Journal of Alloys and Compounds 739 (2018) 62e68

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Wire electrical discharge machining of 3Y-TZP/Ta ceramic-metal

composites
A. Smirnov a, b, *, P. Peretyagin b, J.F. Bartolome

a
a
Instituto de Ciencia de Materiales de Madrid (ICMM), Consejo Superior de Investigaciones Científicas (CSIC), C/ Sor Juana In

es de la Cruz 3, 28049, Madrid,
Spain
b
Moscow State University of Technology STANKIN, Vadkovskij per. 1, Moscow Oblast, 101472, Moscow, Russian Federation

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

Article history: Dense (>98 th%) and homogeneous ceramic/metal composites were obtained by spark plasma sintering
Received 25 October 2017 (SPS) using ZrO2 and lamellar metallic powder of tantalum (20 vol%) as starting materials. Composites
Received in revised form showed a fracture toughness value of 16 MPa m1/2 mainly due to crack bridging of the elasticeplastic
19 December 2017
deformations of ductile metal particles. This fracture toughness was accompanied by a simultaneous
Accepted 21 December 2017
Available online 22 December 2017
enhancement in damage tolerance and fatigue resistance of 3Y-TZP/Ta composites.
Besides exceptional mechanical properties, SPS sintered 3Y-TZP/Ta composites also showed the elec-
trical conductivity suited to wire electrical discharge machining (WEDM). Therefore, they are suitable to
Keywords:
Ceramic-metal composites
be produced in mechanically performant, complex shape components with the required tolerance while
Spark plasma sintering (SPS) reducing machining costs. The aim of this work was the study of the electrical properties of the materials
Wire electrical discharge machining as well as the characteristics of the machining process and the machined surfaces influence on the
(WEDM) bending strength of composites. The results show that workpieces can be machined with high accuracy
Surface roughness and without a drop in mechanical strength.
© 2017 Elsevier B.V. All rights reserved.

1. Introduction example, ductile-phase toughening, transformation toughening, or

Stabilized zirconia ceramics have been demonstrated to display
the highest strength and toughness amongst oxide ceramics due to
a polymorphic phase transformation that occurs in doped zirconia
and known as phase transformation toughening [1].
Besides exceptional mechanical properties, stabilized zirconia
also showed excellent resistance against erosion, friction and
thermal shock that makes this material very attractive for a wide
range of applications [2] in the fields of manufacturing and cutting
tools [3e5], punches [6], biomedical applications [7,8] and even
automobile and aerospace [9].
Nevertheless, the application of these ceramic materials is still
remained in some cases limited by their high sensitivities to crack
propagation. One of the most effective methods to increase fracture
toughness in monolithic ceramics is to incorporate ductile metal
particles reinforcement [10,11]. The mechanical properties of the
ceramic matrix toughening by means of various mechanisms, for
* Corresponding author. Moscow State University of Technology “STANKIN”,
Vadkovskij per. 1, Moscow, 101472, Russian Federation.
E-mail address: a.smirnov@stankin.ru (A. Smirnov).
crack blunting allow design composite with improved mechanical
performance [12e16].
In the previous studies, it was reported that addition of
tantalum lamellar shape metal particles (20 vol%) allow design
zirconia-metal composite with improved mechanical performance
due to the interactions between transformation toughening of
zirconia and crack bridging mechanisms [17,18]. Moreover, spark
plasma sintered zirconia based ceramic-metal composites were
evaluated from the point of view of their mechanical behavior
under monotonic and cyclic loading with artificial induced flaws.
3Y-TZP/Ta composites have demonstrated simultaneous enhance-
ment in damage tolerance and fatigue resistance [19]. Furthermore,
in our earlier results obtained in an in vitro study [20] suggest that a
new zirconia-Ta biocomposite displays biocompatibility. Despite
the presence of high crack resistance of 3Y-TZP/Ta composites,
another factor limiting the application of these ceramics is the
inability to attain sufficient dimensional control during net-shape
fabrication. Common machining methods for producing ceramic
parts rely on finish machining using diamond tools. However, the
high hardness and brittleness of ceramics makes conventional
machining very difficult or even impossible. Therefore, for
manufacturing of advanced ceramics many different shaping

https://doi.org/10.1016/j.jallcom.2017.12.221
0925-8388/© 2017 Elsevier B.V. All rights reserved.
 A. Smirnov et al. / Journal of Alloys and Compounds 739 (2018) 62e68
technologies can be used. Such shaping technologies can be
pressing (e.g. cold and hot isostatic pressing, uniaxial pressing),
casting (pressureless casting, pressure casting, tape casting),
extrusion, injection moulding, green machining, up to high so-
phisticated processes like rapid prototyping or manufacturing,
freeze gelation, printing technologies and many others [21,22].
However, due to ceramic shrinkage it extremely difficult to fabri-
cate product to final net shape, hence their final cost will be
increased. Thus, in order to obtain sophisticated shaped products
advanced machining methods should be used instead of traditional
machining techniques, because of associated advantages that
include reduced processing costs, reduced waste, high precision,
versatility and degree of automation [23].
Wire electrical discharge machining (WEDM) is such a tech-
nique that can be successfully applied to machining of single-phase
ceramics, cermets and ceramic matrix composites [24]. An impor-
tant feature to remember with WEDM is that it will only work with
materials that are electrically conductive. For being electrical
discharge machinable, the materials' electrical resistivity should be
lower than 100e300 $cm [25]. In case of a composite, a mixture of
conducting and insulating phases becomes conducting when the
volume fraction of conducting phase exceeds a ‘percolation
threshold’ of 16%, the minimum amount to give a continuous path
across the whole sample. This threshold is independent of the size
and shape of the conducting phase, as long as its particles are
equiaxed. If the conducting phase consists of long thin particles, the
chance of contact increases, this reduces the percolation threshold
so that conduction occurs at much lower loading [26e28]. Conse-
quently, electrical discharge machining offers production of intri-
cate ceramic composite parts regardless of their high hardness and
is therefore ideally suited for machining ceramic based composites,
requiring only sufficient electrical conductivity.
In comparison with conventional machining techniques, WEDM
achieves higher removal rates for these materials with respect of
surface integrity and tolerances of below 1 mm have been achieved
as well [25]. However, difficulties also arise with respect to the
surface finish conditions [29,30], the corrosion of these materials
during machining [31], and the influence the machining parame-
ters in the surface damage, i. e. cracks produced within the ther-
mally affected zone (recast layer and adjacent regions) beneath the
shaped surface.
The aim of this study was to assess the WED-machinability of
3Y-TZP/Ta composite obtained by Spark Plasma Sintering (SPS) and
their surface microstructural quality and final strength.
2. Experimental procedure
2.1. Starting materials
Commercially available powders were used as raw materials: (1)
t-ZrO2 polycrystals (3Y-TZP, 3 mol% Y2O3; TZ-3YE, Tosoh Corp.,
Tokyo, Japan), with an average particle size d50 ¼ 0.26 ± 0.05 mm,
and (2) tantalum (99.97% purity, Alfa Aesar, Karlsruhe, Germany)
with an average particle size d50 ¼ 44 mm.
Tantalum raw powder (Fig. 1A) was milled by high-energy
milling that was performed using 3 mm diameter zirconia balls
and teflon vial using isopropyl alcohol as liquid media. A ball-to-
powder weight ratio (BPR) of 8:1 was used. Rotational speed and
milling time were kept constant during all milling operations as
1350 rpm and 4 h, respectively. The aspect ratio of flake-shaped
milled metallic particles was obtained from Scanning Electron
Microscopy (SEM) image analysis. The results showed that flake-
like deformed Ta particles had a mean size of 42 mm with a high
aspect ratio around 50:1 (Fig. 1B).
63
2.2. Powder processing
To fabricate the zirconia matrix reinforced with lamellar Ta
particles, 3Y-TZP powder was wet mixed with 20 vol% of the ball-
milled Ta powder. Details of the ceramic/metal slurry processing
were reported elsewhere [18]. The obtained powder was placed in a
die-punch setup made from isostatic graphite (grade С4, DonCarb
Graphite, Rostov, Russia) and compacted by spark plasma sintering
(SPS, FCT Systeme GmbH, HPD25, Effelder-Rauenstein, Germany) in
vacuum (z1  102 mbar) at 1400  C, applying a heating rate of
200  C/min and a uniaxial pressure of 80 MPa. The final tempera-
ture and pressure were maintained for 3 min. The temperature was
controlled during sintering by a pyrometer situated at the top of the
machine and focused at the center of the blank (3 mm over the top
surface). The as-sintered sample disks showed diameters of 50 mm
and a thickness of approximately 3e4 mm.
2.3. XRD characterization
The tantalum powder before and after milling was analyzed by
X-ray diffraction (XRD). The specimens for the XRD (D8 diffrac-
tometer, Bruker AXS Inc., Madison, WI, USA, Cu-Ka radiation,
wavelength 1.5405981 Å, accelerating voltage 40 kV, beam current
30 mA) measurements were prepared by suspending a small vol-
ume of Ta powder in acetone directly on a Si (510) single-crystal
wafer within a specially made supporting assembly and drying
the suspension by evaporating the acetone. An evenly spread dis-
tribution on Ta powder was observed.
The X-ray diffraction powder and sintered composites patterns
were collected at diffraction angles 2q ranging from 20 to 70 .
Qualitative analyses of the crystal phases were found using the
following Powder Diffraction Files (PDF) from the International
Center for Diffraction Data (ICDD): ICDD-PDF 01-083-0113 (t-ZrO2),
ICDD-PDF 00-024-1165 (m-ZrO2), ICDD-PDF 00-035-0789
(tantalum) and ICDD-PDF 00-35-1193 (Ta2O5). The compounds
formed on the EDM'ed surface were determined through XRD as
well. The amount of m-ZrO2 after WED machining was evaluated
from the XRD diffractograms (2q range 27 e33 ) according to
Garvie and Nicholson method [32]:
 
Im ð111Þ þ Im 1 11
Xm ¼   (1)
Im ð111Þ þ Im 1 11 þ It ð101Þ
where It and Im represent the integrated intensities (areas under the
reflections) of the tetragonal (101)t as well as the monoclinic (111)m
and (111)m reflections. Its volume fraction Vmtot was calculated as
proposed by Toraya et al. [33]:
1:311Xm
Vmtot ¼ (2)
1 þ 0:311Xm
2.4. Microstructural and mechanical characterization
The density of the sintered samples was measured using the
Archimedes' method. The measurements were carried out in
distilled water on an analytical balance (Sartorius YDK01, Goettin-
gen, Germany). Scanning electron microscopy (SEM) characteriza-
tion was carried out on polished down to 1 mm surfaces by a
microscope (Phenom G2, Eindhoven, The Netherlands). The
bending strength, sf, was determined by using the three-point
bending test as specified by the ASTM specification C1161e13
64 A. Smirnov et al. / Journal of Alloys and Compounds 739 (2018) 62e68
Fig. 1. SEM micrograph of tantalum powder before (A) and after wet ball-milling for 4 h (B).
[34]. The tests were performed at room temperature using a uni-
versal testing machine (Shimadzu AutoGraph AG-X 5kN, Japan).
The specimens in the form of bars with dimensions of
3.0  4.0  45 mm3 were loaded to failure with a crosshead speed
of 0.5 mm/min and a span of 40 mm. Some of WEDM cut bars were
directly used as bending test samples, but some others were
traditional prepared and then went to bending test for comparison
purpose. Traditional preparation means that SPS sintered discs
were cut into bars using diamond saw, ground and polished with
1 mm diamond paste. The strength was calculated from the failure
loads, F (N), and the specimen dimensions, using the equation:
3FL
sf ¼
2bh2
where N is the failure load, L is the span, b is the width and h is the
height. The strength results were averaged over 10 specimens. The
formulas and calculation procedures used in the measurements of
fracture toughness (KIc) have been reported in previous publica-
tions [35].
2.5. Measurement of electrical resistance and wire-electroerosion
machining (WEDM)
To measure the electrical resistivity, four point probe method
was used. The four point probe setup consists of four equally spaced
tungsten carbide electrodes. These electrodes have a diameter of
0.4 mm and separated by a distance of 1 mm. A power source with a
high internal resistivity sends a constant current through the two
outer electrodes. The current output can be obtained by an ammeter.
The second set of electrodes is used for sensing and since negligible
current flows in these probes e only voltage drop e thus accurate
resistance is measured. A resistance of the sample between inner
electrodes is the ratio of the voltage registering on the voltmeter to
the value of the output current of the power supply. In the present
work, the electrical resistance of sintered ceramic-metal composites
was measured with a four-wire (Kelvin) connection method using a
separate current source (Keithley 6220, Cleveland, OH, USA) and a
two-channel nanovoltmeter (Keithley 2182A, Cleveland, OH, USA).
Wire EDM experiments on the commercial machine (Seibu
M500SG, Seibu Electric & Machinery Co., Koga, Japan) have been
performed. Commercial thin brass wire electrodes were used
(Osaka Brasscut A500, 0.25 mm diameter). Metallic wire and sin-
tered disk are both electrodes separated by a deionized water with
conductivity of 0.1 mS/cm and subjected to an electric voltage
(270 V) and intensity (0.05 A). The machining via EDM is a multi-
stage process. In order to find optimal working parameters the
system database which includes various parameters (workpiece
material, thickness, wire diameter, etc.) was used. However, ma-
chine manufacturer's manual has not provided enough information
for machining of ceramic-metal composites. For this reason, three
cutting conditions of the wire EDM of the ZrO2-Ta composites were
chosen (Table 1). The input parameters such average working
voltage, average working current and pulse off time were consid-
ered for analysis, while other parameters remain constant.
Optical microscope (Leica, Wetzlarý, Germany) was used to
study WEDM machined pieces and detailed analysis of heat
affected regions has been done by using SEM equipped with the 3D
(3)
Roughness Reconstruction application. The field of view area for
the height map calculation was 490 mm2 (550).
3. Results and discussion
3.1. XRD study
The ball-milled Ta powder can be textured by the milling pro-
cess. This texture of the deformed metal particles is revealed by
XRD (Fig. 2A and B).
A strong preference for the deformed crystallites to have their
(200) reflection parallel to the specimen surface occurred. A strong
preference for the {100} type of lattice planes to be parallel to the
surface was reported for cold-rolled polycrystalline bcc metals [36].
Ball-milling and cold-rolling imply that the material is flattened in
between compressing surfaces; that is, the balls in the ball-milling
equipment used here and both rolls in rolling apparatus. The
texture can be explained as follows. The most particles that
deformed were flattened into flakes, which, after being suspended
in acetone (in the procedure for specimen preparation for XRD
analysis), position on to the Si substrate with strong tendency for
their flat sides to be parallel to the surface of the Si substrate. On the
other hand, the measurements of the Ta powders showed that the
XRD lines become substantially broadened upon ball-milling
(Fig. 2B). This broadening can be ascribed to the introduction of
lattice microstrain.
Fig. 3 shows diffractograms obtained from wet mechanically
mixed 3Y-TZP/Ta powder (A) and from polished surfaces of sintered
composite (B) where the complete conversion of the monoclinic
ZrO2 into tetragonal ZrO2 is revealed.
There were no other or new phases than initial powders' phases
observed. In addition, graphite die-punch setup can act as planar
 A. Smirnov et al. / Journal of Alloys and Compounds 739 (2018) 62e68 65

Table 1 3.2. Microstructural characterization and toughening mechanism

Wire electrical discharge machining parameters.

Machining Average working Average working Off time Dense (>98 th.%) and homogeneous ceramicemetal composites
conditions voltage (V) current (A) (ms) were initially fabricated from 3Y-TZP and tantalum (20 vol%)
1 cut 120 2.1 8 powders. Electron scanning micrographs of polished surface of 3Y-
2 cut 100 1.2 4 TZP/Ta composites are shown in Fig. 4A. Different surface mor-
3 cut 85 0.4 2 phologies can be observed depending on the analyzed orientation:
perpendicular or parallel to the pressure direction applied in SPS
(Fig. 4A and B, respectively).
The metallic particles are preferentially oriented due to the ef-
fect of the applied pressure during spark plasma sintering process.
Moreover, during flexural test the polished surface of the com-
posites was used as the tensile side, i.e. was perpendicular to the
SPS-direction. The tantalum particles are uniformly dispersed in
the matrix and no porosity is observed. It was found that the
addition of 20 vol % of Ta particles to the 3Y-TZP matrix produces
reinforcement effect which appears as increase of fracture tough-
ness up to 16 MPa m1/2. The SEM observations of the fracture sur-
faces showed the major toughening mechanism is the plastic
deformation with further partial debonding of tantalum particles
(Fig. 4B). In earlier studies, have been shown that addition of Ta
particles to the zirconia matrix produces reinforcement effect due
to the anticipated contributions between crack bridging of ductile
phase and 3Y-TZP stress-induced phase transformation, which
appears as increase of fracture crack growth resistance [19].

3.3. Electrical resistivity measurements and WEDM results

Fig. 2. XRD analysis of Ta raw powder before (A) and after milling (B). The 200 and 110
reflections of Ta for an as-received and milled powder. Upon ball-milling, pronounced
texturing and broadening occurs as a result of deformation and the increase of lattice
strain.
Fig. 3. XRD analysis of the 3Y-TZP/Ta powder as prepared (A) and polished surface of
sintered composite (B). Labelling “t” and “m” denotes tetragonal and monoclinic zir-
conia, respectively. “-” marks tantalum metal reflections.
sources of graphitic carbon, the presence of which can affect the
composition of the subsurface layers of the sintered material.
However, the X-ray diffraction patterns do not show the presence of
any carbon-containing phase (carbides) in sintered and polished
samples, as can be seen in Fig. 3B. It is likely that carbon-affected
layer with negligible thickness was removed by polishing from
the sintered compact.
The electrical resistivity of composites was equal to 2  104 ±
1 $cm. This value is about five orders of magnitude lower than the
limit of 100e300 $cm, consequently, the addition of 20 vol% of
conductive phase makes the material suitable for WEDM. Optical
photo of WEDM machined piece with complex geometry is pre-
sented in Fig. 5A.
The machined surface of ceramic-metal composite has been
analyzed by using tabletop SEM and XRD. WEDM process is based
on thermoelectric energy between the work piece and an electrode.
A pulse discharge occurs in a small gap between the work piece and
the electrode and removes the unwanted material from the work-
piece through melting and vaporizing. The machined surface after
third cut was examined using a SEM for detailed analysis. Fig. 5BeD
shows the effects of the wire over the material surface after cutting.
When the distance between electrodes is reduced, the discharge
flows between the two electrodes. Once the discharge starts,
plasma is formed in the neighborhood of the machined front and
there are places where the wire has caused materials fusion
(Fig. 5D). The surface topography of the machined composite is a
recast layer with discharge craters.
The SEM cross-sectional view and corresponding XRD spectrum
image of the EDM surface layer for the 3Y-TZP/Ta ceramic-metal
composite is presented in Fig. 6A and B, respectively.
The XRD pattern showed that the WEDM surface layer consists
of tetragonal and monoclinic zirconia, Tantalum and a minor
amount of Ta2O5. The monoclinic volume fraction for EDM'ed sur-
face was about 68 vol%. Unlike the polished sintered samples in
which the negligible amount (6 vol%) of m-ZrO2 was found, after
WEDM this amount was higher due to the presence of solid solu-
tion of Ta2O5 which enhance destabilization of the zirconia from
the tetragonal to the monoclinic phase, resulting in the formation
of microcracks [37,38]. Therefore, transformed zirconia leads to a
volume increase, stressing the neighboring grains and produces the
micro crack formation on the wire-electrical discharge machined
surface. In addition, cracking could also be attributed to the field of
tensile residual stresses resulting from thermal effects due to the
rapid heating and quenching cycles induced during the WEDM
66 A. Smirnov et al. / Journal of Alloys and Compounds 739 (2018) 62e68

Fig. 4. SEM micrographs of a polished (A) and a fractured (B) surface of 3Y-TZP/Ta composite. Zirconia: dark-gray; tantalum: light-gray inclusions. White arrows show decohesion
between the matrix and the metallic particles. Yellow arrows show plastic deformation of Ta. (For interpretation of the references to colour in this figure legend, the reader is
referred to the Web version of this article.)

process (Fig. 5D). However, the occurrence of surface cracks on the
machined surface after wire-EDM was only evidenced in the recast
layer (Fig. 6A).
The values of average bending strength of WEDM specimens
with surface roughness are presented in Table 2. From these values,
it is obvious that polished samples have the highest bending
strength. Meanwhile for WEDM cut bars strength increase as the
machining parameters and surface roughness decrease. However,
despite that fine polishing can give materials higher strength and
high reliability the difference between strength values is not

Fig. 5. Optical photo of WEDM'em 3Y-TZP/Ta composite (A) with complex geometry. SEM micrograph showing 3Y-TZP/Ta surface finishing (B, C (topographic view) and D). White
arrows show cracks formed on composite's surface machined.
 A. Smirnov et al. / Journal of Alloys and Compounds 739 (2018) 62e68 67

Fig. 6. SEM cross-sectional view (A) and corresponding XRD pattern of the EDM'ed surface (B) after third cut.

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