Materials and Design 50 (2013) 223–229

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Materials and Design

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The mechanism of anneal-hardening phenomenon in extruded

Zn–Al alloys
Yangming Zhang, Lijing Yang, Xuduo Zeng, Bizhang Zheng, Zhenlun Song ⇑
Zhejiang Province Key Laboratory of Magnetic Materials and Application Technology, Key Laboratory of Magnetic Materials and Devices, Ningbo Institute of Material Technology
and Engineering, Chinese Academy of Sciences, 519 Zhuangshi Road, Ningbo 315201, PR China

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

Article history: An anomalous anneal-hardening phenomenon was studied in extruded Zn–Al alloys. The extruded Zn–Al
Received 22 December 2012 alloys were isothermally heated above the eutectoid point for 10 h, and then cooled with furnace. The
Accepted 24 February 2013 anneal-hardening phenomenon was observed in specimens with aluminum content ranging from 5 wt%
Available online 5 March 2013
to 25 wt%. Microstructure evolution during the annealing process was investigated. The annealing–harden-
ing phenomenon was accompanied by phase transformation from a suspensive Zn-rich a2 phase to an equi-
Keywords: librium Al-rich a1 phase and a Zn-rich g phase. The hardness of the alloys increased with the decreasing
Extruded Zn-based alloys
volume fraction of the a2 phase. The hardness of the a1 phase and the g phase was measured and the hard-
Anneal-hardening
Phase transformation
ness of the a2 phase was calculated. The mechanism of the anneal-hardening phenomenon in extruded Zn–
Al alloys can be attributed to phase transformation from the soft a2 phase to the harder a1 + g phases.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction Recently, it has been found that the matrix phase transforma-
tion during the annealing process may lead to the hardening phe-
Zinc–aluminum based alloys have been widely used for several nomenon in eutectoid Cu–Al alloys [14], near-eutectic Al–Si alloys
decades [1,2]. Extruded Zn–Al alloys could provide potential appli- [15], eutectoid Ti–Cu alloys [16] and deformed nanocrystalline Ni
cations for instead of brass and cast iron, due to their favorable alloy [17]. Compared with the precipitation hardening which relies
comprehensive characteristics (low melting point, exceptional on fine particles of an impurity phase precipitated from an initially
castability, super plasticity, easy machinability, moderate strength, supersaturated solid solution at the low temperature [18], the ma-
and excellent wear resistance) [3–7]. However, as we know, the trix phase transformation induced hardening is caused by the in-
two properties—plasticity and hardness—are usually contradictory. crease of the phase volume fraction of the matrix phase which
So developing Zn–Al alloys, which not only have high hardness, but has higher hardness.
also keep high plasticity, is advantageous to extend the application. For Zn–Al alloys, heat treatments usually result in the decrease
Annealing is a heat treatment which can relieve the residual of the hardness and strength because of the reduction in the dislo-
stress, reduce the structure defects, and homogenize the composi- cation density and the coarsening of grains [19–22]. Recently, an
tion. Usually, annealing can improve the plasticity and reduce the anneal-hardening phenomenon was observed in rolled (90%) Zn–
hardness. However, annealing may harden alloys in some cases. 22Al (22 wt%Al) alloys [23]. Annealing at 250 °C, the hardness of
The anneal-hardening phenomenon was found in copper-based al- Zn–22Al alloys increased when the heating time was smaller than
loys, which was explained by the solute segregation to the stacking 180 min. Grain size increased during the annealing process. How-
faults formed by deformation [8–10] and the re-establishment of ever, the detailed mechanism of the hardening phenomenon in
the short range ordering partially destroyed by deformation Zn–Al alloys has not been well studied.
[11,12]. The mechanism of anneal-hardening in dilute copper al- In this work, the conditions required for the anneal-hardening
loys was investigated by Vitek and Warlimont [13]: (1) the solute phenomenon in extruded Zn–Al alloys were explored. The micro-
segregation to dislocations and the resulting binding force is the structure evolution during heat treatments was investigated. The
primary cause, (2) the short range ordering is not a primary cause mechanism of the hardening phenomenon can be attributed to a
but may contribute to it. decomposition of a soft suspensive Zn-rich a2 (fcc) phase. The
present study can help people understand the relationship be-
tween the phase structure and the properties in Zn–Al alloys,
which is combined with experimental verification. High plastic-
⇑ Corresponding author. Tel.: +86 574 87911131; fax: +86 574 86685159. ity and high hardness can be obtained by controlling the phase
E-mail address: [email protected] (Z. Song). volume fractions using proper heat treatments.

0261-3069/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2013.02.069
224 Y. Zhang et al. / Materials and Design 50 (2013) 223–229

2. Experimental procedure to 22 wt% (the eutectoid point). The anneal-hardening phenome-

non was more notable in specimens with more lamellar structures.
A medium frequency induction furnace was used to produce the Fig. 5 shows the dependence of the hardness of extruded Zn–
Zn–Al alloys (the aluminum content ranges from 5 wt% to 40 wt% 20Al alloys of various isothermal temperatures on cooling rate. Ex-
with a step width of 5%) by melting the corresponding amounts truded Zn–20Al specimens were isothermally heated at 250–
of Zn (99.99% purity) and Al (99.90% purity). Then the alloys were 320 °C for 10 h and then cooled at various rates (0.02–50 K s1).
obtained by casting the melt in a steel mold. The ingots were sub- When the isothermal temperature was below the eutectoid point
sequently hot extruded at 280 °C by a 315 T vertical extruder with (277 °C), the hardness of Zn–20Al specimens decreased with the
a deformation ratio of 1:28. decreasing cooling rate. Previous reports found that heat treat-
The extruded specimens were subjected to an annealing pro- ments (aging below the eutectoid point) led to the decrease of
cess: isothermally heated at 300 °C for 10 h, and then cooled strength and hardness in Zn–Al alloys [19–22]. The softening was
slowly to room temperature with furnace. explained by the relief of the residual stresses [20,21], the decrease
Vickers hardness (applying load of 1.96 N, 10 s) of the speci- of the structure defects [21] and the grain-coarsening [22]. How-
mens was measured following each heat treatment according to ever, when the isothermal temperature was above the eutectoid
ISO 6507-1:2005(E) standard [24]. At least 10 points were taken point, the hardness of Zn–20Al specimens increased with the
for each specimen to obtain an average value. decreasing cooling rate. Similar results were found in eutectoid
The specimen for tensile testing was 10 mm (within the gauge Cu–Al alloys [14], near-eutectic Al–Si alloys [15], and eutectoid
length) in diameter with 50 mm gauge length according to ISO Ti–Cu alloys [16]. The hardness was dependent on the kinetics of
6892-1:2009(E) standard [25]. Tensile specimens were machined the eutectoid decomposition in Cu–Al alloys [14], the amount of
parallel to the extrusion direction. The tensile deformation was dendritic a-Al phase in Al–Si alloys [15], and the volume fractions
carried out at room temperature with a crosshead speed of of eutectoid structure and martensite in Ti–Cu alloys [16].
7.00  103 mm s1. Each test was repeated five times and the Considering the Zn–Al phase diagram [28], it suggests that the
mean value was taken. decomposition of the suspensive a2 phase may play an important
The electrical conductivity measurements were carried out by a role in the anneal-hardening phenomenon in extruded Zn–Al
SB2230 DC digital resistance tester according to IEC 60468:1974 alloys.
standard [26]. The system was calibrated on the calibration blocks Fig. 6a–c shows the SEM observations of extruded Zn–20Al al-
with known conductivity values. The measured values were con- loys isothermally heated at 250 °C (below the eutectoid tempera-
sidered to be accurate within ±0.05% International Annealed Cop- ture) for 10 h and then cooled in (a) water, (b) air, and (c)
per Standard (IACS). furnace, respectively. It can be found that the grain size increased
The morphologies of the specimens were observed by a Hitachi slightly with the decreasing cooling rate. The hardness decreased
S-4800 field emission microscope (SEM). Ground and polished with the decreasing cooling rate (shown in Fig. 5).
specimens were etched for 30 s in 3%HNO3 + 3%HCl aqueous Fig. 6d–f shows the SEM observations of extruded Zn–20Al al-
solution. loys isothermally heated at 300 °C (above the eutectoid tempera-
The phase structures of the specimens were investigated by a ture) for 10 h and then cooled in (d) water, (e) air, and (f)
FEI Tecnai F20 transmission electron microscope (TEM) with an furnace, respectively. Granular structures transformed into lamel-
accelerating voltage of 200 kV. lar structures as the cooling rate decreased. The hardness increased
The single-phase specimens of the a1 phase and the g phase with the decreasing cooling rate (shown in Fig. 5).
were characterized by XRD (D8 Advance X-ray diffractometer). Fig. 7 shows the TEM observations of extruded Zn–20Al alloys
isothermally heated at 300 °C for 10 h and then cooled in (a) water
and (b) furnace, respectively. In the water-cooled specimen (shown
3. Results and discussion in Fig. 7a), the granular structure was consisted with three kinds of
phases: suspensive Zn-rich a2 phase (the dark area), equilibrium
Fig. 1 shows the changes of the mechanical properties ((a) ten- Al-rich a1 phase (the bright area) and equilibrium Zn-rich g phase
sile strength, (b) elastic modulus, (c) elongation, and (d) hardness) (the dark area). The a1 phase and the a2 phase have the face-cen-
of Zn–Al alloys with increasing aluminum content for both ex- tered cubic lattice with almost the same lattice parameters. The
truded state and annealed state. The tensile strength and the elas- two phases can be distinguished from the EDX spectrums. The g
tic modulus of the extruded Zn–Al specimens with the aluminum phase has the close-packed hexagonal lattice. From the EDX spec-
content ranging from 10 wt% to 25 wt% were improved after the trums (the test was repeated five times to obtain the average va-
annealing. The elongation of the extruded Zn–Al specimens was re- lue), the a1 phase is Al-rich phase (94.9 ± 1.0 wt% Al, balance Zn),
duced after the annealing. An anneal-hardening phenomenon took the a2 phase is Zn-rich phase (79.9 ± 1.1 wt% Zn, balance Al) and
place in the extruded Zn–Al specimens with the aluminum content the g phase is Zn-rich phase (98.2 ± 0.5 wt% Zn, balance Al).
ranging from 5 wt% to 25 wt%. It suggests that the suspensive a2 phase and the equilibrium
Fig. 2 shows the changes of the electrical conductivity of Zn–Al a1 + g phases were co-existed in the water-cooled specimens. In
alloys with increasing aluminum content for both extruded state the furnace-cooled specimen (shown in Fig. 7b), the lamellar struc-
and annealed state. The electrical conductivity of the extruded ture was consisted with the equilibrium Al-rich a1 phase and the
Zn–Al specimens was improved by the annealing, which can be equilibrium Zn-rich g phase. The suspensive a2 phase cannot be
attributed to the decrease of electronic scattering from structure found in lamellar structures.
defects [27]. From the mentioned results, it suggests that the suspensive a2
Figs. 3 and 4 show the SEM images of the Zn–Al alloys with the phase has not completely decomposed into the equilibrium
aluminum content ranging from 5 wt% to 40 wt% for both extruded a1 + g phases by rapid cooling. After annealing, the hardening phe-
state and annealed state. Cracks paralleling to the extrusion direc- nomenon takes place in specimens containing lamellar structures.
tion were found in extruded Zn–Al specimens. After annealing, the The lamellar structure is consisted by equilibrium a1 + g phases.
amount of cracks was reduced. It should be noticed that lamellar To further study the relationship between the phase structure
structures were found in annealed Zn–Al specimens with the alu- and the hardness of Zn–Al alloys, the volume fraction of the a2
minum content ranging from 10 wt% to 30 wt%. The amount of phase was measured using SEM. Because both of the a2 phase
lamellar structures increased as the aluminum content was close and the g phase are Zn-rich phases, the two phases cannot be dis-
 Y. Zhang et al. / Materials and Design 50 (2013) 223–229 225

Fig. 1. Mechanical properties ((a) tensile strength, (b) elastic modulus, (c) elongation, and (d) hardness) versus aluminum content curves for the extruded and the annealed
Zn–Al alloys. The annealing process was: isothermally heated at 300 °C for 10 h and then cooled with furnace.

The proportion of the volume fraction of the a1 phase and the g

phase is (the a1 phase and the g phase can approximate to pure
aluminum and pure zinc respectively):
fa1 wa1 =qAl ð20  0Þ=2:7 0:40
¼ ¼ ¼ ð1Þ
fg wg =qZn ð100  20Þ=7:1 0:60
The volume fraction of the a2 phase can be calculated as:
fa1
fa2 ¼ 1  ðfa1 þ fg Þ ¼ 1  ð2Þ
0:40
Fig. 8 shows the relationship between the volume fraction of
the a2 phase and the hardness of extruded Zn–20Al specimens iso-
thermally heated at 300 °C for 10 h and then cooled by different
rates. It can be seen that the hardness increased with the decreas-
ing volume fraction of the a2 phase. It suggested that the suspen-
sive a2 phase has higher plasticity and lower hardness than the
equilibrium a1 + g phases. The decomposition of a2 phase during
the annealing can cause the reduction in plasticity and the
Fig. 2. Electrical conductivity versus aluminum content curves for the extruded and
improvement in hardness.
the annealed Zn–Al alloys. The annealing process was isothermally heated at 300 °C
for 10 h and then cooled with furnace. To determinate the hardness of the a1 phase and the g phase
respectively, the single-phase specimens were produced with the
corresponding elemental contents based on the EDX spectrums
tinguished by the appearance directly. However, the Al-rich a1 in TEM observations. Fig. 9 shows the XRD patterns and the hard-
phase can be measured directly from the photographs. Therefore, ness of the single-phase specimens. The hardness of the a1 phase
the volume fraction of the a2 phase can be calculated by the lever and the g phase was about 143.5 HV and 63.2 HV respectively. It
rule. indicated that the a1 phase was the hardening phase. It also coin-
226 Y. Zhang et al. / Materials and Design 50 (2013) 223–229

Fig. 3. SEM images of the extruded Zn–Al specimens via different aluminum contents: (a) Zn–5Al, (b) Zn–10Al, (c) Zn–15Al, (d) Zn–20Al, (e) Zn–25Al, (f) Zn–30Al, (g) Zn–35Al,
and (h) Zn–40Al.

Fig. 4. SEM images of the annealed Zn–Al specimens via different aluminum contents: (a) Zn–5Al, (b) Zn–10Al, (c) Zn–15Al, (d) Zn–20Al, (e) Zn–25Al, (f) Zn–30Al, (g) Zn–35Al,
and (h) Zn–40Al. The annealing process was isothermally heated at 300 °C for 10 h and then cooled with furnace.

cided with the hardness results in Fig. 1. The hardness of the Zn–Al
alloys increased with the increasing aluminum content, because
the volume fraction of the a1 phase increased with the increasing
aluminum content.
The hardness of the alloy containing mixture phases can be cal-
culated by the rule of mixture (ROM) based on the iso-strain model
when the hardness of the hard phase is much higher than that of
the soft phase [29]:
 1
fs fh
H¼ þ ð3Þ
Hs Hh

where H is the hardness of the mixture, fs and fh are the volume frac-
tion of soft and hard phases, and Hs and Hh are the hardness of soft
and hard phases, respectively.
For the extruded Zn–Al alloys, the a2 phase can be considered as
the soft phase and the equilibrium a1 + g phases can be considered
as the hard phases. And the hardness of annealed specimens can be
considered as the hardness of the equilibrium a1 + g phases. Based
on the results in Fig. 8, the hardness of the a2 phase can be calcu-
Fig. 5. Dependence of the hardness of extruded Zn–20Al alloys of various
isothermal temperatures on cooling rate. Extruded Zn–20Al specimens were
lated, which was about 30.1 HV.
isothermally heated at 250–320 °C for 10 h and then cooled at various rates Therefore, a model can be suggested for the anneal-hardening
(0.02–50 K s1). phenomenon in extruded Zn–Al alloys. In the hot extrusion, a
 Y. Zhang et al. / Materials and Design 50 (2013) 223–229 227

Fig. 6. SEM images of the extruded Zn–20Al specimens isothermally heated at 250 °C for 10 h and then cooled in (a) water, (b) air, and (c) furnace; and SEM images of the
extruded Zn–20Al specimens isothermally heated at 300 °C for 10 h and then cooled in (d) water, (e) air, and (f) furnace.

Fig. 7. TEM images of the extruded Zn–20Al specimens isothermally heated at 300 °C for 10 h and then cooled in (a) water and (b) furnace, respectively.

part of the softer a2 phase was formed in Zn–Al alloys with the influenced the hardness more than the above-mentioned soften-
aluminum content ranging from 5 wt% to 25 wt%, because the ing effects. Therefore, the increase of the hardness caused by the
hot extrusion temperature (280 °C) was above the eutectoid phase transformation was at least about 6.9–19.9 HV (12–32%),
temperature (277 °C). After the annealing, the softer a2 phase respectively. The corresponding volume fraction of the a2 phase
decomposed into the harder equilibrium a1 + g phases, which can be calculated.
caused the hardening phenomenon. A similar model was re-
ported in deformed nanocrystalline Ni alloy [17]. A soft a phase 4. Conclusion
was obtained in the deformation process, and transformed into a
hard c phase in the annealing. That leads to the work-softening In the present study, the mechanism of anneal-hardening phe-
and the anneal-hardening of nanocrystalline Ni alloy. nomenon in extruded Zn–Al alloys was investigated. The conclu-
The changes of hardness after the annealing and the corre- sions can be drawn as following:
sponding calculated volume fraction of the a2 phase was shown
in Fig. 10. For the extruded Zn–Al specimens (Al: P30 wt-%), the (1) For extruded Zn–Al alloys showing the anneal-hardening
hardness decreased after the annealing. That can be explained by phenomenon, the aluminum content should range from
the grain-coarsening and the removal of crystal defects and the 5 wt% to 25 wt% and the isothermal heating temperature
internal stresses. For the extruded Zn–Al specimens (Al: 5– should be above 280 °C. The electrical conductivity was
25 wt-%), the phase transformation induced hardening effect improved after the annealing.
228 Y. Zhang et al. / Materials and Design 50 (2013) 223–229

Fig. 8. Relationship between the volume fraction of the a2 phase and the hardness of extruded Zn–20Al specimens isothermally heated at 300 °C for 10 h and then cooled by
different rates.

(2) The annealing-hardening phenomenon was accompanied by decreases, the a2 phase decomposes into equilibrium
phase transformation from a suspensive Zn-rich a2 phase to a1 + g phases. The hardness of the alloys increased with
an equilibrium Al-rich a1 phase and a Zn-rich g phase. After the decreasing volume fraction of the a2 phase. The hardness
isothermal heating above the eutectoid point for 10 h, the a2 of the a1 phase and the g phase was measured and the hard-
phase can be obtained by rapid cooling. As the cooling rate ness of the a2 phase was calculated. The suspensive a2 phase
has higher plasticity and lower hardness than the equilib-
rium a1 + g phases.
(3) A model can be suggested for the anneal-hardening phe-
nomenon in extruded Zn–Al alloys. In the hot extrusion, a
part of the softer a2 phase was formed in Zn–Al alloys with
the aluminum content ranging from 5 wt% to 25 wt%,
because the hot extrusion temperature (280 °C) was above
the eutectoid temperature (277 °C). After the annealing,
the softer a2 phase decomposed into the harder equilibrium
a1 + g phases, which caused the hardening phenomenon.
The plasticity and hardness of extruded Zn–Al alloys can
be manipulated by modifying the phase structures using
proper heat treatments.

Fig. 9. XRD patterns (a) and hardness (b) of the single-phase specimens (the a1 Fig. 10. Changes of hardness of extruded Zn–Al alloys after the annealing and the
phase and the g phase). corresponding calculated volume fraction of the a2 phase.
 Y. Zhang et al. / Materials and Design 50 (2013) 223–229 229

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