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Acta Materialia 55 (2007) 63386344

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Enhancing strength and ductility of magnesium by integrating


it with aluminum nanoparticles
X.L. Zhong, W.L.E. Wong, M. Gupta

Department of Mechanical Engineering, National University of Singapore, 9 Engineering Drive 1, Singapore 117576, Singapore
Received 30 May 2007; received in revised form 18 July 2007; accepted 18 July 2007
Available online 12 September 2007

Abstract
Nano-size aluminum powder (Alp) reinforced magnesium composites were successfully synthesized using a powder metallurgy technique. Microstructural characterization of the materials revealed fairly uniform distribution of reinforcement. Mechanical properties
characterization revealed that the presence of aluminum nanoparticles 61 vol.% leads to an increase in hardness, 0.2% yield strength
and ultimate tensile strength of magnesium. The average ductility of the composites was higher when compared with pure magnesium
60.75 vol.% and decreased thereafter. An attempt was made in the present study to correlate the presence of nano-size aluminum reinforcement particles and their increasing number with the microstructural, physical and mechanical properties of magnesium.
 2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Keywords: Powder consolidation; Transmission electron microscopy; Metal matrix composites; Magnesium; Mechanical properties

1. Introduction
Magnesium-based materials are being actively pursued
for weight-saving applications owing to their low density
and high specic mechanical properties. High demand for
energy saving has led to extensive research on lightweight
materials, as conventional materials are no longer able to
meet the requirements of aerospace and automobile industries. In electronic and communication industries, lightweight metals are used in applications as replacements
for plastics [1,2]. Growing demand from the electronic,
aerospace and automobile industries has signicantly
fueled research activities in recent years for their further
development [25]. Advantages of magnesium include high
specic mechanical properties, high dimensional stability,
high thermal conductivity, superior damping characteris-

Corresponding author. Tel.: +65 65166358.


E-mail address: mpegm@nus.edu.sg (M. Gupta).

tics, good machinability, good electromagnetic shielding


characteristics and recyclability. The limitation of magnesium includes its low elastic modulus, rapid loss of strength
with increase in service temperature, poor creep resistance
and poor ductility. These limitations are often circumvented by using stier and stronger reinforcements based
on ceramic and metallic materials [69]. However, the
addition of ceramic reinforcements on a micron scale
usually deteriorates the intrinsic limited ductility of magnesium without reasonable improvement in strength
[3,68]. In recent studies, it has been observed that the
addition of nano-size reinforcements such as ceramic oxides, SiC and carbon nanotubes can lead to a simultaneous
increase in the strength and ductility of magnesium [1012].
No studies have been carried out to develop and investigate magnesium reinforced with nano-size aluminum
particulates.
Accordingly, the primary aim of this study was to synthesize magnesium-based composite materials containing
nano-size aluminum particulates using a powder metallurgy technique and to study the eect of volume fraction
of reinforcement on the properties of the composites.

1359-6454/$30.00  2007 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.actamat.2007.07.039

X.L. Zhong et al. / Acta Materialia 55 (2007) 63386344

6339

2. Experimental procedures

2.6. X-ray diraction

2.1. Materials
Pure magnesium powder of 98.5% purity with a size
range of 60300 lm (Merck, Germany) was used as the
matrix material. Aluminum powder 18 nm in mean size
(Nanostructured & Amorphous Materials Inc., USA) was
used as the reinforcement. The amount of nano-size Al particulates (Alp) was varied from 0.25 to 1 vol.%.

X-ray diraction (XRD) analysis was carried out on the


polished samples of extruded monolithic Mg and Mg/Alp
composites using an automated Shimadzu XRD-6000 diffractometer. The samples were exposed to Cu Ka radiation
) at a scanning speed of 2 min1. The Bragg
(k = 1.54056 A
angle and the values of the interplanar spacing d obtained
were subsequently matched with the standard values for
Mg, Al and other related phases.

2.2. Primary processing

2.7. Mechanical behavior

Monolithic magnesium and magnesium nanocomposites


(Mg/Alp) were synthesized using a powder metallurgy technique. Four dierent volume percentages (0.25, 0.5, 0.75
and 1) of aluminum powder were blended with magnesium
powder for 5 h at a speed of 50 rpm using a V-blender. The
blended powders were uniaxially compacted using a pressure of 97 bar (50 tons) on 35-mm-diameter ingots with
a height of 40 mm. Colloidal graphite was used as a lubricant. The compacted ingots were then sintered using a
Carbolite tube furnace at 500 C for 2 h in an inert argon
atmosphere. Pure magnesium was compacted and sintered
using the same parameters as the composite formulations
for comparison purposes.

The mechanical behavior of monolithic and composite


samples was assessed in terms of hardness and tensile properties. Hardness measurements were performed on the polished Mg and Mg/Alp samples. Hardness was measured on
the Rockwell 15T Supercial Scale using a 1.58 mm (1/
16 in.) steel ball indenter with test load of 15 kgf and dwell
time of 2 s. Hardness measurement was carried out using a
Future-Tech FR-3 Rockwell Type Hardness Tester in
accordance with ASTM standard E18-02.
Tensile tests were conducted on round tension test specimens 5 mm in diameter and with a 25 mm gauge length
using an automated servohydraulic testing machine (MTS
810) with a crosshead speed set at 0.254 mm min1. The
tensile properties of the monolithic magnesium and composite materials were determined in accordance with
ASTM standard E8M-01. A clip-on type extensometer
was used for strain recording.

2.3. Secondary processing


The sintered compacts of pure magnesium and its composites were soaked at 400 C for 1 h in a constant temperature furnace followed by hot extrusion at 350 C using a
150 ton hydraulic press. An extrusion ratio of 25:1 was
used to produce extruded rods 7 mm in diameter.
2.4. Density measurements
The densities of the extruded samples were determined
in accordance with Archimedes principle [9]. Three polished samples randomly selected from each extruded composite formulation were weighed in air and when immersed
in distilled water, using an A&D ER-182A electronic balance with an accuracy of 0.0001 g. The theoretical densities of the samples were calculated using rule-of-mixture.
2.5. Microstructural characterization
Microstructural characterization studies were conducted
on polished specimens of pure magnesium and its composite formulations in the extruded condition to investigate the
presence of porosity, grain size, grain morphology and the
distribution of reinforcement particulates. The microstructure of the samples was investigated using an Olympus
metallographic microscope and Hitachi S4100 eld-emission scanning electron microscope. Scion Image Analyzer
software was used to determine the grain size and morphology from representative micrographs.

2.8. Fracture behavior


Fractography was performed on the tensile fractured
surfaces of samples to provide an insight into the various
possible fracture mechanisms operating during the tensile
failure of the samples using a JEOL JSM-5600LV scanning
electron microscope.
3. Results
3.1. Macrostructural characteristics
Macrostructural characterization conducted on the assintered billets revealed the absence of macrostructural
defects such as circumferential or radial cracks. Following
extrusion, no observable macro defects were observed on
Mg and Mg/Alp samples. The outer surface was smooth
and free of circumferential cracks.
3.2. Density measurements
The results of the density measurement are shown in
Table 1. The experimental and theoretical values of the
composites were found to be almost identical. This indicates that near-dense composites can be obtained using
the fabrication methodology adopted in the present study.

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X.L. Zhong et al. / Acta Materialia 55 (2007) 63386344

Table 1
Results of density and grain size measurements
Material

Alp (wt.%)

Experimental density (g cm3)

Theoretical density (g cm3)

Porosity (%)

Grain size (lm)

Aspect ratio

Mg/0.00Alp
Mg/0.25Alp
Mg/0.50Alp
Mg/0.75Alp
Mg/1.00Alp

0.00
0.38
0.76
1.16
1.52

1.731 0.012
1.738 0.004
1.746 0.009
1.751 0.003
1.755 0.011

1.74
1.74
1.75
1.75
1.75

0.5
0.2
0.4
0
0

23 6
17 5
17 8
16 7
16 6

1.3 0.5
1.3 0.6
1.5 0.3
1.2 0.2
1.4 0.6

3.3. Microstructural characteristics


Microstructural studies conducted on the extruded specimens showed fairly uniform distribution of aluminum particulates with a limited amount of clustering (represented
by white spots in Fig. 1) in the matrix. Grain size studies
indicated a reduction in grain size from 23 lm in the case
of pure Mg to 16 lm in the case of Mg/1.00Alp composite
(see Table 1). No signicant change was observed in the
aspect ratio of the grains with the addition of reinforcement. Transmission electron microscopy (TEM) investigation revealed good matrixreinforcement interfacial
integrity between the Mg matrix and the Al nanoparticulates (see Fig. 2). Observations also revealed a minimal
presence of porosity in composite materials consistent with
the results of density measurements. XRD analysis
revealed the absence of intermetallic and oxide phases.
Representative XRD diractograms of selected materials
are shown in Fig. 3.

Ambient temperature tensile tests revealed simultaneous


improvement in 0.2% yield strength (YS), ultimate tensile
strength (UTS), failure strain and work of fracture
(WOF) (calculated based on the area under the stress
strain curve using EXCEL software) of magnesium with
the addition of nano-size Al particulate reinforcement
(see Table 2). Among the composite formulations, magnesium reinforced with 0.5% of Al nanoparticulates showed
the best overall improvement, with an increase of 62% in
0.2% YS, 43% in UTS, 35% in failure strain and 109% in
WOF.
3.5. Fracture behavior
The fracture surface investigation showed typical brittle
failure exhibited by Mg samples and mixed mode failure in
the case of Mg/0.5Alp composite samples. Representative
SEM fractographs of the samples are shown in Fig. 4.
4. Discussion

3.4. Mechanical behavior


4.1. Microstructural characterization
The results of the hardness measurements conducted on
extruded Mg and Mg/Alp samples revealed increasing
hardness with an increase in volume percentage of nanosize Al particulate reinforcement, as shown in Table 2.

Fig. 1. Representative FESEM micrograph showing the distribution of


aluminum particulates (represented by white spots) in Mg/1.00Alp
composite.

Microstructural characterization of extruded composite


samples are discussed in terms of: (a) distribution of reinforcement, (b) grain size and morphology, (c) presence of
pores and (d) interfacial integrity between the reinforcement and the matrix.
The reasonably uniform distribution of reinforcement
particulates (see Fig. 1) can be attributed to suitable blending parameters and the high extrusion ratio used in secondary processing. In theory, homogeneous distribution of
reinforcements can be obtained, irrespective of the size difference between the matrix powder and the reinforcement
particulates, provided a large deformation load is applied
during secondary processing [13]. However, a limited
amount of clustering of reinforcement is unavoidable in
this case, owing to the high surface energy associated with
the nanoparticles (see Fig. 1). Minimal standard deviation
in density measurement results also reects the uniform distribution of reinforcement in the synthesized materials.
Marginal grain renement (see Table 1) in composite
samples as a result of the presence of particulates can be
attributed to: (a) the ability of nano-size Al particulates
to nucleate magnesium grains during recrystallization;
and (b) the restricted growth of the magnesium grains
due to grain boundary pinning [3,1416]. Within the

X.L. Zhong et al. / Acta Materialia 55 (2007) 63386344

6341

500
400

Al

300
200

O
Mg

100
0
0

10

500
400

Mg

300
200

100
0
0

10

Mg/1.0Alp

Mg (211)

Mg (210)

Mg (004)

Mg (200)
Mg (112)
Mg (201)

Mg (103)

Mg (102)

1500

Mg (002)

Intensity / arb. units

2000

Mg (110)

Mg (101)

2500

Mg (100)

Fig. 2. TEM micrograph showing good interfacial integrity between Mg matrix and nano-Al particulates. The EDX spectrum veries the presence of
nano-aluminum particulate.

1000

Mg/0.5Alp
500

Mg/0.0Alp
0

30

40

50

60

70

80

90

100

Theta-2 Theta (deg)

Fig. 3. Representative XRD diractograms of selected materials synthesized in this study.

composite samples, however, the increase in the number of


aluminum nanoparticulates did not aect the grain size.
Microstructural study revealed minimal porosity in
composite materials. This is also supported by the density
measurement results shown in Table 1. The results suggest
the appropriateness of processing parameters used for
compaction, sintering and extrusion. TEM study revealed
good interfacial integrity between nano-size Al particulates
and the Mg matrix (see Fig. 2). Energy dispersive X-ray
(EDX) analysis conrmed the presence of aluminum, as
represented by the dark-colored phase in Fig. 2. XRD analysis on the synthesized samples revealed the absence of
reaction phases and the presence of pure Mg peaks only
(see Fig. 3). The absence of Al peaks can be attributed to

the limitation of the ltered X-ray to detect phases with


amount <2 vol.% [17].
4.2. Mechanical characterization
The results of hardness measurement revealed that the
hardness of the magnesium composites increases with an
increasing amount of reinforcement (see Table 2). The
increase in hardness of the magnesium composites with
increasing volume fraction of nano-size Al particulate reinforcement can be attributed primarily to: (a) the presence
of harder Al nanoparticulates (36.6HV for magnesium
and 44.4HV for aluminum [18]; (b) higher constraint to
the localized matrix deformation during indentation due

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X.L. Zhong et al. / Acta Materialia 55 (2007) 63386344

Table 2
Results of the room temperature mechanical properties of Mg and Mg/Alp samples
Materials

UTS (MPa)

46 3
54 1
57 1
60 1
61 1

134 11
181 14
218 16
202 7
185 9

190 10
221 15
271 11
261 10
226 12

4.6 0.6
4.8 0.4
6.2 0.9
5.0 1.6
3.3 1.0

7.6 1.6
10.5 1.9
15.9 2.1
13.1 2.9
7.9 1.8

Micron-size reinforcement
AZ91/10SiC [8]
AZ91/10.0SiC [27]
ZC63/12SiC [28]
Mg/21.3SiC [29]

71.47

82.2 1.1

135
120
148
128 1.9

152
135
197
176 3.5

0.8a
0.47a
0.7a
1.4 0.1a

3.3 0.8

Nano-size reinforcement
Mg/1.1Al2O3 [10]
Mg/1.0SiC [12]
Mg/0.3CNT [11]
Mg/0.6Cu [23]
Mg3.0SiCb [30]

59.7 0.5

44 0
57 1

194 5
157 22
146 5
237 24
180

250 3
203 22
210 6
286 8
220

6.9 1.0a
7.6 1.5a
8 1a
5.4 1.2a
3.0

15.5 2.6

15.8 1.8
16.5 3.1

a
b

Failure strain (%)

WOF (MJ m3)

0.2% YS (MPa)

Mg/0.00Alp
Mg/0.25Alp
Mg/0.50Alp
Mg/0.75Alp
Mg/1.00Alp

Hardness (15HRT)

Ductility values.
Values inferred from tensile graph.

Fig. 4. Representative SEM fractograph of: (a) Mg matrix and (b) Mg/0.5% Alp samples.

to the presence of Al nanoparticulates; and (c) reduced


grain size. These results are consistent with the ndings
reported by other researchers [10,12,15].
Room temperature tensile testing revealed signicant
improvement in 0.2% YS and UTS (see Table 2) of pure
magnesium owing to the presence of nano-size Al particulates as reinforcement. The increase in tensile strength can
be attributed to the coupled eects of: (a) Orowan strengthening [3,7]; (b) grain renement; (c) formation of internal
thermal stress due to dierent CTE values between the
matrix and the reinforcement particles (28.9 106 K1
for Mg and 26.49 106 K1 for Al [19]); (d) eective load
transfer between the matrix and the reinforcement; and (e)
hardening due to the strain mist between the reinforcing
particulates and the matrix. The contributions to the
increase in the YS of the composites by the various
strengthening mechanisms could be taken as a simple summation or the root of the sum of squares of the dierent

mechanisms, and have been discussed in several recent


studies [7,2023].
Owing to the presence of the dispersed nano-size particles
in the matrix, dislocation loops form as dislocation lines bow
and bypass the particles. The eect of this process on the
yield stress of the material is described by Orowan strengthening. The increase in yield stress can be expressed as [20]
0:4  G  b lnd=b
p
1
1  vMg
pk
p
where d 2=3d , M is the mean orientation factor for
magnesium, G is the shear modulus of the matrix, b is
the Burgers vector, vMg is Poissons ratio of the matrix,
and kpis
the mean inter-particle distance given by

k d rp=4f  1.
The renement in grain size arises as a result of the presence of reinforcing particles which act as nucleation sites
rOrowan M 

X.L. Zhong et al. / Acta Materialia 55 (2007) 63386344

during recrystallization and the pinning of grain boundaries [3,14,23]. The contribution to the increase in YS due
to grain size strengthening can be described by the Hall
Petch equation [20,23]:
rHP KD1=2

where K is the HallPetch coecient, and D is the grain


diameter.
The coecient of thermal expansion (CTE) mismatch
between the matrix and nano-size Al particles lead to an
increase in dislocation density around the reinforcement
particles during cooling from the elevated processing temperature. The plastic deformation caused by CTE mismatch thus improves the strength of the composite.
Increase in yield stress due to dislocations with density
qth which are created from the relaxation of thermal expansion mismatch between the matrix and the reinforcement
particles is expressed as [20]
1=2

rCTE A  M  G  b  qth

where A is a constant characterizing the transparency of


the dislocation forest for basalbasal dislocation interaction in magnesium [20]. The dislocation density qth can
be p
estimated
by assuming that dislocation loops of radius

d= 2 are punched by spherical particles of diameter d with


volume fraction f to relax the thermal mismatch due to the
dierence in thermal expansion coecients Da for a temperature excursion DT [24].
p
12 2  Da  DT  f
qth
4
b  d  1  f
Eective load transfer depends largely on interfacial
bonding between the matrix and the reinforcement. In this
study, good interfacial bonding is achieved (see Fig. 2).
Using the modied shear lag model, the composite YS
based on the load transfer mechanism can be expressed
by the equation [25]:


1
rcy rmy f s 2 1  f
5
2
where rcy is composite YS, rmy is the matrix YS, and s is
the aspect ratio of reinforcement. Therefore the increment
in YS due to load transfer eect rLT can be calculated as
follows:
rLT rcy  rmy

It may be noted that, based on the contributions by the


above-mentioned strengthening mechanisms, the YS of the
composites should increase with increasing volume fraction
of reinforcement. However, when the volume fraction of
nano-aluminum particulates is increased from 0.5% to
1%, the strength and ductility of the composites drops
but remains higher when compared with pure Mg. This
may be due to the agglomeration of aluminum nanoparticulates with increasing volume fraction, which reduces the
Orowan strengthening eect [3].

6343

The results of room temperature tensile testing also


reveal an increase in the average failure strain of pure magnesium with addition of 60.75% nano-Al particulates. The
best improvement was obtained in the case of Mg/0.5Alp
sample (35%). Pure magnesium has limited dislocation
mobility, and crack generation is relatively easy. Typically,
the addition of micron-size reinforcements leads to an
improvement in strength and decreases the ductility of
the material. However, recent studies have shown that
the addition of Al2O3, Y2O3, ZrO2 and SiC nanoparticles
[10,12,14] and carbon nanotubes [11] in certain volume
fraction leads to a simultaneous improvement in strength
and ductility. The increment in ductility of the magnesium
matrix by reinforcement particulates may be attributed to
the activation of a non-basal slip system [26].
The ability of each material to absorb energy up to fracture is indicated as the WOF. It is calculated by the area
under the stressstrain curve in this study. It can be
observed that the WOF was improved with the addition
of nano-Al particulates (61 vol.%) when compared with
pure Mg, and the optimum value is obtained with the addition of 0.5% Alp, resulting in an improvement of 119%. The
large improvement in WOF is due to the simultaneous
improvement of strength and ductility of the composite.
These results reveal that Mg reinforced with 0.5% Al nanoparticulates may be useful for potential weight critical
applications targeted for strength and damage-tolerant
designs (higher YS and WOF when compared with
magnesium).
A comparison of the mechanical properties of the Mg/
Alp composites synthesized in this study with other Mg
composites strengthened with micron-size [8,2729] and
nano-size [1012,23,30] reinforcements is shown in Table 2.
The strength and ductility of Mg/Alp composites are superior when compared with Mg composites reinforced with a
larger volume fraction of micron-size SiC particulates. This
is extremely advantageous, because a low volume fraction
of nano-size reinforcement does not signicantly compromise on the lightweight properties of magnesium, and the
relative contribution to the mechanical properties surpasses
that of using micron-size reinforcement. Comparison of
the Mg/0.5Alp composite synthesized in this study with
other nanoparticulate-reinforced magnesium composites
revealed that similar or superior combinations of tensile
properties assessed in terms of WOF can be obtained (see
Table 2).
4.3. Fracture behavior
The results of the tensile fracture surface analysis on the
Mg samples revealed typical brittle cleavage fracture (see
Fig. 4a). This can be attributed to the hcp structure of magnesium which restricts the plastic deformation predominantly to basal slip. The fracture surfaces in the case of
Mg/0.5Alp composite samples revealed a mixed mode type
of failure with increased evidence of plastic deformation
(see Fig. 4b). The switch from brittle to mixed mode type

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X.L. Zhong et al. / Acta Materialia 55 (2007) 63386344

Fig. 5. Representative SEM fractographs showing: (a) predominantly straight lines due to slip in the basal plane of pure Mg and (b) uneven lines due to
the combined eect of basal and non-basal slip in Mg/0.5Alp composite.

of fracture can be attributed to the activation of non-basal


slip system due to the presence of critical amount of
nano-size reinforcement [10,11]. This is also evident in
the fractographs shown in Fig. 5. For pure magnesium
samples, predominantly straight lines indicating slip on
the basal planes were observed (see Fig. 5a) while, in the
Mg/0.5Alp composite samples, uneven lines due to slip in
basal and non-basal planes can be observed (see Fig. 5b).
This phenomenon was also observed in earlier studies,
where an increase in the ductility of magnesium was
reported with the addition of nano-size reinforcements
[10,14]. For other composite samples (Mg/0.25Alp, Mg/
0.75Alp and Mg/1.00Alp), fracture surfaces were not distinctly dierent from that of pure Mg.
5. Conclusions
The following conclusions can be made from the experimental ndings of this study.
1. Blend-press-sinter-extrusion powder metallurgy technique was successfully used to synthesize magnesium
composites containing nano-size Al particulates.
2. Microstructural characterization revealed a reasonably
uniform distribution of nano-Al particulates with
good interfacial integrity between the matrix and the
reinforcement.
3. The results of mechanical characterization revealed that
the addition of nano-Al particulates to magnesium
matrix leads to a signicant improvement in the overall
combination of hardness and tensile properties.
4. The threshold for optimum mechanical properties of the
composite formulation was obtained at 0.5 vol.% of Al
reinforcement, with an increase of 62% in 0.2% YS,
43% in UTS, 35% in failure strain and 109% in WOF.
5. Fractography revealed that the fracture behavior of the
Mg matrix changes from a typical brittle mode to mixed
mode when 0.5 vol.% of nano-aluminum particulates
were added to the Mg matrix.

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