Rare Met.

https://doi.org/10.1007/s12598-020-01481-7 RARE METALS

ORIGINAL ARTICLE

Microstructures and mechanical properties of a cast Al–Cu–Li

alloy during heat treatment procedure
Shu-Wei Duan , Kenji Matsuda, Tao Wang* , Yong Zou*

Received: 15 March 2019 / Revised: 17 April 2019 / Accepted: 29 May 2020

Ó The Nonferrous Metals Society of China and Springer-Verlag GmbH Germany, part of Springer Nature 2020

Abstract Al–Cu–Li alloy is a huge potential alloy for Keywords Al–Cu–Li alloy; Heat treatment;
aerospace industry due to its low density and excellent Microstructure; Mechanical property; Precipitate
comprehensive performances. In this study, the
microstructures and mechanical properties of a novel cast
Al–Cu–Li alloy during the heat treatment were investi- 1 Introduction
gated. Results showed that most of the secondary phases
along grain boundaries in as-cast state were dissolved into The lithium (Li) element, as the lightest metal in the world,
the Al matrix after homogenization and solution treatment, was added into the aluminum (Al) alloy; it not only greatly
while the Cu-rich phases were slightly segregated once reduced the density of alloy, but also obtained excellent
again on grain boundaries after aging. A relatively good comprehensive performances. The third generation of Al–
combination of strength and ductility (average ultimate Cu–Li alloy has been extensively used as structural mate-
tensile strength of 430 MPa and elongation of 8.9%) was rial for aerospace industry and attracted many researchers
obtained after natural aging. Transmission electron to study various aspects of them. The precipitates, espe-
microscopy (TEM) results revealed that there was a com- cially T1 (Al2CuLi) and h0 (Al2Cu), in this kind of alloy
plicated precipitate distribution in this cast alloy after played vital roles on its superior performances [1–5].
natural aging. Compared with the similar alloys which In recent years, most studies related to Al–Cu–Li alloy
introduced dislocations before aging, the density of T1 are mainly focused on two aspects: (1) relationship of
(Al2CuLi) phases was decreased but the size was increased. microstructure evolution and mechanical properties; (2) the
The low volume fraction of d0 phase, medium density of structure and formation mechanism of various precipitates
needle-shaped precipitates and relativity narrow precipi- during their evolution. The first aspect was almost spe-
tates-free zone with varying widths near grain boundary are cialized in rolled or wrought state due to that they are the
the reasons accounting for the improvement of actual states of alloy application, but when it comes to the
performances. second aspect, researchers seemed not to be very concerned
about the state of alloy. For example, in the study of the
growth mechanism of T1 precipitate, rolled alloy was
employed in Refs. [6, 7], while in Refs. [8, 9] cast alloy
S.-W. Duan, T. Wang*, Y. Zou*
MOE Key Laboratory for Liquid–Solid Structure Evolution and was used. Besides, some scholars directly introduced the
Materials Processing, Institute of Materials Joining, Shandong dislocation into the as-cast alloy by pre-stretching in their
University, Jinan 250061, China researches, such as Gumbmann et al. [10]. However,
e-mail: wxm689wxm@sdu.edu.cn whether the state of the alloy would affect the behavior of
Y. Zou precipitates is a question worthwhile to be further explored.
e-mail: yzou@sdu.edu.cn Casting Al–Cu–Li alloys can be used to manufacture
K. Matsuda many complex-shaped products simply, and it is of great
Department of Materials Science and Technology, Faculty of practical value for aviation industry due to their low
Engineering, University of Toyama, Toyama 930-8555, Japan

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 S.-W. Duan et al.

density. Previous studies [11] have shown that the dislo- treatment was performed by two steps: two-stage homog-
cation could greatly promote the nucleation of T1 precipi- enization treatment and then water-quenched artificial
tate and suppress the width of precipitates-free zone (PFZ) aging followed by 6-month natural aging. The specific
in the grain boundary. However, the cast products are not parameters of the heat treatment are shown in Fig. 1.
allowed via pre-strength or rolling before aging consider- The metallography specimens were prepared according
ing its complex shape. Therefore, it is more reasonable to to the standard metallography procedures. The samples
improve the performances merely using the heat treatment were etched using Keller0 s etchant (2.5 vol% HNO3 ?
process. 1.5 vol% HCL ? 1 vol% HF ? 95 vol% H2O) for 30 s
Up to now, few researches concentrated on improving and then observed using optical microscope (OM, VHX-
the performance of cast Al–Cu–Li alloys through the heat 500F Keyence) and scanning electron microscope (JMS-
treatment procedure directly. Chen et al. [12] studied the 6610LA SEM) attached energy-dispersive spectroscope
heat treatment of cast Al–3Li–1.5Cu–0.2Zr alloy, and the (EDS). The Vickers hardness of the artificial aging for
ultimate tensile strength (UTS) obtained was 382 MPa at different times was measured on a DHV-1000 digital
peak aging, but the elongation was only 2.9%. On this hardness tester under a load of 0.98 N and a holding time
basis, the microstructure and mechanical properties of cast of 15 s. The standard tensile specimens were prepared after
Al–2Li–2Cu–0.5Mg–0.2Zr alloy during the heat treatment peaking artificial aging and followed by 6 months of nat-
were investigated by Zhang et al. [13]; although their UTS ural aging. Then, room-temperature tensile test was per-
increased to 440 MPa at peak aging, the elongation was formed on a WDW-100E instrument. The fractured
still only 4.5%. Both of them selected high Li content in surfaces were also examined by SEM. X-ray diffraction
order to obtain low density, but high Li content (C 2 wt%) (XRD, Miniflex 600) was employed with the scanning ratio
may also lead to poor ductility and insufficient damage of 10 (°)min-1.
tolerance, which would restrict the application in aerospace The 0.8-mm-thick slices were cored from the samples
industry due to the high requirements for toughness [1]. after peaking aging followed by natural aging and then
Therefore, reducing Li content of cast alloy to the level of mechanically thinned to 120 lm. Transmission electron
the third-generation Al–Li alloys and studying the suit- microscopy (TEM) samples were obtained by single-jet
able heat treatment procedure are of significance. thinning conducted with two kinds of electrolyte: one
In this study, a third generation of Al–Cu–Li cast alloy comprises 25 vol% HNO3 and 75 vol% CH3OH; another
with relatively low Cu/Li ratio and complex minor alloying comprises 10 vol% HClO4 ? 90 vol% C2H5OH. The
elements were employed. A heat treatment procedure was operating temperature was below 273 K. TEM micro-
implemented to gain better mechanical properties, and the graphs, including the selected area diffraction (SAD) and
microstructure features were investigated. Considering bright-field (BF) images, were taken with EM-002B TEM
there have been abundant researches on the evolution of operated at 120 kV.
microstructure and mechanical properties of the Al–Cu–Li
alloy during its aging already, we have not paid much
attention to details in the heat treatment process, but
focused on three aspects: (1) effect of the heat treatment on
precipitates in grain boundaries, (2) the optimal mechanical
properties achieved and (3) the final precipitate character-
istics obtained.

2 Experimental

The investigated material was a novel Al–Cu–Li cast alloy,

its Cu/Li ratio was further reduced in order to get low
density, and the composition is shown in Table 1. The heat Fig. 1 Heat treatment procedures

Table 1 Chemical composition of the investigated alloy (wt%)

Cu Li Mn Zr Ti Mg Fe Si Sn Be Al

2.8 1.4 0.28 0.11 0.03 0.07 0.04 0.03 0.009 0.003 Bal.

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Microstructures and mechanical properties of a cast Al–Cu–Li alloy

Fig. 2 a–c OM images and d–f SEM images of different stages during heat treatment: a, d as-cast alloy; b, e as-quenched alloy; c, f after aging

3 Results and discussion that the serious segregation of elements and secondary
phases happened in there when the alloy is solidifying.
3.1 Effect of heat treatment on microstructures Elemental map-scanning distributions in grain boundary
and its neighboring areas of as-cast alloy are displayed in
OM and SEM images of initial as-cast alloy are shown in Fig. 3a. We can see evident Cu in grain boundaries and
Fig. 2a, d. The microstructure of as-cast alloy is charac- accompanied by partly segregation of Fe. EDS point scans
terized by explicit and wide grain boundaries. It may mean in Fig. 4 further illustrate this phenomenon, it is found that

Fig. 3 Elemental map-scanning distributions of different stages during heat treatment: a as-cast, b as-quenched, and c after aging

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Fig. 4 EDS point scans results: a in grain boundary and within grain of as-cast alloy, b in grain boundary of as-quenched alloy, and c in grain
boundary of after aging alloy

most microalloying elements are segregated to some extent demonstrate that the ideal result is achieved by the
on grain boundaries in as-cast alloy, and the content of homogenization and solution treatment.
intergranular Cu and Fe is significantly higher than the that The samples after natural aging were studied in the same
of intragranular regions. way. In the optical microstructure (Fig. 2c), the number of
In order to eliminate serious segregation of elements and fine black spots and lines increases the grain boundaries,
secondary phases constituents in the as-cast alloy mean- indicating that the secondary phases on grain boundaries
while making the alloying elements be dissolved into the have slightly precipitated again after aging. Similar results
matrix as much as possible, two-stage homogenization and are also displayed in SEM image (Fig. 2f), and the white
solution treatment were employed. OM and SEM images of areas are slightly increased compared to the state of as-
as-quenched alloy are presented in Fig. 2b, e. Compared to quenched. Moreover, the results of elemental map-scan-
the as-cast alloy, it can be observed that the grain bound- ning distributions (Fig. 3c) and EDS point scans (Fig. 4c)
aries became relatively clean and only a little amount of indicate that although some grain boundary precipitates
second phases remained. Elemental map-scanning distri- occurred after aging, there is no serious segregation of
butions of samples after homogenization shown in Fig. 3b alloying elements, so the precipitation at grain boundaries
also illustrate the result of the homogenization. The seg- in aging is only in a small scale.
regation of Cu and Fe in grain boundaries in as-cast alloy is XRD results of the studied alloy at different heat treat-
also effectively decreased. The effects of homogenization ment conditions are shown in Fig. 5. It can be observed
and solution on elements at the grain boundaries are also that the main peaks of as-cast alloy are a-Al and Al3Li
verified in EDS point scans results (Fig. 4), it can be seen phases. Previous studies [14] have reported that other
that Al and Cu become main elements at the grain phases such as Al2Cu, Al2CuMg, AlLi and Al6CuLi3
boundary, and the content of Cu decreased from 28.5 at% should also be existed in the as-cast alloy, but there are no
(as-cast) to 3.75 at% (as-quenched). All of these responses visible peaks of these phases probably because of their

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Microstructures and mechanical properties of a cast Al–Cu–Li alloy

Fig. 5 XRD results of different stages during heat treatment Fig. 7 Tensile properties after all treatments

relatively small amounts. The most significant aspect in caused by the dissolution of solute clusters, especially
this graph is the diffraction peaks of the secondary phases Cu-rich clusters. Results of previous studies [16] have
which declined obviously after homogenization and solu- also demonstrated that the precipitation of a large
tion treatment, revealing that most intermetallic phases amount of precipitates, such as T1, h0 and d0 (Al3Li), is
have dissolved into the Al matrix. And after aging, the T1, directly accounted for the rapid rise of hardness subse-
h0 and d0 (Al3Li) phases precipitated with a large number, quently, and their coarsening during over aging resulted
and their characteristic diffraction peaks play the main role in the decline of hardness.
in XRD patterns. The level of the eventual tensile properties after a series
of heat treatments is also what we are concerned about.
3.2 Optimal mechanical properties achieved Figure 7 provides the engineering stress–strain curve of a
representative sample after all treatments. The average
Figure 6 provides the hardness evolution curve of the UTS has achieved a relatively ideal level (430 MPa). The
alloy in the process of artificial aging at 175 °C. It can be most significant aspect is that the mean elongation reaches
seen that the hardness increases continuously with aging 8.9%; it is a noticeable improvement compared to 2.9% or
time before peak aging except a slight decline in early 4.5% in previous researches [12, 13]. SEM images of the
periods of aging. The maximum hardness is occurred fracture surface are shown in Fig. 8, and it can be seen that
after aged for 24 h, and the value is * HV 136. More- small and densely distributed shallow dimples are present
over, the hardness of samples with peak-aging state can on the fracture surface, accompanied by many smooth
be further increased to HV 144 in subsequent 6-month surfaces. It is the typical intergranular-dimple mixed-type
natural aging. Decreus et al. [15] also observed a sig- fracture mode. The occurrence of a large amount of dim-
nificant softening in the early artificial aging of 2198 and ples also indicates that the relatively good ductility has
2196 alloys. According to their research, it is mainly been attained on the other hand.

Fig. 6 Hardness evolution of studied alloy: a artificial aging at 175 °C and b natural aging of artificial peak aged alloy

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Fig. 8 SEM images of fracture surfaces of tensile sample with different magnifications

Fig. 9 BF images, SAD patterns and corresponding schematic models with a [100] zone axis and b [110] zone axis

3.3 Final precipitate features obtained In addition, other rare precipitates including the phase of
the variant of h0 and the r (Al6Cu5Mg2) phase are also
The final microstructure features of precipitates are also observed. It can be seen that four orientations of needle-
interesting research focus due to that the precipitates play shaped precipitates occur in BF image of Fig. 10. Previous
a crucial factor in performances of Al–Cu–Li alloy. The study [21] has clarified that two orientations belong to two
BF images, SAD patterns and corresponding schematic variants of T1 phase and one is regular h0 phase with the
models of the alloy after all treatments are given in Fig. 9. orientation relationship of (100)h0 //(100)a and [001]h0 //
At least four sets of diffraction patterns are found, which [001]a in Al–Cu–Li alloy when viewing along [110]Al.
are from the Al matrix, the T1, h0 and d0 precipitates, However, the precipitate marked by blue line has another
respectively [17, 18]. These precipitates can also be orientation, which is the variant of h0 and it seems that only
explicitly observed in the BF images. The T1 phase is the direction of c-axis rotates 90° compared to the common
hexagonal and present as platelets on Al plane [19], and h0 h0 phase. Two orientations of h0 are apparent in almost all
phase is tetragonal and semi-coherent with the matrix, related studies of the binary Al–Cu systems when viewed
appearing as disks lying on the {100}Al planes, which are in the [100] direction, such as the researches by Ma et al.
two major strengthening phases in the Al–Cu–Li alloy. [22] and Bourgeois et al. [23]. However, the h0 variant
The d0 phase is spherical and may coexist with a small which is perpendicular to regular h0 phase when viewed in
amount of b0 (Al3Zr) in the form of core/shell particles the [110] direction is rarely reported, and it may be due to
[20]. its instability of occurrence and little amount.

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Microstructures and mechanical properties of a cast Al–Cu–Li alloy

Fig. 10 TEM images of precipitate seening to h0 variant viewed in [110] direction with different magnifications

Fig. 11 a TEM image of r phase viewed in [100] direction; b FFT image of framed area in a; c FFT image after filtering; d inverse FFT images;
e, f corresponding image intensity contrast distribution in two vertical directions marked by green lines in d

Meanwhile, another phase with extremely small amount precipitates around r phase as shown in Fig. 11 is not the
is also observed in Fig. 11. Fast Fourier transform (FFT) state as we expected.
and inverse FFT images indicate that this phase has cubic As stated above, most precipitates contained in the alloy
structure and seems semi-coherent with matrix, then it is have been expounded, but the main reason for the
considered to be r phase. The lattice parameters in two improvement of elongation after the natural aging is still
vertical directions of the phase are estimated to be 0.784 not explicit. So, we evaluated the other information of the
and 0.797 nm by spacing of image intensity, which are precipitates. The presence of large area fractions of grain
close to the value of 0.794 nm calculated by Li et al. [16]. boundary precipitates (GBP) and soft precipitates-free zone
Although r phase is thought to be beneficial to the stability (PFZ) nearby is considered to be the important reason
of the alloy due to its coarsening resistance of high tem- which caused the decrease in plasticity and toughness in
perature [24], the high concentration of Cu in r phase may aging aluminum alloy [25, 26]. Therefore, the TEM images
also facilitate it competing for Cu atoms with T1 and h0 of grain boundary and adjacent zone are observed, and the
phases in the vicinity. The area lacking of needle-shaped results are shown in Fig. 12. It can be seen that the

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Fig. 12 TEM images around grain boundary from different views

Fig. 13 a One of BF image for precipitates measurement viewed in [110] direction; b length distribution of T1 precipitates; c length distribution
of h0 precipitates

relatively large GBP situates in some grain boundaries, the shows, there is a significant difference of the distribution
width of PFZ is relativity narrow and the width changes shape between two phases. Further calculation indicates
greatly with grain boundaries variation. The existence of that the average planar density of needle-shaped precipitate
GBP may be beneficial to facilitate the intergranular frac- observed in [110]Al direction is 58.9 lm-2
-2 0 -2
ture, but the relativity narrow PFZ with varying widths can (T1 * 43 lm , h * 15.9 lm ), and the average length
reduce the sensitivity of strain localization under plastic size of needle-shaped precipitate observed in [110]Al
deformation; thus, it is a reason which helps to the direction is 142.7 nm (T1 * 146.7 nm and h0 * 131.9
enhancement of ductility. nm). Compared to related values in previous researches on
In addition, the length distribution of the T1 and h0 rolled or pre-strength alloys (size and density information
precipitates in the [110] direction is estimated. As Fig. 13 of T1 precipitates in some studies are counted in Table 2
[11, 15, 18, 27, 28]), the average length of needle-shape
Table 2 Size and density information of T1 precipitates in rolled Al– precipitates is greatly increased, but the density is
Cu–Li alloy decreased to some extent. This may be due to the fact that
Alloy Mean size/nm Density information Refs.

2198-T8 50.7 4.9 vol% [27] Table 3 Size of d0 particles in cast Al–Cu–Li alloy and corre-
2198-T81 90 – [28] sponding mechanical properties
2196-T351 60 – [15] Alloy Average UTS/ Elongation/ Refs.
2198-T351 40 – [15] size/nm MPa %
2195-T8 63 1696 lm-3 [18] Al–3Li–2Cu–0.2Zr 32 415 2.7 [29]
Weldalite 049-T6 126.6 2012 lm-3 [11] Al–2Li–2Cu– 21.5 443 4.5 [13]
Weldalite 049-T8 93.8 6392 lm-3 [11] 0.5Mg–0.2Zr

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Microstructures and mechanical properties of a cast Al–Cu–Li alloy

there is no introduction of dislocations, resulting in few aging is characterized by the presence of massive T1, h0 and
nucleation sites in studied alloys, and leading to continuous partial d0 precipitates, and some rare precipitates including
growth in the diameter direction of precipitates during h0 variant and r phase also exist. Low volume fraction of d0
aging. It should be emphasized that though the density of phase, medium density of needle-shaped precipitates and
strengthening precipitates in this study is not as high as that relativity narrow PFZ with varying widths near grain
of rolled, extruded or pre-deformation Al–Cu–Li alloys, it boundary are the reasons which could improve the
still has a noticeable increase compared to that of the cast ductility.
alloys mentioned in Refs. [12, 13, 29]. Moreover, as shown
in BF image of Fig. 9b, the volume fraction and size of Acknowledgements This study was financially supported by the Key
Research and Development Project of Shandong Province (No.
spheroidal d0 particles in this research are much less than 2018CXGC0403).
those in previous, as shown in Table 3 [13, 29], which is
mainly due to relatively lower Li content in the studied
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