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2015 - Effects of Two-Step Homogenization On Precipitation Behavior of Al3Zr Dispersoids and Recrystallization Resistance in 7150 Aluminum Alloy
2015 - Effects of Two-Step Homogenization On Precipitation Behavior of Al3Zr Dispersoids and Recrystallization Resistance in 7150 Aluminum Alloy
Materials Characterization
journal homepage: www.elsevier.com/locate/matchar
a r t i c l e i n f o a b s t r a c t
Article history: The effect of two-step homogenization treatments on the precipitation behavior of Al3Zr dispersoids was in-
Received 16 December 2014 vestigated by transmission electron microscopy (TEM) in 7150 alloys. Two-step treatments with the first step
Received in revised form 20 February 2015 in the temperature range of 300–400 °C followed by the second step at 470 °C were applied during homogeniza-
Accepted 23 February 2015
tion. Compared with the conventional one-step homogenization, both a finer particle size and a higher number
Available online 25 February 2015
density of Al3Zr dispersoids were obtained with two-step homogenization treatments. The most effective dis-
Keywords:
persoid distribution was attained using the first step held at 300 °C. In addition, the two-step homogenization
7150 aluminum alloy minimized the precipitate free zones and greatly increased the number density of dispersoids near dendrite
Al3Zr dispersoids grain boundaries. The effect of two-step homogenization on recrystallization resistance of 7150 alloys with dif-
Two-step homogenization ferent Zr contents was quantitatively analyzed using the electron backscattered diffraction (EBSD) technique.
Recrystallization It was found that the improved dispersoid distribution through the two-step treatment can effectively inhibit
the recrystallization process during the post-deformation annealing for 7150 alloys containing 0.04–0.09 wt.%
Zr, resulting in a remarkable reduction of the volume fraction and grain size of recrystallization grains.
© 2015 Elsevier Inc. All rights reserved.
1. Introduction The effects of both the Zr content and the homogenization condition
on the precipitation of Al3Zr dispersoids and the recrystallization of Al
7xxx series aluminum alloys have high strength to density ratio and alloys have been investigated in previous studies [14,16–20]. The con-
excellent mechanical properties, such as high strength, high fracture ventional homogenization treatment (one-step) is mainly intended to
toughness and good resistance to stress corrosion, and are widely dissolve low melting eutectic phases and to redistribute the solutes in
used in the aeronautical and astronautic industries [1–4]. However, re- aluminum matrix, but not necessary to optimize the precipitation of
crystallization can significantly deteriorate mechanical properties of Al3Zr dispersoids. The high homogenization temperature of the conven-
heat-treated materials; moreover, the fracture toughness of 7xxx alloys tional practice causes both high solubility and diffusion rate of zirconi-
decreases with the increase of the recrystallization degree that occurs um, which results in a low volume fraction of large dispersoids and
during the hot-forming process and solution heat treatment [4]. wide precipitate free zones. To improve the distribution of Al3Zr disper-
Small quantities of Zr are commonly added into 7xxx Al alloys as a soids, some approaches to stepwise homogenization were explored in
recrystallization inhibitor, in which thermally stable Al3Zr dispersoids the literature [12,19–22]. The first step was used to create a favorable
precipitate during the homogenization of cast ingots. Al alloys with Zr condition of dispersoid precipitation for developing an optimized distri-
additions can retain their deformed structure and prevent recrystalliza- bution. The subsequent step then completed the homogenization of the
tion, due to the presence of Al3Zr dispersoids, even when annealed at alloy in the conventional manner. However, the nucleation, growth and
high temperature [5]. The effectiveness of Al3Zr dispersoids strongly de- distribution of dispersoids during the homogenization process are not
pends on their size, number density and distribution [6]. It is recognized well understood and the related recrystallization behavior of deformed
that Zr tends to segregate and enrich in the dendrite centers during materials was not quantitatively examined.
solidification [7–9]. It is difficult to remove Zr concentration gradients In the present study, the effects of one-step and various two-step ho-
during conventional homogenization due to Zr's low diffusivity in Al mogenization treatments on the precipitation behavior of Al3Zr disper-
[10,11]. Therefore, the precipitation of Al3Zr dispersoids often concen- soids in the 7150 alloy were investigated. Particular attention was paid
trates in the center of dendrite grains and the precipitate free zone to the formation of Al3Zr dispersoids during the first step of homogeni-
(PFZ) of dispersoids forms in dendrite grain boundaries [12–15]. zation, which was designed to promote the nucleation of dispersoids
and thus to improve the overall distribution of Al3Zr dispersoids in the
⁎ Corresponding author. final homogenization step. The influence of two-step homogeniza-
E-mail address: [email protected] (X.-G. Chen). tion conditions on the recrystallization resistance of 7150 alloys
http://dx.doi.org/10.1016/j.matchar.2015.02.016
1044-5803/© 2015 Elsevier Inc. All rights reserved.
Z. Guo et al. / Materials Characterization 102 (2015) 122–130 123
(a)
(b) (c)
(d) (e)
Fig. 1. Typical TEM centered dark field images of Al3Zr dispersoids in 7150–0.09Zr alloy after both one-step and two-step homogenization treatments: (a) 470 °C/24 h with an inset of SAD
pattern, (b) 300 °C/48 h + 470 °C/24 h, (c) 300 °C/72 h + 470 °C/24 h, (d) 400 °C/48 h + 470 °C/24 h and (e) 400 °C/72 h + 470 °C/24 h.
The diffusion rates of Zr in Al matrix at the studied temperatures of 300, precipitates are also verified being Al3Zr by the SAD pattern, as pre-
400 and 470 °C are 6.34 × 10− 24 , 1.20 × 10− 20 and 7.07 × sented in the inset of Fig. 3a. However, all Al3Zr dispersoids already
10− 19 m2 s− 1, respectively. grow to a relatively large size (Fig. 3a) due to a high diffusion rate of
After the first step treated at 400 °C, the number of dispersoids is Zr at 400 °C (1.20 × 10− 20 m2 s− 1), and it is difficult to find small
clearly increased relative to the one-step homogenization. The dispersoids between the existing ones (Fig. 3b). The number of
Z. Guo et al. / Materials Characterization 102 (2015) 122–130 125
Table 3
Average radius, number density and volume fraction of Al3Zr dispersoids in 7150–0.09Zr alloy after homogenization treatments.
Homogenization conditions Homogenization parameters Average radius Number density Volume fraction f/r
r (nm) N (μm−3) f (%) (μm−1)
dispersoids observed after first step treated at 400 °C is almost iden- the first step treated at lower temperatures is considerably higher be-
tical to that after the completed two-step treatment. cause the Zr supersaturation is largely increased at lower temperature.
During homogenization, there are two main factors influencing the Therefore, a larger number of dispersoids can be formed by the first
dispersoid precipitation: (1) the supersaturation of the solid solution step treatment. Moreover, the lower the temperature at the first step,
(driving force for nucleation) and (2) the diffusivity of the solute in the higher the driving force for the nucleation but the lower the growth
the matrix (for growth and coarsening). When treated at the high tem- rate of the dispersoids are. The first step treatment at 300 °C produced
perature of the conventional one-step practice, fewer dispersoids can more Al3Zr nuclei than that at 400 °C. However, those small dispersoids
form due to a low supersaturation of Zr in solid solution but they can only slowly grow at this temperature. The subsequent second step
grow faster and may also coarsen because of the high diffusion rate of treatment provides a normal condition for their growth. Overall, as
Zr solutes at 470 °C (7.07 × 10−19 m2 s−1). Compared with the one- shown in Table 3, much denser and finer dispersoids were obtained
step homogenization, the driving force for dispersoid nucleation by when the first step temperature was reduced from 400 to 300 °C.
(a) (b)
Area A
Fig. 2. TEM centered dark field images of Al3Zr dispersoids precipitated after the first step treated at (a) 300 °C for 48 h and (b) enlarged area A.
(a) (b)
Area B
Fig. 3. TEM centered dark field images of Al3Zr dispersoids precipitated after the first step treated at (a) 400 °C for 48 h with an inset of SAD pattern and (b) enlarged area B.
126 Z. Guo et al. / Materials Characterization 102 (2015) 122–130
(a)
Grain boundary
1u m
(b)
Grain boundary
1u m
Fig. 4. TEM dark field images of the Al3Zr dispersoid distribution in grain boundary regions, subjected to different homogenization treatments: (a) one-step, 470 °C/24 h, (b) two-step,
300 °C/48 h + 470 °C/24 h.
The precipitate free zone (PFZ) of Al3Zr dispersoids in the dendrite interdendritic region. Therefore, the precipitation of Al3Zr dispersoids
grain boundary can be clearly observed after one-step homogenization principally occurs in the dendrite cores and the precipitate free zone
at 470 °C (Fig. 4a). Having a solid–liquid partition coefficient, k0 = 2.5, (PFZ) of Al3Zr dispersoids forms near the interdendritic grain boundary
larger than unity, Zr as a peritectic element segregates inversely from during homogenization. The widths of PFZ are in the range of 2 to 3 μm
the dendrite center to the interdentritic boundary during solidification, and the distribution of dispersoids near PFZ is non-uniform. Close to the
resulting in solute-rich dendritic cores surrounded by solute-depleted boundary, only few dispersoids with large interparticle space can be
(a) (b)
200um 200um
(c) (d
200um 200um
Fig. 5. Orientation maps of 7150 alloys with different Zr contents for one-step homogenization: (a) the base alloy (0% Zr); (b) 0.04% Zr; (c) 0.09% Zr; (d) 0.16% Zr. High angle boundaries
(N15°) and low angle boundaries (1–15°) shown as black line and white line, respectively.
Z. Guo et al. / Materials Characterization 102 (2015) 122–130 127
the dendrite grain boundary, leading to a narrow PFZ and a dense distri-
bution of dispersoids after two-step homogenization.
(a) (b)
200um 200um
(c) (d)
200um 200um
Fig. 7. Orientation maps of 7150–0.04% Zr alloy homogenized at: (a) 300 °C/48 h + 470 °C/24 h; (b) 300 °C/72 h + 470 °C/24 h; (c) 400 °C/48 h + 470 °C/24 h; (d) 400 °C/72 h + 470 °C/24 h.
128 Z. Guo et al. / Materials Characterization 102 (2015) 122–130
3γGB
PZ ¼ ð f =r Þ ð1Þ
2
where γGB is the specific grain boundary energy, f is the volume fraction
and r is the average radius of dispersoids. Eq. (1) indicates that a high
volume fraction of small dispersoids (i.e., a high f/r value) is necessary
to achieve a high PZ on grain boundary migration for retarding the
growth of recrystallized grains. PZ can be greatly increased by maximiz-
ing the volume fraction (f) and minimizing the dispersoid size (r). Com-
pared with the one-step homogenization, higher f/r values of Al3Zr
dispersoids are obtained when two-step homogenization treatments
are applied (Table 3), particularly for the first step treated at low tem-
perature (300 °C). The f/r value increases from 0.16 of the one-step ho-
mogenization sample to 0.32 of the two-step homogenization samples
with first step treated at 300 °C. In the alloys subject to two-step homog-
enization treatments, a great number of fine Al3Zr dispersoids dispersed
in the aluminum matrix, and they played a major role in inhibiting re-
crystallization. On the other hand, the recrystallization often occurs
near dendrite grain boundaries where few dispersoids are present and
the PFZ locates (a low local f/r value). The two-step homogenization
treatment can reduce the width of PFZ and increase the number of dis-
persoids near dendrite grain boundaries (Fig. 4), leading to a high local
f/r value and hence an increased PZ in the region. As a consequence,
samples subject to two-step homogenization treatments display a re-
markably high recrystallization resistance. The highest recrystallization
resistance is obtained when first step treated at 300 °C due to the
highest number density and finest size of dispersoids.
4. Conclusions
Fig. 8. Volume fraction and average size of recrystallized grain of 7150–0.04% Zr alloy for (1) The conventional one-step homogenization used for the 7150
both one-step and two-step homogenization treatments: (a) volume fraction and alloy produced a low number density and non-uniform dis-
(b) average grain size.
tribution of Al3Zr dispersoids. Compared with the one-step ho-
mogenization treatment, both a finer particle size and a higher
number density of Al3Zr dispersoids were obtained with the
homogenization, the recrystallized fractions of the two-step homogeniza- two-step homogenization treatments. When the first step was
tion samples are generally reduced, indicating a clear increase in the treating at 300 and 400 °C, the number density of dispersoids in-
recrystallization resistance of the samples with two-step homogenization creased by 7–8 and 3–3.5 times, respectively. The most effective
treatments. Moreover, the samples with the first step treated at 300 °C dispersoid distribution was attained using the first step held at
show more obvious effects that that treated at 400 °C. Both the recrystal- 300 °C.
lized fraction and grain size with first step treated at 300 °C are remark- (2) The two-step homogenization treatment minimized the precipi-
ably reduced relative to the one-step homogenization sample. Results tate free zones and greatly increased the number density of dis-
also show that the holding time for the 300 °C and 400 °C conditions persoids near dendrite grain boundaries, leading to a significant
has a negligible impact on recrystallized fraction and grain size of recrys- improvement of dispersoid distribution in aluminum matrix.
tallization grains. (3) The improved dispersoid distribution through the two-step ho-
The microstructure evolution of Alloy C (0.09% Zr) with the two-step mogenization treatments can effectively inhibit the recrystalliza-
homogenization treatments is shown in Fig. 9. When the samples are tion process during post-deformation annealing for 7150 alloys
subject to two-step homogenization treatments, their microstructure containing 0.04–0.09% Zr. Compared with the one-step homoge-
becomes a main recovery structure with few isolated recrystallized nization, both volume fraction and grain size of recrystallization
grains emerging. Compared with the sample subject to the one-step grains with two-step homogenization treatments were remark-
homogenization that is partially recrystallized (Fig. 5c), the recrystalli- ably reduced. The first step treated at low temperature (300 °C)
zation process is almost inhibited with two-step homogenization was found to be the most effective to increase the recrystalliza-
treatments. The measured recrystallized fraction and grain size are tion resistance.
also displayed in Fig. 10. The recrystallized fraction and grain size are re-
duced to approximately 2% and 25 μm, respectively, for both first steps
treated at 300 °C and 400 °C. For the sample of Alloy C (0.16% Zr), the Acknowledgments
recrystallization resistance of the alloy is already very high with the
one-step homogenization and the recrystallized fraction is only approx- The authors would like to acknowledge the financial support from the
imately 1% (Figs. 5d and 6). Therefore, no two-step homogenization Natural Sciences and Engineering Research Council of Canada (NSERC)
treatments were applied. and from Rio Tinto Alcan through the NSERC Industrial Research Chair
Z. Guo et al. / Materials Characterization 102 (2015) 122–130 129
(a) (b)
200um 200um
(c) (d)
200um 200um
Fig. 9. Orientation maps of 7150–0.09% Zr alloy homogenized at: (a) 300 °C/48 h + 470 °C/24 h; (b) 300 °C/72 h + 470 °C/24 h; (c) 400 °C/48 h + 470 °C/24 h; (d) 400 °C/72 h + 470 °C/24 h.
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Fig. 10. Volume fraction and average size of recrystallized grains of 7150–0.09% Zr Al alloy
for both one-step and two-step homogenization treatments: (a) volume fraction and
(b) average grain size.