4.5. In order to avoid sample passivation,
3. Results the pH of the solution was periodically adjusted to 2. The
complete dissolution of the Alclad layer occurred after 90 days
As shown in Figure 3, the microstructure of the peak-aged
of immersion when the pH was kept constant at a measured
(T6) sample involves two different particles. One type of
value of about 2.5 at the end of the test period. EDS results
particle had a very fine transgranular morphology with
showed a higher percentage of oxygen inside the Alclad layer
uniform dispersion and the other exhibited coarse precipitates
(Figure 6(b)) compared to the interface (Figure 6(c)).
located at grain boundaries (Figure 3(b)). As also is evident in
The fracture surface of the T6-treated sample in the
Figure 3(a), in addition to the transgranular particles, certain
U-bend test is shown in Figure 7. Stress-corrosion cracks
other fine particles were visible at grain boundaries.
were observed after 155 days of immersion. The specimen
Figure 1 The heat treatment cycles used for the samples failed 20 days after cracks were detected.
Figure 8 shows the fracture surface of a T6-treated sample
after failure (region 1 in Figure 7). Figures 9 and 10 show the
corrosion products close to cracks in the fractured surface
(region 2 in Figure 7). Two different kinds of corrosion
products were evident, i.e. spongy (Figure 9(a)) and cracked-
mud (Figure 10(a)). In Figure 9(b), the EDS results suggest
that the products were aluminum oxide or hydroxide.
According to Figure 10(b), the cracked-mud type of
corrosion product could be aluminum oxide or hydroxide.
These products were very thin and looked like a continuous
cracked layer, due to the tension exerted by the residual stress
resulting from bending loads.
For the T73-treated samples immersed in the same
solution, no cracks were detected on the bent area even

232
 Effects of heat treatment on corrosion of Al 7075 Alclad alloy Anti-Corrosion Methods and Materials
M. Askari-paykani, M. Meratian, M. Shayan and K. Raeissi Volume 59 · Number 5 · 2012 · 231 –238

Figure 3 Microstructure of the Al 7075 T6-treated sample showing Figure 4 The microstructure of Al 7075 T73-treated sample showing:
(a) very fine transgranular and intergranular precipitates, (b) coarse (a) fine transgranular precipitates, (b) coarse precipitates, and (c) the
intermetallics at the grain boundaries, and (c) a cross section of the cross section of the specimen showing the Alclad layer on top of the
specimen showing the Alclad layer on top of the specimen specimen

(a) (a)

(b)
(b)

(c)
(c)

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 Effects of heat treatment on corrosion of Al 7075 Alclad alloy Anti-Corrosion Methods and Materials
M. Askari-paykani, M. Meratian, M. Shayan and K. Raeissi Volume 59 · Number 5 · 2012 · 231 –238

Figure 5 EDS analysis of coarse intermetallics shown in Figure 4b Figure 6 The microstructure of the Alclad layer on the T6-treated
sample (a) after two days of immersion in NaCl solution, (b) EDS
cps/eV
analysis of the Alclad layer inside the layer, and (c) at the interface
30 Point 2 Element Series unn. C norm. C Atom. C
[wt. –%] [wt. –%] [at. –%]
Aluminium K series 64.53 68.09 80.68
Iron K series 18.24 20.38 11.57
Copper K series 3.93 8.80 4.19
Zinc K series 2.41 2.70 1.31
20 Fe Zn
Cu Al

10

0
0 2 4 6 8 10
KeV

after 210 days of exposure as seen in Figure 11(a). According

to the EDS results (Figure 11(b)), the presence of a thin layer
of aluminum oxide (hydroxide) deposited on the whole
surface of the specimen again was confirmed.

4. Discussion
The Al 7075 alloy treated under T6 and T73 cycles has been
reported to contain mainly the Al7Cu2Fe, (Al,Cu)6(Al,Fe)
(a)
and Mg2Si precipitates. Very fine transgranular precipitates
that are shown in Figures 3 must be h́ phases with small cps/eV

amounts of GP zones, and h phase. Two types of GP zones, 10 Point 1 Element Series unn. C norm. C Atom. C
[wt. –%] [wt. –%] [at. –%]
with different GPI and GPII structures, reportedly exist in Oxygen K series 49.97 57.75 69.94

artificially-aged Al-Zn-Mg-(Cu) alloys. The main hardening 8 Aluminium K series 35.29 42.25 30.86

precipitate, h́, is a metastable hexagonal phase, semi- 6 o

Al

coherent with the aluminum matrix. The coarse particles

at grain boundaries (Figure 3(b)) consist of two types of 4
bright (Fe/Cu/Si-rich) and dark (Mg/Si-rich) intermetallics, 2
as shown by the arrows in the figure. Figure 12 shows the
EDS analysis of bright (Figure 12(a)) and dark 0
(Figure 12(b)) intermetallics of Figure 3(b). The Fe/Cu/Si- 0 2 4 6 8 10
rich and Mg/Si-rich intermetallics can be considered as KeV
phase compositions for the bright and dark precipitates, (b)
respectively. cps/eV
By means of the over-ageing heat treatment (T73), the fine 25 unn. C norm. C Atom. C
Point 2 Element Series
[wt. –%] [wt. –%] [at. –%]
precipitates obtained mostly becomes h phase with small Oxygen K series 8.67 10.75 17.84
amounts of h́ . It is believed that the T73 treatment causes 20 Aluminium
Copper
K series
K series
67.02
11.47
72.42
12.39
74.83
5.44
Zinc K series 4.10 4.44 1.89
coarsening of the precipitates inside the grains and at grain Zn
Cu Al
15 o
boundaries. The same treatment seems to convert the
metastable h́ to stable h particles. As seen in Figure 4(c), 10
the thickness of cladding on the T73-treated Alclad sample
measured approximately 60 mm. 5
The corrosion of aluminum in aqueous media can be 0
considered as the sum of two electrochemical reactions, 0 2 4 6 8 10
i.e. oxidation and reduction as follows: KeV
(c)
Al ! Al3þ þ 3e2 ð1Þ
þ 2
3H þ 3e ! 3=2 H2 ð2Þ holding the sample in the passivation region for two days and
þ
Al þ 3H ! Al 3þ
þ 3=2 H2 ð3Þ protected it from further corrosion attack.
Dimples on top of the surface of the T6-treated samples
According to equation (3), aluminum corrosion results the (Figure 8) represent ductile fracture, most probably occurring
increased H2 concentration but decreased Hþ concentration due to mechanical overloading at the end of the test period.
in the electrolyte. This can be attributed to the observed Conversely, the signs of the brittle intergranular fracture
variation in pH from 2 to 4.5, indicating that the Alclad layer and the observed cleavage-like surfaces are characteristic
was under strong dissolution. Increasing pH occurred after of IGSSC. Secondary cracks that develop normal to the

234
 Effects of heat treatment on corrosion of Al 7075 Alclad alloy Anti-Corrosion Methods and Materials
M. Askari-paykani, M. Meratian, M. Shayan and K. Raeissi Volume 59 · Number 5 · 2012 · 231 –238

Figure 7 U-bend and fractured surfaces of the T6-treated sample Figure 9 (a) The sponge-like corrosion products and stress corrosion
cracks on the fractured T6-treated sample and (b) EDS analysis of
corrosion products

(a)
cps/ev

10 Element Series unn. C norm. C Atom. C

[wt. –%] [wt. –%] [at. –%]
Oxygen K series 30.80 55.50 70.12
8 Aluminium K series
Zinc
20.21
4.22
36.90
7.60
27.53
2.35
K series

6 o Zn Al

2
Figure 8 Fracture surfaces of T6-treated samples
0
0 2 4 6 8 10
KeV
(b)

Figure 10 (a) “Cracked mud”-like corrosion products on the fractured

T6-treated sample and (b) EDS analysis of corrosion products

(a)

(a)
cps/ev

6 Point 1 Element Series unn. C norm. C Atom. C

[wt. –%] [wt. –%] [at. –%]
Oxygen K series 7.56 21.26 33.45
Magnesium K series 5.72 12.95 15.47
Aluminium K series 12.08 27.34 29.42
4 Zn
Cu Al
Silicon K series 2.70 6.11 6.32
o mg Si Copper K series 6.18 13.99 6.39
Zinc K series 8.11 18.35 8.15

0
(b) 0 2 4 6 8 10
Notes: (a) Ductile and brittle fractures with secondary KeV
cracks; (b) dimples and cleavage like structures (b)

235
 Effects of heat treatment on corrosion of Al 7075 Alclad alloy Anti-Corrosion Methods and Materials
M. Askari-paykani, M. Meratian, M. Shayan and K. Raeissi Volume 59 · Number 5 · 2012 · 231 –238

Figure 11 (a) SEM micrograph on top of the surface of the T73-treated sample and (b) EDS analysis of corrosion products

(a)
cps/ev

Point 1 Element Series unn. C norm. C Atom. C

10 [wt. –%] [wt. –%] [at. –%]
Oxygen K series 49.15 60.36 74.72
Aluminium K series 24.09 29.59 21.72
8 Silicon K series 0.24 0.29 0.20
Iron K series 1.09 1.34 0.48
Fe Zn Si Copper K series 4.96 6.09 1.90
o Cu Al
6 Zinc K series 1.00 1.22 0.37

0
0 2 4 6 8 10
KeV
(b)

rolling directions can be seen in Figure 8(a). Some cracks also .

were detected on the surface that seemed to have grown
through the grain boundaries. It was concluded therefore that
the grain boundaries in the T6-treated samples acted as
suitable paths for IGSCC. It is reported in the literature that
Al 7075-T6 is susceptible to both intergranular corrosion and
IGSCC. This is attributed to the presence of solute-depleted
zones and/or precipitates at the grain boundaries that act as
anodic or cathodic sites with respect to the adjacent matrix.
Thereby, dissolution is localized at the grain boundaries,
which constitutes a pre-existing active path for IGSCC.
5. Conclusions
.
The T6-treated microstructure is characterized by two
kinds of precipitates: very fine transgranular particles with
a uniform distribution and coarse precipitates that are
located at grain boundaries and which consist of two types
of bright (Fe/Cu/Si-rich) and dark (Mg/Si-rich)
intermetallics.
The T73-treated microstructure is characterized by
fine transgranular precipitates and coarse intermetallics
with a light grey appearance and a Fe/Cu-rich
composition.
.
The dissolution of the Alclad layer in corrosion media
altered the pH of the corrosive solution and caused the
sample to be transferred to the passivation region, which
protected it against further corrosion attack. The heat
treatment caused further diffusion of Alclad layer into the
substrate.
.
SCC occurred only in the T6-heat treated samples.
The corrosion products were spongy and had an
appearance similar to cracked mud. The presence of
surface cracks indicated that the grain boundaries acted
as preferential paths for the SCC in the T6-treated
sample.
. Based on microstructural and SCC resistance properties
obtained by the heat treatments, the T73 heat treatment
with a tempering temperature of 1078C for 7 h as the first
step and 1708C for 19 h as the second step can be
recommended for Al 7075 Alclad sheets.

236
 Effects of heat treatment on corrosion of Al 7075 Alclad alloy Anti-Corrosion Methods and Materials
M. Askari-paykani, M. Meratian, M. Shayan and K. Raeissi Volume 59 · Number 5 · 2012 · 231 –238

Figure 12 EDS analysis of intermetallics, (a) bright precipitates and (b) dark precipitates shown in Figure 12(b)
cps/eV

Point 1 Element Series unn. C norm. C Atom. C

25 [wt. –%] [wt. –%] [at. –%]

Aluminium K series 57.69 66.81 79.86

Silicon K series 2.53 5.83 3.35
Chromium K series 1.92 0.23 1.38
20 Manganese K series 0.86 0.10 0.58
Iron K series 17.95 20.82 11.98
Fe Copper K series 5.36 6.21 3.14
Mn Si
15 Cr Cu Al

10

0
0 2 4 6 8 10
KeV
(a)
cps/eV

25 Point 2 Element Series unn. C norm. C Atom. C

[wt. –%] [wt. –%] [at. –%]

Magnesium K series 5.87 10.44 9.07

Aluminium K series 67.02 73.36 77.23
20 Silicon K series 2.11 8.44 6.40
Copper K series 1.07 1.32 1.41
Zinc K series 4.10 6.44 5.89
Zn
Cu Al
15 Mg Si

10

0
0 2 4 6 8 10
KeV
(b)

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Viana, F., Pinto, A.M.P., Santos, H.M.C. and Lopes, A.B.
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Further reading
Andreatta, F., Terryn, H. and de Wit, J.H.W. (2004),
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aluminium alloy”, Electrochimica Acta, Vol. 49, pp. 2851-62.
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Waterloo, G., Schryvers, D. and Wallenberg, L.R. (2001),
“GP-zones in Al-Zn-Mg alloys and their role in artificial
ageing”, Acta Material, Vol. 49, pp. 3443-51.
Dey, S., Gunjan, M.K. and Chattoraj, I. (2008), “Effect of
temper on the distribution of pits in AA7075 alloys”,
Corrosion Science, Vol. 50, pp. 2895-901.
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corrosion behaviors of Al-Zn-Mg alloy”, Scripta Materialia,
Vol. 56, pp. 305-8.
Li, X. and Starink, M.J. (2000), “Analysis of precipitation
and dissolution in overage 7xxx aluminium alloy using
DSC”, Material Science Forum, Vol. 331-337, pp. 1071-6.
Ofioro, J. and Ranninger, C. (1999), “Stress-corrosion
cracking behavior of heat-treated Al-Zn-Mg-Cu alloy with
temperature”, Materials Science, Vol. 35, pp. 509-14.
Park, J.K. and Ardell, A.J. (1999), “Microstructure of the
commercial 7075 Al alloy in the T651 and T7 tempers”,
Metallurgical Transactions A, Vol. 14, pp. 1957-65.
Puiggali, M., Zielinski, A., Olive, J.M., Renauld, E. and
Desjardins, D. (1998), “Effect of microstructure on stress
corrosion cracking of an Al-Zn-Mg-Cu alloy”, Corrosion
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Sha, G. and Cerezo, A. (2004), “Early-stage precipitation in
Al-Zn-Mg-Cu alloy (7050)”, Acta Material, Vol. 52,
pp. 4503-19.

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 Effects of heat treatment on corrosion of Al 7075 Alclad alloy Anti-Corrosion Methods and Materials
M. Askari-paykani, M. Meratian, M. Shayan and K. Raeissi Volume 59 · Number 5 · 2012 · 231 –238

Song, R.G., Dietzel, W., Zhang, B.J., Liu, W.J., Tseng, M.K.
and Atrens, A. (2004), “Stress corrosion cracking and
hydrogen embrittlement of an Al-Zn-Mg-Cu alloy”, Acta
Materialia, Vol. 52, pp. 4727-43.
Wang, D., Ni, D.R. and Ma, Z.Y. (2008), “Effect of pre-strain
and two-step ageing on microstructure and stress corrosion
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an Al-Zn-Mg alloy”, Material Science and Engineering A,
Vol. 293, pp. 267-74.
Corresponding author
M. Askari-paykani can be contacted at: paykani2004@
yahoo.com

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