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Journal of Magnesium and Alloys 5 (2017) 48–55
www.elsevier.com/journals/journal-of-magnesium-and-alloys/2213-9567

Full Length Article

Microstructure, mechanical response and fractography of AZ91E/Al2O3 (p)
nano composite fabricated by semi solid stir casting method
Sameer Kumar D. a,*, Suman K.N.S. b, Tara Sasanka C. a,*, Ravindra K. a, Palash Poddar c,
Venkata Siva S.B. d
a
Department of Mechanical Engineering, R.V.R. & J.C. College of Engineering, Guntur, India
b
Department of Mechanical Engineering, Andhra University College of Engineering, Visakhapatnam, India
c
CSIR-National Metallurgical Laboratory, Jamshedpur, India
d
Department of Mechanical Engineering, Narasaraopeta Engineering College, Narasaraopet, India
Received 18 July 2016; revised 24 November 2016; accepted 24 November 2016
Available online 13 December 2016

Abstract
The present study confers to the fabrication and its characterization of magnesium alloy (AZ91E) based nano composites with nano Al2O3
particulate reinforcements. A novel Semi Solid stir casting technique was adopted for the fabrication of the composite. An average particle size
of 50 nm was used as reinforcement to disperse in matrix. The effects of change in weight fraction of reinforcements on the distribution of particles,
particle–matrix interfacial reactions, physical as well as mechanical properties were reported. The SEM and EDS analysis has shown the uniform
distribution of particles in the composite along with the presence of elements. The mechanical properties of reinforced and unreinforced composite
were evaluated and presented. Fractography of tensile specimens was also discussed.
© 2017 Production and hosting by Elsevier B.V. on behalf of Chongqing University. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Keywords: Magnesium alloys; Nano composites; Semi solid stir casting; Al2O3 particle

1. Introduction alloy with good cast ability and with wide range mechanical
properties at room temperature [6] but does not retain the same
In the recent years, the research on product development for
properties at elevated temperatures >120 °C [7]. Preparing
improved vehicle performance in automotive and aerospace
composites by magnesium alloys appears to be a good alterna-
sector has been considerably increased. The use of alternative
tive for improving their thermal stability [5].
materials is the best cost effective solution. The selection of
Reinforcement particles should be stronger and stiffer than
material to the particular application should focus on function-
the matrix material, so as to produce the expected strengthening
ality, cost and environmental impact. The research on magne-
effect. However, the selection of material, type, size and volume
sium as a substitute to cast iron, aluminum and polymers is
fraction of the reinforcements as well as its interactions with
going on at rapid pace [1–4,22].
matrix is essential to get desirable properties. With good
Magnesium offers good strength with low density. The
thermal stability, ceramic particles as reinforcements are the
recyclability with reduced CO2 emissions has also an added
most desirable due to high hardness, strength and melting point
attraction for magnesium. But pure magnesium is rarely used
[8]. With due considerations on cost and applications are on
due to its poor mechanical properties and high reactivity [5].
mind SiC, Al2O3 reinforcements are popular in magnesium
The addition of zinc and aluminum to magnesium as alloying
composites [9]. A number of research reports are available on
elements overcomes the demerits. AZ91 is popular commercial
SiC particle reinforced magnesium MMC. The composites are
observed to be highly brittle in nature because of SiC particles
[8,11,12,23]. On the other hand Al2O3 particles have the advan-
* Corresponding authors. Department of Mechanical Engineering, R.V.R. &
J.C. College of Engineering, Guntur, India. Fax: +91-863 2288274.
tages of low cost, exhibit high specific stiffness and excellent
E-mail addresses: me2meer@gmail.com (Sameer Kumar D.); tarasasankac oxidation resistance [9]. Al2O3 particles can exist in many crys-
@gmail.com (Tara Sasanka C.). talline phases and produces the most stable hexagonal alpha
http://dx.doi.org/10.1016/j.jma.2016.11.006
2213-9567/© 2017 Production and hosting by Elsevier B.V. on behalf of Chongqing University. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
 Sameer Kumar D. et al. / Journal of Magnesium and Alloys 5 (2017) 48–55
phase at elevated temperatures. Al2O3 particles promise
strength as well as enhanced ductility in magnesium composites
[10], which will be useful in structural applications.
At present, particulate reinforced composites are being pre-
pared by different methods, such as stir casting [8,11,12],
powder metallurgy [13], spray deposition technique, microwave
sintering and die castings [4,11,14]. Among these methods, stir
casting is found to be easily adaptable because of low cost and
high production rate. This method also produces the near-net
shape formation of the composites. Stirring temperature plays a
prominent role in the distribution of particles over the matrix.
When stirring is done above the liquidus temperature, porosity,
particle clusters and high oxide inclusions may occur. Hence a
modification to stir casting method called Semi Solid Stir
Casting was developed to reduce the conventional casting
defects [11,15].
Wettability is also another key factor in enhancing the prop-
erties. Wettability between the matrix and reinforcement can be
improved by decreasing the surface tension of the molten metal
or by increasing the surface energy of the reinforcement par-
ticles. Compared to aluminum, molten magnesium has low
surface tension [11]. Surface energy of the reinforcement par-
ticle can be enhanced by preheating before pouring into the
molten magnesium alloy [11]. The stirring during semi solid
state helps to spread the liquid metal on the surface of Al2O3
particulates and thus good wettability is achieved in Semi Solid
Stir Casting.
The research on Mg–matrix composites was limited due to
the high chemical activity of Mg in fabrication. For the past
decade the research and development on magnesium compos-
ites is remarkably increasing [14]. But, still very little amount
of work was contributed on the development and characteriza-
tion of magnesium alloy based composites by the semisolid stir
casting process. This paper aims on the fabrication of Mg MMC
Table 1
Chemical composition of AZ91E alloy.
Alloy Al Zn Mn Cu Si Fe Mg
%wt. 8.93 0.86 0.28 <0.001 0.13 < 0.001 Remaining
a. Melting Furnace with Argon gas arrangement
Fig. 1. Stir casting experimental setup.
49
with highly corrosion resistive and high purity grade AZ91E
Mg alloy with nano Al2O3 reinforcements via Semi Solid Stir
Casting Method. Metallurgy, physical as well as mechanical
responses of the as cast composites with changes in weight
fractions were addressed in the following sections.
2. Experimentation
2.1. Samples preparation
AZ91E alloy was bought from M/s Exclusive Magnesium
Pvt. Ltd. Hyderabad with chemical composition obtained by
performing wet analysis was given in Table 1.
The preparation of composite was carried out in a mild steel
crucible kept in a resistance furnace (Fig. 1a) under a cover of
flux (20% KCl, 50% MgCl2, 15% MgO, 15% CaF2, wt.%) and
with a high purity (99.98%) argon gas (IOLAR-1) supplied by
Linde India Limited, Jamshedpur. The raw materials, moulds,
flux were preheated to avoid the casting defects. At a furnace
temperature of 250 °C, the preheated AZ91E (10 wt% excess
material to compensate oxidation losses) and 1 wt% flux was
added. The temperature of the furnace was then raised to
700 °C and the melt was homogenized for about 20 minutes.
The liquidus and the solidus temperature of the AZ91 alloy are
found to be 596 °C and 468 °C [15]. So, the melt was slowly
cooled down to 590 °C to keep the material in the semi solid
condition. After cleaning the surface of the melt, the slurry was
stirred. The preheated Al2O3 particulates (avg. size 50 nm)
wrapped in an aluminum foil were submerged beneath the melt,
in corresponding wt%. Afterwards the mixture was stirred
using a four blade mechanical stirrer (Fig. 1b) with a rotation
speed of 450 rpm for 3 minutes and poured into a permanent
steel mould to form the ingots of 15 mm diameter with 150 mm
length. Similar procedure was done for all the reinforcements to
get the samples.
2.2. Porosity measurement
Porosity was measured in accordance with the theoretical as
well as experimental densities by using equation (1) [11,12].
The theoretical density was calculated by Rule of Mixtures
(ROM) with Al2O3 particles density as 3.9 g cm−3. The densities
b. Automatic stirrer
50 Sameer Kumar D. et al. / Journal of Magnesium and Alloys 5 (2017) 48–55
of cast composites were measured by Archimedes principle
with distilled water as immersion fluid. The samples were pol-
ished and weights were measured by using an electronic
balance. For each sample 8 density readings was recorded and
the average value was noted.
% porosity = 1 − ( measured density theoretical density ) × 100
(1)
2.3. Microstructural examination
Microstructural characterization was carried out for alloy as
well as for reinforced composites. The samples were polished
using an automatic polisher (Tegramin – 25, Struers, Denmark)
to produce mirror like surface. Particle distribution and matrix/
particle interfaces were examined using field emission scanning
electron microscope (FESEM) coupled with EDS (SUPRA 55,
Carl Zesis, Germany). The phase analysis was carried out using
X-ray diffractometer (SMART Lab, Rigaku, Japan) with a scan
speed of 3 deg/min between a scanning range of 20–90 degrees.
2.4. Mechanical properties evaluation
Mechanical properties of the composite with different
weight fractions of reinforcements were evaluated in terms of
micro hardness, macro hardness and tensile properties. Hard-
ness studies were carried out to study the effect of reinforce-
ment and its quantity on hardness. Micro hardness and macro
hardness were evaluated for a load of 100 gf and 10 kg respec-
tively with a loading period of 15 s. The hardness values were
measured by taking an average of 8 readings. Tensile testing
was done as per ASTM B 557 Standard on UTN 40, FIE
machine. Three readings for each composition were noted for
tensile testing. Fracture surfaces of tensile specimens were ana-
lyzed using FESEM images.
3. Results and discussions
3.1. Density and porosity
Table 2 shows the comparison of measured density and
theoretical density and porosity. The low porosity indicates
effective casting. It is observed that the porosity increases with
increase in the wt% of reinforcements. The same trend was
reported for AZ91D/SiC composites [11]. The casted compos-
ite density values are lower than the calculated densities
by ROM. It was further noticed that the nano particles as rein-
forcements enhance the porosity due to the presence of
Table 2
Porosity results of AZ91E alloy and processed composite.
Material Theoretical Experimental
density density (g cm−3)
(g cm−3)
AZ91E 1.810 1.806
AZ 91E + 1 wt % nano Al2O3 1.830 1.820
AZ 91E + 1.5 wt % nano Al2O3 1.841 1.829
AZ 91E + 2 wt % nano Al2O3 1.851 1.832
AZ 91E + 2.5 wt % nano Al2O3 1.862 1.838
AZ 91E + 3 wt % nano Al2O3 1.872 1.844
interstitial voids in clusters and discontinuity during stirring
and in pouring into the moulds as gasses entrapment [15].
3.2. Microscopy results
The surface morphology of cast as well as composites is
presented in Fig. 2. A closer observation by SEM combined
with EDS showed that the microstructure consisted of primary
α-Mg with divorced intermetallic eutectic phase ß-Mg17–Al12,
as shown in Fig. 2(a). The precipitates were hard and brittle
which had certain contribution to the hardness of the alloy [16].
Fig. 2 (b, c and d) shows the microstructure of composites
containing different percentages of nano-sized Al2O3 from 1 to
3 wt. %. It has been observed that the distribution of particles in
the composite samples is uniform and the un-uniformity
increases by increasing the reinforcement percentage above
2 wt %. The increase in the reinforcement percentage causes
clustering of particles due to increase in surface energy and
weakens the bonding between reinforcement and matrix there
by wettability decreases.
In Fig. 2(c) it is noticed that there is uniform distribution of
Al2O3 particles and also the refinement of dendritic structures
which may result in better improvement of properties. Fig. 3
shows the EDS analysis of the spectrum for composite with
2 wt % of reinforcement. Peaks of Mg, Al, Zn and O of mag-
nesium matrix composite were observed. The peaks obtained by
X- ray diffraction of composite sample [Fig. 4] are compared
with JCPDS (Joint Committee for Powder Diffraction Stan-
dards) data. From Table 3, the peaks of Al2O3, Mg and Mg17Al12
are identified in the prepared composite.
3.3. Mechanical properties
The reduced strength and stiffness of the magnesium alloys
put a limit on its applications in the field of automobile and
aerospace industries. Magnesium alloy composites can over-
come such difficulties with improvement in mechanical prop-
erties. The hardness, tensile properties, including ultimate
tensile strength, yield strength, elastic modulus (stiffness) and
ductility for AZ91E and for all the reinforcements were mea-
sured and presented in this section.
3.3.1. Hardness
Table 4 presents both macro and micro hardness values for
different weight percentages of reinforcement. It elucidates that
both the macro and micro hardness values increase along with
percentage of reinforcement when compared with base alloy.
Hardness value of pure AZ91 alloy was 80.87 VHN. Compos-
ites reinforced with Al2O3 particles at 3 wt % show the lowest
hardness value (82.14 VHN) while composites reinforced with
Al2O3 particles at 2 wt % show the highest hardness (99.038
% Porosity
VHN). The maximum observed increase in hardness of com-
posites compared to unreinforced magnesium alloy was
22.45%. The micro hardness was increased 19.5% as compared
0.22
0.58 with base material.
0.66 The observed increase in hardness was due to the presence
1.05 of hard Al2O3 particles, which aid to the load bearing capacity
1.28 of the material and also restricts the matrix deformation by
1.51
constraining dislocation movement [11]. After 2% of weight
 Sameer Kumar D. et al. / Journal of Magnesium and Alloys 5 (2017) 48–55 51

Mg17Al12

Al2O3
Mg

Mg17Al12

(a) (b)

Al2O3
Agglomerated
Al2O3

(c) (d)

Fig. 2. SEM images of (a) as cast magnesium alloy (b) AZ91 with 1% Al2O3 reinforcement (c) AZ91 WIth 2% Al2O3 reinforcement (d) AZ91 with 3% Al2O3
reinforcement.

Element Weight% Atomic%

OK 5.78 8.77
Mg K 77.69 77.57
Al K 15.73 13.21
Zn L 0.8 0.45
Totals 100.00

Fig. 3. EDS analysis of AZ91 magnesium alloy.

52 Sameer Kumar D. et al. / Journal of Magnesium and Alloys 5 (2017) 48–55

Fig. 4. XRD pattern of AZ91E–Al2O3 composite.

fraction, the increase in reinforcement results in decrease of Table 4

hardness due to improper distribution of Al2O3 nano particles. It Results of harness measurement.
may also be noted that hardness trend obtained in the present Material Macro hardness HV: 10 kg Micro hardness HV: 100 gf
study is similar to the findings reported for ceramic reinforced 0 80.878 ± 5 64.946 ± 3
magnesium matrices when the reinforcement is in the microm- 1 89.724 ± 3 72.116 ± 1
eter and nanometer length scales [17]. 1.5 92.318 ± 2 73.61 ± 2
2 99.038 ± 2 77.618 ± 3
2.5 94.077 ± 4 75.45 ± 3
3 82.141 ± 4 73.774 ± 2
Table 3
JCPDS data of AZ91E–Al2O3 composite.
S. No. Element JCPDS File No. 2 theta Intensity hkl
1 Corundum Al2O3 75–0787 25.794 692 012 3.3.2. Yield strength
2 35.471 999 104
Yield strength of the composites is observed to be increasing
3 38.091 472 110
4 43.732 956 113 with the increase in volume percentage of hard Al2O3 ceramic
5 53.026 473 024 particles in magnesium alloy (AZ91E) composite. The strength
6 58.049 930 116 of the composite always depends on the size of the particle and
7 67.139 354 214 the interfacial bond between the matrix and the reinforcement
8 68.632 534 300
[18]. Greater strength can be achieved by reduction in particle
9 77.715 151 1 0 10
10 Magnesium Mg 65–3365 32.185 242 100 size [9]. If the bonding between the matrix and the reinforce-
11 34.398 268 002 ment is good enough, then the applied stress can be transferred
12 36.619 999 101 from the soft magnesium alloy matrix to the hard Al2O3 particle.
13 47.820 142 102 The higher strength of Al2O3 particle protects the relatively soft
14 57.384 148 110
magnesium alloy matrix. The yield strength (0.2% offset) of
15 63.072 153 103
16 68.646 149 112 base material is observed to be 96 MPa while the highest yield
17 70.024 104 201 strength observed is 150 MPa for 3% weight fraction (Fig. 5). It
18 Aluminium 73–1148 36.113 999 411 was clear that with increase in the volume percent more loads
19 magnesium 40.079 286 332 can be transferred to the reinforcement which also results in
20 Al12Mg17 64.940 199 721
higher yield strength [11].
 Sameer Kumar D. et al. / Journal of Magnesium and Alloys 5 (2017) 48–55
(a)
Fig. 5. Variation of (a) yield and tensile strength (b) % of elongation w.r.t. % of reinforcement.
3.3.3. Tensile strength
The main aim of preparing the composite material is excel-
lent strength. A strong internal stresses are developed using
tensile load and these may create a localized failure when the
local stress exceeded the strength of the material. The uniform
distribution of the reinforcement particles bears the stress dis-
tribution and delays the formation of localized damage [11]. It
can be observed that the volume percentage of the Al2O3
increases the stress distribution to hard phase, which in turn
increases the tensile strength.
Fig. 5 shows the variation of yield and tensile strength for
alloy and the composite. The tensile strength of casted AZ91E
is 162 MPa while for 2% reinforcement it was 205 MPa and
decreased to 188 MPa for 3% reinforcement. It is clear that
tensile strength of composites is greater when compared to as
cast AZ91.With increase in Al2O3 content the agglomerations
are increased so that the defects induced around the Al2O3
particles due to the differences in the thermal expansion coef-
ficients of AZ91 and Al2O3 might result in debonding of the
interface and decrease in UTS in the composites. The same was
also observed by Senthil et al., with the Al2024 using nano
Al2O3 reinforcement [19].
If the percentage of reinforcement reaches certain level the
reaction in magnesium alloy with Al2O3 ceramic particle can
cause the formation of transition layers. These layers, although
enables a bond between Al2O3 and magnesium alloy, but they
are not tough enough to carry loads and thus they often con-
tribute to lowering the tensile properties of composites [11].
3.3.4. Ductility
The reinforcement affects the ductility of the magnesium
alloy composite. The % of elongation is decreased from 3.08 to
1.94 as shown in Fig. 5b. The decrease in ductility can be
ascribed because of void nucleation with increasing amount of
reinforcement. The high stress concentration at the tip of the
cracked particles can also contribute to a decrease in the duc-
tility in the composite. The exact reason for this variation may
be due to the fact that alumina particles act like stress concen-
trators. This role is promoted as particles lead to be agglomer-
ated. Thus, during tensile loading, the magnitude of stress
53
(b)
increases drastically near the agglomerated nanoparticles and
making the debonding between matrix and reinforcement.
3.3.5. Elastic modulus
Stiffness is the rigidity that can be measured through
Young’s modulus of the composite. As expected, addition of
Al2O3 particles to magnesium alloy (AZ91E) leads to the
improvement of modulus. The distribution of the fine and hard
reinforcement particles in the matrix blocks the motion of the
dislocations and strengthens the magnesium alloy composite.
The percentage of reinforcement, distribution in the matrix,
shape and size will affect Young’s modulus [9,11]. The predic-
tion of modulus of elasticity can be done by the rule of mixtures
and Halpin–Tsai equations. The Rule of Mixtures (ROM)
expression is most suitable for continuous reinforcements and
while the other is for discontinuous reinforcements [11] .
The Halpin–Tsai Equation:
Ec = ( E m (1 + 2S ∗ q ∗ Vp )) (1 − q ∗ Vp ) (2)
where:
q = ( E p E m − 1) ( E p E m ) + 2S) ; S indicates Aspect Ratio.
The Rule of Mixtures Equation:
Ec = E m Vm + E p Vp (3)
The rule of mixtures is simple and considers only volume
fraction and elastic modulus while Halpin–Tsai considers
aspect ratio of the reinforcement particle also. The modulus of
elasticity was calculated by the both methods for all the rein-
forcements. Fig. 6 shows the data of experimental and calcu-
lated modulus of elasticity to the proposed reinforcements. The
difference in both practical and calculated values is also attrib-
uted to the uncertainty in the appropriate value for the modulus
of the particle reinforcement.
3.3.6. Fractography of tensile specimens
Fig. 7 shows the microscope images of fracture surfaces of
alloy and the composite. It is clear from the figure that the
AZ91E magnesium alloy shows the ductile type of fracture.
The addition of hard Al2O3 particles to the matrix increases the
54 Sameer Kumar D. et al. / Journal of Magnesium and Alloys 5 (2017) 48–55

Fig. 6. Variation of modulus of elasticity using experimental, ROM and Halpin–Tsai model.

(a) AZ91E alloy (b) AZ91E+2 wt% Al 2 O 3 Reinforcement

Fig. 7. FESEM images of tensile fractured surfaces.

strength of the composite reducing the ductility. High magnifi-
cation of SEM fractographs indicated the composite with
2 wt % has mixed mode of shear and brittle fracture [20]. The
shallow dimples with varying sizes in the matrix over the frac-
ture surface can be clearly seen in Fig. 7(b). The same case was
observed with nano Al2O3 particle reinforced Al7075 matrix
[21]. At higher percentages, the particles will form clusters and
due to poor bonding and with increase in porosity, ductility
decreases even though the strength did not increase. Micro-
scopic cracks and voids of varying sizes with a noticeable
population of dimples were observed in the region of overload
indicative of locally ductile and brittle failure mechanisms.
4. Conclusions
2 The micro structural studies revealed the uniform distribu-
tion of the nano particles in the matrix system with the
method adopted.
3 Hardness, yield and tensile strengths of the composites were
found to increase with increased nano Al2O3 up to 2%, then
decreased with the addition of nano particles because of
cluster formation.
4 The 2 wt% Al2O3 reinforced AZ91E composite has good
mechanical properties than other reinforcements mentioned
with an increment of 22.5% macro hardness and 26.54 % in
tensile strength.
5 It is understood from fractographs that the unreinforced
AZ91E alloy exhibits the ductile type of fracture, whereas
the composites show a mixed mode of shear and brittle.

The following conclusions were made from the experiment Acknowledgements

conducted.
The authors are grateful to University Grants Commission,
1 AZ91E/ Al2O3 composites were successfully fabricated New Delhi, for granting the research project. The authors are
by Semi Solid stir casting technique with various weight also thankful to Dr. K. L. Sahoo, Principal Scientist, Metal
percentages. Extraction & Forming (MEF) Division, National Metallurgical
 Sameer Kumar D. et al. / Journal of Magnesium and Alloys 5 (2017) 48–55
Laboratory (NML), Jamshedpur, INDIA for the providing
facilities in the preparation of Composites. He has been very
helpful throughout the work.
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