Journal of Alloys and Compounds 345 (2002) 246–251 L

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Development of ductile magnesium composite materials using

titanium as reinforcement
S.F. Hassan, M. Gupta*
Department of Mechanical Engineering, The National University of Singapore, 10 Kent Ridge Crescent, 119260 Singapore
Received 7 January 2002; received in revised form 26 February 2002; accepted 26 February 2002

Abstract

In the present study, elemental and titanium particulate reinforced magnesium materials were synthesized using an innovative
disintegrated melt deposition technique followed by hot extrusion. Microstructural characterization of the composite samples showed
reasonably uniform distribution of titanium particulates in the matrix material, strong interfacial integrity of magnesium matrix with
titanium particulates, and the presence of minimal porosity. Physical property characterization revealed that addition of titanium as
reinforcement marginally improves the dimensional stability of pure magnesium. Tensile behavior characterization revealed that the
presence of titanium reinforcement led to an improvement of 0.2% yield strength and ductility while the UTS was adversely affected. An
attempt is made in the present study to correlate the effect of titanium as reinforcement and its increasing amounts with the
microstructural, physical and tensile properties of magnesium.
 2002 Elsevier Science B.V. All rights reserved.

Keywords: Alloys; Composite materials; Microstructure; Mechanical structures

1. Introduction hexagonal closed packed structure. The addition of harder

Magnesium based composites due to their inherently
low density and ensuing potential to exhibit high specific
mechanical properties are actively sought for weight-criti-
cal structural applications. Increasing demand for fuel
economy and lower level emissions in the automobile
industry has favorably increased the use of these materials
in recent years. A recent industrial review revealed that
there are 60 different types of components, from instru-
ment panels to engine components, in which magnesium is
used or is being developed for use. The use of magnesium
in automobile parts is predicted to increase globally at an
average rate of 15% per year [1]. Magnesium based
materials also exhibit good damping characteristics, di-
mensional stability, machinability, and low casting costs.
Despite these advantages, magnesium based composites
normally exhibit limited ductility at room temperature
[2,3], which bars them from many potential applications.
The limited ductility of magnesium may be attributed to its
*Corresponding author. Tel.: 165-874-6358; fax: 165-779-1459.
E-mail address: mpegm@nus.edu.sg (M. Gupta).
and stiffer ceramic phases such as SiC further adversely
affects the ductility [4]. It is well established that the end
properties of any given composite formulation depend
critically on the nature of reinforcement [5,6]. The results
of a search of the existing literature revealed that a number
of investigations have been conducted on ceramic re-
inforced magnesium and its alloys and the tensile testing
results reveal that the addition of ceramic reinforcement, in
common, reduces the UTS and ductility of the matrix
[4,7–9] and enhances the yield strength and elastic
modulus. The net effect of these variations is a significant
reduction in the work of fracture for the composite
formulation. The result of the literature search also re-
vealed that no study has been carried out to investigate the
effect of the addition of metallic reinforcement on the
expansivity and tensile behavior of the magnesium matrix.
Accordingly, the primary aim of the present work was to
synthesize titanium particulate reinforced magnesium
composite using an innovative disintegrated melt deposi-
tion technique followed by hot extrusion. The materials
thus synthesized were examined for microstructural, phys-
ical and tensile properties. Particular emphasis was placed

0925-8388 / 02 / $ – see front matter  2002 Elsevier Science B.V. All rights reserved.
PII: S0925-8388( 02 )00413-9
 S.F. Hassan, M. Gupta / Journal of Alloys and Compounds 345 (2002) 246–251
on correlating the effect of titanium as reinforcement with
the microstructural, thermal and tensile properties of pure
magnesium.
2. Experimental procedures
2.1. Materials
In this study, elemental magnesium turnings of .99.9%
purity were used as the base material and elemental
titanium particulates of 99% purity with 19610-mm size
range were used as reinforcement phase.
2.2. Processing
Synthesis of monolithic and reinforced magnesium
containing two different volume percentages of titanium
was conducted using the method of disintegrated melt
deposition (DMD) [10]. The synthesis of the composites
involved superheating the magnesium turnings with re-
inforcement particulates (placed in multi-layer sandwich
form) to 750 8C under Ar gas atmosphere in a graphite
crucible. Resistance heating furnace was used. The super-
heated slurry was stirred at 460 rpm for 8 min using a twin
blade (pitch 458) mild steel impeller to facilitate the
incorporation and uniform distribution of reinforcement
particulates in the metallic matrix. The impeller was coated
with ZIRTEX 25 (86% ZrO 2 , 8.8% Y 2 O 3 , 3.6% SiO 2 ,
1.2% K 2 O and Na 2 O and 0.3% trace inorganic) to avoid
iron contamination of the molten metal. The melt was then
released through a 10-mm diameter orifice at the base of
the crucible and disintegrated by two jets of argon gas,
orientated normal to the melt stream and located 265 mm
from the melt pouring point, and subsequently deposited
onto a metallic substrate located 500 mm from the
disintegration point. The argon gas flow rate was main-
tained at 25 l / min. Ingot of 40-mm diameter was obtained
following the deposition stage. The synthesis of monolithic
magnesium was carried out using steps similar to those
employed for the reinforced material except that no
reinforcement particulates were added. The ingots obtained
following the casting process were machined to a diameter
of 36 mm and then hot extruded at 350 8C employing an
extrusion ratio of 20.25:1.
2.3. Density measurements
Density measurements were performed on polished Mg
and Mg / Ti P samples taken from extruded rods using
Archimedes’ principle [10]. Samples were weighed using
A&D ER-182A electronic balance with an accuracy of
60.0001 g. Distilled water was used as the immersion
fluid.
247
2.4. Quantitative assessment of titanium
Retained Ti in extruded composite was determined by
the inductively plasma atomic emission method, using
three randomly selected samples. This method involved (a)
dissolving a known amount of sample in the nitric acid, (b)
atomizing the solution into plasma, and (c) analyzing the
plasma in the inductively coupled plasma spectrometer,
which detects the wavelength of Ti.
2.5. Microstructural characterization
Microstructural characterization studies were conducted
on metallographically polished extruded composite sam-
ples to investigate reinforcement distribution, interfacial
integrity between the matrix and reinforcement, and the
presence of porosity. JEOL JSM-5800 LV scanning elec-
tron microscope (SEM) equipped with energy dispersive
spectroscopy (EDS) was used. Digitizing the scanning
electron micrographs into binary image form followed by
cumulative image analysis using Quantimet 520 system
was applied on 15 micrographs to determine the volume
percentage of porosity in extruded composites.
2.6. X-ray diffraction studies
Extruded Mg and Mg / Ti P samples were exposed to Cu
Ka radiation ( l51.5418 A)˚ with a scan speed of 28 / min
on an automated Shimadzu LAB-X XRD-6000 diffrac-
tometer. The Bragg angles and the values of interplanar
spacing, d, obtained were subsequently matched with
standard values [11] for Mg, Ti, and other related phases.
2.7. Coefficient of thermal expansion
Coefficient of thermal expansion (CTE) of Mg and
Mg / Ti P materials was determined using an automated
SETARAM 92-16 / 18 thermomechanical analyzer. Dis-
placement of materials samples, each of 1062 mm in
length, was measured as a function of temperature (in the
range of 50–400 8C, 5 8C / min heating rate) using an
alumina probe under argon atmosphere (flow rate 1.2
l / min) to determine CTE.
2.8. Tensile behavior
The smooth bar tensile properties of the extruded Mg
and Mg / Ti P samples were determined in accordance with
ASTM test method E8M-96. The tensile tests were con-
ducted on round tension test specimens of diameter 5 mm
and gauge length 25 mm using Instron 8516 machine with
a crosshead speed set at 0.254 mm / min. The strain during
the tensile testing was recorded using Instron 2630-100
Series Clip-On type extensometer.
248 S.F. Hassan, M. Gupta / Journal of Alloys and Compounds 345 (2002) 246–251

Table 1
Density, X-ray diffraction studies and CTE measurement results for Mg and Mg / Ti P
Material Reinforcement Density (g / cm 3 ) Porosity Matching peaks CTE (310 26 / 8C)
(vol.%)
(wt.%) (vol.%) Mg Ti
Mg – – 1.73960.001 0.047 9[3] – 28.660.1
Mg / 5.6Ti P 5.6 2.2 1.81560.004 0.103 a 9[3] 1[1] 27.960.9
Mg / 9.6Ti P 9.6 4.0 1.89160.018 0.036 a 9[3] 2[2] 26.161.9
Numbers in square brackets indicate the number of main peaks matched.
a
Result of cumulative image analysis conducted on 15 representative SEM micrographs.

2.9. Fracture behavior 3.3. Quantitative assessment of titanium

Fracture surface characterization studies were carried
out on the fractured tensile samples to provide an insight
into the various possible fracture mechanisms operating
during the tensile loading of the samples using a JEOL
JSM-T330A SEM equipped with EDS.
Results of inductively coupled plasma spectrometer
showed successful retention of titanium in the extruded
composite matrices (Table 1).
3.4. Microstructural characterization

The distribution of titanium particulates, Ti P –Mg inter-

3. Results
3.1. Macrostructure
The result of macrostructural characterization conducted
on the as-deposited unreinforced and composite samples
did not reveal any presence of macropores or shrinkage
cavity. Following extrusion, there was also no evidence of
any macrostructural defects.
facial integrity and the presence of minimal porosity in the
extruded rod can be assessed from the scanning electron
micrograph shown in Fig. 1. Fig. 1b shows a typical
scanning electron micrograph illustrating Ti P –Mg interfa-
cial characteristics with EDS area and line maps.
3.5. X-ray diffraction studies
The X-ray diffraction results corresponding to the Mg
and Mg / Ti P samples are shown in Table 1.

3.6. Coefficient of thermal expansion

3.2. Density measurement
The results of the density and porosity measurements
(Table 1) indicate that near dense materials can be
obtained using the fabrication methodology adopted in the
present study.
The results of CTE measurements of extruded mono-
lithic and reinforced magnesium samples (Table 1) showed
a marginal improvement in dimensional stability of mag-
nesium matrix as a result of the presence of titanium
particulates.

Fig. 1. Representative SEM micrographs showing: (a) distribution of Ti P in Mg / 9.6Ti P and (b) the interfacial characteristics of Ti P –Mg interface with
area-map and line-map (refer to slanted black line) in the case of Mg / 5.6Ti P composite.
 S.F. Hassan, M. Gupta / Journal of Alloys and Compounds 345 (2002) 246–251 249

Table 2
Room temperature tensile properties
Materials Reinforcement 0.2% YS UTS Ductility Work of
(vol.%) (MPa) (MPa) (%) fracture (J / m 3 )a
Mg – 10064 258616 7.761.2 20.262.6
Mg / 5.6 Ti P 2.2 163612 24869 11.161.4 25.762.9
Mg / 9.6 Ti P 4.0 154610 23965 9.560.3 20.761.4
a
Determined from engineering stress–strain diagram using EXCEL software.

3.7. Tensile behavior predominance of fractured particulates and the occasional

The results of ambient temperature tensile tests revealed
that the ductility and 0.2% YS of magnesium were
significantly increased with the addition of titanium as
reinforcement (Table 2). The UTS of magnesium matrix,
however, was adversely affected with the presence and
increasing amounts of reinforcement.
3.8. Fracture behavior
Results of fractography, in common, reveal the cleavage
type of failure mode of the matrix (Fig. 2a and b), the
presence of debonded particulates (Fig. 2c and d).
4. Discussion
4.1. Synthesis of Mg and Mg /TiP
Synthesis of Mg and Mg / Ti P materials was successfully
accomplished by DMD process followed by hot extrusion.
Important features revealed in the present study are (a)
minimal oxidation of magnesium, (b) absence of macro-
pores and blowholes, and (c) no detectable reaction
between Mg or Mg / Ti P melts and the graphite crucible.

Fig. 2. Representative SEM micrographs taken from the tensile fracture surface of composites showing: (a) and (b) cleavage marks indicative of brittle
fracture in pure Mg and Mg / 9.6Ti P , respectively, (c) fractured particulates in the case of Mg / 5.6Ti P , and (d) Ti P –Mg interfacial debonding in the case of
Mg / 9.6Ti P (marked with arrow) composite.
250 S.F. Hassan, M. Gupta / Journal of Alloys and Compounds 345 (2002) 246–251
The inert atmospheric condition used during melt process-
ing, dispersion, deposition and solidification was in-
strumental in the prevention of reaction between air / oxy-
gen and Mg melt. The absence of macropores, blowholes,
and segregation or agglomeration of reinforcement par-
ticulates due to the effect of gravity indicates the suitability
of stirring conditions in the crucible and the realization of
good solidification conditions during deposition. The ab-
sence of reaction between Mg and Mg / Ti P with the
graphite crucible can be attributed to the inability of
temperature–time cycle used during DMD process to
trigger the reaction and also to the inability of magnesium
to form stable carbides [5]. The results, in essence, indicate
the feasibility of the DMD process as a potential fabrica-
tion technique for the Mg / Ti P metal matrix composites
(MMCs).
4.2. Microstructure
The results of the microstructural characterization
studies conducted on the extruded Mg / Ti p samples are
discussed in terms of (a) distribution of reinforcement, (b)
reinforcement–matrix interfacial characteristics, and (c) the
presence of porosity. The results of scanning electron
microscopy revealed a reasonably uniform distribution of
titanium. The reasonably uniform distribution of Ti par-
ticulates realized in the present study can be attributed to:
(a) limited agglomeration of reinforcement during melting
of matrix due to thin layered arrangement of raw materials
in crucible for melting, (b) minimal gravity-associated
segregation due to judicious selection of stirring parame-
ters which ensured uniform incorporation of Ti particulates
in matrix melt, (c) good wetting of reinforcement by the
matrix melt [12], and (d) disintegration of the composite
slurry by argon jets into droplets, and subsequent deposi-
tion in metallic mold. The microstructural characterization
result, however, still revealed a lot of scope for further
improving the distribution of Ti P in the Mg matrix (Fig.
1a). XRD results indicated the absence of any reaction
between reinforcement particulates and the magnesium
melt (Table 1). These findings are consistent with those
reported elsewhere [13]. The results of microstructural
characterization of composite material also revealed a near
defect free interface formed between reinforcement and
matrix (Fig. 1). The interfacial integrity was assessed in
terms of interfacial debonding and presence of microvoids
at the particulate–matrix interface. The results of scanning
electron microscopy also revealed extremely limited mutu-
al solubility between Ti P and Mg matrix during processing,
which is supported by EDS area mapping and line scan-
ning analysis (Fig. 1b). The presence of minimal porosity
in Mg / Ti P composite material (Table 1) can be attributed
to: (a) good compatibility between Ti P and Mg [12], and
(b) the use of an appropriate extrusion ratio. It has been
established convincingly in earlier studies that an extrusion
ratio even as low as 12:1 can nearly close the micrometer-
size porosity associated with as-solidified metal-based
materials [5,10].
4.3. Coefficient of thermal expansion
The results of CTE measurements in the temperature
range of 50–400 8C revealed that the presence and an
increasing percentage of titanium reduces the CTE value of
magnesium matrix (Table 1). This can be attributed to: (a)
lower coefficient of thermal expansion of titanium (27.03
10 26 / 8C and 9.1310 26 / 8C for Mg and Ti [14], respective-
ly), (b) uniform distribution of reinforcement particulates,
and (c) good interfacial integrity between reinforcement
and matrix. The results obtained in the present study
indicate the feasibility of using titanium particulates in
enhancing the dimensional stability of magnesium matrix.
4.4. Tensile behavior
The results of tensile behavior studies revealed that there
was a significant increase in 0.2% YS as a result of the
presence of titanium as reinforcement. This can be attribu-
ted to: (a) the presence of high dislocation density in
matrix due to the large difference of coefficient of thermal
expansion between matrix and reinforced materials (27.03
10 26 / 8C and 9.1310 26 / 8C for Mg and Ti [14], respective-
ly), and (b) the presence of well-bonded strong rein-
forcement particulates (the elastic modulus and yield
strength of Ti P are 102.2 GPa [14] and 586 MPa [16],
respectively, compared to 44.7 GPa and 100 MPa [14] for
Mg). In general, the yield stress of material is the stress
required to operate dislocation sources and is governed by
the presence and magnitude of all the obstacles that restrict
the motion of dislocation in the matrix [15]. Under the
applied stress, the high density of dislocation required
higher initial stress to operate the dislocation and the
presence of strong second phase further restricts the
initiation of motion of dislocation in the matrix to increase
the 0.2% YS [7,15]. The results obtained in the present
study clearly reveal that the presence of titanium par-
ticulates within the limit of 9.6 wt.% serves the two roles
mentioned above thereby increasing the resistance of
material towards deformation up to a strain level of 0.002.
As the applied tensile load increases beyond yield point, a
strong internal stress identical to that of elastic range is
developed between titanium particulates and magnesium
matrix and increases to a certain level that initiates local
damage, i.e. particle cracking (Fig. 2c), matrix cracking,
and interface debonding (Fig. 2d). The onset of this
localized damage relaxes the internal stress around the Ti
particulates and their coalescence leads to the final fracture
of the composites. Absence of this localized damage in
unreinforced magnesium is believed to be the reason for
higher UTS when compared with the reinforced compos-
ites (Table 2). However, the results of tensile property
characterization revealed that the ductility of composite
 S.F. Hassan, M. Gupta / Journal of Alloys and Compounds 345 (2002) 246–251
materials was notably increased when compared to that of
pure magnesium (Table 2). Increase in ductility of the two
composites is thought to be related to the softening of
magnesium matrix due to diffusional dissolution of Ti
[17]. The work of fracture computed using stress–strain
diagram reveals that Mg–Ti P composite with 5.6 wt.% of
titanium is distinctly superior when compared to unrein-
forced magnesium. In the case of Mg / 9.6Ti P composite,
work of fracture was found to be similar to that of Mg
indicating that the presence of Ti P does not adversely
affect the fracture resistance of magnesium. In essence, the
results of tensile testing revealed that titanium can be used
as reinforcement in magnesium for the development of
materials for strength based designs (higher yield strength
when compared to magnesium) and damage tolerant
designs (similar or higher work of fracture when compared
to magnesium).
4.5. Fracture behavior
The results of fracture analysis revealed typical brittle
fracture in the case of Mg and its composite samples (Fig.
2). This can be attributed to the HCP crystal structure of
Mg that restricts the slip to the basal plane. The presence
of small steps and microscopically rough fracture surface
indicates the inability of magnesium to cleave on any
single plane. These findings are consistent with those
reported elsewhere [4,18]. The presence of broken Ti
particulates (Fig. 2c) is indicative of strong interfacial
bond realized between the Ti particulates and the mag-
nesium matrix due to good wetting phenomenon ex-
perienced in the present experimental methodology. How-
ever, debonded titanium particulates were also observed
occasionally on the fracture surface of the composite
samples (Fig. 2d).
5. Conclusions
(1) Disintegrated melt deposition technique coupled
with hot extrusion can be used to synthesize elemental
titanium reinforced magnesium composites.
(2) The reasonably uniform distribution of Ti particu-
lates, strong Ti P –Mg interfacial integrity and the presence
of minimal porosity in the composite microstructure
indicate the suitability of primary processing and sec-
ondary processing parameters used in the present study.
251
(3) Results of coefficient of thermal expansion measure-
ment indicate that the increasing presence of titanium is
able to marginally improve the dimensional stability of
pure magnesium.
(4) The results of mechanical characterization revealed
that the presence of titanium in magnesium matrix lead to
an improvement in 0.2% YS and ductility while the UTS
was marginally lowered.
(5) The results of fracture surface characterization of
Mg / Ti P composites revealed that particle breakage was the
dominating reinforcement-associated failure mechanism
under tensile loading.
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