Composites Science and Technology 69 (2009) 22562264

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Composites Science and Technology

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Mechanical and fracture properties of an AZ91 Magnesium alloy reinforced

by Si and SiC particles
Z. Trojanov a,*, V. Grtnerov a,1, A. Jger a,1, A. Nmeny b, M. Chalupov b, P. Palcek b, P. Lukc a
a
Department of Physics of Materials, Faculty Mathematics and Physics, Charles University, Ke Karlovu 5, CZ-121 16 Praha 2, Czech Republic
b
Department of Materials Engineering, Faculty of Mechanical Engineering, University of Zilina, Velky Diel, SK-010 26 Zilina, Slovak Republic

a r t i c l e i n f o a b s t r a c t

Article history: A commercial AZ91 magnesium alloy (nominal composition Mg9%Al; 1%Zn; 0.3%Mn, balance Mg in
Received 20 April 2009 weight percent) reinforced with SiC particles and modied by the addition of Si has been used in this
Received in revised form 14 June 2009 study. Formation of an in situ composite (MgMg2Si) results in strong bonding between Mg2Si and
Accepted 19 June 2009
the matrix interface. Samples were deformed in compression in the temperature interval from room tem-
Available online 26 June 2009
perature up to 300 C. Stress relaxation tests were performed with the aim to reveal the thermally acti-
vated processes. Reinforcing effect of SiC and Mg2Si particles decreases with increasing temperature. The
Keywords:
estimated values of the activation volume as well as the activation enthalpy indicate that the main ther-
A. Metal matrix composites
B. Plastic deformation
mally activated process is connected with a rapid decrease of the internal stress. Fracture properties were
C. Stress relaxation studied in impact tests at various temperatures. A ductility enhancement was found at 200 C and tem-
D. Scanning electron microscopy peratures above 200 C.
E. Casting 2009 Elsevier Ltd. All rights reserved.
Magnesium alloy
Composite
Mechanical properties
Thermally activated process
Fractography

1. Introduction Solid solubility of Al in Mg is about 2.1 wt.% (1.9 at.%) at

Mechanical properties of magnesium alloys decrease rapidly
with increasing temperature. Remarkable improvement of
mechanical properties can be reached by the addition of reinforc-
ing phases (bres or particles) which may improve stiffness, wear
resistance, thermal expansion coefcient (CTE) and deformation
properties at elevated temperatures [17].
AZ91 magnesium alloy is the most popular commercially avail-
able magnesium alloy. This alloy shows superior castability and
good mechanical properties combined with good corrosion resis-
tance for the high purity versions of the alloy. Typical applications in-
clude transmission casings, valve covers, intake manifolds, brackets,
pumps, etc. MgAlZn based alloys like AZ31, AZ61, AZ80 and AZ91
are, in general, utilized for applications at ambient or slightly ele-
vated temperatures primarily in the automotive and electronic
industry. They successfully combine acceptable mechanical proper-
ties with good castability and relatively low production costs.
* Corresponding author. Tel.: +420221911357; fax: +420221911490.
E-mail address: ztrojan@met.mff.cuni.cz (Z. Trojanov).
1
Present address: Institute of Physics, Academy of Sciences Czech Republic, Na
Slovance 2, 182 21 Praha 8, Czech Repubic.
ambient temperature [8]. Exceeding of solid solubility of Al gives
rise to Mg17Al12 intermetallic phase in the lamellar form. An
addition of Zn, (its solubility limit in Mg is about 0.8 at.% at RT
[9]) further improves the mechanical properties of the MgAl
system. The Si additions lead to the improvement of mechanical
properties at elevated temperatures (up to about 150 C). The re-
sult of negligible solubility of Si in Mg matrix is the formation of
the Mg2Si intermetallic phase [10]. By this way it is possible to
obtain relatively cheap alloys with acceptable mechanical prop-
erties for some thermally and mechanically exposed parts in
the transport industry [11].
It is generally accepted that during deformation of a composite,
deformation process occurs in the matrix and short ceramic bres
deform only elastically. An increase in the ow stress in the com-
posite is caused mainly by the following four reasons:
 Load transfer from the matrix to bres.
 Direct impact of bres as impenetrable obstacles for the disloca-
tion motion.
 Inuence of bres on the development of the dislocation sub-
structure in the matrix.
 Inuence of bres on the microstructure formation.

0266-3538/$ - see front matter 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compscitech.2009.06.016
 Z. Trojanov et al. / Composites Science and Technology 69 (2009) 22562264
While the intrinsic mechanical and physical properties of a rein-
forcement (stiffness, strength, and thermal expansion) are dictated
by its chemical nature, the geometric and topological parameters
of the reinforcement (shape, size, volume fraction, spatial orienta-
tion, and distribution) can be altered during processing.
According to the dislocation theory, the applied stress r neces-
sary for deformation of any polycrystalline material can be divided
into two components: the internal (athermal) stress ri and the
effective stress r*, i.e. one can write
r ri r : 1 the intermetallic phase (Mg2Si), formed during the manufacture
The internal stress ri, resulting from long-range internal stres-
ses impeding the plastic ow can be written as
r a1 Gbqt1=2 ; 2 2. Experimental procedure
where G is the shear modulus, a1 is a constant describing interac-
tion between dislocations, b is the Burgers vector of dislocations
and qt is the total dislocation density. The effective shear stress r*
acts on dislocations during their thermally activated motion when
they overcome short range obstacles. The mean velocity of disloca-
tions v is connected with the plastic strain rate by the Orowan
equation:
e_ 1=wqm bv ; 3 dard T6 thermal treatment (annealing for 18 h at 413 C in the pro-
where qm is the density of mobile dislocations and w is Taylor ori-
entation factor. The most common equation used in describing the
average dislocation velocity as a function of the effective stress is an
Arrhenius type. The plastic strain rate e_ for a single thermally acti-
vated process can be expressed as:
e_ e_ 0 expDGr =kT; 4 stress along a stressstrain curve. Duration of the SR was 300 s.
where e_ 0 is a pre-exponential factor containing the mobile disloca-
tion density, the average area covered by the dislocations in every
activation act, the Burgers vector, the vibration frequency of the dis-
location line, and the geometric factor. T is the absolute tempera-
ture and k is the Boltzmann constant. DG(r*) is the change in the
Gibbs free enthalpy depending on the effective stress r* = r  ri
and the simplest form is
DGr DG0  V r DG0  Vr  ri : 5
Here DG0 is the Gibbs free enthalpy necessary for overcoming a
short range obstacle without the stress and V = bdLc is the activation
volume where d is the obstacle width and Lc is the mean length of
dislocation segments between obstacles.
The stress relaxation technique is very useful method to study
the thermally activated processes and to reveal the dominant pro-
cess occurring during plastic deformation. In a stress relaxation
(SR) test, the specimen is deformed to a certain stress, r0, then
the machine is stopped and the stress is allowed to relax. The stress
decreases with the time t. The specimen can be again reloaded to a
higher stress (load) and the SR test may be repeated. The time
derivative r_ = dr/dt is the stress relaxation rate and r = r(t) is
the ow stress at time t during the SR. The stress relaxation tests
are very often analysed under the assumption that the SR rate is
proportional to the strain rate e_ , according to [12], as:
e_ r_ =M; 6 conventional mechanical polishing and etching using glycol solu-
where M is the combined modulus of the specimenmachine set.
The stress decrease with the time during the SR can be described
by the well known Feltham equation [13]:
Drt r0  rt alnbt 1; 7 for 3060 s by an electrolytic method at the current
where r(0)  r0 is the stress at the beginning of the stress relaxa-
tion at time t = 0,
2257
kT
a ; 8
V
 
M e_ 0 V DG0  V r 0 M e_ 0
b exp  ; 9
kT kT a
where e_ (0) the plastic strain rate at the beginning of the
relaxation.
In the present work, the microstructure, mechanical and frac-
ture properties of the AZ91 alloy-based composite consisting of
process and reinforcing SiC particles were studied.
A commercially available AZ91 magnesium alloy (the nominal
composition Mg9%Al; 1%Zn; 0.3%Mn; balance Mg in weight per-
cent) was reinforced with 10 vol.% of SiC particles (SiCp) and an
addition of 3 wt.% of Si. The size of the SiCp exhibited about
20 lm. Composite was prepared by the squeeze cast technology.
The preform was inltrated by the liquid alloy using two-stage
application of the pressure. The samples were subjected to a stan-
tective argon atmosphere, then ageing for 8 h at 168 C [11])
Compression tests were carried out at an initial strain rate of
3.3  105 s1 over a wide temperature range from room temper-
ature (RT) to 300 C. Dimensions of the samples used in compres-
sion tests were 5  5  10 mm3.
Sequential stress relaxation tests were performed at increasing
Ductility of the alloy at room temperature is very low and there-
fore the SR tests were performed at elevated temperatures. On
the other hand, recovery during the SR test was observed at
300 C and hence, the results obtained at this temperature were
not taken into account because the above given equations
describing the SR were derived under an assumption that the
internal stress ri is constant during the SR. Only in the rst SR
test at 300 C, recovery may be considered to be negligible, i.e.
ri is constant.
Components of the applied stress (ri, r*) were estimated using
Lis method [14,15]. The SR curves were tted to the power law
function in the form:
1 1
r  ri am  11m t t0 1m ; 10
where a, t0 and m are tting parameters.
The impact tests were performed by the Charpy pendulum in
the temperature range from RT to 300 C. The samples with dimen-
sions of 10  10  55 mm3 were machined from the billet using
standard tools. The U-type notch has been created by the electro
erosive cutting to 2 mm depth. High temperature tests were con-
ducted with the preheated samples in an electric furnace. The frac-
ture surfaces were investigated immediately after the impact tests
using a scanning electron microscope (SEM) in order to prevent
possible oxidation.
Samples for the microstructure analysis were prepared by the
tion (1 ml HNO3, 24 ml water, 75 ml ethylene glycol). In order to
obtain detailed three-dimensional morphology the surfaces of
samples were deeply etched using a mixture of 36 ml phosphoric
acid (H3PO4) and 64 ml ethyl alcohol. The samples were etched
I = 0.05 mA cm2 and the voltage of 0.7 V. For the phase identica-
tion, a SEM analysis was performed on the samples that undergone
both etching and deep etching procedure.
2258 Z. Trojanov et al. / Composites Science and Technology 69 (2009) 22562264
Fig. 1. The initial microstructure of experimental material, etched using glycol
solution: SiC particles (dark grey); primary Mg2Si coarse dendritic phase (light
grey); Chinese script of Mg2Si; c-phase (lightest) surrounded by lamellae discon-
tinuous precipitate (c + d).
3. Results and discussion
3.1. Microstructure analysis
A representative view of microstructure of the AZ91alloy based
composite with 3%Si and 10 vol.% of SiCp is shown in Fig. 1. Micro-
structure of the AZ91 alloy (see Fig. 1) consists of the d-phase (solid
solution of Al in the Mg), the c-phase (intermetallic compound
Al12Mg17, see the detail in Fig. 2c and the discontinuous precipitate
(lamellae of c + d phase). (It should be noted that in many papers,
Mg17Al12 phase is called the b-phase.) The addition of 3%Si gives
rise to the Mg2Si phase formed as eutectic particles in the form
of Chinese script type (Figs. 1, 2b and c), or primary Mg2Si coarse
Fig. 2. (a) SEM micrograph of initial microstructure etched using glycol solution; (b) Chinese script type particle; (c) c-phase (electron compound Al12Mg17) and lamellae
discontinuous precipitate (c + d); (d) primary Mg2Si coarse dendritic crystal entrapped by d-Mg.
dendritic particles (Figs. 1, 2d, and 4a). Similar morphology of
Mg2Si compound was also found also by Jiang et al. [16]. The Mg2Si
phase is situated usually in the d-phase grains interior, and also of-
ten the islands of the entrapped d-phase are often present in some
Mg2Si coarse dendritic crystals (Figs. 1 and 2d).
The c-phase is distributed mainly around the grain boundaries
(Fig. 1 and 2a) and discontinuous precipitate lamellae (DP) were
often adjacent to the c-phase or the grain boundaries. The DP mor-
phology corresponds with the Crawley and Millikens observation
of the precipitation morphology in the aged AZ91 alloy [17].
Fig. 3a illustrates the same site of microstructure as Fig. 2a after
deep etching. The deep etching revealed the three-dimensional
shape of the components. The details in Fig. 3bd correspond to
details in Fig. 2bd. Note that the Chinese script particles and the
coarse dendrites of Mg2Si were etched more rapidly than the rest
of the other microstructure. The c-phase lamellae of DP and
c-phase itself are the most resistant components to etching
(Fig. 3c). It is interesting to note that coarse Mg2Si dendrites are
etched inhomogeneously due to the entrapped d-phase (Figs. 4b
and 5a).
From Figs. 1 and 4 it is obvious that the matrix/SiCp interface
has a waved character. Candan [18] pointed out that aluminium
may create black-colored Al4C3 particles as a reaction product at
the matrix/SiCp interface. The waved interface can arise during
the matrix inltration. According to references [18,19], the reaction
between Al and SiCp is a common feature observed during the fab-
rication of Al matrix composites reinforced by SiCp. The reaction
occurs as follows [19]:
4Al 3SiC ! Al4 C3 3Si: 11
This reaction depends on the processing parameters, especially
on temperature and chemical composition of both the matrix and
the reinforcement [19].
SEM energy dispersive analysis was used in order to analyse the
chemical composition of the matrix/SiCp interface. The mapping
(Fig. 5) revealed segregation of Al atoms in the vicinity of the SiCp
 Z. Trojanov et al. / Composites Science and Technology 69 (2009) 22562264 2259

Fig. 3. SEM micrographs of the same places as shown in Fig. 2 after using deep etching.

Fig. 4. SEM micrographs represent SiC particle with serrated interface and primary Mg2Si coarse dendritic crystal after using glycol etching (a) and deep etching (b).

Fig. 5. The sample under observation using SEM energy dispersive analysis: (a) SEM image and (b) map of Al distribution. Note higher concentration of Al in the zones
adjacent to SiCp and no occurrence in the vicinity of Mg2Si, the concentration of Al in the c-phase (Al12Mg17) is appropriate.
2260 Z. Trojanov et al. / Composites Science and Technology 69 (2009) 22562264

interface and indicated a possible occurrence of Al4C3 carbide. The 500

excess of Si from Eq. (11) can contribute to the formation of the
Mg2Si phase. The segregation of Zn has not been observed. 02
400
max
3.2. Stressstrain curves

(MPa)
300
The true stresstrue strain curves obtained in compression at
various temperatures are shown in Fig. 6. Samples were deformed 200
either to fracture at temperatures up to 200 C or to predetermined
strain at higher temperatures. A at shape of the stressstrain 100
curves obtained at higher temperatures than 150 C is obvious
from Fig. 6, indicating the equilibrium between hardening and
softening. The temperature dependence of the yield stress as well 0
0 50 100 150 200 250 300 350
as the maximum stress is introduced in Fig. 7. A weak temperature
dependence of the yield stress up to 200 C is followed by the more temperature (C)
rapid decrease at higher temperatures (Fig. 7). It is interesting to
Fig. 7. Temperature dependence of maximum stress and yield stress.
note that the softening and the transition from brittle to ductile
behaviour above 200 C corresponds with the onset of plasticity
of Mg2Si as published by Takeuchi et al. [20] (see also [21]). How-
ever, the dislocation glide in non-basal slip planes in the Mg ma- Bf DaDT 1
qT ; 12
trix, which is usually observed at higher temperatures (higher b1  f t0
than about 200 C) [2224], may involve not only the increased where t0 is the minimum size of the reinforcing phase particles, b is
compression plasticity but also the observed transition from brittle the magnitude of the Burgers vector of the newly created disloca-
to ductile behaviour as well. The Mg matrix with the hexagonal tions, B is a geometrical constant, Da is the difference between
structure provides only two independent basal slip systems at the two thermal expansion coefcients and DT is the temperature
ambient temperature. Non-basal slip systems activity strongly de- variation. A higher dislocation density in the composite material
pends on structural parameters like grain size, texture, alloying yields in a higher level of the internal stress. For the strengthening
elements and strain gradients which may arise in the vicinity of due to the presence of dislocations generated by the differential
inclusions. A comparison of the temperature dependence of the CTE, the following equation may be used:
yield stress of the alloy and composite is introduced in Fig. 8. As
it follows from Fig. 8, the addition of the reinforcing phase in- DrT a1 wGbqT 1=2 : 13
creases the yield stress of the monolithic alloy. The difference be-
Strengthening mechanisms in MgSi alloys prepared by rapid
tween the yield stresses of the composite and alloy decreases
solidication procedure were studied by Mabuchi and Higashi
with increasing temperature. The composite strengthening de-
[28]. They calculated various contributions to strengthening and
pends on the geometrical parameters of composites (size and
found that the main strengthening effect has the small grain size
shape of bres or particles, volume fraction of the reinforcement,
and the small Mg2Si particles. Rapid decrease of the strength at
interparticle distance), on the physical properties of the all compo-
temperatures higher than 200 C has been attributed to the coars-
nents (thermal expansion coefcient, bonding at the matrixrein-
ening of particles. Larger particles (>110 lm) or very small parti-
forcement interface), microstructure and mechanical properties
cles (<50 nm) are required to attain high strength at elevated
of all components [25].
temperatures above 200 C.
Metal matrix composites are characterized by a large difference
The reinforcing phase contributes to strengthening mainly
in the thermal expansion coefcient (CTE) of the matrix and cera-
through an increased dislocation density (arising from the ther-
mic reinforcement (CTE of Mg exhibits 26  106 K1 [20],
mal and geometrical mismatch). The load transfer from matrix
CTE(SiC) = 6.6  106 K1 [26] and CTE(Mg2Si) = 7.6  106 K1
to reinforcing particulates plays in this composite only a mar-
[19]). Even small temperature changes generate thermal stresses
ginal role.
in the matrix. Thermal stresses can be partially released by disloca-
tion generation in the vicinity of the interface. The density qT of
thermal dislocations in the matrix can be calculated [27].

200
400 RT 50C AZ91
100C AZ91+SiC+Si
160
300
150C
02 (MPa)
(MPa)

120
200
200C

250C 80
100
300C
0 40
0.00 0.04 0.08 0.12 0 50 100 150 200 250 300 350
temperature (C)

Fig. 6. Compression true stresstrue strain curves at initial strain rate Fig. 8. Temperature dependence of the yield stress of composite in comparison
e_ 8:3  105 s1 . with the unreinforced alloy.
 Z. Trojanov et al. / Composites Science and Technology 69 (2009) 22562264 2261

300 40
150C 35
250
ap 150C
30
200 250C
(MPa)

25

V/b3
150
i 20
100
15
50
10

0 5
0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.00 0.05 0.10 0.15 0.20 0.25 0.30

Fig. 9. A part of the true stresstrue strain curve obtained at 150 C. The points of Fig. 11. Strain dependence of activation volume obtained for two temperatures.
rap on the curve indicate the stresses at which the SR tests were performed, ri and
r* are the internal and effective stresses.
atures are plotted against the effective stress, r*, the values appear
to lie at one line master curve (Fig. 12). Kocks et al. [30] sug-
3.3. Stress relaxation tests
gested an empirical equation between the Gibbs enthalpy DG
and the effective stress r* in the following form:
A part of the true stresstrue strain curve of the alloy measured
   p q
at 150 C with points indicating the stresses at which the SR tests r
DG DG 0 1  ; 14
were performed is shown in Fig. 9. Components of the applied 
r0
stress the internal stress, ri,, and the effective stress, r*, are given
in Fig. 9. It is obvious that the internal stress ri is a substantial con- where DG0 and r0 are Gibbs enthalpy and the effective stress at 0 K.
tribution to the applied stress rap at the onset of the stressstrain For the effective stress it follows:
curve. The internal stress, ri, increases with increasing strain up to "  1=q #1=p
  kT e_ 0
approximately 5% of the plastic strain, than decreases with increas- r r 0 1 ln ; 15
ing strain. On the other hand, the effective stress component DG0 e_
increases with increasing strain and at e = 0.25 ri = r*. Similar
where p and q are phenomenological parameters reecting the
curves estimated at 250 C are shown in Fig. 10. The effective stress
shape of a resistance obstacle prole.
component is higher than the internal stress and it increases with
The possible ranges of values p and q are limited by the condi-
increasing strain while the internal stress decreases with increas-
tions 0 < p 6 1 and 1 6 q 6 2. Ono [31] suggested that Eq. (14) with
ing strain for e > 0.007. The internal stress of several magnesium
p = 1/2, q = 3/2 describes a barrier shape prole that ts many
alloys has been studied by Milicka et al. [29] in creep experiments.
predicted barrier shapes. Thermodynamics generally denes the
They found that the internal stress ri reects the creep resistance
activation volume as
of the materials. Experimental internal stresses determined in      
creep well correspond to those determined in SR tests under com- dDG d ln e_ d lnr_
V  kT kT : 16
parable testing conditions. dr T
 dr  dr
T
The activation volumes V were estimated using Eqs. (7) and (8).
Eq. (16) can be rewritten as
As usual, the values of V divided by b3 for samples deformed at 150
and 250 C are plotted against strain in Fig. 11. It can be seen that   p q1  p1
DG0 pq r r
the activation volumes decrease with increasing strain for both V 1 : 17
r0 r0 r0
temperatures measured. If the activation volumes for both temper-

50
250C
120
40
ap 150C
(MPa)

250C
80 30
* fit
V/b3

20
40 i
10

0
0.00 0.04 0.08 0.12 0.16 0
20 40 60 80 100 120

* (MPa)
Fig. 10. A part of the true stresstrue strain curve obtained at 250 C. The points of
rap on the curve indicate the stresses at which the SR tests were performed, ri and Fig. 12. The plot of the activation volume against the thermal stress r* estimated
r* are the internal and effective stresses. for two deformation temperatures and t of all experimental points using Eq. (17).
2262 Z. Trojanov et al. / Composites Science and Technology 69 (2009) 22562264

Fig. 13. Fractographic observation (SEM): (a) surface perpendicular to the fracture surface of specimen fractured at RT shows the Mg2Si dendrite with many microcracks (see
arrows); (b) cleavage fracture of primary Mg2Si dendritic crystal entrapped by d-phase, fractured at 300 C; (c) and (d) the opposite sites of fractured specimen at 200 C with
pyramid-like shape of primary Mg2Si dendritic crystal (c) and rest of Mg2Si in opposite site of fracture surfaces (d).

The values of the activation volume should lie at the curve given
by Eq. (17). Using binominal expansion in Eq. (17), the activation
volume should depend on the effective stress Vapp / (r*)n. All data
estimated for the activation volume at both temperatures studied
are introduced in Fig. 12 together with the t according to Eq.
(17). The activation enthalpy calculated from Eq. (17) has been
estimated to be DG0 = 0.95 0.05 eV. Similar activation enthalpy
was found for AX41 magnesium alloy reinforced by 13 vol.% of
short Safl bres [32]. The values of the activation volume and
the activation enthalpy may help to identify thermally activated
processes. The dislocationdislocation interaction mechanism has
an activation volume ranging between 102104b3, with the activa-
tion volume and enthalpy varying with strain. A rapid decrease in
the internal stress with temperature (see Fig. 10) indicates that
softening is connected with dynamic recovery.
3.4. Impact tests
The observation of fracture surfaces may help to identify operating
fracture mechanism (s) of constituents at different temperatures and
the bonding abilities of their interfaces. The investigation was concen-
trated on the U-notch side of the fracture surface, where bending stres-
ses are assumed to be generated during the impact testing. Specimens
were fractured predominantly in a brittle manner even at 300 C. The
measured fracture energies were almost identical for all temperatures
tested (about 1 J). This implies that on one hand the composite parti-
cles contribute to the stiffness, and on the other hand they serve as
the crack initiators. The main features of fracture surfaces in the inves-
tigated temperature range were similar: brittle fracture of SiCp and
Mg2Si phases (see Figs. 13 and 14) and slightly ductile fracture of the
d-phase (see Figs. 15 and 16).

Fig. 14. (a) Microcracks (arrows) between matrix and SiC particles near the fracture surface at RT; (b) brittle fracture of SiCp (300 C) with serrated interface and (c) teeth in
the surface after delamination of SiCp at RT (SEM).
 Z. Trojanov et al. / Composites Science and Technology 69 (2009) 22562264
Fig. 15. SEM micrograph of specimen failed at 100 C shows the cleavage
transcrystalline fracture of c-phase with ne secondary microcrack (pointed out
by arrows), transcrystalline ductile fracture with ne dimples morphology of
discontinuous precipitate (c + d), and transcrystalline ductile fracture of d-phase.
Cracks were mostly initiated at the Mg2Si phase (Fig. 13). Coarse
dendritic crystals and Chinese script particles failed by the trans-
crystalline cleavage fracture at all temperatures tested. The inter-
face between the d-phase and the Mg2Si is unlikely to be
coherent since the lattice constants and the crystal structures are
different [28]. In spite of this, the bonding strength of the Mg
matrix/Mg2Si interface is high as documented in Figs. 13a and c
and d by comparison of the opposite surfaces of the fractured spec-
imen. It appears that the development of crack within Mg2Si coarse
dendrites is easier than the debonding at the interface. The rest of
Mg2Si phase after rupture is clearly seen in Fig. 13d. The strong
bonding between matrix and Mg2Si may be a result of an
in situ formation. Plastic deformation of the matrix and/or high
velocity of main crack propagation may result in a large number
of secondary cracks in the Mg2Si coarse dendritic crystals as
observed in Fig. 13a. Furthermore, the pyramid-like shape of the
cracks of the Mg2Si dendrites (Fig. 13c) was observed after failure
in the entire temperature range. Notice in Fig. 13b that the
entrapped d-phase inside the brittle fractured primary Mg2Si
coarse dendritic crystal failed plastically.
The second main contribution to the crack propagation comes
from SiCp, Fig. 14. Fracture mechanisms did not change throughout
the temperature range RT to 300 C. In comparison with Mg2Si, SiC
particles cracks are developed mainly by the delamination of
interfaces with the Mg matrix (Fig. 14a). However, trancrystalline
cleavage fracture was observed as well (Fig. 14b). The interface ser-
rations observed by light microscopy (see Fig. 1) and SEM (Fig. 13b)
were revealed after the delamination of SiCp from the matrix in the
form of ne teeth (Fig. 14c).
Fig. 16. Comparison of d-phase breakage at RT (a) and 300 C (b), mechanism for both is transcrystalline ductile fracture with plastically transformed walls (SEM).
2263
Minor contributions to the crack propagation are from the
c-phase, the d-phase and the discontinuous precipitates (Fig. 15).
The transcrystalline cleavage of the c-phase with secondary micro-
cracks and the transcrystalline ductile fracture with the ne
dimples morphology of the discontinuous precipitates (c + d) were
observed in the entire investigated temperature range. It is inter-
esting to note that Grtnerova et al. [33] observed a change in frac-
ture mechanisms of the c-phase from transcrystalline to
interphase cleavage at and above 200 C for AZ91 reinforced by
Safl bres and SiCp. In this study, no change of fracture mecha-
nisms of the c-phase between RT and 300 C was observed. This
may be attributed to the higher amount of more brittle constitu-
ents (Mg2Si Chinese script particles, primary Mg2Si coarse
dendritic crystals, c-phase and discontinuous precipitate).
The nature of d-phase fracture varied with temperature
(Fig. 16a and b) but this change was not signicant; generally
the higher the temperature the more plastic fracture surface,
which corresponds with anticipated activity of other slip systems
at higher temperatures (200 C [34,35]). The fracture mechanism
was identied as transcrystalline ductile with dimples morphology
accompanied by plastically transformed walls. As temperature in-
creased the walls become higher and the dimples spread out. How-
ever, in comparison with [36] the plasticity of walls with
temperature change is not as signicant as in the case of Safl or
hybrid composite. Furthermore, slip bands were not observed on
the walls at higher temperatures as in [36]. The most probable rea-
son for such behaviour is that brittle components present in con-
siderable amount impede the plastic straining of the relatively
ductile matrix. The increased plasticity of the matrix with temper-
ature rise is in agreement with the deformation behaviour
observed in compression (see Fig. 6).
4. Conclusions
The microstructure observation revealed:
 Mg2Si phase is present in two forms: the coarse dendritic crys-
tals and Chinese script type particles.
 Aluminium tends to react at the matrix/SiCp interface.
 The consequence of this reaction is the weak bonding between
SiC particles and matrix.
Mechanical properties:
 The presence of Si in the matrix improves the thermal stability
of the composite at temperatures up to 200 C due to strong
bonding between Mg2Si/matrix.
 A ductility enhancement was found at and above 200 C.
2264 Z. Trojanov et al. / Composites Science and Technology 69 (2009) 22562264
 The strength improvement is very probably due to the increase
of dislocation density (thermal and geometrically necessary
dislocations).
Stress relaxation tests:
 The internal stress estimated from the stress relaxation tests
decreases with increasing deformation temperature.
 The values of the apparent activation volumes are in the order of
101102b3.
Fracture properties:
 The composite studied is very brittle at all temperatures as
proved by impact tests.
 The Mg matrix exhibits a slightly plastically deformed fracture
surface at and above 200 C.
 The main contribution to fracture comes from the primary Mg2Si
dendritic crystals and from the matrix/SiCp interface.
 The effect of SiCp seems to be harmful rather than benecial.
Acknowledgements
This work received a support from the Ministry of Education,
Youth and Sports of the Czech Republic by the project MSM
0021620834. The authors are grateful also for the support offered
by the Czech and Slovak authorities under the Exchange Pro-
gramme MEB 0808116. P.P. and M.C. would like to acknowledge
the nancial support of the Slovak Grant Agency for Science under
the contract VEGA 1/0249/09.
References
[1] Trojanov Z, Grtnerov V, Lukc P, Drozd Z. Mechanical properties of Mg
alloys composites reinforced with short Safl bres. J Alloys Compd
2004;378:1926.
[2] Trojanov Z, Szraz Z, Lbr J, Lukc P. Deformation behaviour of an AS21 alloy
reinforced by short Safl bres and SiC particles. J Mater Sci Technol
2005;162163:1318.
[3] Hassan SF, Gupta M. Development of high performance magnesium nano-
composites using nano-Al2O3 as reinforcement. Mater Sci Eng A
2005;392:1638.
[4] Zheng MY, Wu K, Liang M, Kamado S, Kojima Y. The effect of thermal exposure
on the interface and mechanical properties of Al18B4O33w/AZ91 magnesium
matrix composite. Mater Sci Eng A 2004;372:6674.
[5] Ho KF, Gupta M, Srivatsan TS. The mechanical behavior of magnesium alloy
AZ91 reinforced with ne copper particulates. Mater Sci Eng A
2004;369:3028.
[6] Trojanov Z, Drozd Z, Kdela S, Szraz Z, Lukc P. Strengthening in MgLi
matrix composites. Compos Sci Technol 2007;67:196573.
[7] Trojanov Z, Lukc P, Szraz Z. Strengthening and recovery in AX41 magnesium
alloy reinforced with short Safl bres. Kovove Mater 2007;45:28391.
[8] Raynor GV. The physical metallurgy of magnesium and its alloys. Pergamon
Press; 1959. p. 33.
[9] Okamoto H. In: Massalski TB, editor. Binary alloy phase diagrams. ASM
International; 1990.
[10] Nayeb-Hashemi AA, Clark JB. MgSi (MagnesiumSilicon). In: Massalski TB,
editor. Binary alloy phase diagrams. ASM International; 1990.
[11] Polmear IJ. Magnesium alloys and applications. Mater Sci Technol
1994;10:116.
[12] Dotsentko VI. Stress relaxation in crystals. Phys Status Solidi (b)
1979;93:1143.
[13] Feltham P. Stress relaxation in magnesium at low temperatures. Phys Status
Solidi 1963;3:13406.
[14] Li JCM. Dislocation dynamics in deformation and recovery. Can J Appl Phys
1967;45:493509.
[15] De Batist R, Callens A. On the analysis of stress relaxation experiments. Phys
Status Solidi (a) 1974;21:5915.
[16] Jiang QC, Wang HY, Wang Y, Ma BX, Wang JG. Modication of Mg2Si in MgSi
alloys with yttrium. Mater Sci Eng A 2005;392:1305.
[17] Crawley AF, Milliken KS. Precipitate morphology and orientation relationships
in an aged Mg9% Al1% Zn0.3% Mn alloy. Acta Metall 1974;22:55762.
[18] Candan S. Effect of SiC particle size on corrosion behavior of pressure
inltrated Al matrix composites in a NaCl solution. Mater Lett
2004;58:36015.
[19] Liu Y, Liu X, Xiufang B. Grain renement of MgAl alloys with Al4C3SiC/Al
master alloy. Mater Lett 2004;58:12827.
[20] Takeuchi S, Hashimoto T, Suzuki K. Plastic deformation of Mg2Si with the C1
structure. Intermetallics 1996;4:S14750.
[21] Lee JC, Byun JY, Park SB, Lee HI. Prediction of Si contents to suppress the
formation of Al4C3 in the SiCp/Al composite. Acta Mater 1998;46:177180.
[22] Yoshinaga H, Horiuchi R. On the ow stress of a solid solution Mg Li alloy
single crystals. Trans JIM 1963;4:13441.
[23] Courret A, Caillard D. An in situ study of prismatic glide in magnesium I. The
rate controlling mechanism. Acta Metall 1985;33:144754.
[24] Courret A, Caillard D. An in situ study of prismatic glide in magnesium II.
Microscopic activation parameter.. Acta Metall 1985;33:145562.
[25] Trojanov Z, Grtnerov, Drozd Z, Szraz Z, Lukc P. Short bres and particles
impact on compressive behaviour of an AZ91 alloy. Inter Foundry Res
2008;60:4452.
[26] Lide DR. editor. Handbook of chemistry and physics. 73rd ed.; 19921993.
[27] Arsenault RJ, Shi N. Dislocation generation due to differences between the
coefcients of thermal expansion. Mater Sci Eng 1986;81:17587.
[28] Mabuchi M, Higashi K. Strengthening mechanisms of MgSi alloys. Acta Mater
1996;44:46118.
[29] Milicka K, Trojanov Z, Lukc P. Internal stresses during creep of magnesium
alloys at 523 K. Mater Sci Eng A 2007;462:2159.
[30] Kocks UF, Argon AS, Ashby MF. Thermodynamics and kinetics of slip. Prog
Mater Sci 1975;19:1288.
[31] Ono K. Temperature dependence of dispersed barrier hardening. J Appl Phys
1968;39:18036.
[32] Trojanov Z, Lukc P, Szraz Z. Strengthening and recovery in AX41
magnesium alloy reinforced with short Safl bres. Kovov Mater
2007;45:28391.
[33] Grtnerov V, Chalupov M, Jger A, Trojanov Z. Inuence of temperature on
fracture mechanisms of magnesium composites. Mat Sci Forum
2005;482:3758.
[34] Balk J, Lukc P, Bohlen J, Kainer KU. Effect of temperature on tensile properties
of hot rolled AZ31 Mg alloy sheets. Kovove Mater 2007;45:13540.
[35] Yoo MH, Agnew SR, Morris JR, Ho KM. Non-basal slip systems in HCP metals
and alloys: source mechanisms. Mater Sci Eng A 2001;319321:8792.
[36] Palcek P, Chalupov M, Hadzima B. Cracks propagation in AZ91 and AZ31
magnesium alloys. In: 21th Symposium DanubiaAdria on experimental
methods in solid mechanics, Brijuni/Pula, Croatia, September 2004.