Composites Science and Technology 68 (2008) 33963400

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Composites Science and Technology

journal homepage: www.elsevier.com/locate/compscitech

Deformation and failure behavior of a hydrostatically extruded

Zr38Ti17Cu10.5Co12Be22.5 bulk metallic glass/porous tungsten phase
composite under dynamic compression
Y.F. Xue a, H.N. Cai a, L. Wang a,*, F.C. Wang a, H.F. Zhang b, Z.Q. Hu b
a
School of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China
b
Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China

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

Article history: Hydrostatic extrusion of a Zr38Ti17Cu10.5Co12Be22.5 bulk metallic glass/porous tungsten phase composite
Received 25 June 2008 was performed, and the dynamic compressive deformation and fracture behavior of the as-extruded
Received in revised form 11 September 2008 composite were investigated in detail at room temperature by means of the Split Hopkinson Pressure
Accepted 18 September 2008
Bar (SHPB). In comparison with the as-cast composite, the as-extruded composite presented a much
Available online 26 September 2008
higher ow stress without sacricing plasticity under dynamic compression, exhibiting ductility incre-
ment, but evidence of work softening was observed. The specimen for the as-extruded composite failed
Keywords:
by axial splitting with occasional shear fracture in some regions. It is suggested that the increase in ow
Amorphous materials
Mechanical properties
stress and ductility of the as-extruded composite is attributed to the extrusion process which introduced
Fractography hardened condition and texture in the tungsten phase as well as the 3D net structure of the porous tung-
Extrusion sten phase. The work softening mechanism appears to be essentially associated with the large number of
microcracks and voids under dynamic compression.
2008 Elsevier Ltd. All rights reserved.

1. Introduction
Recently, bulk metallic glasses (BMGs) have attracted increasing
attention because of the basic science and potential engineering
application as structural materials. This class of materials has
many promising properties, e.g., extremely high strength and hard-
ness, large elastic strain limit combined with relatively high frac-
ture toughness, as well as good wear and corrosion resistance
[15]. However, BMGs loaded under unconstrained conditions usu-
ally fail catastrophically with little global plasticity [69], which
deformation behavior signicantly limits the application of BMGs
as engineering materials. The motivation to improve the ductility
of these monolithic BMGs leads to the development of BMG based
composites, such as composites reinforced with refractory metals
or metal bers, ceramic particles or carbon nano-tubes, in situ
formed ductile dendritic phase or in situ formed nanocrystals
[1014]. In those composites, the reinforced phase is expected to
hinder the propagation of the single shear band within BMGs
and seed the initiation of multiple shear bands throughout the
specimens. Recently, Zhang et al. [15] and Xue et al. [16] reported
the Zr-based metallic glass/porous tungsten phase composite,
respectively, which exhibited excellent ductility compared to those
* Corresponding author. Tel./fax: +86 10 68913257.
E-mail address: wanglu@bit.edu.cn (L. Wang).
of all the previous tungsten reinforced metallic glass matrix com-
posites both under quasistatic and dynamic compression.
In order to improve the mechanical properties of BMGs, except
for optimizing the composition of alloys and developing compos-
ites, deformation processing could also be available, for example,
cold rolling, swaging, and hydrostatic extrusion. Yokoyama et al.
[17] reported the cold rooling process was concluded to be a valu-
able method for improving the ductility and plasticity of
Zr55Cu30Al10Ni5 BMG. Recently, Xue et al. [18] reported a new Zr-
based metallic glass/porous tungsten phase composite deformed
by hydrostatic extrusion, which exhibited improved strength com-
pared to the as-cast composite under quasistatic compression.
In the present study, hydrostatic extrusion of a Zr38Ti17Cu10.5-
Co12Be22.5 BMG/porous tungsten phase composite was performed
and its effect on microstructure and mechanical properties of the
composite under dynamic compression was investigated.
2. Experimental procedures
Ingots of the Zr38Ti17Cu10.5Co12Be22.5 alloy were prepared by
combining element metals in an induction furnace with the purity
of 99.8% or higher in a Ti-gettered Argon atmosphere. The porous
tungsten with 80 vol.% tungsten was made by power metallurgy,
which is noted that the porous tungsten exhibits a 3D net struc-
ture. The Zr38Ti17Cu10.5Co12Be22.5 BMG/porous tungsten phase
composite was prepared by pressure inltration. The specic

0266-3538/$ - see front matter 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compscitech.2008.09.026
 Y.F. Xue et al. / Composites Science and Technology 68 (2008) 33963400
procedure for making the as-cast composite was described in de-
tail in Ref. [16]. The as-cast composite rods were then hydrostati-
cally extruded at 663 K with section area reductions of 53.8%,
and no further processing was carried out. A detailed description
of preparing the as-extruded composite can be found elsewhere
[18].
The microstructure of the as-extruded composite is shown in
Fig. 1. The micrograph in the plane perpendicular to the extruded
direction is fairly equiaxed; it appears that the dark metallic glass
phase is surrounded by the grey W phase, as seen in Fig. 1a. How-
ever, the longitudinal plane in Fig. 1b shows a strongly elongated
structure in the direction of the extrusion. The X-ray diffraction
patterns of the as-extruded composite are given by Xue et al.
[18], which demonstrate that no other phases were detected with-
in the sensitivity limits of X-ray diffraction.
A wire electro-discharge machine (WEDM) was used to cut
cylindrical specimens 5 mm in diameter and 5 mm in length (the
aspect ratio was kept as 1) from the composite rods and the as-ex-
truded specimen was machined with the long axis parallel to the
extruding direction. A Split Hopkinson Pressure Bar (SHPB) was
used to study the dynamic compressive behavior of the composites
at a strain rate about 103 s1 at room temperature. The details of
the SHPB testing of metals can be found in elsewhere [16]. To en-
sure that the stress state in the BMG specimens reaches equilib-
rium before failure occurs, a copper insert was placed between
the striker bar and the input bar to increase the rise time by shap-
ing the incident pulse. Further details about the mechanical tests of
the pure metallic glass under dynamic compression are given by
Xue et al. [19]. To avoid the repeated impact of the input bar on
the specimen, an aged maraging steel stopper ring was xed to
preserve the fracture surface. Further information on the use of
stopper rings for high strain rate compression testing is given in
Ref. [20].
3. Experimental results
Typical true stresstrue strain curve for the as-extruded com-
posite under dynamic compression is shown in Fig. 2. For compar-
ison, Fig. 2 also shows curves of the pure metallic glass, the pure W,
and the as-cast composite. Both the as-cast composite and the as-
extruded composite show greater plastic deformation and ow
stress than the unreinforced metallic glass and the pure W, respec-
tively. It should be noted that the oscillations in the early part of
the stressstrain curves are a result of the experimental technique
itself due to elastic wave dispersion and lack of stress equilibrium
during the beginning of wave propagation, which do not represent
material behavior. It is noted that the pure W exhibits a gradual
softening behavior after reaching a peak stress level, but compared
to the pure W, the as-cast composite shows greater ow stress and
nearly no work softening behavior up to strain about 20% during
dynamic compressive deformation. Compared to the yield stress
Fig. 1. Micrographs of the as-extruded composite (a) transverse section and (b) longitudinal section.
3397
3000
3.6103 s-1
2500
True stress (MPa)
2000
3.6103 s-1 3.5103 s-1
1500 560s-1
(a) Pure metallic glass
(b) Pure tungsten
1000
(c) As-cast composite
(d) As-extruded composite
5%
(d) (c) (b) (a)
500
True statin
Fig. 2. Typical true stresstrue strain curves of the pure metallic glass, the pure
tungsten, the as-cast composite, and the as-extruded composite.
of 2073 MPa for the as-cast composite, the as-extruded composite
shows a dramatic increased yield stress of 2630 MPa, and the frac-
ture strength also increases from 1960 MPa for the as-cast compos-
ite to 2149 MPa for the as-extruded composite. The ow stress of
the as-extruded composite remains constant up to a true strain
about 0.1 without any appreciable strain hardening and then be-
gins to decrease gradually. It is clear from Fig. 2 that the extrusion
process provides an improvement of ductility without a loss in
plasticity for the present BMG composite under dynamic
compression.
Fractographic analysis reveals that the specimen for the as-ex-
truded composite fractured mainly as a consequence of axial split-
ting with occasional shear fracture in some regions. The axial
splitting fracture surfaces of both as-extruded composite and as-
cast composite are illustrated in Fig. 3. The splitting fracture sur-
face of the as-extruded composite is very hackly with numerous
microcracks (marked by arrows) parallel to the loading direction,
as seen in Fig. 3a. Typical splitting fracture surface of the as-ex-
truded composite at high magnication is shown in Fig. 3b, which
exhibits that the W phase failed mainly by a mixture of intergran-
ular cleavage and transgranular cleavage (arrows). However, com-
pared to the splitting fracture surface of the as-extruded composite
in Fig. 3a at same magnication, there are nearly no splitting
microcracks were formed on the splitting fracture surface of the
as-cast composite under dynamic compression, as seen in Fig. 3c.
Typical higher magnication view corresponding to the region in
Fig. 3c is shown in Fig. 3d, compared to the splitting fracture mor-
phologies of the as-extruded composite in Fig. 3b, the W phase in
the splitting fracture surface of the as-cast composite fractured by
predominately intergranular cracks, transgranular cracks were
only occasionally observed in large W particles. No obvious differ-
ences were observed in the metallic glass phase between the
as-extruded composite and the as-cast composite under dynamic
compression.
3398 Y.F. Xue et al. / Composites Science and Technology 68 (2008) 33963400

Fig. 3. Axial splitting fracture morphologies of the specimens under dynamic compression (a) the image of failed specimens for the as-extruded composite at low
magnication, revealed numerous splitting microcracks (indicated by arrows) on the splitting fracture surface, (b) typical fracture morphology at high magnication in
Fig. 3a, exhibited a mixture of transgranular cleavage and intergranular cleavage in W phase, (c) the image of failed specimens for the as-cast composite at low magnication,
revealed nearly no splitting cracks on the splitting surface and (d) typical higher magnication view corresponding to the region in Fig. 3c revealing the W phase failed mainly
by intergranular cleavage from W grain boundary sources.

The transverse section of the as-extruded composite shows, the

inset in Fig. 4 that macrocracks form quickly, starting at the spec-
imen perimeter and propagating towards the center. The close-up
examination in the macrocrack tip (marked by the rectangle in the
inset to Fig. 4) is shown in Fig. 4, there exists three kinds of fracture
modes in the as-extruded composite: interface dissociation be-
tween tungsten phase and metallic glass phase (marked by arrows
1), tungsten phase separation (marked by arrows 2), including
intergranular cleavage and transgranular cleavage, as shown in
Fig. 3b, and metallic glass phase avulsion (marked by arrows 3).
Both the density of arrows 1 and arrows 2 are greater than that
of arrows 3, respectively, which indicate that the microcracks pre-
ferred to propagate through the tungsten phase or along the inter-
face between the two phases rather than through the metallic glass
phase in the as-extruded composite.
Occasionally, small shear fracture in the as-extruded composite
under dynamic compression could also be found, as seen in the in-
set to Fig. 5, which exhibits that the shear fracture is relatively at.
The typical high magnifying fracture morphology of the shear frac-
Fig. 5. Typical shear fracture morphology at high magnication revealing the area
ture (marked by the rectangle in the inset to Fig. 5) in Fig. 5 shows
marked by the rectangle in the inset covered by the W phase and the metallic glass
that the shear fracture surface covered by two areas which ap- phase which appeared alternately. (Inset: low magnication SEM image of failed
peared alternately: the W phase and the metallic glass phase. specimens for the as-extruded composite on the shear fracture surface under
dynamic compression).

The W phase is sheared smoothly due to shear stress, which is sug-

gested to fracture primarily along the interface between the two
phases. The metallic glass phase softened and owed in the direc-
tion of shear stress, forming liquid ow layers, indicating that the
temperature during shear band failure is much high under dy-
namic compression.

4. Discussion

Fig. 4. SEM polished photograph magnied the crack tip mark by the rectangle in
the inset revealing microcracks propagating mainly along the interface between the
glass phase and the W phase (arrows 1) or in W phase (arrows 2). (Inset: low
magnication SEM image of failed specimens for the as-extruded composite on the
transverse section under dynamic compression).
As seen in Fig. 2, compared to the pure W, the as-cast composite
exhibits nearly same yield point but greater ow stress and
fracture strain under dynamic compression, which indicate that
the W phase plays a dominant role in the deformation of the as-
 Y.F. Xue et al. / Composites Science and Technology 68 (2008) 33963400
cast composite due to its large volume. Compared to the gradual
work softening behavior of the pure W after reaching a peak stress
level, the as-cast composite shows greater ow stress and nearly
no obvious work softening behavior under the same loading case.
The pure Zr38Ti17Cu10.5Co12Be22.5 BMG fractured at about 1.6 GPa
at strain rate of 560 s1, which is lower than that of both the pure
W and the as-cast composite. Xue et al. [21] reported that Zr38Ti17-
Cu10.5Co12Be22.5 BMG shows negative strain rate sensitivity, indi-
cating that 20% vf Zr-based BMG could provide little contribution
to the higher bearing capacity of the as-cast composite at strain
rate about 3.5  103 s1. The description referred above suggests
that the greater ow stress and nearly no obvious work softening
behavior of the as-cast composite in comparison with the work
softening behavior of the pure W under dynamic compression is
attributed to the 3D net structure of the porous tungsten, which
obstructs the micro-shear banding and microcracks propagating
difcult.
In comparison with the true stresstrue strain curve of the as-
cast composite, the as-extruded composite shows much higher
ow stress, one reason may be due to the extrusion process which
induced a hardened condition, containing a higher dislocation den-
sity in W phase. The bonding state at the interface between the W
phase and the metallic glass phase and the dislocation density in
the W phase for the as-extruded composite had been examined
by TEM in Ref. [19], which exhibit a more stable interface between
the two phases and a higher dislocation density in the W phase
compared to the as-cast composite.
Lennon and Ramesh [22] performed SHPB experiments on ex-
truded and recrystallized polycrystalline tungsten, and found the
fracture strain of the as-extruded tungsten is lower than that of
the recrystallized tungsten. Ramesh and Coates [23] also observed
that the total plasticity of the swaged 91pct W alloy (WNiFe) is
relatively low in comparison with the as-sintered alloy during dy-
namic compression. However, different phenomena were observed
in the present study. Compared to the fracture strain of 30.0% for
the as-cast composite under dynamic compression, the as-ex-
truded composite shows a comparable fracture strain of 33.5%,
which is considered to be attributed to the change of failure mech-
anism compared to the as-cast composite. Lankford and co-work-
ers [24,25] have also found that micro-structural inuences can
signicantly alter the dynamic deformation and failure of tungsten
heavy alloys.
Xue et al. [16] reported that the as-cast composite failed by a
mixture of one major shear band and axial splitting under dynamic
compression. However, the as-extruded composite fractured by ax-
ial splitting with occasional shear fracture in some regions. The
transition of failure mode for the as-extruded composite may be
attributed to the elongated grain structure (Fig. 1b), which makes
it geometrically very difcult to propagate a crack along the shear
stress direction, but comparably easy to propagate a crack along
the loading direction which is parallel to the grain elongated direc-
tion, as seen in Fig. 3a. Close-up examination of the fracture surface
in the as-extruded composite was performed and discussed later in
this section.
Compared to the smooth splitting fracture surface of the as-cast
composite in Fig. 3c, the microcrack number density is obviously
greater on the splitting fracture surface in the as-extruded compos-
ite in Fig. 3a. Not like the crack propagation of pure W or W alloys
by extrusion along the elongated structure continuously under dy-
namic compression, due to the 3D net structure of the porous tung-
sten for the as-extruded composite obstructing crack propagating
effectively and promoting substantive microcracks initiated,
numerous microcracks were formed. Those microcracks are paral-
lel to each other, not linking together, and distributing uniformly
on the fracture surface. It is proposed that the 3D net structure,
which hinders the crack motion, thereby delays the onset of frac-
3399
ture and increases the plastic strain to failure, is the major reason
for the improved plasticity of the as-extruded composite under dy-
namic compression. It is suggested that much of the stress concen-
tration at the crack tip is taken up by micro-plasticity. Propagation
of those microcracks requires further deformation, since the driv-
ing tensile stress is exhausted continuously corresponding to the
microcrack is initiated and grows. It is likely that those numerous
microcracks absorb a considerable amount of fracture energy and
may accounts for the large fracture strain for the as-extruded com-
posite under dynamic compression.
The numerous microcracks formed in the as-extruded compos-
ite during dynamic compression could also give rise to its gradually
softening behavior. It appears that the observed softening behavior
in the as-extruded composite with increasing strain under dy-
namic compression is due to the competition between the evolu-
tion of the dislocation substructure (work hardening in W phase)
and the development of axial microcracks. A very large number
of uniformly distributed microcracks were formed in the as-ex-
truded composite under dynamic compression, which results in
the softening by microcracks accumulated within the specimen is
greater than that of hardening, so work softening behavior was ob-
served in the as-extruded composite under dynamic compressive
loading case.
From comparison Fig. 3b with Fig. 3d, it is found that the trans-
granular cleavage density for the as-extruded composite under dy-
namic compression is greater than that of the as-cast composite,
which is suggested to be attributed to the h1 1 0i crystallographic
texture in W phase induced by extrusion. Body-centered-cubic
metals (e.g., polycrystalline tungsten) exhibit a fairly strong
h1 1 0i texture in either the rolling, swaging or extrusion direction
[26,27]. It is believed that the as-extruded composite with 80% vf
polycrystalline tungsten also has a fairly strong h1 1 0i crystallo-
graphic texture in extrusion direction. Dmmer et al. [27] reported
that twin formation is associated with transgranular fracture in
tungsten under dynamic compression. Subhash et al. [28] also re-
ported that the deformation of the polycrystalline tungsten in
h1 1 0i orientation under high strain rate loading is characterized
by extensive twinning, and twintwin intersection yielding trans-
granular fracture, however, ne grain polycrystalline specimens
failed in a typical brittle manner with grain boundaries. It is con-
cluded that the increment of transgranular cleavage in W phase
for the as-extruded composite under dynamic compression is
due to the h1 1 0i texture in W phase by extrusion. Based on those
reasons above, the texture in W phase for the as-extruded compos-
ite under dynamic compression which induced the increment of
transgranular cleavage is also suggested to be one reason for the
larger ductility of the as-extruded composite, since the resistance
through a grain body is stronger than that along a grain boundary.
It is interesting to note that during dynamic loading for the as-
extruded composite, localized shearing occurs occasionally within
the specimen. Compared to the shearing fracture surface of the as-
cast composite in Ref. [16], the shearing fracture surface of the
present composite is smoother, especially the metallic glass phase
exhibits more softening behavior, indicting that higher shearing
stress is applied and higher temperature was reached in the local-
ized shearing zones for the as-extruded composite.
5. Conclusion
The deformation and failure behavior of the Zr38Ti17Cu10.5-
Co12Be22.5 BMG/porous tungsten phase composite by hydrostatical
extrusion was investigated under dynamic compression. It is found
that the extrusion process is an effective route to improve the duc-
tility of the Zr38Ti17Cu10.5Co12Be22.5 BMG/porous tungsten phase
composite under dynamic compressive loading case. In compari-
son with the W phase in the as-cast composite fractured by a pre-
3400 Y.F. Xue et al. / Composites Science and Technology 68 (2008) 33963400
dominantly intergranular separation along grain boundaries under
dynamic compression, W phase in the as-extruded composite
failed with mixed intergranular and transgranular cleavage. The
increment of transgranular cleavage in the as-extruded composite
is attributed to the texture in W phase induced by extrusion pro-
cess, which is suggested to play an important role in improving
the ductility of the as-extruded composite under dynamic com-
pression. Except for the hardened condition and texture in the W
phase introduced by extrusion process itself, 3D net structure of
the porous tungsten is also found to be one very important factor
for the plasticity improvement for the as-extruded composite un-
der dynamic compression, which obstructs the crack propagation
effectively and promotes more microcracks formed, thereby delays
the onset of fracture and increases the plastic strain to failure.
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