Strojnícky časopis – Journal of MECHANICAL ENGINEERING,

VOL 70 (2020), NO 1, 29 - 38

PERFORMANCE EVALUATION OF SURFACE MODIFIED NANO

Al2O3 (p) REINFORCED AZ91E COMPOSITES UNDER IMPACT AND
FATIGUE LOADING CONDITIONS

Sameer Kumar D1, Suman K N S 2, PALASH Poddar3, Tara Sasanka C 4

1
Department of Mechanical Engineering, Bapatla Engineering College,
Bapatla, INDIA, e-mail: me2meer@gmail.com
2
Department of Mechanical Engineering, Andhra University College of Engineering, Visakhapatnam, INDIA
3
Principal Scientist, CSIR - National Metallurgical Laboratory, Jamshedpur, INDIA
4
Department of Mechanical Engineering, R.V.R. & J.C. College of Engineering, Guntur, INDIA

Abstract: This paper confers to compare the behavior of AZ91E, AZ91E with 2 wt. % plain and surface
modified alumina reinforced composites under different loading conditions. The composites were prepared and
specimens were cut in accordance with standard procedures to conduct impact and fatigue tests. Surface
modified alumina reinforced AZ91E magnesium based composites resulted in improved impact and fatigue
strength because of good interactions between the matrix and reinforcement. The results are discussed.

KEYWORDS: Metal Matrix Composites, Magnesium composites, AZ alloys, Alumina, Nickel coating,
Impact, Fatigue

1 Introduction
The role of magnesium in automotive sector is increasing day by day because of higher
specific density when compared against aluminum and iron. Several studies are done on
magnesium and its alloys as a substitute material to gain the advantage of less weight for the
sake of improved fuel economy and reduced CO2 emissions [1, 2]. Though magnesium
materials exhibited many positive characteristics, its reactivity and low strength at higher
temperatures restricted the further usage. Researchers identified that these problems can be
overcome with the usage of Magnesium composites [3, 4].
Composite materials are known for improved properties provided the interactions between
the matrix and reinforcement phases are good enough to carry the loads [5]. Bond strength
and defects around the matrix and reinforcement constituents influence the behavior of the
composite [6]. Particularly with ceramic reinforcement, wettability is a major challenge to the
researchers. Metallic coating on the ceramic practices is observed to be simple and effective
solution to promote good interfacial characteristics [7].
Most commonly used ceramic particles to reinforce metal matrix composites are Al2O3,
SiC,B4C,TiB2,TiC,Mg2Si,ZrB2[8]. Among these Al2O3 and SiC have more compatibility with
Magnesium [9]. Al2O3 particles are considered in the present work. These particles are coated
with Nickel to provide hardness, fatigue and wear strength. Pang et al. [10] mentioned the
importance of sensitization and activation conditions in successful implementation of Nickel
coating on nano particles by electro less plating route. The research on development of coated
ceramic reinforced composites is very less and it is much limited in case of Magnesium and
its alloy matrix materials. Sameer et al. [11] made composites with nickel coated nano
alumina ceramic particles as reinforcement in the AZ91E magnesium alloy in different weight
fractions. An overall improvement of 20-30 % was seen at 2wt. % in the basic mechanical

DOI: 10.2478/scjme-2020-0003, Print ISSN 0039-2472, On-line ISSN 2450-5471 ©2020 SjF STU Bratislava
properties of surface modified composite over monolithic alloy and composites without any
coating [12]. Though the basic mechanical properties of surface modified reinforcement
induced composites are promising further studies have to be evolved to focus on the failure of
composites. Simulation studies can also be conducted to analyze the mechanical behavior and
failure of composites [13]. However, the experimental studies are carried in the present study.
The present work deals with the extensive development of the surface modified (nickel
coated) alumina reinforced AZ91E magnesium composites in view of impact and the fatigue
behavior. The detailed experimental facilities, methodology and results are explained in the
subsequent sections. The failure mechanism of proposed composites is discussed through
fractography with microscopical analysis.

2 Materials and Methods

2.1 Preparation of surface modified alumina reinforcement

Alumina particles with an average size of 50nm supplied were considered as one of the
soured of reinforcement (Figure 1(a)). These particles are coated with electro less nickel to
increase the wettability in the matrix. The nickel coating on the reinforcement was done using
the electro less plating method with SnCl2, PdCl2 mode of sensitization and activation
conditions. Nickel chloride hexahydrate (NiCl2.6H2O) is the source of Nickel while Sodium
hypophosphite (NaH2PO2.H2O) is the reducing agent to reduce Nickel from electro less bath.
Un coated powder was immersed into electro less bath at 850c with the pH value 8. Coating
procedure and related characterization studies are discussed in detail by Sameer et al. [14].
The surface modified particles are shown in Figure 1(b).

(a) Nano Alumina (b) Surface modified Alumina

Fig. 1 Reinforcement [11,14]

2.2 Matrix Material

Matrix selection is always crucial in deciding the characteristics of composite. Among
various methods available, the selection of particular material is always a difficult task and
MADM methods make decision making easier [15, 16]. AZ91 magnesium alloy has been
selected as matrix material [17] among which AZ91E is observed to have excellent corrosion
resistance among the all AZ91 series alloys [1, 2]. The chemical composition of AZ91E is
depicted in Table 1.
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 Balance

30 ©2020 SjF STU Bratislava Volume 70, No. 1, (2020)

2.3 Preparation of Composites
The composites were prepared with AZ91E as matrix material along with coated and
uncoated nano alumina as reinforcements. Semi solid stir casting method has been adopted to
fabricate the composites because of improved properties and uniform texture of reinforcement
over matrix [18, 19]. The particles are pre heated and added in 2 wt. % were added to the
AZ91E melt at 5900C. The semi solid slurry was stirred with an automatic mechanical stirrer
and poured into molds of 150 mm in length and 15 mm in dia.

2.4 Impact Testing

The impact testing is used to measure the energy absorbed by the material before it breaks
or fractures. Brittle materials absorb lesser energy and breaks quickly while ductile materials
need more energy to fracture. The IZOD type of testing procedure is considered in the current
work. The IZOD specimens are 12.7 X 12.7 X 63.5 mm with a 45° included-angle notch,
which is 2-mm/0.079-inch deep as shown in Figure 2 (a & b).

(a) Specimen dimensions (b) Prepared specimens

Fig. 2 Impact Specimens

2.5 Fatigue Testing

The fatigue testing was done according to DIN 50113 standards (Figure 3 (a & b)). Fatigue
Testing was conducted on rotary bending type fatigue testing machine (Model No: TM 7001)
supplied by M/s DUCOM Material Characterization Systems, Bangalore. The failure life of
the proposed composites at different predetermined stress levels was measured and considered
to calculate the fatigue data. The statistical design of the experiments was planned to select
the minimum no of specimens and the analysis of variance was conducted to observe the
quality of data [20].

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 (a) Specimen dimensions (b) Prepared specimens
Fig. 3 Fatigue Specimens as per DIN 50113

2.6 Micro structural Examinations

The characterization of fractured surfaces (both fatigue and impact) was done using Field
Emission Scanning Electron Microscope (FESEM) attached with Energy Dispersive
Spectroscopy (EDS) (Model: TESCAN-MIRA 3 LMH, 2014 coupled with QUANTAX 200
with XFlash BRUKER, 2014).

3 Results and Discussions

3.1 Impact Behavior

The impact strength in terms of the impact energy absorbed in Joules during the IZOD
impact test of the monolithic AZ91E alloy and the composites prepared with 2 wt. %
uncoated and nickel coated alumina was tabulated in Table 2.
Table 2. Impact strength of the proposed composites

Impact Energy (J) - IZOD method

Sample Standard
Sample 1 Sample 2 Sample 3 Mean
Deviation
AZ91E 3.4 3.1 3.2 3.233 0.152
AZ91E with 2 wt. %
2.9 2.5 2.6 2.666 0.208
Al2O3
AZ91E with 2 wt.%
4.2 4.4 4.4 4.333 0.115
Ni Coated Al2O3
The impact energy of the composite reinforced with surface modified alumina was found
to be increased. The impact energy of the cast AZ91E is 3.233 J while for a 2% Al2O3
reinforcement, it was 2.666 J and in the case of 2% of the nickel coated reinforcement it was
4.333 J. An improvement of 34.02 % was seen in nickel coated alumina composites compared
to the base alloy. The impact energy values of plain alumina are lesser than the monolithic
material due to the presence of ceramic reinforcement and the reduced ductility values
[11,12]. The hard ceramic alumina particles act as stress concentrators can produce unstable
cracks resulting in lower energy absorption and impact energy in refuse to go along with the
applied load. The gaps at the interfaces of reinforcement and matrix particles also led to the
interfacial debonding and the failure phenomena indicate weak particle–matrix interactions.
However, the Ni coating over the surface of alumina help to slow down the failure mode

32 ©2020 SjF STU Bratislava Volume 70, No. 1, (2020)

which is dominated by the particle cracking and poor ceramic and matrix interactions. The
coating on the particles helps in absorbing more energy because of the stronger interface
resulting in higher impact energy than the monolithic alloy as well as the composite with plain
alumina. Ozden et al. reported that strong matrix – reinforcement interactions will provide
greater impact values. The similar kind of mechanism is observed in this current work. These
results are also in accordance with the literature where it was reported that the better matrix–
reinforcement interfacial bonding provides greater impact energy values [21].

a) d)

b) e)
cracks

c) f)

Fig. 4 Impact analysis (a-c) fractured specimens (d-f) fractogrphy of AZ91E alloy, AZ91E
with 2 wt. % Al2O3 reinforcement, AZ91E with 2 wt. % nickel coated Al2O3 reinforcement

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3.1.1 Impact fractography
The impact fractured specimens were shown in Figure 4(a-c), while the FESEM
morphology is shown in Figure 4(d-f). The microscopic cracks were observed in the fracture
morphology of uncoated alumina reinforced composites (Figure 4(e)) as a result of poor
interfacial bonding characteristics. The improved ductility of AZ 91E with Ni Coated Al2O3
alloy (Table 2) makes it to undergo plastic deformation which is reason for the high energy
impact. The FESEM fractography of Ni coated alumina reinforced composites shows a ductile
fracture with dimples over the surface (Figure 4 (f)).

3.2 Fatigue Behavior

Fatigue testing is analyzing the material behavior under repeated loads, Raju et al. used
statistical analysis to determine minimum no of samples to measure the fatigue strength of Al
alloy and associated composites [20]. Sameer et al. [22] observed that 3 to 4 samples were
enough to measure the fatigue strength of proposed composites with in the vicinity of
assumptions. The number of cycles before fracture are recorded and the results obtained are
validated with the use of statistical tables. The S-N curves of the proposed composites are
shown in Figure 5.

Fig. 5 Generation of S-N curve for AZ91E and its composites

Mathematical equations are developed (Equations 1-3) using MINITAB in order to analyze
the fatigue behavior at 108 cycles which is the most common measurement of fatigue data for
Aluminum and Magnesium alloys.
σ = 408.6 - 94.51 L + 6.632 L2 (1)

σ = 492.2 - 111.8 L + 7.734 L2 (2)

σ = 532.1– 123.2 L + 8.731 L2 (3)

Where σ is the stress and L is Log Life.

34 ©2020 SjF STU Bratislava Volume 70, No. 1, (2020)

 From the equations 1-3, the fatigue life of AZ91E and its proposed composites was found
to be 76.96 MPa, 92.57 MPa and 105.2 MPa respectively at 108 cycles. The AZ91E
composites prepared with surface modified alumina reinforcement exhibited an improvement
of 36.69% in the endurance stress limit over the monolithic AZ91E alloy. The Ni Coating on
the ceramics provided good interactions and can take entire load. A good amount of load
transfer can also be happened between matrix and reinforcement phases and this phenomenon
increased the no of cycles before fracture [23].

a) d)

b) e)

c) f)

Fig. 6 Fatigue analysis (a-c) fractured specimens (d-f) fractogrphy of AZ91E alloy, AZ91E
with 2 wt. % Al2O3 reinforcement, AZ91E with 2 wt. % nickel coated Al2O3 reinforcement

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3.2.1 Fatigue fractography
The specimens were cut and the fatigue fractured specimens of the proposed composites
were shown in Figure 6 (a-c) while the FESEM fatigue morphology of these specimens were
shown through Figure 6(d-f). The FESEM images of the high cycle fatigue fracture surface of
AZ91E are showing (Figure 6 (a)) striation-like features. The presence of striations is an
indicative of plastic deformation. The observation of AZ91E with alumina reinforced
composites showing (Figure 6 (b)) fine microscopic cracks representing locally brittle failure
mechanism. The overall failure morphology of the AZ91E matrix with coated alumina
reinforcement (Figure 6 (c)) was flat and revealed both smooth and rough regions which were
a suggestive of fatigue deformation. At higher magnification, the fatigue fracture surface of
surface modified alumina reinforced AZ91E composites revealed well-defined pockets of
randomly dispersed striations. These intrinsic features are representing both brittle and ductile
failure mechanisms at the fine microscopic level.

CONCLUSION
The mechanism of impact and fatigue failure of AZ91E magnesium based Surface
modified alumina reinforced composites was discussed in this paper. The Nickel coating on
the reinforcement was had a strong impact in improving the mechanical properties because of
strong metallic interactions. Good bond strength developed between the matrix and composite
constituents promoted increased load transfer from the ductile AZ91E magnesium alloy metal
matrix to hard and brittle alumina particle reinforcements. The coating on reinforcements also
resulted in delay of crack initiation and propagation compare to AZ91E and AZ91E with
uncoated alumina. An overall improvement of 34.02% in impact and 36.69% in fatigue
response was observed in Ni coated alumina reinforced composites compared to monolithic
material. Locally ductile mechanism has been observed via shallows and dimples in case of
composites as compared to the monolithic alloy.

ACKNOWLEDGEMENTS
The authors would like to express sincere thanks to the concerned persons of CSIR –
National Metallurgical Laboratory (NML), Jamshedpur for the preparation of castings,
Narasaraopet Engineering College, Narasarao Pet, VFSTR University, Vadlamudi for Fatigue
and Impact experiments and Centre for Nano and Soft Matter Sciences, Bangalore for their
support to carry out micro structural examinations.

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