Journal of Alloys and Compounds 821 (2020) 153125

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Microstructure evolution and mechanical behavior of AleLi alloy

fabricated by laser melting deposition technique
Shikun Jiao a, c, Xu Cheng a, b, Shuxin Shen a, b, Xin Wang a, b, Bei He a, b, Dong Liu a, b, *,
Huaming Wang a, b
a
National Engineering Laboratory of Additive Manufacturing for Large Metallic Components, Beihang University, School of Materials Science and
Engineering, Beihang University, 37 Xueyuan Road, Beijing, 100083, China
b
Beijing Engineering Technological Research Center on Laser Direct Manufacturing for Large Critical Metallic Components, 37 Xueyuan Road, Beijing,
100083, China
c
Beijing Xinghang Electro-mechanical Equipment Co., Ltd, NO.9 Dongwangzuo North RD, Fengtai District, Beijing, 100074, China

a r t i c l e i n f o a b s t r a c t

Article history: This paper systematically studies the microstructure evolution, tensile property and microhardness of
Received 2 September 2019 Aluminum-lithium (AleLi) alloy with dimension of 80 mm
30 mm
80 mm manufactured by laser
Received in revised form melting deposition (LMD) technology. Results indicate that the microstructures of the as-deposited AleLi
17 November 2019
alloy are variable from the top to the bottom of the plate. At the top region, a fully dendritic structure is
Accepted 20 November 2019
observed with underdeveloped secondary arms. And the copper-rich precipitates with irregular stripe
Available online 21 November 2019
morphology appear in the inter-dendritic areas. Attributing to the thermal cycle during laser deposition
process, as distance increasing away from the top, the number of irregular stripe phases reduces with the
Keywords:
Laser melting deposition
massive precipitation of needle-like TB phases (soft and brittle). At the bottom of the plate, dendritics of
Aluminum-lithium alloy as-deposited AleLi alloy obviously coarsened, TB phases fully decorate the entire grains with a few re-
Microstructure evolution sidual copper-rich precipitates. Attributing to the different microstructures, the micro-hardness firstly
TB phase increases from 121 HV to 134 HV at a distance of 30 mm, and then decreases to about 98 HV at the
Microhardness bottom of the deposited AleLi alloy plate. The ultimate tensile strength of the as-deposited AleLi alloy
Tensile property (longitudinal direction, at the middle-bottom part of the plate) is comparable to the hot-rolled AleLi
alloy (244 MPa). However, the yield strength and elongation of the as-deposited AleLi alloy are rela-
tively poor due to the embrittlement of copper-rich phases as well as TB phase.
© 2019 Elsevier B.V. All rights reserved.

1. Introduction promising candidate material using in the next generation aero-

space application. Casting technology is one of the most common
AleLi alloy has good combination of low density, high elastic methods to fabricate AleLi alloy components. However, the high
modulus, enhanced specific strength and rigidity, excellent fracture chemical activity of lithium may cause serious oxidation and even
toughness and fatigue crack growth resistance [1e3]. In general, explosion when directly contacting with oxygen or water vapor
around 1 wt.% Li addition could provide approximately 3% [4,5]. In addition, due to slow cooling rates and improper selection
decreasing in density and 6% increasing in Young’s elastic modulus of processing parameters, the as-casted Al alloy always presents
of aluminum alloy [1]. Thus, AleLi alloy is considered as a coarsened-grains with randomly distribution of defects such as gas
pores and shrinkage holes [5,6].
Laser melting deposition manufacturing (LMD) is one of a rapid
prototyping manufacturing methods [7]. During the process of
* Corresponding author. National Engineering Laboratory of Additive
Manufacturing for Large Metallic Components, Beihang University, School of Ma- LMD, laser is utilized to create a melt pool at the surface of a sub-
terials Science and Engineering, Beihang University, 37 Xueyuan Road, Beijing, strate within an inert atmosphere accomplished by delivering co-
100083, China. axial powders from powder nozzles. Near-net-shape metal
E-mail addresses: [email protected] (S. Jiao), [email protected] components are consequently built in a layer-by-layer mode by
(X. Cheng), [email protected] (S. Shen), [email protected] (X. Wang),
melting and solidification via computer numerical control system
[email protected] (B. He), [email protected] (D. Liu), [email protected]
(H. Wang). (CNC) [7e10]. Attributing to the advantages of no mold, few

https://doi.org/10.1016/j.jallcom.2019.153125
0925-8388/© 2019 Elsevier B.V. All rights reserved.
2 S. Jiao et al. / Journal of Alloys and Compounds 821 (2020) 153125

material wastes, short production cycle and great designing flexi- Table 2
bility, LMD is fast developed and has been successfully apply to Experiment parameters of LMD process.

titanium alloy [11e13], ultra-high strength steel [14] and superalloy Parameters Values
[15,16]. Laser power P (W) 4000e6000
However, compared with aforesaid alloys, the fabrication of Laser beam diameter D (mm) 6e7
aluminum alloys have many intrinsic problems [6,17] such as high Scanning speed Vs (mm/min) 600e900
reflectivity, low laser energy absorption and poor oxidation resis- Powder feeding rate Vf (g/min) 8e12
Atmosphere condition (ppm) O2  50; H2O  50
tance, which raise the difficulties of production Al based compo-
Scanning strategies snakelike
nents. The most reported Al alloys, preparation by additive Powder size 150 mesh
manufacturing (AM) process, are AleSi based alloys [18e20]. For Thickness of deposition layer (mm) 2
example, J Li [20] successfully fabricated a Ale5SieCueMg alloy
component using the LMD technique. Compared with AleSi alloy, Li
element in Al alloy has high chemical activity and low melting Beihang University with the processing parameters are listed in
temperature, which easily evaporate during LMD process. Besides, Table 2. A plate with dimension of 80 mm
30 mm
80 mm
high cooling rates and unstable thermal cycles can cause unpre- (Fig. 2) was fabricated on a pure Al plate substrate and the chemical
dictable microstructure thus influence mechanical property of alloy compositions of as-deposited AleLi alloy are also listed in Table 1.
[21e23]. For example L Cui [22] suggested that during fast cooling,
some un-wanted phases of d0 appeared in fusion line when welding 2.3. Microstructure characterization
of AleLi alloy. Hence, many efforts are required to put forward to
fabricate AleLi alloy using LMD technique. Microstructures of the longitudinal direction (YOZ section) of
In this study, by adjusting the working parameters and powder as-deposited samples were investigated. Metallographic specimens
compositions, a third generation AleLi alloy (based on 2A97 alloy) with dimension of 10 mm
10 mm
10 mm were cut at different
is fabricated by LMD technique. The microstructure evolution and position by wire-electrode discharge cutting machine, which were
mechanical behavior of LMDed AleLi alloy are carefully analyzed then ground by SiC abrasive paper and mechanically polished using
and which will offer some fundamental knowledge for the subse- diamond polishing paste. After that, the polished samples were
quent heat treatment. etched using Keller’s reagent which consisted of 1.0 mL HF, 2.5 mL
HNO3, 1.5 mL HCl and 95 mL H2O. Optical microscopy (OM, Leica-
DM 4000 M), scanning electronic microscopy (SEM, JSM 6010 and
2. Methods
CS 3400) equipped with an energy dispersive spectrometer (EDS)
were used to observe the microstructure and fracture surfaces of
2.1. Powder material
alloy. Identification of precipitations were conducted using a
transmission electron microscopy (TEM, JEOL-2100). Before the
An AleLi alloy (r ¼ 2.64 g/cm3) was designed on the basis of
test, TEM foils of 3 mm in diameter were mechanically polished to
2A97 alloy (a third generation AleLi alloy [24,25]) with less lithium
around 200 mm and then ion-milled. Composition of AL-Li alloy was
but more Cu element addition in order to obtain lower anisotropy
identified using the x-ray diffraction machine (XRD, Rigaku D/MAX
and improve weldability than traditional AleLi alloy [23]. AleLi
2500). And XRD test was conducted with Cu Ka radiation, scanning
alloy powders used in this study were produced by plasma
rates 6 /min, voltage 40 kV and current 150 mA.
rotating electrode process (PERP) with size around 150 mesh. The
surface and cross-section morphology of these powders are pre-
2.4. Mechanical test
sented in Fig. 1, and the chemical composition is listed in Table 1.

The average Vickers microhardness of the sample (YOZ section)

2.2. Laser melting deposition manufacturing process was measured using a load of 100 gf for a dwell time of 10 s. The
average microhardness at particular position was calculated from
Deposition experiment was carried out using a LMD-V system in seven indents. Room-temperature tensile properties were
measured using an AG-250 KNIS universe tensile testing machine
with an extension rate of 1 mm/min. Specimens with dimensions of
f6 mm
47 mm were machined along deposition direction (Fig. 2
(a)). In order to minimize the measurement errors, three specimens
were tested under same condition.

2.5. Heat treatment

Heat treatment were taken to investigate the precipitation

behavior of need-like TB phase. The temperature of solution treat-
ments was identified by the results of DSC (differential scanning
Fig. 1. (a) Surface morphology of as-received AleLi alloy powders; (b) cross-section calorimeter) around 520  C. Samples were firstly heat treated to the
morphology of AleLi alloy powders. temperature of 520  C for 2 h. Then they were cooled to room

Table 1
Chemical compositions of powders and as-deposited AleLi alloy (wt. %).

Cu Li Mg Zn Mn Zr Be Ti Fe Si Al

AleLi Powder 4.40 1.38 0.45 0.50 0.26 0.10 e e 0.076 0.043 Bal.
As-deposited AleLi alloy 4.41 1.32 0.48 0.36 0.28 0.11 e e 0.080 0.034 Bal.
2A97 2.0e3.2 0.8e2.3 0.25e0.5 0.17e1.0 0.2e0.6 0.08e0.2 0.0001e0.1 0.0001e0.1 <0.15 <0.15 Bal.
 S. Jiao et al. / Journal of Alloys and Compounds 821 (2020) 153125 3

Fig. 2. (a) Schematic illustration of the LMDed AleLi alloy thick plate, scanning strategy and deposition direction, (b) as-deposited plate.

temperature by quenching in water. After that, they were re-heated (Fig. 3(beg)). At the top region (Fig. 3 (b, e)), the microstructure
to the temperatures of 360  C, 400  C, 435  C, 460  C, 500  C for 5 h shows a fully dendritic structure with underdeveloped secondary
respectively to study the precipitation of need-like TB phase [26]. dendritic arms, and the primary arm spacing ranges from 27.8 mm
to 40.8 mm. Some precipitations with irregular morphology appear
3. Results along the inter-dendritic areas. At the middle region (Fig. 3 (c, f)),
the dendritic structure gradually disappears, and some needle-like
3.1. Microstructural features and phase identification phases with length around 7 mm appear at the inter-dendritic areas.
As distance increasing away from the top, the irregular inter-
The as-deposited grain morphologies and microstructures of dendritic phases reduce further with the massive precipitation of
AleLi plate along the deposition direction are illustration in Fig. 3. needle-like phases until the entire grains are fully decorated (Fig. 3
Uni-directional aligned columnar grains are observed epitaxial (d, g)).
growth from substrate with variation of microstructures Backscattered electron microcopy with EDS analysis shown in

Fig. 3. Solidification microstructures of the as-deposited AleLi alloy (a) overview of sample, (b, e) top region, (c, f) middle region and (d, g) bottom region.
4 S. Jiao et al. / Journal of Alloys and Compounds 821 (2020) 153125

Fig. 4. EDS analysis at the top position of the as-deposited AleLi alloy plate (at.%).

Fig. 5. TEM images and SAD pattern at bottom region of deposited AleLi alloy. (a) Bright Field image of needle-like TB phase, taken along [100]a, (b) SAD patterns view along [110]a
zone axis. (c) Bright Field image of needle-like T1 phase, (d) SAD patterns view along [100]a zone axis.

Fig. 4 indicates that these irregular phases at grain boundaries are

mainly consisted of a light grey phase (spectrum 1 and 2) and a dark
grey (spectrum 3) phase. EDX analysis point out that the inter-
dendritic intermetallics are rich in copper. The light grey phase
containing high amount of Cu (~33 at.%) with Al: Cu around 2:1,
which probably the q0 (Al2Cu) phases or R phase (Al5CuLi3) phases
[27,28]. The dark grey phases with high amount of Cu and Mg
suggested probably to be S’phase [29,30]. However, due to the light
atomic weight, Li element is hardly to be detected in EDS test [31].
TEM bright field images and corresponding SAED patterns are
further carried out to identify the needle-like phases in alloy, as can
be seen from Fig. 5. The diffraction patterns corresponding to the
matrix and needle-like phases are obtained along [100]a and [110]a
zone axis. The needle-like phases have a face-centered cubic
structure with lattice constant a ¼ 0.583 nm, which is identified as
TB (Al7Cu4Li) phase. The orientation relationship of TB phase and a-
Al matrix follows: (100)TB//(110)Al, (001)TB//(001)Al [31]. Besides,
another needle-like phase with much thinner width and a hexag-
Fig. 6. XRD analysis of the LMDed AleLi alloy at different position. The disappearance of
onal closed-packed structure with lattice constant of a ¼ 0.496 nm (220)a and (311)a peaks at top-middle position may due to the different cutting direction.
 S. Jiao et al. / Journal of Alloys and Compounds 821 (2020) 153125 5

appear with the increase peak intensity. The different types of

phases are attributed to thermal cycles during laser deposition
process.

3.2. Mechanical property

Microhardness distribution of the as-deposited AleLi alloy

along the vertical section (YOZ section) are shown in Fig. 7. The
microhardness increases gradually from 121 HV from the top of the
plate to 134 HV at a distance of 30 mm, and then decreases to about
98 HV at the bottom of the plate. The variations of micro-hardness
of alloy is closely related to the precipitations such as TB phase, T1
and Copper-rich phases which could also influence the tensile
property of alloy.
The room-temperature tensile properties of the as-deposited
alloy (bottom-middle position) are illustration in Table 3. The ul-
timate tensile strength (UTS), yield strength (YS), and elongation
(EL) are 244 MPa, 168 MPa and 5.0% respectively. Compared with
the hot rolled 2A97 alloy [32], the ultimate strength is comparable
Fig. 7. Microhardness from top to bottom region of the as-deposited AleLi alloy. but the yield strength and elongation are poor. Fracture surface of
LMDed AleLi alloy is shown in Fig. 8. Necking is observed, and some
small dimples are found on the fracture surface which indicate the
Table 3 failure mode of the alloy belongs to the ductile fractures.
Tensile properties of LMDed AleLi alloy.

Sample UTS, (MPa) YS, (MPa) El, (%) 4. Discussion

As-deposited AleLi alloy (L direction) 244 ± 16 165 ± 3 5.0 ± 1.6
Hot-rolled 2A97 282 261 18.2 4.1. Rapid solidification behavior of AleLi alloy during LMD process

In this study, the as-deposited AleLi alloy shows an obvious

and c ¼ 0.935 nm is also found in the alloy matrix, which is
dendritic microstructure with underdeveloped secondary arms at
confirmed as T1(Al2CuLi) phase. The crystallographic orientation
top region (Fig. 3 (b)), which is significantly different from tradi-
relationship of T1 and a-Al matrix is (1120)T1//(21 1)Al [30]. And T1
tional casting process. It is due to the directional distribution of
phase is one of the critical strengthening phase in AleLi alloy.
temperature gradient with a super-quick cooling rate of around
To further identify the phases, XRD patterns at top-middle and
105e106 K/s [20]. The same microstructure can also be observed in
bottom-middle region of the as-deposited plate were conducted. As
arc welding of AleLi alloy [31].
it can be seen in Fig. 6, phases at top-middle position (black curve)
In Fig. 3(bed), copper-rich phases appear at the inter-dendritic
mainly is consisted of a-Al matrix. Whereas for bottom-middle
areas, which is related to equilibrium solute atomic partition co-
position (red curve), phases of TB(Al7Cu4Li) and T1(Al2CuLi)
efficient of elements in Al alloy. As is well known, the equilibrium

Fig. 8. Fracture surface of LMDed AleLi alloy (a) low magnification of fracture surface, (b) high magnification of fracture surface, (c) low magnification of fracture section, and (d)
high magnification of fracture subsurface.
6 S. Jiao et al. / Journal of Alloys and Compounds 821 (2020) 153125

Fig. 9. Dissolution of Copper-rich precipitations at different positions, (a) 6 mm from the top, and (b) 12 mm from the top.

solute atomic partition coefficient of Cu is low (Keq Cu ¼ 0.15) in Al hardness achieved at distance around 72 mm (Fig. 12 stage III to IV).
alloy [33]. According to Sheil law [31], during LMD process, Cu atom When the resident temperature declines to the formation tem-
can be continuously discharged into low melting point liquid perature of T1 phase (Fig. 12 V) [26,34]. A few numbers of T1 phase
through the front edge of the solid-liquid interface. Therefore, the precipitate out, but due to the limited diffusion rate of atoms at
enrichment of Cu atoms at the inter-dendritic regions will promote such temperatures, only a small quantity of T1 phases appear with
the formation copper-rich precipitates. slightly increase of hardness. (Fig. 12 stage IV to V).
Mechanical properties of the as-deposited AleLi alloy at the
middle-bottom region show poor strength and elongation. The loss
4.2. Effect of thermal cycle on microstructure and hardness of alloy
of tensile properties for the as-deposited AleLi alloys are mainly
during LMD process
caused by the formation of cracks at the inter-dendritic areas. AleLi
alloys posses inherent characteristics like large solidification tem-
As mentioned in Fig. 3, the morphologies of LMDed AleLi alloy
perature range, high coefficient of thermal expansion, high
from top to bottom exhibit different characteristics. It is expected
shrinkage stresses, and tendency to form low-melting constituents,
that a significant amount of solid solution and aging can occur
and to the formation of eutectics. Under the non-equilibrium so-
during thermal cycling.
lidification condition during LMD, low melting Cu elements are
At initial stage of deposition, high cooling rate as well as
segregation to the inter-dendritic areas, which promote the for-
directional temperature gradient encourages the formation of
mation of copper-rich precipitates. Because high coefficient of
dendrites with under-developed secondary dendritic arms (Fig. 3
thermal expansion of AleLi alloy leads to high stress and strain
(b)). With continued deposition, thermal cycling and thermal ac-
cumulations allow copper-rich phase to dissolve, as shown in Fig. 9.
And thermal cycling also promotes the formation of TB phase in
grains, as shown in Fig. 3(e, f).
As numbers of thermal cycling increase with decrease of peak
temperature for every cycle, massive precipitation of TB phase are
observed. In order to further identify the precipitation temperature
of TB phase, the as-deposited AleLi samples were first solution-
heated at 520  C for 2 h, and then re-heated at different tempera-
tures of 360  C, 400  C, 435  C, 460  C, 500  C for 5 h respectively.
Fig. 10 shows the microstructures of re-heated samples. As it can be
seen from TEM work in Fig. 11, TB phases appear in alloy when heat-
treated at 360  C. As the temperatures increase from 400  C to
460  C, the number of TB phase decreases with the obvious coars-
ening. And TB phases will not precipitate when the aging temper-
ature reaches to 500  C.
The whole microstructure evolution of AleLi alloy during LMD
process with the change of microhardness is sketched and can be
seen in Fig. 12. At initial stage of deposition, large quantities of Cu-
rich phases formed along the inter-dendritic area (Fig. 12 I). With
continued deposition, heat cycling and thermal accumulations
allow Cu-rich phase to dissolve and the dissolution of Copper-rich
phases will enhance the microhardness of alloy due to the solid-
solution effect (Fig. 12 stage I to II) [34]. And the microhardness
reaches to the maximum value of 134 HV at the distance 16 mm
from the top of the plate. When the resident temperature of ther-
mal cycles fall down to the TB phase precipitation temperature from
500  C to around 360  C, TB phases appear from the inter-dendritic
regions (Fig. 12 III). TB phase has been conformed a high tempera-
ture aging production of AleLi alloy, and which has been proved as
a soft but brittle phase [34]. As a result, the massive transformation Fig. 10. Microstructures at X temperature aging for 5 h after solution-heated at 520  C
of TB phases lead to the decrease of micro-hardness with the lowest for 2 h:((a) X ¼ RT; (b) X ¼ 360  C; (c) X ¼ 400  C; (d) 435  C; (e) 460  C; (f) 500  C).
 S. Jiao et al. / Journal of Alloys and Compounds 821 (2020) 153125 7

Fig. 11. TEM images of the AleLi alloy after aging at 360  C for 5 h. (a) Bright filed; (b) SAD patterns view along [100]a zone axis.

Fig. 12. Sketched phase evolution of a AleLi alloy during laser deposition process.

[21,30,35]. The solidification cracking will generate from inter- The microstructure of the as-deposited AleLi alloy in upper
denderitic areas and lead to the final rupture of the alloy which position of the plate has rapid solidification characteristics. It shows
can be seen in Fig. 11. Besides, missive transformed TB phase with fully dendritic structure with underdeveloped secondary arms.
soft and brittle characteristics can act as the crack initiation sites Copper-rich precipitations appear at the inter-dendritic region. The
during tensile test and further reduce the tensile property. Hence, thermal cycle during subsequent deposition leads to the dissolu-
further study based on parameters of LMD process as well as heat tion of Copper-rich precipitations as well as the precipitation of TB
treatment is required to improve the mechanical property of and T1 phases.
LMDed AleLi alloy. The micro-hardness increases gradually from 121 HV from the
top of the plate to 134 HV at a distance of 30 mm, and then de-
creases to about 98 HV at the bottom of the deposited AleLi plate
5. Conclusion
because of the different microstructures causing by thermal cycling
during LMD process.
In this investigation, an AleLi alloy plate is firstly prepared by
The ultimate tensile strength of the LMDed AleLi alloy
LMD technology. The main conclusions are summarized as follows:
8 S. Jiao et al. / Journal of Alloys and Compounds 821 (2020) 153125

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