Journal of Alloys and Compounds 776 (2019) 536e542

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Journal of Alloys and Compounds

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

Effect of in-situ TiB2 particles on microstructure and mechanical

properties of Mg2Si/Al composites
Rui Du, Du Yuan, Fei Li, Dongcheng Zhang, Shusen Wu*, Shulin Lü
State Key Lab of Materials Processing and Die & Mould Technology, Huazhong University of Science and Technology, 1037 Luoyu Road, Wuhan 430074,
China

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

Article history: This study intends to offer a depth understanding on controlling the morphology of eutectic Mg2Si by
Received 13 September 2018 adding in-situ TiB2 particles into 10 wt% Mg2Si/Al composite. The evolution of the microstructure and
Received in revised form mechanical properties of Mg2Si/Al composites with different TiB2 particles addition from 1 wt% to 5 wt%
21 October 2018
is investigated and the mechanism is also discussed. The results show that coarse eutectic Mg2Si phase
Accepted 23 October 2018
Available online 29 October 2018
can be refined and modified with the addition of TiB2 particles, and the lattice coherence between them
is also confirmed. Besides, the addition of TiB2 particles can greatly enhance multiple mechanical
properties of composites at the same time. With 5% TiB2 particles addition, the modulus, yield strength
Keywords:
In-situ TiB2 particles
and elongation of composites are improved 11%, 59% and 141% respectively compared with Mg2Si/Al
Eutectic Mg2Si composites. Moreover, different addition of TiB2 particles changes gradually the fracture behavior of
Microstructure composites from brittle fracture to quasi-cleavage fracture, and finally to entirely ductile behavior.
Mechanical properties © 2018 Elsevier B.V. All rights reserved.
Fracture behavior

1. Introduction
Particle reinforced aluminum matrix composites (PRAMCs) have
quite broad applications in various fields such as military and
transportation, automobile and aircraft [1,2]. The notable benefits
of composites are well known, from lightweight, high load-carrying
ability with less energy consumption, outstanding mechanical
properties [3,4], as well as their wide applications [5,6].
In-situ processes for synthesizing PRAMCs possess prominent
advantages compared with ex-situ processes, such as uniform
distribution of particles, clean and well-bonded interface between
matrix and reinforcement, stable reaction systems without by-
products [7,8]. The above merits make in-situ routes more attrac-
tive and draw considerable attention recently [9].
Mg2Si has many excellent properties such as high melting
temperature (1085
C), low density (1.99  103 kg/m3), low thermal
expansion coefficient (7.5  106 K1), and comparatively high
elastic modulus (120 GPa) [10]. Besides, using normal casting
method to fabricate in-situ Mg2Si/Al composites also has low pro-
duction cost. Therefore, in-situ Mg2Si/Al composites become a high
potential candidate used in aerospace and automotive applications
* Corresponding author.
E-mail addresses: ruidu@hust.edu.cn (R. Du), ssw636@hust.edu.cn (S. Wu).
[11].
However, Mg2Si phase is quite coarse and brittle, exhibiting
sharp-edge morphology in the composites. Non-treated compos-
ites are prone to crack because coarse Mg2Si phase induces
generally stress concentration on the corner of it [12]. Conse-
quently, crack propagation takes place, resulting in the premature
failure and low strength of the whole composites. Thus, it's crucial
to control the microstructure of Mg2Si/Al in order to improve
ductility and obtain desirable mechanical properties. Various
means have been introduced to modify the morphology of Mg2Si,
for example, superheating treatment [13], remelting process
[14,15], semisolid casting process [16], etc. Nevertheless, the addi-
tion of inoculant directly into the composites alloy is a more
practical approach because it is simpler, cost effective and suitable
for general engineering applications.
The principles for the modification on primary Mg2Si by the
addition of Sr [17,18], P [19,20] and TiB2 [21,22] are well understood,
but the difference between primary Mg2Si and eutectic Mg2Si in-
dicates that the modification methods to treat eutectic Mg2Si
should still be explored. According to what has mentioned above
[22], in-situ TiB2 particles can not only act as the nuclei of Mg2Si but
TiB2 itself is also an excellent reinforcement particle, which can
greatly strengthen aluminum matrix, especially in Young's
modulus. Moreover, Young's modulus of aluminum alloys is a sig-
nificant criterion in structure design which can be greatly promoted

https://doi.org/10.1016/j.jallcom.2018.10.301
0925-8388/© 2018 Elsevier B.V. All rights reserved.
 R. Du et al. / Journal of Alloys and Compounds 776 (2019) 536e542 537

by the addition of Mg2Si and TiB2 [23]. However, the current
research findings about the application of in-situ TiB2 particles in
Mg2Si/Al are still rather limited, especially on mechanical proper-
ties and the corresponding mechanisms.
The present study aimed to investigate the effects of in-situ TiB2
particles on the microstructure and mechanical properties of 10%
Mg2Si/Al composites, especially on fracture behavior. A compre-
hensive understanding about regulating the morphology of
eutectic Mg2Si in aluminum matrix composites was also revealed to
extend our knowledge on these advanced materials. Besides, the
mechanism was investigated as well.
the fracture surface after tensile test was still on the same SEM. A
TEM (Tecnai-G2, FEI) was introduced for observation and identifi-
cation of orientation relationship. TEM thin foils were prepared by
the combination use of mechanical technology and ion beam
thinning.
The phase identification of 10% Mg2Si/Al, 10% TiB2/Al master
composite, and other TiB2þMg2Si/Al final composites was carried
out by X-ray diffraction (XRD-7000S, SHIMADZU) using Cu Ka ra-
diation at 40 KV and 30 mA.
2.5. Mechanical properties tests of composites

2. Experimental procedures The room temperature tensile tests for the samples were per-
formed on a tensile machine (AG-100KN, SHIMADZU) with a 1 mm/
2.1. Preparation of 10% TiB2/Al master composite min crosshead speed. The samples were machined according to
ASTM specification B557M. Extensometer was also used to deter-
K2TiF6 (99.9% purity) powders and KBF4 (99.9% purity) powders mine the Young's modulus of the composites. To ensure the re-
with an accurate molar ratio of 1:2 were mixed sufficiently before petitive of composites, tensile data were taken from the average
experiment. Commercial pure aluminum (99% purity) ingots were value of 5 specimens.
melted in a graphite crucible using an electrical resistance furnace.
When the temperature of the melt reached and remained stable at
3. Results and discussion
840
C, the mixed salts were added into the melt. The amount of the
mixed salts added into the melt corresponded to the composition of
3.1. Microstructure evolution induced by addition of TiB2 particles
10% TiB2/Al master composite. Salt-reaction process lasted gener-
ally for about one hour. After reaction, the slag was skimmed out as
Fig. 1 shows the XRD patterns of 10% TiB2/Al master composite.
completely as possible, and the melt was cooled to 720
C and cast
It is clear that only TiB2 was detected as the newly formed phase
into a preheated permanent mould to get 10% TiB2/Al master
and other intermediate phases or by-products were not observed,
composite.
indicating the salt-metal reaction used in this experiment took
place completely to synthesis in-situ TiB2 particles.
2.2. Preparation of 10% Mg2Si/Al composite
Fig. 2 shows the XRD patterns of 10% Mg2Si/Al composite. It
shows that only Mg2Si was detected in the composite and further
Pure Al ingots and Al-24.5%Si master alloy were melted in a
prove that Mg2Si/Al composite was successfully fabricated by
graphite crucible using an electrical resistance furnace. When the
normal casting method.
temperature of the melt reached and remained stable at 750
C,
Fig. 3(a) and Fig. 3(b) show respectively the microstructure of
commercial pure magnesium (99% purity) ingots were added into
10% Mg2Si/Al composite and 10% TiB2/Al master composite. Fig. 3(a)
the melt wrapped with aluminum foils. After Mg ingots were
reveals that the microstructure of Mg2Si/Al composite consists of a-
completely melted, the melt was degassed using pure argon gas.
Al and eutectic Mg2Si which exhibits coarse flake-like morphology.
Then, the melt was cooled to 720
C and cast into a preheated
In Fig. 3(b), due to the lattice mismatch between TiB2 ceramics and
permanent mould to get 10% Mg2Si/Al composite.
a-Al grains is far over than 5%, it is quite difficult for TiB2 particles to
be engulfed by the moving liquid/solid interface of the a-Al matrix
2.3. The addition of in-situ TiB2 particles into 10% Mg2Si/Al
[25]. Thus, TiB2 particles distributed along the grain boundaries of
composite

Pure aluminum ingots, pure magnesium ingots, Al-24.5%Si

master alloy and 10%TiB2/Al master composite were used to fabri-
cate 10% Mg2Si/Al with 1 wt% TiB2, 3 wt% TiB2 and 5 wt% TiB2,
respectively. These weighted ingots were melted completely in an
electrical resistance furnace at 750
C. It is well known that high-
intensity ultrasonic vibration in the melt can give rise to
nonlinear effect such as cavitation and acoustic streaming, which
can effectively improve the distribution of reinforced particles in
the matrix [24]. Herein, in order to get a uniform distribution of
TiB2 particles, the same ultrasonic vibration treatments for 4 min
with vibration power of 2.8 kW and ultrasound frequency of 20 kHz
were applied in the molten composites. Then the composites was
immediately cast into a permanent mould preheated at about
200
C.

2.4. Microstructure analysis of composites

After casting, specimens were cut from the composites ingots.

The composites were mechanically polished and then were etched
with diluted hydrofluoric acid for 15s to reveal microstructure
morphologies. Microstructure observation for the samples was
implemented by SEM (Nova-450, FEI). Moreover, observation on Fig. 1. XRD patterns of 10% TiB2/Al master composite.
538 R. Du et al. / Journal of Alloys and Compounds 776 (2019) 536e542
Fig. 2. XRD patterns of 10% Mg2Si/Al composite.
a-Al grains. It is also clear from Fig. 3(b) that most of the TiB2
particles were in submicron size and a small portion of them were
nano size, which was in good agreement with our previous
research [26].
Fig. 4 shows the SEM images of unmodified Mg2Si/Al composite
and modified composites with different TiB2 particles addition. The
addition of TiB2 particles into the Mg2Si/Al composite resulted in
two obvious effects on the morphology and size of eutectic Mg2Si:
One was the shape modification and the other was the grain
refinement. As shown in Fig. 4(b), with 1% TiB2 particles addition,
most eutectic Mg2Si remained approximately unchanged and still
kept coarse. However, TiB2 particles were observed to dwell along
the interface between Mg2Si and aluminum matrix, which affected
significantly the morphology of this part eutectic Mg2Si surrounded
by TiB2 particles. Their shape transformed from big flake to small
polygon and the average size of eutectic Mg2Si decrease greatly
from about 20 mm to approximate 5 mm. With the increase of TiB2
particles amount, modification of eutectic Mg2Si was dominant and
the polygon grains became smaller, which could be seen from
Fig. 4(c). While the amount of TiB2 particles reached 5%, it is notable
that big flake-like eutectic Mg2Si could hardly be seen in Fig. 4(d)
and there was only modified small polygon eutectic Mg2Si particles
Fig. 3. Microstructure of 10% Mg2Si/Al composite and 10% TiB2/Al master composite: (a) 10% Mg2Si/Al composite; (b) 10% TiB2/Al master composite.
left, which had finer size compared with Fig. 4(b) and (c).
It is obvious that, on the one hand, the morphology and size of
eutectic Mg2Si had been radically altered by the addition of TiB2
particles. Nevertheless, on the other hand, TiB2 particles agglom-
erations along a-Al grain boundaries in Fig. 3(b) were broken by
eutectic Mg2Si. The interesting phenomenon indicated a mutual
interaction was present between eutectic Mg2Si and TiB2 particles
and this interaction was considered to affect Mg2Si/Al composite
profoundly.
Fig. 5 shows the XRD patterns of composites with different TiB2
particles addition. It can be proved from Fig. 5 that the addition of
TiB2 particles did not change the original phase composition in
Mg2Si/Al composite and introduced only TiB2 particles into the
composites. Thus, the alteration on morphology of eutectic Mg2Si
can be only attributed to the addition of TiB2 particles.
Fig. 6 shows the high magnification SEM images of modified 10%
Mg2Si/Al composite with 3% and 5% TiB2 particles. It confirmed
further that eutectic Mg2Si had been modified and refined. It is also
important to note that some TiB2 particles could be observed to
embed into eutectic Mg2Si in Fig. 6. The above fact may be attrib-
uted to that TiB2 particles can act as heterogeneous nuclei of
eutectic Mg2Si.
In order to determine the orientation relationship between TiB2
and Mg2Si, TEM observation was introduced in Fig. 7 to reveal
micro-mechanism of heterogeneous nucleation. As shown in
Fig. 7(a), the presence of Mg2Si phase was identified and TiB2
particles captured by eutectic Mg2Si were viewed as well. Fig. 7(b)
presents the SAED results of overlap between Mg2Si and TiB2 par-
ticles in Fig. 7(a). The obtained results demonstrate that (2 0 0)
crystal face of Mg2Si is parallel to (0 0 1) crystal face of TiB2 particles
(TiB2 belongs to hexagonal crystal system and the authors also
specially annotate four element coordinates of TiB2 crystal face in
Fig. 7(b)), indicating there is a good coherent relationship existing
between these two phase. The above results were in agreement
with the foregone studies [20,21].
Hence, authors can expound the mechanism and procedure
about regulating the morphology of eutectic Mg2Si by TiB2 parti-
cles. During the solidification of Mg2Si/Al composite with TiB2
particles, TiB2 particles are uniformly distributed in the melt due to
the treatment of high-intensity ultrasonic vibration. After the for-
mation of primary a-Al grains, TiB2 particles are pushed by the
growing solid/liquid interface. When the Al-Mg2Si eutectic reaction
starts, since the lattice orientation relationship between TiB2 par-
ticles and eutectic Mg2Si, TiB2 particles provide heterogeneous
nuclei to promote the nucleation of Mg2Si. Thus, Mg2Si phase is
refined and cannot grow large to exhibit flake-like morphology. The
 R. Du et al. / Journal of Alloys and Compounds 776 (2019) 536e542
Fig. 4. SEM images of composites: (a) 10% Mg2Si/Al composite; (b) 10% Mg2Si/Al composite with 1% TiB2 particles; (c) 10% Mg2Si/Al composite with 3% TiB2 particles; (d) 10% Mg2Si/
Al composite with 5% TiB2 particles.
Fig. 5. XRD patterns of composites: (a) 10% Mg2Si/Al composite; (b) 10% Mg2Si/Al
composite with 1% TiB2 particles; (c) 10% Mg2Si/Al composite with 3% TiB2 particles;
(d) 10% Mg2Si/Al composite with 5% TiB2 particles.
increase of TiB2 particles means the promotion of modification
effect. Therefore, with the increase of TiB2 particles, eutectic Mg2Si
become finer. Not only that, eutectic Mg2Si phase can also capture
TiB2 particles during solidification, which prohibit the formation of
TiB2 particles agglomerations pushed by a-Al grains. In summary, a
more uniformly distributed TiB2 particles and refined eutectic
Mg2Si phase are fabricate in this context through the unique
539
mutual interaction.
3.2. The changes of tensile properties
It is reasonable to predict that the addition of TiB2 particles into
Mg2Si/Al composite will have great impact on its tensile properties,
for instance, Young's modulus, yield strength and elongation. The
tensile curves of 10% Mg2Si/Al composite with different TiB2 par-
ticles addition are respectively shown in Fig. 8. Apparently, without
TiB2 particles addition, Mg2Si/Al composite exhibited poor ultimate
tensile strength and low elongation. With increasing TiB2 particles,
composites were strengthened gradually and the ultimate tensile
strength and elongation were also promoted at the same time. In
contrast, with 5 wt% TiB2 addition, the ultimate tensile strength
reached 298 MPa and increased 95% compared with Mg2Si/Al
composite.
In the case of the modulus of composites, as shown in Table 1, it
can be observed that the modulus of composites was enhanced by
the addition of TiB2 particles. With 5 wt% TiB2 addition, the
modulus of composite reached 82.85 GPa and increased 11%
compared with Mg2Si/Al composite of no TiB2 particles. This sig-
nificant improvement can be only attributed to the presence of TiB2
(Its Young's modulus is 529 GPa) particles. Thus, during the elastic
deformation stage, a-Al and eutectic Mg2Si can bear tensile
strength together with TiB2 particles, promoting the modulus
significantly. Moreover, with more addition of TiB2 particles,
modulus is further improved compared with Mg2Si/Al composite.
As for the yield strength of composites, it can be found from
Table 1 that the yield strength increased with increasing mass
fraction of TiB2 particles. Without TiB2 particles addition, the yield
strength of Mg2Si/Al composite was only 128 MPa. After 1 wt% TiB2
addition, the yield strength reached 167 MPa and increased 30%.
540 R. Du et al. / Journal of Alloys and Compounds 776 (2019) 536e542

Fig. 6. High magnification SEM images of modified 10% Mg2Si/Al composite with 3% and 5% TiB2 particles: (a) Mg2Si/Al composite with 3% TiB2 particles; (b) Mg2Si/Al composite
with 5% TiB2 particles.

Fig. 7. TEM images of modified 10% Mg2Si/Al composite with 5% TiB2 particles: (a) morphology of Mg2Si/Al composite with 5% TiB2 particles; (b) SAED patterns of (a).

Table 1
Some tensile properties of the composites.

Composites Young's modulus Yield strength Elongation

(GPa) (MPa) (%)

10 wt%Mg2Si/Al 74.85 127.56 2.12

10 wt%Mg2Siþ1 wt%TiB2/Al 76.39 167.34 2.86
10 wt%Mg2Siþ3 wt%TiB2/Al 79.29 183.27 3.79
10 wt%Mg2Siþ5 wt%TiB2/Al 82.85 202.68 5.09

with Mg2Si/Al composite of no TiB2 addition. Thus, it can be

Fig. 8. Tensile curves of Mg2Si/Al composite with different TiB2 particles addition.
With 3 wt% TiB2 addition, yield strength increased continuously
and reached 183 MPa. When the addition of TiB2 particles reached
5%, yield strength was 203 MPa and increased even 58% compared
concluded that the addition of TiB2 particles resulted in the increase
of yield strength. Generally, the yield strength of composites is
expected to be influenced by various factors. It has been reported
that coefficient of thermal expansion (CTE) mismatch strength-
ening and Orowan strengthening play the key roles in improving
the yield strength of PRAMCs [27].
Firstly, due to the large difference in the CTE between a-Al
(23.5  106K1) and TiB2 reinforcement phase (7  106K1), re-
sidual stresses were built up during fabrication process (solidifi-
cation of composites), inducing high-density dislocations around
the interface between reinforcement phase and matrix [28].
Therefore, the yield strength of composites was enhanced by the
addition of TiB2 particles. Furthermore, the high-density
 R. Du et al. / Journal of Alloys and Compounds 776 (2019) 536e542
dislocations generated by CTE mismatch depend on the size of
reinforcement phase in some extent [29]. The finer size of eutectic
Mg2Si, the more high-density dislocations will be generated.
Because eutectic Mg2Si could be refined by TiB2 particles, Mg2Si/Al
composite were further strengthened by the addition of TiB2 par-
ticles. Meanwhile, with increasing amount of TiB2 particles, TiB2
particles and refined eutectic Mg2Si would generate more high-
density dislocations to further promote the strength of composites.
The other strengthening mechanism is related to Orowan
strengthening, caused by the resistance for the passing of disloca-
tions generated by closely spaced hard particles. However, Orowan
strengthening is widely thought to be related with submicron size
particles, because micron-size phase are quite coarse and the inter-
particle spacing is too large [30]. Therefore, the Orowan strength-
ening in this context depends mainly on TiB2 particles. With more
TiB2 particles addition, Mg2Si/Al composite can be further
strengthened.
In a word, the modified morphology of Mg2Si and the addition of
TiB2 are the main reasons for the increase of strength. Hence, TiB2
particles can not only strengthen composite through refining
eutectic Mg2Si, but also directly promote the strength of
composites.
The morphology of eutectic Mg2Si plays an important role in
determining elongation and fracture behavior of the composites. It
can be observed from Table 1 that the elongation of composites
increased gradually with the addition of TiB2 particles, and elon-
gation reached 5.09% with 5 wt% TiB2 addition. Moreover, it can be
also concluded in Fig. 9 that the facture behavior of composites
transformed from brittle fracture to quasi-cleavage behavior and
finally became total ductile behavior.
In the case of 10% Mg2Si/Al composite, eutectic Mg2Si exhibited
coarse flake-like morphology (Fig. 4(a)), thereby the mechanical
Fig. 9. SEM fracture images of composite (a) 10% Mg2Si/Al composite; (b) 10% Mg2Si/Al composite with 1% TiB2 particles; (c) 10% Mg2Si/Al composite with 3% TiB2 particles; (d) 10%
Mg2Si/Al composite with 5% TiB2 particles.
541
properties especially the elongation were significantly reduced.
Thus, the elongation of 10% Mg2Si/Al composite was only 2.12%
(Table 1) and the fracture surface of the unmodified composite was
covered by smooth cleavage planes (Fig. 9(a)), suggesting that it
belongs to a brittle fracture mode. Likewise, these features of
fracture explain the low elongation of the unmodified composites
as well. In general, because of its coarse morphology and brittle-
ness, eutectic Mg2Si provide an easy path for crack propagation and
the fracture path goes preferentially through these eutectic regions
[31].
However, with 1% TiB2 particles addition, a part of eutectic
Mg2Si were refined and modified, which was shown in Fig. 4(b).
The finer and polygon shape eutectic Mg2Si phase would generate
less stress concentration and effectively suppress the initiation and
propagation of the cracks, resulting in the improvement of the
elongation. Meanwhile, some dimples could also be viewed in
Fig. 8(b), which means the type of fracture is multiple fracture of
part dimple and part cleavage mechanism. Thus, it can be
concluded that the refinement of eutectic Mg2Si by TiB2 particles
partially converts the fracture behavior of the composites.
With 3% TiB2 particles addition, the composite has more and
even finer modified eutectic Mg2Si, as shown in Fig. 4(c). The
composite does not crack prematurely when they bear tensile
stress. Thus, the elongation of composite can be improved to 3.79%
(Table 1). Not only that, a considerable amount of dimples in
Fig. 9(c) indicates that the dominant fracture behavior of the
refined composite here is ductile fracture. When the amount of TiB2
particles reached 5%, the rough fracture surface and typical dimples
shown in Fig. 9(d) implied the occurrence of plastic deformation on
the fracture surface. According to the microstructures shown in
Figs. 4(d) and Fig. 6(b), most of TiB2 particles are captured and
wrapped by refined and modified eutectic Mg2Si. As illustrated in
542 R. Du et al. / Journal of Alloys and Compounds 776 (2019) 536e542
Fig. 9(d), embedded TiB2 particles are also seen to protrude from
the dimples, suggesting that eutectic Mg2Si and a-Al matrix also
take part in the fracture process. Therefore, the fracture behavior of
composites converts sequentially from brittle fracture to mainly
ductile fracture due to the addition of TiB2 particles.
4. Conclusions
In this study, efforts have been paid to explicate the role of TiB2
particles which play in the refinement of eutectic Mg2Si
morphology and the transformation of composites fracture
behavior. The main conclusions can be summarized as follows:
(1) The suspended TiB2 particles can act as good heterogeneous
nuclei of eutectic Mg2Si due to the coherent lattice rela-
tionship between TiB2 and Mg2Si. Thus, coarse eutectic Mg2Si
can be refined and modified with the addition of TiB2 par-
ticles. With 5% TiB2 particles addition, coarse and flake-like
eutectic Mg2Si in 10 wt% Mg2Si/Al no longer exists.
(2) composites at the same time. The yield strength and elon-
gation of the composites increased 59% and 141% with 5 wt%
TiB2 addition, respectively. Moreover, the modulus of com-
posites also increased 11% with 5 wt% TiB2 addition.
(3) The different addition of TiB2 particles changes gradually the
fracture behavior of composites from brittle fracture to
quasi-cleavage fracture, and finally to entirely ductile
behavior with 5 wt% TiB2 addition.
Acknowledgements
This work was founded by the project 51574129 supported by
National Natural Science Foundation of China, and by the project
JCKY 2016209A001. The authors would also like to express their
appreciation to Analytical and Testing Center, HUST.
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