MECHANICAL PERFORMANCE OF MAGNESIUM …...powder metallurgy using micro-alumina (3%) and varying...

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International Journal of Civil Engineering and Technology (IJCIET)

Volume 8, Issue 8, August 2017, pp. 365–378, Article ID: IJCIET_08_08_037

Available online at http://http://www.iaeme.com/ijciet/issues.asp?JType=IJCIET&VType=8&IType=8

ISSN Print: 0976-6308 and ISSN Online: 0976-6316

© IAEME Publication Scopus Indexed

MECHANICAL PERFORMANCE OF

MAGNESIUM COMPOSITES CONTAINING

HYBRID Al2O3 REINFORCEMENT

E Suneesh

Department of Mechanical Engineering,

Noorul Islam University, Kumaracoil, Tamilnadu, India

M Sivapragash

Faculty of Mechanical Engineering,

V.V College of Engineering, Tisaiyanvilai, Tamilnadu, India

ABSTRACT

Improved ductile properties are recently reported in the magnesium composites

reinforced with nano-particulates. However, nanocluster formation, stress

concentration, and insufficient wet ability restrict the further development of such

composites. The present study investigates the feasibility and effect of using hybrid

reinforcements for synthesizing magnesium MMCs. Composites were prepared via

powder metallurgy using micro-alumina (3%) and varying amounts of nano-Al2O3

(0.5 wt. % & 1 wt. %) powders as hybrid reinforcements and Mg-3Zn-0.7Zr-1Cu alloy

as the base matrix. The properties of the extruded samples were examined by

conducting metallurgical and mechanical characterization studies. A comparative

study of the obtained results was done with micro Al2O3 alone reinforced composite.

Results revealed that hybrid composites with 1 % nano Al2O3 had superior properties

than micro Al2O3 composite. Reasonably well distributed hybrid reinforcements were

also noticed in the metallurgical examination. Hence, the current research suggests

the addition of hybrid reinforcements as a means for improving the overall properties

of magnesium based materials.

Key words: Ductile properties, magnesium composites, nano-particulates, hybrid

reinforcements, metallurgical and mechanical properties.

Cite this Article: E Suneesh, M Sivapragash, Mechanical Performance of Magnesium

Composites Containing Hybrid Al2O3 Reinforcement. International Journal of Civil

Engineering and Technology, 8(8), 2017, pp. 365–378.

http://www.iaeme.com/IJCIET/issues.asp?JType=IJCIET&VType=8&IType=8

1. INTRODUCTION

For the past few decades, researchers had put forth enormous attempts in developing

lightweight materials. Lightweight materials gained much attention in the transportation

industry due to their remarkable energy saving properties. Though aluminum and its alloys

E Suneesh, M Sivapragash


showed signs of future lightweight materials, as a result of global inclination towards the

green environment and significant weight saving properties, magnesium-based materials

received greater acceptance in the modern era [1]. Apart from the lightness, other exceptional

properties of magnesium include easiness for casting, machining, and outstanding damping

capacity [2-3]. Still, magnesium in its pure form is not widely used for many structural

applications considering their insufficient corrosion resistance, poor ductility and inability to

retain high-temperature strength [4-5]. Hence, Mg alloys and composites (Mg-MMCs) are

often prepared through the deliberate inclusion of different alloying elements and

reinforcements to cope up with the desired properties for various applications [1, 6].

Previous studies conducted on Mg-based materials discovered that numerous alloying

elements (Al, Cu, Zn etc.) are accessible to further enhance the properties of magnesium.

Since aluminum had the most favourable influence on magnesium, magnesium-aluminium

alloy composition (AZ series) became more popular among the commercially available

alloys. Copper is also reported to be a potential alloying element which improves the strength

properties. Moreover, AZ alloy series (especially AZ31, AZ61 and AZ91) have found

widespread usage in lightweight and structural applications. Due to the presence of thermally

unstable Mg17Al12 phase, AZ alloys exhibit inadequate high temperatures properties thereby

limiting their industrial applications [7-8]. On a contradictory to the limitations of magnesium

alloys, the availability of different processing methodologies and flexibility in selecting

appropriate reinforcement materials triggers enormous research efforts on magnesium matrix

composites (Mg-MMCs) [9-10]. Literature studies on synthesis of the composite materials

proposed that apart from conventional reinforcements added in micron-level, nano

particulates when mixed with magnesium can also upgrade its high-temperature properties.

Precisely, the addition of nano-alumina is found to be good in yielding excellent mechanical

properties including tensile strength, ductility etc. both at the room as well as elevated

temperatures [9, 11-12]. Nevertheless, poor wettability, lower densities due to clustering of

nanoparticles and stress concentration due to agglomeration, are reported in nano composites

resulting in a significant crack formation [13-15]. This initiates the need for developing

advanced subsidiary reinforcements and in accordance with the recent studies conducted,

hybrid reinforcements were suggested as an efficient competent. Available literature reveals

that a little attempt has been made so far to fabricate Mg-based composites by the

simultaneous incorporation of micro and nano particulate (hybrid) reinforcements in an

economical manner.

Based on the above motivation, an attempt is made in the present research to develop a

magnesium-based composite using hybrid alumina reinforcements (micro Al2O3 + nano

Al2O3). Since the characteristics of Mg-MMCs based on AZ series alloys has been reported

widely, a new magnesium alloy (Mg-3Zn-0.7Zr-1Cu) having Cu as a potential alloying

element was employed as the matrix material. Blend-press-sinter based powder metallurgy

followed by hot extrusion was used for fabricating the composite. Extruded samples were

subsequently characterized for investigating their metallurgical and mechanical properties.

The current work primarily aims at investigating the effects of hybrid reinforcement and the

varying amounts of nano Al2O3 on the structural behaviour of the composites developed. In

addition, a comparative study between mechanical and metallurgical characteristics of micro

alumina alone and hybrid alumina (micro Al2O3 + nano Al2O3) reinforced magnesium

composites was conducted in this research. For the comparative analysis, micro Al2O3 alone

reinforced Mg-3Zn-0.7Zr-1Cu alloy composite was prepared prior to the fabrication of the

hybrid composite.

Mechanical Performance of Magnesium Composites Containing Hybrid Al2O3 Reinforcement


2. EXPERIMENTAL PROCEDURES

2.1. Materials

Magnesium-Zinc-Zirconium alloy with copper inclusion (Mg-3Zn-0.7Zr-1Cu) was identified

as the matrix material and the matrix composition includes 95.3 wt. % of Mg, 3 wt. % of Zn,

0.7 wt. % of Zr and 1wt. % of Cu. Metallic powders for the matrix composition were acquired

from MEPCO Metal Powder Company, India (Mg, Zn & Cu) and Tritrust Industrial, China

(Zr). Multi-sized alumina particles (micro and nano size) were used as reinforcement

materials. Micro alumina was procured from Alfa Aesar, USA (size 20-50 μm and purity:

99.9%). For making the hybrid reinforcements, nano alumina powders were prepared using a

planetary ball milling machine with a ball-to-powder ratio of 3:1 and milling speed of 200

rpm.

2.2. Processing

Blend-press-sinter powder metallurgy process followed by hot extrusion was employed for

the fabrication purpose. Hybrid composites were fabricated by simultaneously reinforcing the

Mg-3Zn-0.7Zr-1Cu base matrix with different weight ratios of micro and nano alumina

particles as shown in Table 1.

Table 1 Composition of composites

Designation Title

Composition (wt. %)

Base alloy Al2O3

Micron Nano

Mg-3Zn-0.7Zr-1Cu/Al2O3 A 97 3 0

Mg-3Zn-0.7Zr-1Cu/Al2O3 B 96.5 3 0.5

Mg-3Zn-0.7Zr-1Cu/Al2O3 C 96 3 1

Atomized powders of Mg (Size: 50-65 μm, Purity: 97%), Zn (Size: 45-75 μm, Purity:

97.5%), Zr (Size: 50 mesh, Purity: 99.5%) and Cu (Size: 45-75 μm, Purity: 99%) were

initially weighed and mixed with the micro/hybrid alumina reinforcements during the

blending process. Proper quality mixtures were achieved by blending them in a mechanical

alloying machine for 1-hour duration at a speed of 200 rpm. Powder compaction involves

compacting the metal powders with high pressure using a dedicated die and punch setup.

Cylindrical samples used for the different characterization studies were obtained by the

compaction process. Compacts were prepared in a 150-ton hydraulic press at a pressure of 50

to 60 N/m2 using a suitable punch and die assembly as shown in Fig. 1 (a & b). As the density

of the compacted powder is proportional to the pressure applied, pressure is maintained

constant throughout the compaction process. Billets (Fig. 1 (e)) having 65 mm diameter and

35 mm length were obtained after the compaction process which aree used for the further

processing. Compacted samples are sintered in an electric muffle furnace (Fig. 1 (c)) at 400ºC

for a period of 1 hour. Samples (Fig. 1 (f)) are then allowed to be cooled to the room

temperature in the furnace itself. In order to reduce the tendency of magnesium-oxygen

reaction inside the furnace, compacted specimens were wrapped with aluminium foil prior to

the sintering process.



Figure 1 Images of the experimental procedure (a) Schematic image of hydraulic press (b) Punch and

die for compaction (c) Sintering (d) Hot extrusion and (e), (f), (g) & (h) Samples obtained after

compaction, sintering and extrusion respectively

Secondary processing involves hot extrusion of the sintered billets and subsequent heat

treatment process. Hot extrusion was carried out at a temperature of 400ºC in a hydraulic

press using an extrusion ratio 25:1 (Fig. 1 (d)). In order to avoid unwanted sticking of the

sintered samples to the die and facilitate a smooth extrusion process, colloidal graphite was

used as the lubricant. Extruded rods (Fig. 1 (h)) measures about 12.5 mm diameter and 500-

800 mm length. These rods were then subsequently stress relieved at 260°C for 15 minutes in

a muffle furnace [16] and sent for further characterization. For conducting the comparative

analysis, micro alumina alone reinforced composite was also prepared using the same

fabrication technique.

2.3. Density and Porosity Measurements

Experimental density values of the samples were determined using Archimedes’ principle.

Three randomly selected polished samples were used for evaluating the experimental density

and their weights were recorded initially in the air and then in distilled water using an

accurate electronic balance. Theoretical densities and porosity values of the samples were

calculated using rule-of-mixture principle.

2.4. Metallurgical Characterization

Polished samples were used for metallurgical studies in order to investigate the morphological

characteristics of grains, distribution of reinforcement, interfacial integrity between matrix

and reinforcements and distribution of secondary phases. Polished samples for the analysis

were prepared according to the standard metallographic procedures as followed in the

previous studies. A standard solution containing 70ml ethanol (95%), 10ml acetic acid, 10 ml

distilled water and 0.4 g picric acid was used as the etchant to reveal the detailed

microstructure of the surface layer [17-18]. ZEISS EVO 18 Scanning electron microscope

equipped with Quantax 200 with X-Flash – Bruker energy dispersive X-ray spectroscope was

used for the structural and elemental analysis of the hybrid composites whereas JEOL (JSM -

6390LV) Scanning electron microscope was utilized for the characterization of the micro

alumina composite.



2.5. XRD Studies

X-ray diffraction (XRD) analysis was carried out on the powdered composite samples with

micro and hybrid reinforcements for identifying the different phases present. Reinforcement-

matrix reaction and the presence of secondary phases were investigated using a

PANALYTICAL X’PERT Pro Powder X’Celerator Diffractometer. The powdered samples

were exposed to a Cu-Kα1 (λ=1.5406 Aº) radiation with an applied voltage of 40 kV and a

beam current of 30 mA. The XRD spectrum was acquired from 10 to 80º 2θ at a 0.017º step

size.

2.6. Mechanical Characterization

The mechanical characterization tests such as measurement of tensile and hardness properties

were conducted on the samples. Polished sintered samples were used for evaluating micro

hardness values. Each sample tested had an average dimension of 12 mm diameter and 8 mm

thickness. Micro hardness measurements were taken using an SIOMM HVD-1000MP digital

micro hardness tester equipped with a Vickers diamond indenter as shown in Fig. 2 (a, b &

c).The test was conducted under an applied load of 500 gf, an included angle of 136º and with

a dwell time of 15 s. Hardness values were taken at five different locations and average values

were computed. The test was conducted according to ASTM standard E384-16 and readings

were taken at room temperature [20].

Figure 2 Vickers micro hardness measurement (a) Specimen loaded under Vickers diamond indenter,

(b) Vickers micro hardness test conditions and (c) indentation measurement [19]

For evaluating the tensile properties of the composite specimens, tensile tests were

conducted at room temperature using a ‘DAK UTB9103’ automated mechanical testing

machine with a crosshead speed of 0.25 mm/min. Round specimens were used and the

samples were prepared in accordance with respective ASTM standard E8 [21]. The tensile

samples measures around 5mm diameter and 25mm gauge length (Fig. 3 (a)). The fracture

behaviour of the samples failed under tension was studied using a JEOL (JSM - 6390LV)

Scanning electron microscope.

3. RESULTS AND DISCUSSIONS

The hybrid magnesium composites containing two different length scales of alumina

(microand nano) reinforcements was successfully synthesized using blend-press-sinter

powder metallurgy technique followed by hot extrusion.



3.1. Density and Porosity Results

The experimental and theoretical densities along with the calculated porosity values are listed

in the Table. 2.

Table 2 Density and porosity values of fabricated composites

Sl No Material Theoretical

density (g/cc)

Experimental

density (g/cc) Porosity (%)

1 Composite A 1.8346 1.8289 ± 0.0026 0.31 ± 0.006

2 Composite B 1.8392 1.8321 ± 0.009 0.38 ± 0.006

3 Composite C 1.8442 1.8346 ± 0.0012 0.52 ± 0.001

Experimental density values are found to be very close to the theoretical values. The effect

of nano alumina percentage on the density of the different composite samples can be observed

from Fig. 4 (a). Results revealed that density of hybrid composites is higher than that of micro

alumina alone reinforced composite. Improved density values are essential for composites to

have distinctive properties. Also, a slight increase in density was observed in hybrid

composites with an increase in wt. % of nano alumina. Relatively higher densities of added

constituents such as alumina, Zn, Zr, Cu etc. and grain refinement may be the reason for the

improved density values. Slight amount of porosity (Table. 2) observed in the newly made

composites may be due to (i) entrapment of gases during the blending process (ii) evolution of

hydrogen, and (iii) shrinkage of the composite during its solidification after the secondary

processing [22-24]. Resulting porosity values were reported to be minimum for Mg-3Zn-

0.7Zr-1Cu alloy as shown Fig. 4 (b). The obtained density and porosity results were

comparable with that of pure Mg and Mg alloys and this confirms the successful

incorporation of powder metallurgy process for producing magnesium based near dense

hybrid nano-composites [8].

Figure 4 Effect of nano-alumina wt. % on (a) Density and (b) Porosity of the composite samples.

3.2. Metallurgical Studies

3.2.1. SEM Analysis

The results of microstructural characterization studies conducted on the composite samples

with micro and hybrid reinforcements are shown in Figs. 5 and 6 respectively. Fairly uniform

distribution of micro alumina particles with some micro pores can be observed from Fig. 5.

1.825

1.83

1.835

1.84

1.845

1.85

0 0.5 1 1.5

Den

sity

(g/

cm3)

Wt.% of nano alumina (a)

0.15

0.25

0.35

0.45

0.55

0 0.5 1 1.5

Po

rosi

ty (

%)

Wt.% of nano alumina (b)



Figure 5 SEM micrographs of Mg-3Zn-0.7Zr-1Cu + 3% micro Al2O3 composite.

The representative SEM micrographs shown in Fig. 6 (a &b) revealed that micro and nano

Al2O3 particles were distributed well enough with limited porosity in the hybrid composites.

This homogenous distribution of the reinforcements is quite essential for a composite to have

unique properties. Resultant composite structure with finely sized grain particles could be

possibly attributed to the presence of fewer segregation problems and efficient ball milling,

extrusion & sintering process. High extrusion ratio can also result in uniform distribution of

grains as reported in the previous studies [25-26]. Fig. 6 (c&b) shows the magnified images of

the SEM analysis for understanding the distribution of nano-particles. It shows that as-

received micro alumina particles were was broken down, flattened and their edges were round

off due to the loading and flattening effect of ball milling process [27]. Some amount of

clustered nano Al2O3 particles can be observed as shown in Fig. 6 (d) in the 1% nano Al2O3

reinforced hybrid composite. Particle pulls out during grinding and polishing may be the

cause for the clustering of the reinforcements [28]. However, clustering of micron Al2O3

particles was not evident in the single reinforcement composite. Available magnifications of

the SEM were not enough to detect the nature of interfacial integrity between matrix and

reinforcement.

Figure 6 SEM micrographs showing distribution of reinforcements in (a) Composite B (b) Composite

C and (c & d) high magnification images of (a) &(b).



3.2.2. EDAX Analysis

EDAX profiles of the hybrid composites are portrayed in Fig. 7 (a & b). Profiles taken

revealed the presence of Mg, Al, Cu, Zn and oxygen peaks in the EDAX spectrum. Thus it

was clear that the added constituents are well preserved even after the powder metallurgy

process. Due to the lower weight fraction in the hybrid composite, Zr peaks were not obtained

from the EDAX analysis. The observed N peaks may be due to the presence of undisposed

remains from the applied etchant during the SEM analysis. Similar observation was also

observed from Fig. 7 (b).Oxygen and aluminium were found to be rich in the matrix

proposing the considerable distribution of micro and nano alumina particles.

So after the detailed metallurgical studies conducted on the extruded micro and hybrid

alumina composite samples, we can presume that the blend-press-sinter powder metallurgy

process appeared to be a successful method for incorporating of alumina particles into the

Mg-3Zn-0.7Zr-1Cu alloy matrix.

Figure 7 EDAX profiles of (a) Composite A and (b) Composite B.

3.3. XRD Results

Figure 8 X-ray diffraction patterns for the as-extruded composite specimens (A) Micro alumina

composite, (B) Hybrid composite B and (C) Hybrid composite C.

Diffraction patterns obtained from the XRD studies conducted on the micro and hybrid

composites were detailed in the Fig. 8 (a, b & c). The XRD diffractograms revealed the

presence of Mg and Al2O3 phases in the composites. In addition to the above two phases,

secondary phases such Cu2Mg, Cu5Zn8 and one ternary phase Al0.93Cu1.07Mg was also



observed. None of the zirconium peaks was detected for both micro and hybrid alumina

composites. Results of XRD analysis confirms the presence of dispersed phases of precipitate

components in the matrix phase.

3.4. Mechanical Responses

3.4.1. Microhardness

The results of room temperature micro hardness tests are presented in Table. 3 and Fig. 9.

Micro hardness of the hybrid composites is found to be superior when compared to micro

alumina alone reinforced composite. Micro hardness values are also seen to be increased with

increase in nano alumina content as shown in Fig. 9. Improved micro hardness values could

be possibly attributed to the presence of hard ceramic particles, minimal porosity, reduction in

grain size and restriction offered by the hard einforcement particles to the localized matrix

deformation during indentation [29-30].

Figure 9 Effect of nano-alumina wt. % on the mcrohardness of the composite samples.

3.4.2. Tensile Properties

The results of the room temperature tension test as shown in the Table. 3 revealed that the

hybrid reinforcements can enable increments in the 0.2% yield strength (YS) and ultimate

tensile strength (UTS) of the composites formed. Superior tensile strength properties were

noticed for hybrid composites containing 0.5% nano-alumina in comparison with micro

alumina composites. Based on the previous studies, it is evident that improvement in strength

properties of magnesium-based materials depends on the simultaneous action of several

mechanisms rather than a single unique mechanism. Henceforth, in the present work,

significant increase in tensile properties of Mg-MMCs with the addition micro and nano-

alumina particulates can be the result of the following mechanisms.

Grain refinement and reasonably well-distributed reinforcement particulates.

Interaction between the hard oxide particles finely dispersed within the grain and the moving

dislocations (orowan strengthening mechanism) [31-33],

Interaction between the grain boundary and moving dislocations (hall–petch strengthening

mechanism) and

Increased dislocation density due to the thermal property mismatch between the reinforcement

and matrix in the nanocomposite (increased dislocation density strengthening) [31, 34-35].

96

98

100

102

104

106

108

0 0.5 1 1.5

Mic

ro h

ard

nes

s (H

V)

Wt.% of nano alumina



Table 3 Results of room temperature hardness and tension tests

Material

Reinforcement

Vol. % Micro-

hardness

(HV)

Tensile YS

(Mpa)

UTS

(Mpa)

Failure

strain

(%) Nano Micro

Composite A ... 3 93 ± 3 154 ± 8 214 ± 7 4.5 ± 1.8

Composite B 0.5 3 102 ± 3 159 ± 4 232 ± 5 6.5 ± 1.8

Composite C 1 3 106 ± 2 141 ± 4 200 ± 8 3.5 ± 1.4

Mg/Al2O3a 0.5 4.5 57 ± 1 139 ± 27 187 ± 28 1.9 ± 0.2

Mg/Al2O3a 0.75 4.25 87 ± 1 138 ± 13 189 ± 15 2.4 ± 0.1

Mg/Al2O3a 1 4 74 ± 1 157 ± 20 211 ± 21 3.0 ± 0.3

a Wong, W. L. E., S. Karthik, and M. Gupta (2005) [36]

Excellent ductility of Mg-3Zn-0.7Zr-1Cu matrix as observed with the addition of micro

and nano-Al2O3 (0.5%) reinforcement particles could be the result of homogeneous

distribution of fine Al2O3 particles in the matrix, reduction in grain size and non-basal slip

activation [34, 37]. Stress-strain curves for composite specimens are plotted in Fig. 10 and it

is observed that maximum tensile elongation is obtained for the hybrid composite containing

0.5 % of nano alumina. However, the tensile properties decreases when the nano-alumina

content was increased to 1%. This could be possibly due to the clustering of alumina particles

as observed in the SEM micrographs and the considerable porosity as observed in the table. 2.

Figure 10 Stress-strain curves for composite specimens containing micro and hybrid reinforcements

3.4.3. Fracture Behaviour

The microscopic fracture surfaces of the tension test failed samples are shown in Fig. 11 (a, b

& c). The presence of micro cracks and their propagation through the matrix can be easily

detected from the fractographs. It is also revealed that mixed mode of failure occurs in both

micro and hybrid reinforcement composites rather than brittle mode as observed in pure Mg

with the presence of dimples and micro cracks indicating a plastic deformation at the

microscopic level. In addition, the presence of fine micro cracks can be responsible for the

increased yield and tensile strength properties of the hybrid composites [38].



Figure 11 Representative SEM fractographs of tensile failure (a, b & c) of the composite specimens

4. CONCLUSIONS

Based on the current study focused on understanding the influence of hybrid reinforcements

on mechanical and metallurgical behavior of the Mg-3Zn-0.7Zr-1Cu alloy, the following

conclusions can be made.

Magnesium composite with hybrid reinforcements (micro and nano Al2O3) can be successfully

synthesised using blend-press-sinter powder metallurgy technique.

Reasonably uniform distribution of micro and nano alumina particles with a limited porosity

are observed in both micro alumina and hybrid reinforcement composites.

SEM studies revealed clustering of nano Al2O3 particles in the 1 % nano Al2O3 reinforced

hybrid composite owing to the particle realignment during grinding and polishing.

The experimental density and porosity values are comparable with that of pure Mg and Mg

alloys and confirmed the successful incorporation of powder metallurgy process for producing

magnesium based near dense nano-composites.

Effectiveness of hybrid reinforcements are clearly indicated by the significant improvement in

mechanical properties such as hardness and tensile properties of the hybrid composite

samples.

However, the tensile properties decreases when the nano-alumina content was increased to

1%. This could be possibly due to the clustering of alumina particles and the presence of

considerable porosity in the composite samples.

ACKNOWLEDGEMENTS

Authors wish to acknowledge Mechanical Department of Noorul Islam University

(Kumarcoil, Tamil Nadu) for providing necessary assistance and support while conducting the

research.

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