Journal of Materials Processing Technology xxx (2004) xxxxxx

The influence of hot deformation on the exfoliation

corrosion behaviour of aluminium alloy 2025

T.Y. Liu a, , J.S. Robinson b , M.A. McCarthy c

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a Materials and Surface Science Institute, University of Limerick, Ireland

Department of Materials Science and Technology, University of Limerick, Ireland
Department of Mechanical and Aeronautical Engineering, University of Limerick, Ireland
b

Abstract

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The influence of hot deformation and alloy composition on the tensile properties and exfoliation corrosion susceptibility of the aluminium alloy 2025 has been investigated. Five casts of 2025 were used to make extrusion billets. These were designated, low manganese,
high manganese (with low copper), high chromium, high titanium and, outside the permitted range but reflecting more modern alloy
design, high zirconium. Billets were then hot extruded and hot forged at a range of temperatures expected to produce unrecrystallised,
partially recrystallised and fully recrystallised microstructures. The main objective of the compositional variation was to alter the wrought
grain refining intermetallic phase. After the application of a standard heat-treatment, tensile properties were determined, and exfoliation
tests were performed in accordance with ASTM-G34. The exfoliation susceptibility and mechanical properties of AA2025 showed a
marked dependence on microstructure developed during hot forming and heat-treatment. Higher forming temperatures resulted in coarser
recrystallised microstructures, which tended to reduce the susceptibility to exfoliation corrosion, but adversely affected tensile properties.
2004 Published by Elsevier B.V.

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Keywords: 2025 Aluminium alloys; Hot deformation; Exfoliation corrosion; Tensile properties

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1. Introduction

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The aluminium alloy 2025 is a wrought, heat-treatable,

medium-strength material that is used in aerospace applications. Its main application is fixed and variable pitch
propeller blades. The operational environment of propeller
blades in service requires materials to have good fatigue
resistance, mechanical strength, and corrosion resistance.
The manufacture of these blades is normally by hot extrusion and hot forging. The resulting structure may make
the blades susceptible to exfoliation corrosion attack. Exfoliation corrosion is a form of environmentally assisted
subsurface attack that proceeds along multiple narrow paths
parallel to the fabricated surface of the product. Corrosion
attack normally occurs inter-granularly but can also be
influenced by stringers of constituent particles. Its visible
characteristics are lifting of the surface layers by corrosion
products, leading to leafing and delamination. Severe exfoliation can result in greatly decreased service life. Factors
leading to exfoliation corrosion include a highly directional

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Corresponding author.
E-mail addresses: tianying.liu@ul.ie (T.Y. Liu), jeremy.robinson@ul.ie
(J.S. Robinson), michael.mccarthy@ul.ie (M.A. McCarthy).

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microstructure and a corrosive environment. A consensus

has not yet been reached on the mechanism of exfoliation corrosion, and several views have been proposed. It
has been suggested that exfoliation corrosion belongs in
the same category as inter-granular corrosion (IGC) and
stress corrosion (SCC). Severe inter-granular corrosion will
promote exfoliation, and the wedging stress caused by corrosion products plays a significant role in development of
exfoliation. An equiaxed grain structure has been shown to
be less susceptible to exfoliation corrosion [13]. Wrought
aluminium alloy 2025 with markedly elongated grain structure is prone to this kind of attack. The primary objective
of the present research is to investigate the influence of
hot forming parameters and grain refining elements on the
exfoliation resistance and mechanical properties of 2025
wrought product.

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2. Experimental

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2.1. Materials

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The 2025 aluminium alloys in the present research were

supplied by Mettis Aerospace Group, Redditch, UK. The

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0924-0136/$ see front matter 2004 Published by Elsevier B.V.

doi:10.1016/j.jmatprotec.2004.04.316
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T.Y. Liu et al. / Journal of Materials Processing Technology xxx (2004) xxxxxx

Table 1
Chemical composition corresponding to the 2025 aluminium alloy specification and chemical analysis results of the five 2025 variants (wt.%).

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81
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83
84
85
86
87
88
89
90
91
92
93
94
95
96
97
98
99
100
101
102
103

Zr

Ti

Al

0.501.2
0.8
0.78
0.78
0.78
0.81

1.0 max
0.19
0.23
0.19
0.2
0.2

3.95.0
4.14
4.51
4.49
4.58
4.67

0.401.2
1.05
0.69
0.64
0.61
0.64

0.05 max
<0.01
<0.01
<0.01
<0.01
<0.01

0.1 max
0.01
0.01
0.07
<0.02
0.01

0.02
0.02
0.02
0.02
0.02

0.25 max
0.01
0.01
<0.01
0.04
0.01

0.15 max
0.01
<0.01
<0.01
0.05
0.12

Bal.
Bal.
Bal.
Bal.
Bal.
Bal.

specification chemistry of 2025 and chemical analysis results of five 2025 variants are listed in Table 1. Alloy 2025H
corresponds to a standard composition, with the Mn content
at the high-end of the range, and lower copper than the other
variants. Alloys 2025HC, 2025HT and 2025HZ have high
chromium, titanium and zirconium compositions, respectively. It was decided to add 0.12% Zr for 2025HZ which,
though outside the allowable range, is at a level which has
a strong effect on recrystallisation and grain structure. LM
composition has lower Mn content compared with the H
composition as do the other variants.
2.2. Experimental procedures
The same procedures of casting, hot extrusion and hot
forging as those detailed in [9] were applied to manufacture the tested specimens. The extrusion billets were hot extruded at either 360 or 440 C. Hot forging was conducted at
250, 300, 360, 400 and 440 C. Sections from the forgings
were solution heat-treated for 6 h at 515 5 C, followed
by cold water quenching (<40 C). The forgings were then
artificially aged for 10 h at 170 C.
Exfoliation testing was conducted in accordance with the
guidelines in ASTM G3499 [5]. The testing specimen was
roughly equivalent to a quarter of the forging. To remove
any influence of peripheral coarse grain arising from the extrusion process, 2 mm was milled off the surface of the face
to be tested. This specimen was then degreased, and etched
for 1 min in 5 wt.% NaOH solution at 80 C, rinsed in water,
desmutted for 30 s in concentrated nitric acid at room temperature, rinsed with distilled water, and air dried. A protective lacquer was applied to both underside and sides of the
specimens. The exfoliation tests were conducted in a chamber that maintained the temperature at 25 3 C. The specimens were visually inspected at regular intervals (5, 12, 24,
48, 72 and 96 h), and the development of exfoliation corrosion was assessed by reference to the standard photographs
in ASTM G34 corresponding to: N (no appreciable attack),
P (pitting), EA (superficial exfoliation), EB (moderate exfoliation), EC (severe exfoliation), and ED (very severe exfoliation).
The characterization of microstructure was performed
mainly by optical microscope and scanning electron microscope (SEM). Quantitative metallographic analysis was
conducted using a Buehler Omnimet Image Analyser. Hard-

0.01
<0.01
<0.01
0.12
<0.01

ness testing was performed on an Instron Wolpert Testor 930

calibrated with a test-block to the requirements of ASTM
E92-92. Tensile tests were conducted at room temperature
on a computer controlled Dartec machine, in accordance
with ASTM standard B55784. Cylindrical tensile test specimens were made from forgings after heat-treatment. The
orientation of the specimens was parallel to the extrusion
direction and the longitudinal direction (L) of the forgings.
The gauge length and diameter were 30 and 6 mm, respectively. The loading direction was along the symmetrical axis
of the test pieces, and the loading rate was 0.01 mm/s. The
0.2% proof stress (Rp0.2 ), tensile strength (Rm ), elongation
(A), and reduction of area (Z) were obtained by analysis of
test results.
Finite element (FE) simulations of the extrusion and
forging processes were carried out using ABAQUS with
the aim of predicting the strain development during hot
forming. A two-dimensional extrusion FE model and a
three-dimensional forging FE model were created. The
extrusion billet and forging billet were considered the deformable part in each case. For the extrusion billet, plane
strain four-noded reduced integration elements (CPE4R)
were used and for the forging billet, hexahedral eight-noded
reduced integration elements (C3D8R) were used. Extrusion die, container and forging dies were assumed to be
rigid. Contact between the die and billet was modelled
including friction. The friction coefficient used was 0.06
since lubricant was applied to the platens during forging.
The material plastic properties were adopted from [8]. The
simulations were performed using the ABAQUS explicit
code. Adaptive meshing techniques were applied to modify
overly distorted elements since both extrusion and forging
are large deformation operations.

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3. Results and discussion

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3.1. Microstructural evaluation in hot processing

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The examination of microstructure as extruded and as

forged was carried out before heat-treatment. Both transverse sections (perpendicular to the extrusion direction) and
longitudinal sections (parallel to extrusion direction) were
examined. Transverse sections taken from front of the extrudate were examined to gain microstructural information

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Zn

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Ni

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Cr

EC

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Mg

RR

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Mn

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Cu

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Fe

PR

2025
2025H
2025LM
2025HC
2025HZ
2025HT

Si

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Fig. 2. 2025H forging longitudinal section (extruded at 360 C, forged at

440 C, no heat-treatment).

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aligned with the direction of material flow. This directional

microstructure became more appreciable at higher forging
temperatures (400 and 440 C), with coarse intermetallic
particles forming aligned stringers (Fig. 2).
No sign of recrystallisation during the hot forging stage
was detected on most specimens, which suggests that dynamic recovery rather than dynamic recrystallisation dominated the hot forging processes. It is well known that aluminium alloys are high stacking fault energy metals. More
active dynamic recovery mechanisms occur during hot forming decreasing the dislocation density and thus, reducing the
driving force for recrystallisation.
In addition, the FE simulations provided supporting
information that the forming temperature alters the microstructure. FE simulation results displayed an inhomogeneous plastic strain distribution over the forging billet
caused by non-uniform deformation. There was a higher
localised strain near the center of the billet. As expected,
strain energy accumulated through the hot forming process varied with forming temperature. Fig. 3 illustrates that
the strain energy increased progressively during forming,
and reached the highest level near the end of forming.
Lower forming temperatures gave rise to higher strain
energy, which will promote recrystallisation in subsequent heat-treatment. The results predicted by FE were
in agreement with the microstructural observation that a
fully recrystallised grain structure, with varied grain size,
was evident in all specimens forged at lower temperatures (250, 300, and 360 C) after heat-treatment, due to
the higher strain energy. At higher forging temperatures,
only partially recrystallised or unrecrystallised grain structures were observed. Furthermore, relatively smaller recrystallised grains were noted at materials forged at lower
temperatures, which was attributed to increased grain nucleation.

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about the homogenized ingot and the microstructure prior to

extrusion. A large volume fraction of coarse second-phase
was observed in these specimens, some with dendritic
and script morphology. The predominant phases were pale
pink and light grey with a very small amount of dark grey
phase. The SEM with energy dispersive X-ray spectroscopy
(SEMEDS) analysis indicated that these second phase particles were a Cu-rich phase that was assumed to be CuAl2 ,
a Fe-bearing phase, and an intermetallic compound of Mn,
Fe, Si and Al.
Examination of longitudinal sections where the microstructure was representative of the influence of extrusion
displayed elongated phase particles along the extrusion direction (Fig. 1). In the extrusion transverse sections taken
adjacent to the position where the forging billet was cut,
a larger volume fraction of second-phase was detected
for materials extruded at 360 C. The volume fraction
of second-phase in 2025HC extruded at 360 C was approximately 9%, while in samples extruded at 440 C it
was approximately 7%. Etched sections revealed that the
dendrite-casting network was removed for the majority of
the length of the extrudates.
Etched extrusion transverse sections exhibited a recrystallised layer at the outer surface. The depth of layer in the
2025HZ composition extruded at 440 C (94 m) was less
than that in the 2025H and 2025HT composition extruded
at same temperature (100 m). The average depth of the
recrystallised layer in the 2025HC and 2025LM extruded at
440 C were about 22 and 39 m, respectively. In unrecrystallised areas, a substructure was evident with average sub
grain diameter 34 m in the H, HZ, HC, HT and LM variants extruded at 440 C. An additional observation is that of
a very fine dispersed phase distributed homogenously in the
matrix of 2025 variants extruded at 360 C.
In the longitudinal section of forgings prior to heattreatment, flattened, elongated, constituent particles were

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Fig. 1. 2025H extrusion longitudinal section (extruded at

phase particles elongated into extrusion direction.

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360 C);

second-

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T.Y. Liu et al. / Journal of Materials Processing Technology xxx (2004) xxxxxx

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This part of the research mainly focused on the exfoliation resistance of 2025HT (high Ti) and 2025LM (low Mn),
compared with the other 2025 compositions studied in previous work [9], in order to evaluate the influence on exfoliation behaviour exerted by hot forming conditions. Table 2
displays visual rating results of all 2025 variants.
In specimen 2025HT, extruded at 360 C, and forged at
250 C, with a corrosion rating of EB, full recrystallisation
(Fig. 4) was exhibited. These pancake like grains, were
elongated in both the L and LT directions and were flatter
in the ST direction. The average grain size was 117 72,
88 47, and 34 20 m in the L, LT and ST orientations, respectively. Increasing the forging temperature also
resulted in fully recrystallised grains, but with a larger grain
size. The average grain size in the specimen extruded at the
same extrusion temperature, but forged at 300 C were 127

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Table 2
Visual rating of exfoliation testing specimens
Extrusion
temperature ( C)

Forging
temperature ( C)

ASTM G34 EXCO rating

2025H

2025HZ

2025HT

2025LM

96 (h)

48 (h)

96 (h)

48 (h)

96 (h)

48 (h)

96 (h)

48 (h)

96 (h)

ED
EB
EA
EA
P

N
N
Na
Na
Na

EB
EB
EA
P
EB

N
N
N
N
Na

EB
EB
P
P
EA

N
N
N
N
EA

EB
EB
EA
EA
EC

N
N
N
Na
EB

EB
EB
EA
Pa
ED

N
N
N
N
N

EB
EB
P
P
P

N
N
N
N
N

EB
EB
EA
P
P

N
N
N
N
N

EB
EB
EB
EA
EA

N
N
N
N
Na

EB
EB
EA
P
EC

250
300
360
400
440

EA
EA
EA
Na
Na

440
440
440
440
440

250
300
360
400
440

N
N
Na
N
N

Exfoliation at edge only.

2025HC

48 (h)
360
360
360
360
360

EC

222

RR

221

EA
EB
P
P
P

CO

220

UN

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97, 122 74, and 39 24 m in the L, LT and ST directions, respectively. In specimen forged at 360 C much
larger recrystallised grains appeared, with L, LT and ST dimensions of 222 127, 218 182, and 55 32 m. In this
specimen, exfoliation resistance was improved with a rating
of EA. When forging temperature was increased to 400 C,
partially recrystallised grain structure began to appear with a
large volume fraction of recrystallisation (Fig. 5). The poorest exfoliation behaviour was observed at the highest forging temperature 440 C, and microstructure examination of
2025HT at this temperature revealed an almost fully unrecrystallised structure (Fig. 6). Moreover, the corresponding
rating was EC. The general tendency was that decreased exfoliation corrosion susceptibility was associated with higher
forging temperature with the exception of the forging temperature of 440 C.
The microstructural variation and exfoliation performance
of 2025LM showed a similar pattern. At 440 C forging
temperature, 2025LM did not show improved resistance to

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Fig. 4. 2025HT extruded at 360 C, forged at 250 C. Fully recrystallised.

Fig. 3. FE predicted strain energy (J/m3 ) developed during forging: ()

250 C; () 300 C; () 360 C; () 400 C; () 440 C.

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The results of micro hardness testing of 2025 alloys did

not show much variation. The values of hardness varied between 121 and 135 (the specification for Vickers Hardness
of 2025 alloys is 124). The 2025LM composition displayed
the lowest hardness, and lowest yield strength Rp0.2 and ultimate tensile strength Rm . The detailed cause for this requires
further investigation.
Tensile properties of materials can be affected by several factors, e.g. forming conditions, grain structure, alloy
refining elements, the size and distribution of intermetallic phases, and heat-treatment procedures. Fig. 7 illustrates
part of the tensile test results, which show that tensile properties varied with hot forming temperature and compositions. The yield strength Rp0.2 , of the 2025HZ, 2025HC and
2025HT compositions varied in the range of 236316 MPa,
226292 MPa, and 221293 MPa, respectively, while the ultimate tensile strength Rm of the same compositions varied between 341 and 421 MPa, 342401 Mpa, and 336
423 MPa, respectively.
It can be seen that the Rp0.2 , and Rm , of materials at a
forging temperature of 360 C was lower, for almost all alloys. A coarse fully recrystallised structure was displayed at
this temperature, although the structure behaved well when
subjected to the exfoliation corrosion test. The 2025HZ alloy extruded at 360 C and forged at 400 C showed highest tensile strengths, but with relatively low ductility. When
2025HZ was extruded at 440 C and forged at low temperature, a good tensile strength level was obtained due to a fine
recrystallisation structure at lower forging temperature, and
corresponding ductility at this point was acceptable.
At an extrusion temperature of 360 C, 2025HC and
2025HT also displayed higher tensile properties at a forging
temperature of 400 C, but with low ductility at this point.
Relatively higher levels of Rp0.2 , and Rm , and medium
ductility of 2025HC and 2025HT were obtained at lower

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3.3. Mechanical properties

PR

256

268

EC

255

RR

254

Fig. 6. 2025HT extruded at

tallised.

360 C,

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Partially recrys-

exfoliation and was rated as ED. Examination of the microsection revealed an almost fully unrecrystallised structure.
Another reason was probably that lower Mn content in the
material was not able to inhibit the damaging effects on corrosion performance caused by Fe-rich intermetallic phases
at high temperature.
The influence of extrusion temperature on exfoliation corrosion resistance was also evident by comparing 2025HT
and 2025LM extruded at 360 and 440 C, and forged at the
same temperature. The higher extrusion temperature gave
rise to better corrosion performance since a coarser grain
structure was formed.
For evaluation of the exfoliation corrosion susceptibility
of all the 2025 alloys, comparison of the present research
with previous work in [9] was carried out. It was noted that
all tested materials exhibited the trends already reported in

forged at

440 C.

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forged at

400 C.

[9] toward this form of corrosion attack. At a given extrusion temperature, higher forging temperatures led to more
resistance to exfoliation as a coarser recrystallisation grain
structure was obtained after heat-treatment. However, HZ,
HC, HT and LM compositions exhibited a higher susceptibility at high forging temperatures (440 C) that was not
observed in the H variant. The examination of the microsections of the former forged at 440 C revealed an almost fully
unrecrystallised grain structure. Besides grain structure, another possible reason for this corrosion susceptibility was
that since all these four compositions contained relatively
higher Cu, more CuAl2 precipitation is likely to occur at the
grain boundary during heat-treatment, resulting in Cu depletion at the grain boundary, forming an anodic path that facilitates inter-granular corrosion attack. Severe inter-granular
corrosion develops to exfoliation finally. Generally, a coarse
recrystallised grain structure renders 2025 alloys more resistant to exfoliation attack.

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tallised.

360 C,

Fully unrecrys-

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Fig. 7. Testing results of tensile properties: () Rp0.2 ; () Rm ; () A; ( ) Z.

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forging temperatures (250 and 300 C) when extruded at

440 C; again, finer recrystallised grain structure was observed in these specimens. It is worthwhile to note that both
2025HZ and 2025HT exhibited relatively high Rp0.2 and Rm

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(Fig. 8), which reflected the refining effects of the addition

of Zr and Ti. Microstructural examination confirmed that
both 2025HZ and 2025HT showed finer grain structure.
The addition of Cr did not result in any apparent change in

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4. Conclusions
The exfoliation resistance and mechanical properties of
five 2025 aluminium alloys with grain refining additives
were investigated. The present study focused on the microstructural development during hot forming processing
and heat-treatment with special interest on recrystallisation
grain structure. The above properties of 2025 alloys were
found to be markedly dependent on microstructure resulting
from hot deformation and heat-treatment.
Alloy compositions, extrusion temperatures and forging
temperatures proved to be major factors that had considerable influence on susceptibility to exfoliation corrosion, due
to their effects on microstructure.
Since aluminium alloys are high stack fault energy metals, dynamic recovery was expected to dominate the hot
forming process [7], and this was verified by microstructural examination. Recrystallisation occurred mainly in the
heat-treatment operation.
The finite element (FE) analysis results provided a useful
insight into hot deformation, by revealing that strain energy
built up in the hot forming process was affected by the forming temperature. Lower forming temperature led to higher
stored strain energy at a given deformation rate, which promoted recrystallisation during heat-treatment. In addition,

Uncited reference

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the FE analysis revealed that an inhomogeneous strain field

was developed during hot deformation, which will alter grain
size and distribution.
Good exfoliation corrosion resistance was related to a
coarse fully recrystallised grain structure. The fine fully recrystallised structure did not display high-resistance to exfoliation. The poorest resistance was related to fully unrecrystallised structure. The influence of hot forming temperatures
on exfoliation susceptibility was illustrated by the fact that
higher extrusion temperature and higher forging temperature (below 440 C) improved the resistance of 2025 alloys
to exfoliation. The 2025LM alloy exhibited the worst exfoliation behaviour at a forging temperature of 440 C.
Tensile properties were also affected by the final microstructure. A fine recrystallised structure led to high Rp0.2 ,
and Rm . As noted above, a coarse recrystallised structure
led to better resistance to corrosion but, unfortunately, it
also tended to reduce tensile strength. Moreover, high yield
strength was usually associated with loss of ductility. At high
extrusion temperature, good tensile properties were obtained
at low forging temperatures.
The addition of Zr, Cr and Ti was shown to refine the grain
structure, especially at low extrusion temperature. These refining elements also increased the exfoliation corrosion susceptibility at higher forging temperatures by retarding recrystallisation. The addition of Zr and Ti improved the tensile strength of 2025 alloys slightly, while Cr had little effect
on tensile properties. The high copper low manganese variant 2025LM showed lowest tensile properties but behaved
well regarding ductility, which requires further investigation.

EC

333

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332

tensile properties, which may be due to the relatively small

addition of Cr in the 2025HC alloy.
In short, test results showed the dependence of tensile
properties on the microstructure developed in hot forming and heat-treatment. Further investigation of mechanical
properties is necessary in order to decide if the directional
grain structure will cause anisotropy of properties in 2025
alloys.

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Fig. 8. (a) Rp0.2 of 2025 alloy (extrusion temperature 360 C); (b) Rm of 2025 alloy (extrusion temperature 360 C). () 2025H; () 2025HZ; ( )
2025HC; () 2025HT; () 2025LM.

[4,6].

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Acknowledgements

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The authors wish to acknowledge the support of Mettis

Aerospace Group, Redditch, UK, for supplying the 2025,
Mr. Richard Cudd for technical assistance, and the Materials and Surface Science Institute at the University of Limerick for part-funding the project. For correspondence please
contact jeremy.robinson@ul.ie.

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References

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[1] Annual Book of ASTM Standards, G34-99 (American Society for

Testing and Materials, Philadelphia), Pennsylvania, USA, 1999.

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[2] ASM speciality handbook, in: J.R. Davies (Ed.), Aluminium and Aluminium Alloys (ASM International, OH440730002, USA), 1993, 598.
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[5] H.J. McQueen, Hot working and recrystallisation of face-centred cubic
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[6] Mettis Aerospace Group/HAD Forgings Ltd., UK (unpublished data).
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[8] S.J. Ketcham, I.S. Shaffer, ASTM STP 516, ASTM 1972.
[9] T.Y. Liu, J.S. Robinson, M.A. McCarthy, The influence of processing
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