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Original Article
Article history: An AleZneMgeCu alloy and an AleZneMgeCueSceZr alloy are used to study effects of co-
Received 12 November 2022 addition of minor Sc and Zr on aging precipitates and mechanical properties of AleZneMg
Accepted 21 December 2022 eCu alloys. After solid solution treatment, almost complete recrystallization occurs in the
Available online 27 December 2022 AleZneMgeCu alloy, while recrystallization is significantly inhibited in the AleZneMg
eCu-Sc-Zr alloy, with a recrystallization fraction of 12.6%. The AleZneMgeCueSceZr alloy
Keywords: has remarkably higher strength than the AleZneMgeCueSceZr alloy in the solid solution-
AleZneMgeCu alloy treated and water-quenched state, which is due to the Orwan strengthening of coherent
Recrystallization Al3(Sc, Zr) particles and the grain boundary strengthening for finer grains. At the aging
Al3(Sc, Zr) particles temperature of 120 C,the co-addition of Sc and Zr accelerates the nucleation and growth
Aging precipitates of h0 phases in the grain interior, allowing the aged AleZneMgeCueSceZr alloy to reach its
Strengthening peak strength earlier. At the aging temperature of 140 C, the aging precipitate strength-
ening effect is weaker for the AleZneMgeCueSceZr alloy than for the AleZneMgeCu alloy
because of the accelerated transformation from h0 phases to h phases and growth of h
phases in the grain interior.
© 2022 The Author(s). Published by Elsevier B.V. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
* Corresponding author.
E-mail address: bingliu102@126.com (B. Liu).
https://doi.org/10.1016/j.jmrt.2022.12.133
2238-7854/© 2022 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 2 : 2 9 4 4 e2 9 5 4 2945
particle strengthening caused by the formation of stable L12- at 470 C for 24 h, hot rolling and cold rolling, sheets of the two
ordered Al3Sc particles [6e9]. Despite the many advantages of alloys were prepared with a thickness of 2 mm. Block speci-
Sc addition, Sc cannot be extensively used because of its high mens with dimensions of 15 mm 15 mm 2 mm and tensile
price. Compared with adding Sc alone, co-addition of Sc and specimens were cut from the sheets. The cutting method was
Zr can reduce costs and provide equivalent or even enhanced wire electro-discharge machining, which had the advantage of
effects owing to the formation of more stable Al3(Sc, Zr) par- easily satisfying the geometric and dimensional requirements
ticles [10]. Zr can replace up to 50% of Sc atoms in Al3Sc par- of the specimens with little effect on the mechanical properties
ticles, thereby forming Al3(Sc, Zr) particles [11e13]. Previous [19]. The length direction of the tensile specimens is parallel to
studies have shown that the co-addition of Sc and Zr con- the rolling direction, and a schematic diagram of the tensile
tributes to AleZneMgeCu alloys in two main aspects: (1) grain specimen is shown in Fig. 1. These specimens were solid
refinement due to the formation of primary Al3(Sc, Zr) parti- solution-treated at 470 C for 1 h, immediately water-
cles during casting; (2) inhibition of recrystallization resulting quenched, and then aged at 120 C and 140 C for 0e48 h,
from the precipitation of secondary Al3(Sc, Zr) particles during respectively.
homogenization [14,15]. Deng et al. [15] systematically inves- The block specimens were used for electrical conductivity
tigated effects of Sc and Zr microalloying on the microstruc- and hardness measurements. The electrical conductivity and
ture and mechanical properties of AleZneMg alloys. Based on hardness measurements were performed on a D60 K digital
their work, the addition of 0.10 wt% Sc and 0.10 wt% Zr did not metal conductivity tester and a Wolpert 401MVD micro-
contribute to the grain refinement of ingots but effectively Vickers hardness tester, respectively. At least three hardness
inhibited recrystallization; the addition of 0.25 wt% Sc and measurements were conducted for each specimen. Tensile
0.10 wt% Zr was very effective in refining the grain of ingots properties were measured on a MTS-858 tester with a
and inhibiting recrystallization; the addition of 0.25 wt% Sc stretching speed of 2 mm/min, and three tensile specimens
and 0.10 wt% Zr increased the yield strength of the peak-aged were prepared for each state. The microstructure of the
alloy by 96 MPa, which was associated with grain boundary specimens was studied by a LECIA DFC295 optical microscope
strengthening and Orowan strengthening of secondary Al3(Sc, (OM), a JSM-7900 F scanning electron microscope (SEM) with
Zr) particles. an electron back-scattered diffraction (EBSD) detector, and a
For AleZneMgeCu alloys, aging precipitates provide the TECNAI G2 F20 transmission electron microscope (TEM). The
most significant strengthening effect. At the common tem- specimens for OM observations were mechanically polished
perature (95 Ce180 C) of aging precipitation strengthening, and anodically coated in a mixture of 30 mL HBF4 and
aging precipitates include GP zones, h0 and h phases [16,17]. 200 mL H2O. The specimens for TEM and EBSD observations
Some reports suggest that Sc and Sc þ Zr additions to were first mechanically thinned below 80 mm and then pre-
AleZneMg alloys slow down the precipitation of h0 phases pared by twin-jet electropolishing in a mixture of 30 vol%
somewhat [9], while some reports state that Sc additions HNO3 and 70 vol% CH3OH below 25 C.
significantly speed up the precipitation of h0 phases [18], and
others believe that the addition of Sc has no effect on the
precipitation behavior of h0 phases [15]. It seems that the ef- 3. Results
fects of Sc or Sc þ Zr additions on aging precipitates are un-
certain, and more studies should be conducted on the effects 3.1. Electrical conductivity, hardness and tensile
of Sc or Sc þ Zr additions on aging precipitates. properties
In this work, the effects of co-addition of minor Sc and Zr
on aging precipitates and mechanical properties are investi- Fig. 2 shows the electrical conductivity and hardness of alloys
gated by electrical conductivity, hardness, tensile property #1 and #2 with different aging treatment. As shown in Fig. 2a,
measurements and microstructure observations. Moreover, the electrical conductivity increases with the aging time at
the influential mechanism for the co-addition of minor Sc and 120 C and 140 C for both alloys #1 and #2. The electrical
Zr on the aging precipitates is discussed. conductivity is higher for the alloy #2 than for the alloy #1 in
the same aged state, where at 140 C the electrical conduc-
tivity for the alloy #2 is significantly higher than that for the
2. Experimental alloy #1. In the case of the alloy #1, the hardness increases
with the aging time at 120 C within 48 h, while at 140 C, the
In this work, an AleZneMgeCu alloy (alloy #1) and an hardness reaches a maximum after aging for 24 h. In the case
AleZneMgeCu-Sc-Zr alloy (alloy #2) were used. The chemical
composition of the two alloys is listed in Table 1. After the same
process, including semi-continuous casting, homogenization
Fig. 2 e Electrical conductivity and hardness of alloys #1 and #2 with different aging treatment: (a) electrical conductivity; (b)
hardness.
of the alloy #2, the hardness peaks at both 120 C and 140 C alloy #2 has higher strength but lower hardness than the alloy
after 24 h of aging (Fig. 2b). #1 after the same duration of aging treatment at 140 C (Figs. 2
Fig. 3 shows the tensile properties of alloys #1 and #2 with and 3). This suggests that the relationship between hardness
different aging treatment. It can be seen that the alloy #2 has and strength is not always linear [20], and the Rp data in Fig. 3b
higher Rm (ultimate tensile strength) and Rp (yield strength) are used for subsequent discussion.
but lower A (elongation) than the alloy #1 in the same aged
state. For the alloy #2, the maximum Rm and Rp at 120 C and 3.2. Microstructure
140 C are obtained after aging for 24 h. For the alloy #1, the
peaks of Rm and Rp cannot be observed within 48 h at 120 C, Fig. 4 shows the OM images of alloys #1 and #2 in different
while the peaks of Rm and Rp are obtained after aging treat- states. As shown in Fig. 4a and b, both cold-rolled alloys #1 and
ment at 140 C for 36 h. In addition, it can be found that the #2 exhibit the fibrous structure along rolling direction. The OM
Fig. 3 e Tensile properties of alloys #1 and #2 with different aging treatment: (a) Rm (ultimate tensile strength); (b) Rp (yield
strength); (c) A (elongation).
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 2 : 2 9 4 4 e2 9 5 4 2947
these horseshoe-shaped particles are identified as Al3(Sc, Zr) Fig. 9 exhibits the TEM images for precipitates at grain
particles. The no-contrast lines (Ashby-Brown contrast) for boundaries of alloys #1 and #2 after aging at 120 C and 140 C
the Al3(Sc, Zr) particles in the bright-field image indicate the for 24 h. The aging-induced precipitates at grain boundaries
coherency between the Al3(Sc, Zr) particles and Al matrix [21]. are evident in the alloy #1 after aging at 120 C for 24 h and
These coherent Al3(Sc, Zr) particles precipitate during ho- aging at 140 C for 24 h, and the precipitates at grain bound-
mogenization with high thermal stability and can effectively aries after aging at 140 C for 24 h have clearly larger sizes than
pin dislocations and grain boundaries, thus hindering grain those after aging at 120 C for 24 h. These aging-induced
boundary migration, inhibiting recrystallization and refining precipitates at grain boundaries are stable h phases. The size
grains [15,22,23]. of aging-induced precipitates at boundaries is much smaller
Fig. 7 exhibits the TEM images for precipitates in the grain for the alloy #2 than for the alloy #1 in the same aged state.
interior of alloys #1 and #2 after aging at 120 C and 140 C for Furthermore, some obvious dislocations and Al3(Sc, Zr) par-
24 h. As shown in Fig. 7a, a high density of fine precipitates can ticles can be observed at or near grain boundaries in the alloy
be found in the grain interior of the alloy #1 after aging at #2 (Fig. 9c and d).
120 C for 24 h. These fine precipitates with a size of
3.3 ± 0.6 nm are formed during aging. The streaks along {111}
direction at 1/3 and 2/3 of {220} in the <112>Al SADP and the
diffraction spots at 2/3 of {220} in the <001>Al SADP indicate 4. Discussion
that these fine precipitates are mainly h0 phases (Fig. 8a and b)
[24,25]. In addition, the weaker diffraction spot at {1,7/4,0} in 4.1. Effect of co-addition of Sc and Zr on the mechanical
the <001>Al SADP is visible, which suggests the presence of a properties of solid solution-treated and water-quenched
few GPI zones [26]. For the alloy #1 after aging at 140 C for 24 h, alloys
the streaks from h0 phases are still evident (Fig. 8c); however,
the density of the aging-induced precipitates decreases The mechanical properties of solid solution-treated and
significantly and their size increases to 4.7 ± 0.8 nm (Fig. 7b). water-quenched alloys #1 and #2 are listed in Table 2. Ac-
Similarly, the aging-induced precipitates in the grain interior cording to Table 2, the solid solution-treated and water-
of the alloy #2 after aging at 120 C for 24 h include major h0 quenched alloy #2 has higher hardness, Rm and Rp but lower
phases and minor GPI zones (Fig. 8d and e); as the aging A than the solid solution-treated and water-quenched alloy
temperature increases, the size of aging-induced precipitates #1, where the increments of Rm and Rp are 49 MPa and 51 MPa,
in the grain interior increases from 3.6 ± 0.6 nm to 6.3 ± 0.9 nm respectively.
(Fig. 7c and d), and the intensity of streaks from h0 phases In the case of metallic materials, the strengthening
becomes noticeably weaker (Fig. 8f). mechanisms include solid solution strengthening, precipitate
strengthening, grain boundary strengthening and dislocation
strengthening. Assuming that the contribution of each
strengthening mechanism is independent, the total yield
strength (Rp(total)) of the experimental alloy can be expressed
by Eq. (1):
Fig. 8 e SADPs for precipitates in the grain interior of the alloy #1 after (a, b) aging at 120 C for 24 h and (c) aging at 140 C for
24 h. SADPs for precipitates in the grain interior of the alloy #2 after (d, e) aging at 120 C for 24 h and (f) aging at 140 C for
24 h.
and water-quenched alloy #2. Based on this, the dislocation treated and water-quenched alloy #1 depends on the precip-
strengthening effect is not taken into account in the present itate strengthening and grain boundary strengthening.
work. Therefore, the RP increment of the solid solution-treated Based on the interaction between precipitates and dislo-
and water-quenched alloy #2 relative to the solid solution- cations, the precipitate strengthening mechanism can be
divided into two mechanisms: (1) the mechanism of fine
precipitation sheared by dislocations, which involves order
strengthening, coherency strengthening and modulus
mismatch strengthening; (2) the Orowan dislocation bypass
mechanism for larger precipitates. The Orowan mechanism
operates when the precipitate cannot be sheared by disloca-
tions. Previous literature has shown that the strengthening
mechanism changes from a shearing mechanism to an Oro-
wan mechanism when the diameter of Al3Sc in binary AleSc
alloys exceeds 4e6 nm [4,29,30]. The diameter of Al3(Sc, Zr)
particles in Fig. 6c is 23 ± 4 nm; therefore, the Orowan
mechanism is believed to be responsible for the Al3(Sc, Zr)
particle strengthening in the present work. The yield strength
contributed by the Orowan mechanism (Rp(pre-o)) can be
calculated as follows [31]:
0:4MGb pr
Rp ðpre oÞ ¼ pffiffiffiffiffiffiffiffiffiffiffi ln (2)
pl 1 n 2b
Fig. 10 e TEM images for the precipitates in the grain interior of the alloy #1 after aging at 120 C for (a) 4 h and (b) 48 h and
after aging at 140 C for (c) 4 h and (g) 48 h. TEM images for the precipitates in the grain interior of the alloy #2 after aging at
120 C for (d) 4 h and (e) 48 h and after aging at 140 C for (f) 4 h and (g) 48 h.
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 2 : 2 9 4 4 e2 9 5 4 2951
Fig. 11 e Sizes (equivalent circle diameters), number density and volume fractions of aging precipitates in the grain interior
of alloys #1 and #2 with different aging treatment: (a) sizes (equivalent circle diameters); (b) number density; (c) volume
fractions.
for the alloy #1 and 1.9 mm for the alloy #2) of the two alloys, related to the dislocation density in the grain interior of the
DRp(h-p) of approximately 15 MPa is obtained. alloy #1 and the alloy #2. Due to the almost complete recrys-
Therefore, in the case of the solid solution-treated and tallization of the alloy #1 after solid solution treatment, the
water-quenched alloys, the calculated Rp increment due to the dislocation density in the grain interior is very low. Because of
co-addition of Sc and Zr is approximately 56 MPa, which is in the pinning effect of the coherent Al3(Sc, Zr) particles, a rela-
general agreement with the experimental result (51 MPa). tively high density of dislocations are retained in the grain
interior of the alloy #2 after solid solution treatment. These
4.2. Effect of co-addition of Sc and Zr on the precipitation retained dislocations can serve as preferential nucleation sites
behavior during aging for aging precipitates, accelerating the nucleation and growth
of the aging precipitates [18].
To further determine the effect of co-addition of Sc and Zr on Fig. 12 shows the TEM images for precipitates at grain
the precipitation behavior during aging, the TEM microstruc- boundaries of alloys #1 and #2 after aging at 120 C and 140 C
ture of the two alloys after aging at 120 C and 140 C for for 4 h and 48 h. It is evident that the size of the aging pre-
different times is also studied. Fig. 10 shows the TEM images for cipitates at grain boundaries of the two alloys also increases
precipitates in the grain interior of alloys #1 and #2 after aging with the time and temperature, but the size of the aging pre-
at 120 C and 140 C for 4 h and 48 h, and the sizes (equivalent cipitates at grain boundaries is smaller for the alloy #2 than for
circle diameters) of aging precipitates measured from the TEM the alloy #1 in the same aged state. This is because almost
images are given in Fig. 11. As shown in Figs. 7 and 10 and 11, complete recrystallization occurs in the alloy #1, where the
the size of the aging precipitates in the grain interior of the two grain boundaries are mainly high angle grain boundaries;
alloys increases with the time and temperature, and the size of while the coherent Al3(Sc, Zr) particles significantly inhibit
the aging precipitates in the grain interior is larger for the alloy recrystallization in the alloy #2, where the grain boundaries
#2 than for the alloy #1 in the same aged state, which is more are mostly low angle grain boundaries. The aging precipitates
pronounced at higher temperatures and for longer times. This prefer to nucleate and grow at high angle grain boundaries
suggests a faster nucleation and growth rate of the aging pre- rather than at low angle boundaries owing to the higher free
cipitates in the grain interior of alloy #2, which should be energy of the high angle grain boundaries [36].
2952 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 2 : 2 9 4 4 e2 9 5 4
Fig. 12 e TEM images for the precipitates at grain boundaries of the alloy #1 after aging at 120 C for (a) 4 h and (b) 48 h and
after aging at 140 C for (c) 4 h and (g) 48 h. TEM images for the precipitates at grain boundaries of the alloy #2 after aging at
120 C for (d) 4 h and (e) 48 h and after aging at 140 C for (f) 4 h and (g) 48 h.
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