Materials and Design 80 (2015) 4150

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Materials and Design

journal homepage: www.elsevier.com/locate/matdes

Thermal stability of aluminum after friction stir processing

with SiC nanoparticles
M. Sarkari Khorrami, M. Kazeminezhad , A.H. Kokabi
Department of Materials Science and Engineering, Sharif University of Technology, Azadi Avenue, Tehran, Iran

a r t i c l e

i n f o

Article history:
Received 18 January 2015
Revised 14 April 2015
Accepted 3 May 2015
Available online 4 May 2015
Keywords:
Friction stir processing
Thermal stability
Nanoparticles
Severe plastic deformation
Microstructure
Aluminum alloy

a b s t r a c t
In this research, 1050 aluminum sheets in the conditions of annealed and severely deformed by 2 passes
of constrained groove pressing (CGP) process were used. Two passes of friction stir processing (FSP) were
applied on the specimens. Also, another CGPed specimen was processed by 2 passes of FSP using SiC
nanoparticles. The samples were then heat treated to study thermal stability of base metal, heat affected
zone (HAZ), thermo-mechanically affected zone (TMAZ), and stir zone (SZ). Microstructure examinations
revealed that the annealed base metal was relatively stable upon heating even up to 400 C and a little
grain growth was evident. On the other hand, the CGPed base metal was fairly stable just up to 200 C.
It was also observed that HAZ and TMAZ of annealed specimen exhibited some grain growth while for
CGPed sample, these regions experienced recrystallization and subsequent grain growth during heat
treatment. It was found that the SZ of annealed and CGPed specimens remained ne after heat treatment
even up to 400 C and slight grain growth occurred. Microstructural assessments revealed that using SiC
nanoparticles during FSP had a potential to form ner grain structure at SZ compared with that in specimen FSPed without any particle. Also, it was found that SiC nanoparticles could hinder grain growth during heat treatment provided that a suitable distribution nanoparticles was formed.
2015 Elsevier Ltd. All rights reserved.

1. Introduction
As grain renement is a benecial method to enhance mechanical properties of aluminum alloys, many attempts have been made
for this purpose [15]. Several routes based on severe plastic deformation (SPD) such as equal channel angular pressing (ECAP) [6]
and high pressure torsion (HPT) [7] for bulk materials and accumulative roll bonding (ARB) [8] and constrained groove pressing (CGP)
[9,10] for sheets have been introduced to form ultrane grained
structure in aluminum alloys. In addition, friction stir processing
(FSP) based on friction stir welding (FSW) process has been used
for modifying grain structure of aluminum alloys [1113].
Although both SPD processes and FSP have potential to produce
ultrane grained structure in aluminum alloys, different mechanisms are involved in the grain renement. It has been noted that
in the early stage of SPD processes, the dislocation density
increases by enhancement of strain. Further strain can cause the
generated dislocations to be rearranged and then cell structure
with thick cell walls and low angles of misorientation is formed.
Subsequent deformation leads to reduction in thickness of cell

Corresponding author.
E-mail address: mkazemi@sharif.edu (M. Kazeminezhad).
http://dx.doi.org/10.1016/j.matdes.2015.05.006
0261-3069/ 2015 Elsevier Ltd. All rights reserved.

walls and then subgrains surrounded by low angle grain boundaries (LAGBs) are formed. At very high magnitude of strain
imposed by SPD processes, the misorientation angle between the
subgrains is increased corresponding to the replacement of
LAGBs by high angle grain boundaries (HAGBs). However, it is
believed that HAGBs in SPDed materials have non-equilibrium
structure [14]. In fact, non-equilibrium grain boundaries may be
formed when excessive dislocations (that do not contribute to
the formation of misorientation at a grain boundary) are present
at the grain boundaries [15]. In FSP, as the material in the stir zone
(SZ) experiences high magnitude of strain and strain rate at high
temperature (up to 0.9Tm), the mechanisms based on dynamic
recovery (DRV) [16] and dynamic recrystallization (DRX) including
continuous DRX (CDRX) [17], discontinuous DRX (DDRX) [16,18],
and geometric DRX (GDRX) [19] are responsible for formation of
very ne grain structure in the SZ. It has been reported that the
most of grains formed in the SZ have HAGB character and only
20% of grains in the SZ have LAGB character, in contrast to the
SPDed materials [20].
Considering the different natures of grain structure obtained
with the SPD processes and FSP, it is anticipated the behavior of
grain structures resulting from these processes upon heating differs from each other. Several researches have been carried out
regarding heat treatment of SPDed [2125] and FSWed/FSPed

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M.S. Khorrami et al. / Materials and Design 80 (2015) 4150

[2635] aluminum alloys. As reported by Ren and Shan [36], recovery or recrystallization and subsequent grain growth occur during
heat treatment of SPDed aluminum depending on the annealing
temperature. Also, in the research performed by Kwan et al. [37],
it has been mentioned that heat treatment at low temperature
(up to 200 C) can cause to increase the hardness of ARBed aluminum with low strain value; however, heat treatment at high
temperature can lead to grain growth and then reduction in the
hardness. Therefore, the strain values imposed by SPD processes
along with the heat treatment temperature are dominant factors
determining the behavior of SPDed aluminum upon heat
treatment.
Heat treatment of FSWed/FSPed aluminum has been performed
by investigators to study the following issues. Heat treatment after
FSW of precipitated hardening aluminum alloys can retrieve the
strength of the joint by modifying the shape, size, and distribution
of secondary strengthening particles [38]. Moreover, several
attempts have been made to study thermal stability of FSW joints
upon heat treatment. Some researchers have mentioned that SZ
grain structure can be stable during heat treatment. For example,
Cerri and Leo [30] have reported that SZ heat treated at low temperature (up to 200 C) has comparable mechanical properties with
that in as-FSW condition. Also, Hu et al. [33] have reported that the
ne grain structure formed in the SZ was retained after heat treatment even at 450 C for 2 h; however, abnormal grain growth
(AGG) has been observed in the several studies [27,28] depending
on the aluminum alloy type and also FSW parameters [28]. In
another research, the effect of heat treatment on the microstructural evolutions in the FSPed AlMgTiO2 in-situ nanocomposite
has been studied [39]. It has been reported that the solid-state
reactions were completed during heat treatment. Also, nanoparticles could hinder grain growth during heat treatment; however,
the inuence of distribution of nanoparticles on the thermal stability behavior of the aluminum matrix has not been assessed.
According to the above explanations, it seems that studying the
thermal stability of FSPed aluminum, especially in the case of using
SiC nanoparticles during FSP, in which the base metal is severely
deformed by one of SPD processes gives useful information.
Additionally, there is a lack of understanding about the effect of
secondary particles distribution (i.e., appropriate and agglomerated distributions of SiC nanoparticles) on the thermal stability
of stir zone during heat treatment. For this purpose, in the present
study, the 1050 aluminum sheets in the conditions of annealed and
SPDed by 2 passes of CGP process were processed by 2 passes of
FSP. Moreover, one of CGPed samples was FSPed with incorporation of SiC nanoparticles to examine the effect of nanoparticles
on the thermal stability of SZ. After FSP, specimens were heat treated at various temperatures and thermal stability of base metals,
heat affected zone (HAZ), thermo-mechanically affected zone
(TMAZ), and SZ was discussed in details.

FSP using SiC nanoparticles to study the effect of nanoparticles

on the thermal stability of the SZ. The used nanoparticles had an
average size of 55 nm. A eld emission scanning electron microscopy (FESEM) image from SiC nanoparticles is shown in Fig. 1.
In order to use SiC nanoparticles, a groove with dimensions of
1 mm in width and 1.5 mm in depth was machined at the middle
surface of the CGPed sheet. The groove was completely lled with
a specic quantity of SiC nanoparticles (about 120 mg). After
inserting the nanoparticles in the groove, the top surface of groove
was sealed by performing a single FSP pass using a tool (12 mm
diameter) without pin at rotation and traverse speeds of 1200
and 50 mm/min, respectively. It ensured that the SiC nanoparticles
could not be thrown out of the groove during FSP using a tool with
pin. Afterward, two passes of FSP was carried out with inter-pass
temperature of about 25 C. The FSP parameters were the same
as those considered for FSP without nanoparticles. As a result,
Al/SiC nanocomposite with approximately 1.5 vol. pct. reinforced
particles was achieved.
The acquired specimens were heat treated at various temperatures of 200, 300, and 400 C for 1 h. It is worthy to note that distinct
specimens were prepared for each condition of heat treatment. The
FSP parameters and also the amount of SiC nanoparticles preplaced
in the groove remained constant for all specimens. Moreover, all of
the cross section for further analyses were cut from the same position at the FSP path to eliminate the effect of thermal cycle during
FSP. In order to study the microstructure of as-FSPed and heat treated samples, optical microscopy (OM) using polarized light was
employed. So, the cross section of FSPed samples was prepared
using standard metallography procedures and then electroetched
by a solution of 200 ml distilled water + 4.5 ml HBF4 at voltage of
20 V for 100 s. Also, to observe the distribution of SiC nanoparticles
in the stir zone, FESEM equipped with energy dispersive spectroscopy (EDS) was employed. Moreover, the microhardness of various areas was measured using Vickers microhardness test with
load of 100 g and loading time of 15 s.

3. Results and discussion

3.1. Microstructure evolutions
3.1.1. Before heat treatment
The microstructures of annealed and CGPed base metals before
FSP are shown in Fig. 2. As can be seen, the grain size of annealed

2. Experimental procedures
1050 aluminum sheets with dimensions of 84  50  3 mm
were used as the staring materials. The as-received aluminum
was full annealed at 350 C for 3 h. In order to apply severe strain
to the annealed sheets, two passes of CGP process (the strain magnitude of 2.32) were performed. For more information about CGP
process refer to [10]. Annealed and 2 passes CGPed specimens were
then processed by 2 passes of FSP. For this purpose, FSP tool made
from H13 tool steel with shoulder and pin diameters of 12 and
3 mm, respectively, and pin height of 2.1 mm was prepared. Also,
a tilt angle of 3 was considered. FSP was performed at rotation
and traverse speeds of 1200 rpm and 50 mm/min, respectively. In
addition, one of CGPed specimens was processed by 2 passes of

Fig. 1. FESEM image from SiC nanoparticles.

M.S. Khorrami et al. / Materials and Design 80 (2015) 4150

specimen is about 40 lm and is rened after 2 passes of CGP process. It has been reported that the grain/subgrain size of commercial purity aluminum can be reduced to about 0.9 lm after
applying 2 passes of CGP process [40].
The microstructures from various areas of HAZ, TMAZ, and SZ at
both advancing and retreating sides of annealed and CGPed specimens processed by 2 passes of FSP are presented in Figs. 3 and 4,
respectively. As shown, grain growth occurs at HAZ of annealed
specimen as a result of heat input during FSP. However, the
microstructure of SZ comprises ne equiaxed grains resulting from
dynamic recrystallization phenomenon during FSP with signicantly smaller grain size compared with the annealed base metal.
Also, the microstructure of TMAZ includes elongated grains, particularly at advancing side. This can be due to the scant deformation
and heat during FSP applied in the TMAZ which are not sufcient
for dynamic recrystallization to occur [41]. For CGPed sample,
the microstructure evolutions at various areas are relatively different from those take place in the annealed one. In HAZ of CGPed
specimen, static recrystallization and subsequent grain growth
occur since strain energy is stored in the material during CGP process. This initial stored strain provides sufcient driving force for
recrystallization during heating cycle of FSP. The same phenomenon can occur in TMAZ. Another issue that should be noted
is pertinent to the comparison between the SZ grain structures of
the annealed and CGPed specimens. In the previous study carried
out by the present authors [42,43], it has been reported that the
SZ grain size of annealed sample is relatively lower than that of
CGPed one after 1 pass of FSW. This observation has been attributed to the stored strain energy in CGPed sample leading to the
more grain growth occurrence after dynamic recrystallization.
From this point of view, it can be concluded that CGPed/SPDed
materials are quietly unstable upon FSP, as previously stated in
the literature [4245]. However, considering the SZ microstructures of annealed and CGPed samples after 2 passes of FSP
(Figs. 3 and 4), it is found that the SZ grain size of these specimens

43

is almost the same. Since the stir zone grain size values of annealed
and 2 passes CGPed samples are different after 1 pass of FSP (as
reported by [43]) and it is the same after second pass of FSP, it
can be noted that all of the stored strain energy would be released
after 1 FSP pass and then the initial stored strain cannot have inuence on the microstructural evolutions in the SZ during the second
FSP pass. More detailed descriptions regarding the effect of stored
strain on the fabrication of Al/SiC nanocomposite via various
passes of FSP have been reported by the present authors [46].
One of the CGPed samples is processed by 2 passes of FSP using
SiC nanoparticles to investigate the effect of SiC on the stability of
grain structure in the SZ during FSP and subsequent heat treatment. To do so, two regions in the stir zone with different distributions of nanoparticles, i.e. the areas of center (with proper
distribution) and retreating side (where agglomerated SiC
nanoparticles are formed) are considered. Fig. 5 shows the FESEM
images from the mentioned regions indicating the different distributions of SiC nanoparticles in these regions. Also, EDS analysis
from the selected area shown in Fig. 5(c) signies the existence
of SiC nanoparticles. The microstructure from center of SZ for
CGPed sample FSPed with SiC nanoparticles is shown in Fig. 6. As
can be seen, using SiC nanoparticles during FSP causes to form signicantly smaller grains in the SZ with respect to the CGPed sample FSPed without nanoparticles. This can be due to the pinning
effect of nanoparticles on the grain boundaries which can effectively retard grain growth. Moreover, nanoparticles can lead to
the formation of ne grains via particulate stimulation nucleation
(PSN) mechanism [47]. It is worthy to note that the microstructure
evolutions at HAZ and TMAZ of the specimen FSPed with SiC
nanoparticles are the same as those of CGPed sample.
3.1.2. After heat treatment
Microstructural evolutions occur during heat treatment at 200,
300, and 400 C temperatures in various regions of base metal,
HAZ, TMAZ, and SZ are examined separately as following.

Fig. 2. The microstructures of annealed and 2 passes CGPed base metals.

Fig. 3. The microstructures from various areas of HAZ, TMAZ, and SZ for annealed specimen processed by 2 passes of FSP without SiC nanoparticles.

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M.S. Khorrami et al. / Materials and Design 80 (2015) 4150

Fig. 4. The microstructures from various areas of HAZ, TMAZ, and SZ for 2 passes CGPed specimen processed by 2 passes of FSP without SiC nanoparticles.

Fig. 5. FESEM images from (a) center and (b) retreating side of stir zone for CGPed specimen processed by 2 passes of FSP with SiC nanoparticles; (c) EDS analysis and
chemical composition of where the arrow in (b) is shown.

Fig. 6. The SZ microstructure of 2 passes CGPed sample processed by 2 passes of

FSP using SiC nanoparticles.

3.1.2.1. Thermal stability of the base metals. The microstructures of

annealed and 2 passes CGPed base metals after heat treatment at
temperatures of 200, 300, and 400 C are shown in Figs. 7 and 8,
respectively. Referring to Fig. 7, heat treatment at 200 C leads
the grain size of annealed base metal to increase slightly and
increasing the temperature to 300 and 400 C intensies somewhat this grain growth. Since no initial strain is stored in the
annealed specimen, considerable microstructure evolutions do
not
take
place
upon
heat
treatment.
Comparing
Figs. 2(a) and 8(a), it is observed that the grain structure of
CGPed base metal does not change obviously after heat treatment
at 200 C. However, recrystallization and subsequent grain growth
occurs in the CGPed base metal during heat treatment at more
temperatures, particularly at temperature of 400 C in which
intense grain growth at some areas can be observed. This can be
pertinent to the stored strain in the CGPed base metal. So, it can
be concluded that the CGPed base metal is relatively stable upon

M.S. Khorrami et al. / Materials and Design 80 (2015) 4150

45

Fig. 7. The microstructures of annealed base metal heat treated at various temperatures of (a) 200, (b) 300, and (c) 400 C.

Fig. 8. The microstructures of 2 passes CGPed base metal heat treated at various temperatures of (a) 200, (b) 300, and (c) 400 C.

Fig. 9. HAZ/TMAZ microstructures of annealed specimen heat treated at temperatures of (a) 300 and (b) 400 C.

heating up to 200 C and exhibits quite instability upon heating

above 200 C. These results are fairly consistent with those
reported by others studying the annealing behavior of ARBed aluminum [37,48].
3.1.2.2. Thermal stability of HAZ and TMAZ. In the HAZ and TMAZ of
annealed specimen, some grain growth occurs after heat treatment, especially at temperature of 400 C. For example, the
microstructures of HAZ/TMAZ from retreating side for annealed
specimen after heat treatment at 300 and 400 C are shown in
Fig. 9. As can be seen, grain growth occurs as the width of elongated grains formed in the TMAZ is slightly increased after heat
treatment with respect to as-FSPed condition (shown in Fig. 3).
Fig. 10 indicates the HAZ/TMAZ microstructures of 2 passes
CGPed specimen heat treated at temperatures of 200, 300, and
400 C. As shown in Fig. 10, heat treatment causes the more grain
growth occurrence at HAZ. To indicate better this issue, for example, the higher magnication images from HAZ of CGPed specimen
heat treated at 200 and 400 C are shown in Fig. 11. In addition, by
comparing the TMAZ microstructures in as-FSPed condition shown

in Fig. 4 with those in the heat treated at temperatures of 200

400 C, it is revealed that heat treatment can result in disappearing
of elongated grains at TMAZ and increasing the heat treatment
temperature can intensify this phenomenon. The reason is related
to the some recrystallization that may take place at TMAZ during
heat treatment because of stored strain from CGP process corresponding to disappearing elongated grains. It is noteworthy that
heat treatment at temperature of 400 C leads to some grain
growth after recrystallization at TMAZ. So, it can be concluded that
the TMAZ of annealed sample is relatively stable upon heat treatment while TMAZ of CGPed sample experiences some recrystallization and grain growth during heat treatment.
3.1.2.3. Thermal stability of SZ. The SZ microstructures of annealed
sample heat treated at various temperatures are indicated in
Fig. 12. As can be seen, the SZ grain structure remains ne as that
found in as-FSPed condition; however, the grain size is slightly
increased after heat treatment at temperatures of 300 and
400 C. To show this issue in more details, the SZ grain structures
of annealed specimen in the conditions of as-FSPed and heat

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M.S. Khorrami et al. / Materials and Design 80 (2015) 4150

Fig. 10. HAZ/TMAZ microstructures of 2 passes CGPed specimen heat treated at various temperatures of (a) 200, (b) 300, and (c) 400 C.

Fig. 11. HAZ microstructures of 2 passes CGPed sample heat treated at (a) 200 and (b) 400 C temperatures.

Fig. 12. SZ microstructures of annealed sample heat treated at various temperatures of (a) 200, (b) 300, and (c) 400 C.

Fig. 13. SZ microstructures of annealed specimen in the conditions of (a) as-FSPed and (b) heat treated at temperature of 400 C.

treated at 400 C in higher magnication are presented in Fig. 13.

These observations imply that the grain structure formed in the
SZ has acceptable thermal stability even up to temperature of
400 C for 1 h. This stability does not exist in other regions of base
metal, HAZ, and TMAZ as explained previously.

The microstructures from SZ of 2 passes CGPed specimen heat

treated at mentioned temperatures are illustrated in Fig. 14. In
order to show this issue in more details, for example, the higher
magnication images from SZ of 2 passes CGPed specimen in the
conditions of as-FSPed and heat treated at 300 C are shown in
Fig. 15. As it can be seen, similar to the annealed specimen, the

M.S. Khorrami et al. / Materials and Design 80 (2015) 4150

47

Fig. 14. SZ microstructures of 2 passes CGPed sample heat treated at various temperatures of (a) 200, (b) 300, and (c) 400 C.

Fig. 15. SZ microstructures of 2 passes CGPed specimen in the conditions of (a) as-FSPed and (b) heat treated at temperature of 300 C.

Fig. 16. SZ microstructures of 2 passes CGPed specimen FSPed using SiC nanoparticles in the conditions of (a) as-FSPed and (b) heat treated at 300 C.

SZ of 2 passes CGPed specimen is fairly stable upon heating and

only a slight grain growth occurs during heat treatment. This
observation complies with a model introduced by Humphreys
and Hatherly [49]. It has been noted that when the matrix is free
of any secondary particle the conditions for normal grain growth
may be provided. However, due to the thermal stability of SZ, the
rate of grain growth is almost ignorable. Moreover, above results
signify the thermal stability of SZ regardless of whether the base
metal is in the annealed or in the severely deformed conditions.
This phenomenon can be attributed to the fact that since the
microstructure evolutions in the SZ originate from dynamic recrystallization mechanisms (resulting from high strain and strain rate
at elevated temperature) during FSP, it has been reported that
the ne grain structure with more than 90% HAGBs is formed in
the SZ [18,50]. Moreover, due to high temperature involved in
the FSP, the dislocation density interior the grains surrounded by
HAGBs is very low [41] and HAGBs are expected to have equilibrium structure [20]. As a result, the formed structure can exhibit
superior stability upon heating. In contrast, the grain structure
formed as a result of SPD (such as 2 passes CGPed base metal) consists mainly of subgrains surrounded by LAGBs. In addition, due to

appreciably high density of extrinsic grain boundary dislocations,

HAGBs have non-equilibrium structure [51]. This grain structure
is quite unstable upon heating due to the occurrence of recrystallization and subsequent grain growth phenomena, as discussed
before.
For studying the inuence of SiC nanoparticles on the stability
of the SZ grain structure, 2 passes CGPed specimen is processed
by FSP using SiC nanoparticles. It is found that the SiC nanoparticles are capable to retard grain growth during both FSP and heat
treatment processes. To show this matter, the SZ microstructures
in the conditions of as-FSPed and heat treated at 300 C are shown
in Fig. 16. Comparing the microstructures of some areas of the SZ in
which SiC nanoparticles are not distributed well in as-FSPed and
heat treated conditions (Fig. 16(a) and (b), respectively), it is
revealed that slight grain growth occurs in these regions during
heat treatment. It should be noted that part of this grain growth
is pertinent to the FSP; however, during heat treatment, additional
normal grain growth occurs in the areas with lack of SiC nanoparticles. It is worthy to mention that AGG can be seen at the retreating side of SZ in the specimen FSPed with SiC nanoparticles and
then heat treated at temperature of 400 C (Fig. 17). In the

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M.S. Khorrami et al. / Materials and Design 80 (2015) 4150

AGG even during heat treatment at 400 C. Of course, some normal

grain growth can occur during heat treatment, but due to the pinning effect of SiC nanoparticles, the rate of grain growth is greatly
limited. Therefore, it can be concluded that suitable dispersion
along with sufcient amount of SiC nanoparticles can effectively
stable grain structure during FSP as well as heat treatment.
3.2. Microhardness

Fig. 17. The SZ microstructure from retreating side of specimen FSPed using SiC
nanoparticles followed by heat treatment at temperature of 400 C.

retreating side of SZ, some agglomerated SiC nanoparticles are

formed in some areas (Fig. 6(b)) resulting in the formation of relatively large grains with respect to those in the areas where proper
distribution of SiC nanoparticles exists. In fact, agglomerated SiC
nanoparticles cannot prevent the grain growth during FSP and heat
treatment. This observation can be elucidated by considering a
research carried out by Humphreys and Hatherly [49] which predicts the occurrence of AGG in the material in which sufcient
amount of secondary particles with proper distribution does not
exist. In contrast, there is considerable amount of SiC nanoparticles
with proper distribution in some areas of SZ center preventing the

The microhardness values of base metal, HAZ, TMAZ, and SZ in

the conditions of as-FSPed and heat treated at various temperatures of 200, 300, and 400 C are indicated in Fig. 18.
Referring to Fig. 18(a), it can be seen that the microhardness of
2 passes CGPed sample is obviously more than that of annealed
one in the as-FSPed condition due to the grain renement after
CGP process, as explained in Section 3.1.1. After heat treatment
at temperature of 200 C, the difference in the microhardness values of annealed and CGPed base metals still remains. Of course, a
slight decrease in the microhardness of the CGPed base metal is
observed as a result of the recovery phenomenon during heat
treatment at relatively low temperature. This result is fairly in
agreement with that reported by Kwan et al. [37] concerning
annealing of ARBed aluminum.
It is observed that heat treatment at higher temperature (i.e.,
300 and 400 C) leads to the appreciable decrease in the microhardness of the CGPed base metal because of recrystallization
and subsequent grain growth occurrence as discussed more in
Section 3.1.2.1. This observation implies the instability of CGPed
base metal upon heating above 300 C. It should be noted that

Fig. 18. Microhardness values of (a) base metal, (b) HAZ, (c) TMAZ, and (d) SZ for annealed and 2 passes CGPed specimens in the conditions of as-FSPed and heat treated at
various temperatures.

M.S. Khorrami et al. / Materials and Design 80 (2015) 4150

the microhardness of the annealed sample remains almost constant after heat treatment at various temperatures.
According to Fig. 18(b) and (c), it is revealed that the microhardness values of HAZ and TMAZ for both annealed and CGPed samples are slightly decreased after heat treatment. This can be due
to the grain growth phenomenon during heat treatment as discussed more in Section 3.1.2.2.
The microhardness values of SZ for annealed and CGPed specimens are illustrated in Fig. 18(d). Additionally, the SZ microhardness
of CGPed sample FSPed using SiC nanoparticles is shown in this gure. As can be seen, the SZ microhardness values of annealed and
CGPed specimens processed without nanoparticles are almost the
same. As claried in Section 3.1.1, this can be due to the formation
of the same grain size at the stir zone during the second FSP pass
of these samples. However, using SiC nanoparticles during FSP of
CGPed sample leads to increase in the microhardness of SZ compared with that of CGPed sample FSPed without any particles. The
reason for this observation is pertinent to the pinning effect of SiC
nanoparticles on the grain boundaries of newly dynamic recrystallized grains which can be responsible for forming very ne grain
structure in the SZ. Also, other strengthening mechanisms can be
involved in rising the SZ microhardness of CGPed sample FSPed with
SiC nanoparticles include: (1) pinning of dislocations due to the reinforcement particles (Orowan theory [52]), (2) geometrically necessary dislocation induced as a result of difference in the thermal
expansion coefcients of aluminum matrix and SiC nanoparticles,
and (3) elastic strain in the aluminum matrix-reinforced interface
[53]. Referring to Fig. 18(d), it is found that the SZ microhardness values of annealed and CGPed specimens are reduced somewhat after
heat treatment as a result of small grain growth. Moreover, in the
case of using SiC nanoparticles, although the SZ microhardness is
decreased with increasing the temperature of heat treatment, it is
higher than SZ microhardness of samples FSPed without SiC
nanoparticles even at temperature of 400 C. This observation signies that SiC nanoparticles can improve the mechanical properties of
aluminum at high temperature.
4. Conclusions
In this study, thermal stability of various areas resulted from
FSP of annealed and severely deformed aluminum sheets was
investigated. In addition, to examine the effect of secondary particles on the thermal stability of SZ, the 2 passes CGPed sample was
FSPed using SiC nanoparticles. The chief results achieved from this
research were given as:
1. Annealed base metal was relatively stable upon heat treatment.
However, the 2 passes CGPed base metal was stable just up to
200 C and more heat treatment temperature caused to the
recrystallization and subsequent grain growth signifying instability of CGPed base metal upon heating above 200 C.
2. In the HAZ of annealed and 2 passes CGPed sample, grain
growth occurred after heat treatment. Increasing the heat treatment temperature caused to increase in the grain size of HAZ.
The microstructure of TMAZ for annealed sample consisted of
elongated grains and heat treatment led to increase in width
of elongated grains. However, the TMAZ microstructure of 2
passes CGPed sample included the mixture of elongated and
equiaxed grains as a result of partial recrystallization at TMAZ
during FSP. After heat treatment, recrystallization was completed corresponding to the disappearing of elongated grains.
3. The SZ microstructures of annealed and 2 passes CGPed samples
were quite stable upon heat treatment even up to temperature
of 400 C and only small grain growth occurred after heat
treatment.

49

4. Incorporating SiC nanoparticles into the SZ resulted in the formation of smaller grain size due to the pinning effect of
nanoparticles on the grain boundaries during FSP. These
nanoparticles had capability of retarding grain growth somewhat during heat treatment; however, some normal grain
growth occurred at the center of SZ while AGG took place at
regions where the SiC nanoparticles were not properly
distributed.

Acknowledgment
The authors wish to thank the research board of Sharif
University of Technology Iran for the nancial support and the
provision of the research facilities used in this work.
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