Preparation, thermal analysis and mechanical properties of in-situ
Al2 O3 /SiO2(p) /Al composites fabricated by using zircon tailing sand

Kang Wang, Wenfang Li, Jun Du, Peng Tang, Jiyin Chen

PII: S0264-1275(16)30340-9
DOI: doi: 10.1016/j.matdes.2016.03.064
Reference: JMADE 1542

To appear in:

Received date: 12 January 2016

Revised date: 10 March 2016
Accepted date: 13 March 2016

Please cite this article as: Kang Wang, Wenfang Li, Jun Du, Peng Tang,
Jiyin Chen, Preparation, thermal analysis and mechanical properties of in-situ
Al2 O3 /SiO2(p) /Al composites fabricated by using zircon tailing sand, (2016), doi:
10.1016/j.matdes.2016.03.064

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Preparation, thermal analysis and mechanical properties of in-situ

Al2O3/SiO2(p)/Al composites fabricated by using zircon tailing sand

Kang Wang1, Wenfang Li1, *, Jun Du1, Peng Tang1, Jiyin Chen1

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(1, * School of Materials Science and Engineering, South China University of

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Technology, Guangzhou, China, 510640)

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* Corresponding author: Wenfang Li

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Tel./ fax: +86 20 8711 3747
E-mail addresses: mewfli@scut.edu.cn
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Abstract: Zircon tailing sand (comprised of SiO2 and Al2SiO5) was utilized as
reinforcement precursors to prepare aluminum matrix composites (AMCs) by using
indigenously developed stir casting technique. The Al2O3/SiO2(p)/Al composites were
successfully fabricated at different vol.% (viz. 1.1, 3.2, 5.4, 7.5 and 9.7) of zircon

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tailing sand and their metallurgical and mechanical properties have been analysis. The
SiO2/Al reaction in molten composites was proven by using the cooling curve thermal

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analysis (CCTA). Particles dispersion and wettability at SiO2/Al interface were

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improved with the optimized process parameters (i.e., particles preheating at 700 ℃ ×
1 h, feeding rate at 10 g/min and stirring time for 10 minutes). Optical and SEM

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micrographs revealed the uniform distribution of reinforcements in the matrix. X-ray
diffraction patterns and EDS testing results of the prepared AMCs revealed the
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presence of Al2SiO5, Al2O3, Si and the special duplex phase. The Brinell hardness,
ultimate tensile strength and yield strength (σ0.2%) of the composite were improved
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with the addition of zircon tailing sand in Al matrix. Fractured surface was carried out
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to explain the % elongation reduction and failure mechanism of these composites.

Keywords: Aluminum matrix composites (AMCs); Stir casting; zircon tailing sand;
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SiO2/Al reaction; cooling curve thermal analysis (CCTA); mechanical properties.

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1.Introduction
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Engineering interest in the aluminum matrix composites (AMCs) has increased

[1], owing to their high specific strength, high hardness, and high toughness. The
application potential of AMCs [2] mainly depends on the preparation process [3],
microstructure [4] and properties of the reinforcements [5]. Many methods, such as
squeeze casting [6], powder metallurgy [7], stir casting [8], and spray deposition [9],
have been developed for fabricating particle reinforced AMCs. Among them, stir
casting is widely used to prepare ceramic particles reinforced AMCs. By using this
technique, the ceramic particles (e.g. SiC(p) and Al2O3(p) etc.) whose wettability are
poor can be easily mixed into the molten Al at a relatively low temperature [10, 11].
Traditional researches on stir casting process [12-14] indicated that the dispersion of
the reinforcements in molten Al mainly depended on the rotation speed, temperature
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of the melts and the shape of the stirrer. In order to uniformly disperse the particles
and promote their mechanical properties, researchers have paid their attention on the
wettability at ceramic/Al interface. Geng et al. [15] improved the wettability of
discontinuous reinforcement in molten Al by preheating the reinforcement. Chen et al.

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[16] studied the dispersion and wettability of TiB2 in Al melts at different stirring time.
A special feeder made particles effectively immerse into the melts was designed by

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Tony Thomas et al. [17].

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According to the published reports [18-20], the mechanical properties of the
AMCs could be promoted by incorporating the ceramic particles with high hardness

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(e.g. SiC(p), Al2O3(p), and Al2SiO5 etc.). The SiO2 particles are also favorable to AMCs
fabrication. Without adding any alloying addition, the contact angle at the Al/SiO 2
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interface below 1000 ℃ is 70˚~90˚ [21]. It indicates that SiO2 particles can be
spontaneously wet by molten Al.
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The source of SiO2 is abundantly available. An attempt has been made to prepare
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particle reinforced AMCs reinforced with glass waste (SiO2) [22]. Moreover, several
researchers [1, 23] reported the AMCs with high strength by using the fly ash particles
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(with 49.5% SiO2 [1]) from a power plant. In this study, the reinforcement precursor
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(mainly comprises of SiO2 and Al2SiO5) was collected from the alloy manufacturers
who supplied Zr to the nuclear reactors and aerospace industry. The abundant but
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useless zircon tailing sand was dumped in designated landfills. It has led to a series of
considerable environmental problems. Utilizing the zircon tailing sand in AMCs
industry is good for the cost reduction. Also, it is helpful to solid waste treatment.
To the best of our knowledge, there has been no synthesis of AMCs using the
zircon tailing sand, till date. In order to know the strengthening effect of zircon tailing
sand and the products from SiO2/Al in-situ reaction, pure Al was selected as the
composite matrix. The wettability and dispersion of the particles in molten Al were
improved by the proper stir casting parameters. The cooling curve thermal analysis
(CCTA) [24] was carried out to prove the in-situ reaction in molten Al.
2. Experimental procedure
2.1 Raw materials for AMCs preparation
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The reinforcement precursor, zircon tailing sand, was obtained from the landfills
of a Zr alloy manufacturer. The density of zircon tailing sand was about 2.5 g/cm3.
The XRD pattern and chemical composition of the as-received zircon tailing sand are
shown in Fig. 1. Table 1 shows the chemical composition of the pure Al matrix

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(commercial pure Al with purity of 99.9 wt.% and density of 2.7 g/cm3).

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Fig. 2a shows the morphology of the zircon tailing sand. The main compositions

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of these particles are SiO2 and aluminum silicate. The size of the as-received zircon

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tailing sand was about 300 μm. Fig. 2b shows the morphology of the zircon tailing
sand which has been ball milled for 5 min in a planetary ball mill (with a size of

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520×600 mm). Fig. 2c shows the average size of the ball milled particles is 83.2 μm
(tested by using BACKMAN COULTER LS-13-320). These particles were utilized as
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the reinforcement precursor.
2.2 Apparatus for stir casting and AMCs fabrication
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Fig. 3a shows the stir casting apparatus applied in this study. An electric motor
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with 300 Watts power was used. The temperature error in the electric furnace was
limited to ±5 ℃. Fig. 3b shows a graphite impeller used for generating a vortex in
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molten Al. In order to avoid any contaminants at high temperature, the surfaces of the
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impeller and the graphite crucible were coated with Mica coating. When the Al ingot
(1.5 kg) was molten at 700 ℃, argon gas was supplied into the crucible at a constant
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flow rate of 2 lpm to avoid the reaction of Al melts with the atmospheric air. By the
time the temperature reached 700 ℃, C2Cl6 was added to the molten Al as the
degassing agent. After degassing, oxides on the surface of the melts were thoroughly
skimmed. The impeller was immersed into the crucible to 1/2 its depth of.
A predetermined quantity of zircon tailing sand particles were previously
preheated at 700 ℃ for 1 h by using a muffle furnace in atmospheric air. Then, these
particles were fed into the molten Al by using a hopper placed above the vortex
surface. Particles feeding rate was controlled to 10 g/min by using the hopper. In order
to obtain enough drag force from the vortex, and also to avoid an accidental spilling
out of the Al melts from the crucible, the rotating speed of the impeller was set at 500
rpm. The stirring operation was lasted for 10 min after all of the particles were fed
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into Al melts. Thereafter, composites slurry was poured into a steel permanent mould
(Φ20 mm × 80 mm) which was previously coated and preheated at 300 ℃.
The Al2O3/SiO2(p)/Al composites containing different weight percentages of
zircon tailing sand were fabricated. These samples added with 0 wt.%, 1 wt.%, 3 wt.%,

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5 wt.%, 7 wt.% and 9 wt.% zircon tailing sand were represented by Sample-1,
Sample-2, Sample-3, Sample-4, Sample-5 and Sample-6, respectively. Volume

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fraction ( Vr ) of these composites were calculated by using the equation as follow:

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1
Vr  100% (1)
1 
1  (  1) r

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wt m

where wt is the weight percentage of reinforcement precursor, ρr is the density of

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zircon tailing sand, and ρm is the density of the matrix. These calculation results are
given in Table 2.
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2.3 Thermal analysis of Al2O3/SiO2(p)/Al composites

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Fig. 4 shows the graphite mould used for CCTA experiments. The molten Al
(Sample-1) and the composite melts (Sample-6) at 700 ℃ were decanted to the
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graphite mould that was preheated at 700 ± 5 ℃, respectively. A K-type thermocouple

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was placed in the middle of the surface of the melts and immersed into the position of
55 mm from the bottom of the graphite mould. The thermocouple and the mould were
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fixed on a test stand to avoid any vibration. The temperature-time curves were
recorded at a dynamic rate of 10 Hz/Ch by using NI Thermocouple 9212 Series
Module which connected with NI cDAQ-9171 system. An algorithm was set for
calculating the first derivative and second derivative of the cooling curves. Fraction
solid (ƒs) of the melts at any moment (t) during the solidification course was evaluated
by using Newtonian thermal analysis (NTA) according to the following equation [25]:

1 t dT
fs 
LF 
tss
CV (
dt
 ZN ) dt (2)

where ƒs, tss, CV, dT/dt, LF, and ZN are the fraction solid, onset time of the
solidification course, volumetric heat capacity of the melts, temperature changing rate,
volumetric latent heat and the baseline value at time t, respectively. Volumetric latent
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heat is expressed as:

tes dT
LF   CV (  ZN ) dt (3)
tss dt
The tes in Eq. (3) symbolizes for the end of the solidification course. CV can be

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evaluated from the following equation:

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CV   LCpL (1  f s )   sC ps f s (4)

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where, ρ and Cp signifies density and heat capacity, respectively. The subscript ‘L’ and

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‘S’ represents for ‘liquid’ and ‘solid’, respectively. The values and expressions of ρS,
ρL, CpL and CpS are given in Table 3 [26, 27]. A baseline (ZN) for evaluating the

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fraction solid curve was determined by using a numerical integral algorithm on the
basis of Eq.(2), Eq. (4) and Table 3. These determination procedures have been clearly
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described in reference [24].
2.4 Investigation of process parameters
2.4.1 Preheating process of the zircon tailing sand
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Preheating processes of 300 ℃ × 1 h, 500 ℃ × 1 h and 700 ℃ × 1 h in atmospheric

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air were carried out for zircon tailing sand, respectively. Before preheating, a
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predetermined quantity of zircon tailing sand (5.4 vol.%) was put into a container and
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placed in an electric furnace. After each preheating process, particles were fed into the
molten Al at a feeding rate of 10 g/min. The same operation was conducted by using
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the zircon tailing sand without preheating. The molten composite was mechanical
stirred for 10 min at a fixed stirring speed of 500 rpm. After stirring, the surface
section of the melts was collected and poured into a cast mould. Samples were cut
from the cast composites to carry out the metallurgical characterization.
2.4.2 Feeding rate
The effect of the particles feeding rate on reinforcements distribution in Al matrix
was investigated. The composites was fabricated by using the feeding rate of 10 g/min,
20 g/min, 30 g/min, 40 g/min and 50 g/min, respectively. The predetermined quantity
of zircon tailing sand (preheated at 700 ℃ × 1 h in atmospheric air) was 5.4 vol.% in
each fabricate process. The stirring speed was fixed at 500 rpm. As soon as the
feeding operation was completed, the surface section of the composite melts was
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collected and poured into the cast mould. Specimens for further metallurgical
characterization were cut from the cast composite.
2.4.2 Stirring time
The effect of stirring time on the microstructure of the AMCs were investigated.

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The composites were fabricated with the stirring time of 1 min, 5 min, 10 min and 15
min, respectively. The predetermined quantity of zircon tailing sand (preheated at

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700 ℃ × 1 h in atmospheric air) was 5.4 vol.% in each fabricate process. The feeding

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rate for the particles was controlled to 10 g/min. The stirring speed was fixed at 500
rpm. The stirring time was recorded after the particles were all fed into the melts. As

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soon as the stirring operation was completed, the surface section of the composite
melts was collected and poured into the cast mould. Samples for further metallurgical
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characterization were cut from the cast composite.
2.5 Methodology of structural and mechanical characterization
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The metallographic analysis was carried out by using optical microscope (Leica
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DMI3000-M). In order to clearly observe the particles distribution, specimens were

polished but not etched. The constituents of zircon tailing sand and the composites
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were characterized by using X-ray diffraction (XRD). Scanning Electron Microscopy

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(SEM) along with energy dispersive X-ray spectroscopy (EDS) was used for
morphology observation and fractographic examination. The secondary electron (SE)
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mode was set in SEM testing for clear morphology observation.

Tensile testing was conducted by using SHIMADZU AG-X testing machine at
room temperature (at a strain rate of 6.7 × 10-3 s-1). Tensile testing specimens were
made according to ASTM E8M-04 standards (sub-size sample) [28] as shown in Fig.
5. The Brinell hardness of each sample was measured and analyzed by applying a
load of 250 kgf and maintaining it for 30 s (ASTM E10-07 [29]). The resultant
hardness of each sample was an average of at least five separate measurements, taken
from totally different locations on the sample surface.
3.Results and discussion
3.1 SiO2/Al reaction in Al melts
Fig.6a and b show the cooling curves and their first and second derivative of
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Sample-1 and Sample-6, respectively. The baselines used for evaluating the fraction
solid curves are given in these two diagrams. The cooling rates of these melts are
about 0.5 ± 0.1 ℃/s (calculated from the slope of the cooling curves before liquidus
temperature). Fig. 6c and d show the magnified images of area A and B marked in Fig.

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6a and b. The onset temperature of the nucleate point (TN) was determined by using
the second derivative curve, when the d2T/dt2 curve radically shifted upward and

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intercepted the zero level line. The TNAl in Fig. 6c symbolizes for the temperature at

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which the first primary Al crystals nucleate, stabilize and begin to grow. When the

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second derivative goes down and then goes up and intercepts the zero line again, it

indicates the growth temperature of primary Al ( TGAl ). The TmAlin corresponds to the
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first zero point of dT/dt curve and the crest on d2T/dt2 curve. These feature points that
correlate to the phase transformation of these two samples are given in Table 4. The

points ( TNAl , TmAinl and TGAl ) of Sample-6 are lower than those of Sample-1. The first
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peak revealed in the second derivative in Fig. 6a signifies the onset of solidification
course of α-Al. It also can be found in the corresponding curve of Sample-6. Fig. 6b
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shows one more narrow stage in the cooling curve at about 578 ℃. The first and
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second derivative of the narrow stage suggest the Al-Si eutectic reaction has taken
place. Si atoms were from the SiO2/Al reaction, as shown in Eq. (5) [30]:
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4 Al  3SiO2  2 Al2O3  3Si (5)

According to the thermodynamics theory, the Gibbs free energy ( GT ) of SiO2/Al

reaction [31] is written as :

GT  617977  79.3T (6)

where T is the temperature of SiO2/Al system. Above the melting point of pure Al

(T > 660 ℃) , the value of GT is -543990.1 J. It proves the SiO2/Al reaction can

spontaneously take place during AMCs fabricate process. The decrease of these

feature points ( TNAl , TmAinl and TGAl ) of Sample-6 is due to the colligative property of

Al-Si dilute solution. Fig. 6e shows a smooth fraction solid curve of Sample-1. It
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indicates that no reaction has taken place during the solidification course of molten Al.
An inflexion point at ƒs = 0.82 can be found in Fig. 6f. It is due to the effect of Al-Si
eutectic reaction on the latent heat releasing during solidification course.
3.2 Process parameters determination

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3.2.1 Preheating process
Fig. 7a shows the microstructure of the composite fabricated by using the

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particles without preheating. No obvious particles can be found in this micrograph. It

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indicates the wettability of zircon tailing sand without preheating is extremely poor.
Fig. 7b shows the microstructure of the composite fabricated by carrying out the

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preheating process at 300 ℃ × 1 h. A large cavity is shown in the rectangular area in
this image. The samples fabricated by using zircon tailing sand preheated at 500 ℃ ×
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1 h and 700 ℃ × 1 h were shown in Fig. 7c and d, respectively. In these cases, less
defect can be found with the increase of preheating temperature.
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Fig. 7e shows the defects in the sample fabricated by using 300 ℃ × 1 h particles
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preheating process. It reveals a large particle agglomerate inside a cavity. The defect
was caused by the large temperature difference between particles and the melts. Once
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the particles at a relatively low temperature were fed, the viscosity of molten Al
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outside the particle agglomerates was suddenly promoted. The difficulty in particles
dispersing was resulted from the poor fluidity outside these agglomerates. The
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microstructure of the sample fabricated with 700 ℃ × 1 h particles preheating process

is shown in Fig. 7f. A clean interface between the particles and the matrix can be
observed in the micrograph with a high magnification.
Moreover, Fig. 8a shows the contaminants appeared on the surfaces of the
as-received particles. During the feeding operation, these particles could not be
absorbed into molten Al. Fig. 8b shows the contaminants on the particles are removed
by using preheating process (300 ℃ × 1 h). It indicates the preheating process can
clean the particle surface. Due to the consideration of reducing the temperature
difference between the particles and the melts, preheating at 700 ℃ × 1 h were taken
as the proper parameter.
3.2.2 Feeding rate
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Fig. 9a shows the microstructure of the composite fabricated with a feeding rate
of 10 g/min. It displays a uniformly distributed reinforcement on the Al matrix. Figs.
9b-d are the microstructures of these samples prepared by using the feeding rate of 20
g/min, 30 g/min and 40 g/min, respectively. It is evident that the agglomeration

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tendency of the particles become more and more critical with the increase of feeding
rate. Fig. 9e shows the microstructure of the sample fabricated with a feeding rate of

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50 g/min. It reveals the most critical agglomeration tendency of the particles which

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will results in a serious particles peeling off during polishing procedure. Obviously, a
feeding rate of 10 g/min is the most proper parameter for particles distribution in Al

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matrix.
Dispersion of the particles in molten Al depends on the absorption capacity of the
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vortex. It is usually controlled by the speed of the impeller [12]. Fig. 9 indicates the
particles agglomeration can also be improved without changing the rotating speed.
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The lower feeding rate was applied, the longer time and more sufficient space in the
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vortex would be provided to the particles to interact with Al melts. In contrast, excess
number of particles fed from the hopper in a short moment would lead to the
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formation of particle agglomerates on the surface of molten Al. Thereafter, these

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particle agglomerates would further limit the absorbing capacity of the vortex.
3.2.3 Stirring time
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Figs. 10a and b show the microstructures of the composites prepared with stirring
time for 1 min and 5 min, respectively. As expected, both of the images show the
agglomeration tendency of the particles. Arrows labeled in these two images show the
defects at the particle interfaces. These poor bonding interfaces are resulted from the
non-uniformly dispersed particles. Fig. 10c shows the particles are uniformly
dispersed with the stirring time for 10 min. Few defects can be found at the clear
reaction zone of each particle. Fig. 10d reveals a pore (labeled by the arrows) in Al
matrix with the stirring time for 15 min. Excessive stirring in molten Al facilitated the
reinforcement dispersion, but it also led to gas entrapment and the defects formation.
Due to the consideration of acquiring the composites with uniformly dispersed
particles and fewer defects, a stirring time of 10 minutes is acceptable.
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3.3 Phase identification and microstructure

Table 5 summarizes the most proper process parameters based on the experiments
in section 3.2. These parameters were used for fabricating the Al2O3/SiO2(p)/Al
composites containing different quantity of zircon tailing sand. Fig. 11 shows the

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XRD patterns of the Al2O3/SiO2(p)/Al composites. The peaks of SiO2 and aluminum
silicate are revealed in these patterns. The peaks of Si in XRD results prove the in-situ

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reaction has taken place in molten Al. Fig. 12 shows the optical microstructures (OM)

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of Al2O3/SiO2(p)/Al composites containing different vol.% of zircon tailing sand.
Several pores can be found in the micrographs of Sample-2, Sample-3 and Sample-6

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(labeled with arrows in Fig. 12a, b and e respectively). Since the Sample-2 and
Sample-3 were produced with relatively low vol.% of zircon tailing sand, the
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reinforcements in these samples’ surfaces were not as intensive as the others’.
Particles peeling off in Fig. 12a and b are due to the inhomogeneous shear force
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exerted on the polishing surfaces with non-uniform hardness. The pores in Fig. 12e
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are resulted from the particles agglomerates in Sample-6. Since excessive quantity of
particles were fed, the viscosity of the melts was significantly increased. The particles
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dispersing became more and more difficult with the prominent decrease of the fluidity
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of molten Al.
Fig. 13 shows the typical morphology of Al2O3/SiO2(p)/Al composites. A special
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duplex-phase is presented in Fig. 13a. The SiO2 surrounded by Al2O3 layers in this
structure is resulted from SiO2/Al in-situ reaction. Fig. 13b shows the aluminum
silicate particle which is known as a conventional reinforcement in AMCs [20]. Fig.
13c shows the Al-Si eutectic phase stayed at the grain boundary of α-Al. It suggests
the Si atoms have diffused into molten Al after the SiO2/Al in-situ reaction. Fig. 13d
shows the uniformly distributed Al2O3 particles generated from the interaction of
duplex phase and the molten Al.
3.4 Mechanical properties
Fig. 14 shows the Brinell Hardness (HB) of pure Al matrix and the fabricated
Al2O3/SiO2(p)/Al composites. The Brinell hardness of the pure Al matrix is 20.2 HB
which is close to the value given in reference [32]. The Brinell hardness of Sample-6
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is 43.2 HB which is 114% higher than the pure Al matrix (Sample-1). The Brinell
hardness of Al2O3/SiO2(p)/Al composites linearly increase with the addition of zircon
tailing sand. It is owing to the presence of hard SiO2, Al2SiO5 and the products from
SiO2/Al reaction.

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Fig. 15 reveals the typical engineering stress strain diagrams of pure Al matrix
and Al2O3/SiO2(p)/Al composites. The average yield strength (σ0.2%), ultimate tensile

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strength (UTS) and % elongation of Al2O3/SiO2(p)/Al composites with various vol.%

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of zircon tailing sand are presented in Fig. 16. Both UTS and the yield strength are
increased by the addition of zircon tailing sand. But % elongation of the AMC

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decreases when the amount of zircon tailing sand increases. The UTS of Sample-5 is
96.1 MPa which is 74.4% greater than the pure Al matrix (Sample-1). The UTS of
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Sample-6 is 93.2 MPa which is close to that of Sample-5. The yield strength of
Sample-6 is 66.9 MPa which is 112.2% higher than the Al matrix (Sample-1). On the
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contrary, the % elongation of Sample-6 is only 13.7% that of Sample-1.

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As far as these particles reinforced AMCs, an increase in reinforcement fraction

often results in an increase in dislocation density around the reinforcements during
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solidification [33]. In this case, the influence of a far-field stress offers resistance to
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the motion of both the microscopic level dislocations [34]. Meanwhile, the more
reinforcements were formed, the larger is the magnitude of the resistance offered.
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Besides, a good interfacial bonding at reinforcement/matrix interface will promote the

load bearing capacity of the AMCs [35]. Agglomeration tendency of the particles in
Fig. 12e is more critical than that of the other microstructures in Fig. 12. It indicates
the bonding property at reinforcement/matrix interfaces of Sample-6 is more poor
than that of Samples-5. As a result, a prominent UTS enhancement can not be found
at Sample-6. Fig. 16b shows the yield strength of Sample-2 is smaller than that of
Sample-1. It is known that stress concentration would take place nearby the defects
generated from stir casting process. The composite with such a low reinforcement
fraction can not resist the yielding evolution resulted from the critical stress
concentration.
Fig. 17a reveals the fracture pattern of pure Al matrix (Sample-1). It shows a net
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work of large size dimples which indicate large amount of plastic flow prior to failure.
Fig. 17b reveals the fractured surface of Al2O3/SiO2(p)/Al composites (Sample-5). It
shows a brittle fracture pattern with less area of cavities, indicates that the debonding
of reinforcement is taken place prior to the large amount of plastic flow. The fractured

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surface of Sample-6 is shown in Fig. 17c in which the agglomeration tendency of the
particles is critical. During tensile testing, the defects caused by the particle

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agglomerates led to a serious stress concentration in Al matrix. Besides, the cracking

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of the brittle particles, located by the arrow in Fig. 17c, provides the evidence for %
elongation reduction of the AMCs. These findings also support the slight decrease of

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UTS value of at Sample-6 in Fig. 16a.
4. Conclusions
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The conclusions derived from this research are given below:
1) The uniform dispersion of zircon tailing sand with better wettability in pure Al
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matrix was obtained by using particles preheating at 700 ℃ × 1 h, feeding rate at 10

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g/min and stirring time for 10 minutes.

2) Few pores and particle agglomerates could be found in the fabricated AMCs
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containing 5.4 vol.% and 7.5 vol.% of zircon tailing sand.

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3) The SiO2/Al in-situ reaction has taken place in molten Al during fabricate process.
4) The UTS of Al2O3/SiO2(p)/Al composite containing 7.5 vol. % zircon tailing sand
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was 74.4 % greater than pure Al matrix.

5) The addition of zircon tailing sand enhanced the hardness and tensile strength of
the AMCs, but it reduced the % elongation of the AMCs.

Acknowledgments
The authors are gratefully acknowledge the support of the Science and
Technology plan projects with Grant No.2013B090500091 of Guangdong Province,
China. The raw materials used in this study were acquired as a courtesy from
Guangzhou Kinbon non-ferrous alloy metals Co.Ltd.
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[1] David RSJ, Robinson SDS, Dinaharan I. Microstructure and some mechanical
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properties of fly ash particulate reinforced AA6061 aluminum alloy composites

prepared by compocasting. Mater Des 2013;49:28.
[2] Lloyd DJ. Particle reinforced aluminium and magnesium matrix composites. Int
Mater Rev 1994;39:1.

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Figure Captions:
Fig. 1. XRD pattern of zircon tailing sand
Fig. 2 Morphology and size of the zircon tailing sand.
(a) zircon tailing sand without ball milling, (b) zircon tailing sand after ball

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milling,
(c) particle distribution of the ball milled zircon tailing sand.

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Fig. 3 Stir casting apparatus.

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(a)Schematic diagram of stir casting apparatus, (b)graphite impeller.
Fig. 4 Thermal analysis set up with graphite mould and thermocouple.

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Fig. 5 The dimensions of the tensile specimen as per ASTM E8M-04 standard.
Fig. 6. Cooling curve thermal analysis for the samples.
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(a) Sample-1, (b) Sample-6, (c) Feature points for Sample-1, (d) Feature points
for Sample-6,
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(e) Fraction solid curve for Sample-1, (f) Fraction solid curve for Sample-6.
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Fig. 7 Effect of the preheating process on the microstructure.

(a) without preheating, (b) 300 ℃× 1 h, (c) 500 ℃× 1 h, (d) 700 ℃× 1 h,
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(e) particles peeling off in the sample (with 300 ℃× 1 h),

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(f) clean interface in the sample (with 700 ℃× 1 h).

Fig. 8 Effect of the preheating process on particles morphology.
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(a) The as-received particles, (b) The particles after preheating process.
Fig. 9 Effect of the feeding rate on the microstructure of the composite.
(a) 10g/min, (b) 20g/min, (c) 30g/min, (d) 40g/min, (e) 50g/min.
Fig. 10 Effect of the stirring time on the microstructure of the composite.
(a) 1 min, (b) 5 min, (c) 10 min, (d) 15 min.
Fig. 11 XRD patterns of fabricated Al2O3/SiO2(p)/Al composites.
Fig. 12 Optical microstructure of Al2O3/SiO2(p)/Al composites.
(a) Sample-2, (b) Sample-3, (c) Sample-4, (d) Sample-5, (e) Sample-6.
Fig. 13 The typical morphology of fabricated Al2O3/SiO2(p)/Al composites.
(a) duplex-phase, (b) aluminum silicate, (c) Al-Si eutectic phase, (d) Al2O3
particles.
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Fig. 14 Brinell harness of fabricated Al2O3/SiO2(p)/Al composites.

Fig. 15 Strain stress curves of fabricated Al2O3/SiO2(p)/Al composites.
Fig. 16 Effect of vol.% of zircon tailing sand on:
(a) Ultimate tensile strength, (b)Yield strength, and (c) % elongation.

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Fig. 17 Fracture surface of (a) Sample-1, (b) Sample-5, (c) Sample-6.

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Fig. 1. XRD pattern of zircon tailing sand

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Fig. 2 Morphology and size of the zircon tailing sand. (a)zircon tailing sand
without ball milling, (b)zircon tailing sand after ball milling, (c)particles
distribution of the ball milled zircon tailing sand.
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Fig. 3 Stir casting apparatus. (a)Schematic diagram of stir casting apparatus,

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(b)graphite impeller.

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Fig. 4 Thermal analysis set up with graphite mould and thermocouple.

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Fig. 5 The dimensions of the tensile specimen as per ASTM E8M-04 standard.
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Fig. 6. Cooling curve thermal analysis for the samples.

(b) Sample-1, (b) Sample-6, (c) Feature points for Sample-1, (d) Feature points for
Sample-6,
(e) Fraction solid curve for Sample-1, (f) Fraction solid curve for Sample-6
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Fig. 7 Effect of the preheating process on the microstructure.

(a) without preheating, (b) 300 ℃× 1 h, (c) 500 ℃× 1 h, (d) 700 ℃× 1 h,
(e) particles peeling off in the sample (with 300 ℃× 1 h),
(f) clean interface in the sample (with 700 ℃× 1 h).
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Fig. 8 Effect of the preheating process on particles morphology.

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(a) The as-received particles, (b) The particles after preheating process.

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Fig. 9 Effect of the feeding rate on the microstructure of the composite.

(a) 10g/min, (b) 20g/min, (c) 30g/min, (d) 40g/min, (e) 50g/min.
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Fig. 10 Effect of the stirring time on the microstructure of the composite.

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(a) 1 min, (b) 5 min, (c) 10 min, (d) 15 min.

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Fig. 11 XRD patterns of fabricated Al2O3/SiO2(p)/Al composites.

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Fig. 12 Optical microstructure of Al2O3/SiO2(p)/Al composites.

(a) Sample-2, (b) Sample-3, (c) Sample-4, (d) Sample-5, (e) Sample-6.
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Fig. 13 The typical morphology in fabricated Al2O3/SiO2(p)/Al composites. (a)

duplex-phase, (b) aluminum silicate, (c) Al-Si eutectic phase. (d) Al2O3 particles.
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Fig. 14 Brinell harness of different Al2O3/SiO2(p)/Al composites samples.
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Fig. 15 Strain stress curves of different Al2O3/SiO2(p)/Al composites samples.

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Fig. 16 Effect of vol.% of zircon tailing sand on:

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(a) Ultimate tensile stress, (b)Yield stress, and (c) % elongation

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Fig. 17 Fracture surface of (a) Sample-1, (b) Sample-5, (c) Sample-6.

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Table captions:

Table 1 Chemical composition (wt.%) of commercial pure Al.

Table 2 Volume fraction of the fabricated Al2O3/SiO2(p)/Al composites

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Table 4 Feature points of the cooling curve thermal analysis.

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Table 5 Process parameters for Al2O3/SiO2(p)/Al composites fabrication.

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Table 1 Chemical composition (wt.%) of commercial pure Al

Al Si Fe Cu Mn
99.90 0.02 0.05 0.02 0.01

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Table 2 Volume fraction of the fabricated Al2O3/SiO2(p)/Al composites

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Sample No. Sample-1 Sample-2 Sample-3 Sample-4 Sample-5 Sample-6

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wt.% 0.0 1.0 3.0 5.0 7.0 9.0
vol.% 0.0 1.1 3.2 5.4 7.5 9.7

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Table 3 Physical properties considered during calculation of solid fraction
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S L CpL CpS

(kg/m3) (kg/m3) (J/mol·℃) (J/mol·℃)

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2700 2380 31.748 31.376 -16.393 10-3T - 3.607 10-5T 2  20.753 106 T 2
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Table 4 Feature points of the cooling curve thermal analysis.

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Samples TNAl Al
Tmin TGAl TNAl-Si TmAinl-Si TGAl-Si

Sample-1 675.7 665.9 667.2 — — —

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Sample-6 667.9 653.5 648.6 587.5 578.6 555.9

Table 5 Process parameters for Al2O3/SiO2(p)/Al composites fabrication

Process Stirring Stirring Feeding Preheating Stirring
Parameters Temperature Speed Rate Process Time

Values 700 ℃ 500 rpm 10 g/min 700℃ × 1 h 10 min

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Graphical Abstract

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Highlights

► Zircon tailing sand was used for fabricating the Al2O3/SiO2(p)/Al composites.

► The SiO2/Al in-situ reaction has taken place in molten Al.

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► Suitable process parameters were carried out to uniformly disperse the zircon

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sand in Al melts.

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► Mechanical properties are increased by the addition of zircon tailing sand.

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