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DEVELOPMENT & CHARACTERISATION OF

Mg HYBRID COMPOSITE REINFORCED WITH
n-TiO2/µ-Al2O3 FOR STRUCTURAL AND
BIOMEDICAL APPLICATIONS

ABSTRACT
of the Thesis

Submitted by

NEELA MURALI V K

in partial fulfillment of the requirements for the degree of

DOCTOR OF PHILOSOPHY

FACULTY OF MECHANICAL ENGINEERING

ANNA UNIVERSITY
CHENNAI 600025

JULY 2023
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ABSTRACT

The recent decade has witnessed significant progress in the creation

of high-performance Magnesium (Mg) alloys in cast and wrought form, Mg-
based composites and varied processing processes. Mg ion batteries and bio-
absorbable Mg alloys are examples of such materials. Mg alloys containing
rare earth elements, such as Mg-Gd-Y-Zr alloys demonstrates extremely good
heat resistance. Many experts are now working on producing Mg alloys with
optimal mechanical properties and diverse process parameters. A large
number of extensive studies have been conducted in the last decade to
improve the mechanical characteristics of the Mg Metal Matrix Composites
(MMC). Several conventional and nonconventional techniques were
developed to accommodate various reinforcements with the Mg metal matrix.
The lack of mechanical properties of pure Mg metal could be resolved by
suitable alloying elements. Mg-alloy characteristics could be improved further
by strengthening the alloy matrix with appropriate reinforcements and
composite forming processes.

As a result, the application area of Mg-based alloys and their

composites has widened and it is now used in structural applications such as
automotive, aerospace and biomedical sectors. According to the literature
review, multiple efforts have been undertaken to improve the mechanical
properties of Mg composites by employing various types of reinforcements
and altering their weight % and processing procedures. Mg matrix composites
containing ceramic reinforcements such as Aluminium Oxide (Al2O3), Silicon
Carbide (SiC) and Carbon Nano Tubes (CNT) shown excellent mechanical
characteristics. Although the addition of ceramic reinforcement to the Mg
alloy matrix improved their mechanical and tribological properties by
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improving the interfacial integrity between the matrix and reinforcement

phases, strength and ductility, but the fracture toughness was found to be
limited.

As a result, a novel Mg matrix composite will be created using a

cost-effective technology to address these drawbacks and create a composite
suited for industrial applications. According to recent research, these
limitations can be solved by simultaneously reinforcing the Mg matrix using
hybrid reinforcements. On this basis, new Mg-based hybrid composites with
micro Al2O3 and nano-TiO2 reinforcement were produced. In the first phase, a
unique quaternary alloy Mg-3Zn-0.5Mn was created. Succeeding that, these
alloy-based composites were created in the next step. The alloy was
reinforced with several reinforcement sets consisting of variable micron level
Al2O3 particles hybridized with nano-TiO2 composites. The blend-press-sinter
Powder Metallurgy (PM) processing technique was employed to create the
composites. The characteristics of the alloys and hybrid composites were
investigated independently in their as-extruded and stress-relieving or heat-
treated states.

The following were the primary goals of this study a) Synthesis of

the novel quaternary alloy Mg-3Zn-0.5Mn and the same alloy-based
composite reinforced with micro Al2O3 and hybrid nano-TiO2 particles carried
out by PM route followed by hot extrusion. b) Characterisation of the alloys
and composites based on the mechanical, microstructural and metallurgical
properties in their as-extruded form and after the stress-relieving process.
c) The investigation on the mechanical & corrosion property of the Mg alloy
and hybrid composites after heat treated & stress-relieved. When compared to
pure Mg metal, the mechanical parameters of the produced Mg-3Zn-0.5Mn
alloys showed a significant improvement in the physical, mechanical and
corrosion characteristics.
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The included alloying components improved the density and

porosity of the synthesized alloys. The dense alloys with low porosity
developed shows the efficiency of the PM manufacturing approach. The
presence of MgZnCu intermetallic in the alloys is linked to the alloys superior
thermal characteristics, as demonstrated by X-Ray Diffraction study. Alloys
have a homogeneous distribution of equiaxed grains. However, there was
some porosity and particle clustering found in the alloy matrix. The stress-
relieving method improved the mechanical properties of these alloys. After
stress-relieving, Mg-3Zn-0.5Mn alloys demonstrated good ultimate tensile
strength and fracture strain. The stress-relieving method also significantly
enhanced microhardness, impact strength and compressive strength.

The study's findings confirm the importance of stress-relieving in

improving the mechanical properties of manufactured alloys. Grain refining
during the hot extrusion process and precipitation strengthening were played a
crucial part in the enhancement of the properties. By using the blend-press-
sinter PM technique, hybrid composites Mg-3Zn-0.5Mn/hybrid Al2O3 and
TiO2 were created. Set of hybrid composites were created by altering the
weight percentage of micron level Al2O3 in the composites while maintaining
a constant 0.1% of nano TiO2. The billets were subjected to hot extrusion
process at 400°C as part of secondary processing. Following hot-extrusion,
the samples were subjected to stress-relieving at a temperature of 260°C. The
physical characterisation test revealed that hybrid composites have a higher
density than pure Mg and prepared alloys. The improved density and minimal
porosity indicated that the alloy matrix and the hybrid composite matrix
formed with strong bonding.

The microstructural analysis revealed a well-refined microstructure

with little porosity and consistent distribution of reinforcements along the
grain boundaries of the equiaxed grain structure's alloy matrix. The
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intermetallics discovered in dispersed form along grain boundaries

demonstrated the interfacial integrity between the matrix and reinforcement
phases. According to the mechanical characterisation, increasing the weight
percentage of Al2O3 in the hybrid reinforcement and the stress-relieving
process resulted in significant improvements in the mechanical properties of
the hybrid composites.

The reduced amount of micropores and microvoids after the stress-

relieving process contributed to a significant improvement in the mechanical
properties of the hybrid composites. A nano TiO2 particle in the hybrid
composite also assisted to activate the non-basal slip systems, thus the
samples underwent plastic deformation during tensile loading, resulting in
enhanced ductility of the composite. The fracture mechanism in hybrid
composites under various types of loading was also discussed. Superior
mechanical characteristics were found for stress-relieved alloys reinforced
with 2 wt.% hybrid Al2O3. Hence it shows an appealing potential for
overcoming Mg-based materials weak mechanical properties.

The corrosion study was carried out in two ways: immersion in Stimulated
Body Fluid (SBF) and electrochemical polarization. Both approaches implied
that the corrosion resistance of the generated Mg alloy and Mg hybrid
composites improved after the heat treatment process. When prepared alloys
and hybrid composites were compared, the hybrid composites had higher
mechanical strength and corrosion strength than the prepared alloys. This
study found that the hybrid composite's improved mechanical and corrosion
strength is a suitable metal for bio-medical applications and can be used in
structural applications.