Wear 259 (2005) 1190–1196

Low content and free cobalt matrixes for diamond tools

S. Spriano a,∗ , Q. Chen a , L. Settineri b , S. Bugliosi c
a Dipartimento di Scienza dei Materiali ed Ingegneria Chimica, Politecnico di Torino-Corso Duca degli Abruzzi, 24-10129 Torino, Italy
b Dipartimento di Sistemi di Produzione ed Economia dell’azienda, Politecnico di Torino-Corso Duca degli Abruzzi, 24-10129 Torino, Italy
c Istituto di Scienza e Tecnologia dei Materiali Ceramici—Consiglio Nazionale delle Ricerche—Strada delle Cacce, 73-10135 Torino, Italy

Received 28 July 2004; received in revised form 21 January 2005; accepted 8 February 2005
Available online 10 May 2005

Abstract

In the present work several titanium alloys were evaluated as matrixes for diamond tools. The purpose is to find new metal matrixes
not containing cobalt or with the amount minimised. Due to the low expansion thermal coefficient of titanium, diamond composites were
produced by pressureless sintering, that means a relevant economic saving. The effect of different Ti–Ni ratio and of small aluminum and
cobalt additions on the mechanical properties of the alloys was investigated. The monolithic metal alloys and diamond composites were
characterized by density measurements. The structure was investigated by X-ray diffraction analysis (XRD), the microstructure by optical and
electron microscopy. Hardness as well as erosion tests were performed as mechanical characterization. The diamond retention capability and
the metal-diamond interface were evaluated by electron microscopy on the fracture surfaces of composites. Crack free composites, presenting
high relative density, were obtained. They show a strong diamond-metal interface. No graphitization evidence on diamond particles was
observed. Hardness value and an erosion resistance comparable with that of hot pressed cobalt was registered in some cases.
© 2005 Elsevier B.V. All rights reserved.

Keywords: Diamond tools; Titanium alloy; Metal matrix composites; Sintering

1. Introduction
Cobalt powders are widely employed in the manufac-
ture of metal matrix diamond tools designed for cutting and
drilling of hard rocks and concrete [1]. Due to high toxic-
ity of cobalt, the exposure to metal powders or to metal dust
during the cutting processes is particularly hazardous [2].
So the main objective is to find new metal matrixes present-
ing no toxic risk [3–5]. Chemical composition of the matrix
should be selected in order to obtain the diamond grains held
firmly by the matrix and to make the matrix abraded at a
rate compatible with the diamond breakdown [6–8]. In this
work three series of samples, presenting different chemical
composition, were prepared and characterized. The first se-
ries include binary Ti–Ni alloys, the second series ternary
Ti–Ni–Co alloys and the third series ternary Ti–Ni–Al al-
loys. Titanium based alloys are not common matrixes for di-
amond tools, while pure titanium was employed for diamond
grit coating [9]. In this study titanium was selected because
it is a carbide former and therefore it should form a strong
interface with diamond by a surface chemical reaction. In
addition titanium has a low expansion thermal coefficient,
so pressureless sintering can be applied, with a relevant eco-
nomic saving. Finally its low elastic modulus can also be
advantageous [10] and some intermetallic compounds con-
taining titanium were recently claimed as high wear resis-
tant materials [11]. Ni was added in order to decrease the
sintering temperature of the material, compared to commer-
cial titanium alloys. In fact the sintering temperature must
be lower than 1000◦ , in order to avoid diamond graphitiza-
tion.
2. Experimental procedure

∗ Corresponding author. Tel.: +39 0115644711; fax: +39 0115644699. Two types of samples were prepared for each series of
E-mail address: silvia.spriano@polito.it (S. Spriano). systems: the monolithic matrix and the diamond impreg-

0043-1648/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.wear.2005.02.076
 S. Spriano et al. / Wear 259 (2005) 1190–1196 1191

Table 1 pressure), isothermal step of 5 min (35 MPa applied pres-

Metal powders used for the sintered materials
Metal Powder size (␮m)
Co 40
Ti-I 150
Ti-II 40
Ni 70
Al 70
nated composite. Commercial powders of pure Ti, Ni, Co,
and Al were used as original materials and their sizes were
listed in Table 1. Batches were sufficiently mixed for a good
homogeneity among different metal components. Synthetic
diamond grains (DeBeers) were employed in composites in
the ratio of 0.35 g/cm3 (1.75 Kt/cm3 ). Diamond grain aver-
age dimension was about 0.7–0.8 mm. Batches were pre-
pared according to the chemical compositions listed in the
Table 2. All samples were prepared via cold press (35 MPa)
of a batch of 2 g. All samples were pressureless sintered in
a vacuum furnace. The sintering temperature was 930 ◦ C,
which is lower than the eutectic temperature in the Ti–Ni
phase diagram (942 ◦ C). The thermal treatment consisted
of a linear heating at 10 ◦ C/min up to the sintering tem-
perature, then an isothermal step of 15, 30 or 60 min at
the sintering temperature and as last a linear cooling at
10 ◦ C/min. In the case of Ti–Ni–Al alloy, the effect of a
second isothermal step (600 ◦ C for 1 h) was also tested (F1-
b, F2-b samples). As reference a pure Co sample was hot
pressed under vacuum by using the following process: linear
heating at 5 ◦ C/min up to 700 ◦ C (8 MPa applied pressure),
linear heating at 80 ◦ C/min up to 900 ◦ C (35 MPa applied
sure).
Pureness (%) After sintering, all samples were characterized by means
99.5 of apparent density measurements by using the Archimedes
99.3 method. Rockwell B hardness measurements were performed
99.9 by using an Officine Galileo hardness tester. In some cases the
99.5
99.5
hardness value was out of the Rockwell B scale. In these cases
Brinell measurement was performed and the obtained value
was converted into the Rockwell B scale: that is why values
higher then 100 are reported. The microstructure of the sin-
tered samples was observed by scanning electron microscopy
(SEM—Leica Stereoscan). Quantitative surface analysis was
performed by energy dispersion spectroscopy (EDS). The
crystallographic structure of the materials was investigated
by X-ray diffraction analysis (XRD—X’Pert Philips Diffrac-
tometer), using the Bragg Brentano camera geometry and the
Cu K␣ incident radiation. The estimated mass fractions of the
phases were calculated by semi-quantitative XRD analysis.
The reference intensity ratio (RIR) values (also called I/Ic val-
ues) were used to perform the calculation. Erosion tests were
performed by using a Falex Air Jet Eroder. The nozzle pres-
sure employed was 207 kPa, the abrasive range was 1 g/min,
the distance between the sample and the nozzle was 10 mm.
The employed abrasive powder was DynablastTM (Norton
Company). Two tests were performed on each sample, by ap-
plying a nozzle-specimen angle of 20 or 90◦ . The tests were
performed at steps of 2 min. The total erosion time was 6 min.
Each specimen was weighed both before and after each step
(METTLER AT 201 balance–precision 0.01 mg). The eroded
volume was then calculated by considering the alloy density.
The erosion rate was calculated by linear fitting of the erosion
volume versus time curves.

Table 2
Chemical composition and properties of the matrix samples
Series Sample code Composition (wt.%) Sintering time (min) Relative density (%) RB hardness
I A Ti90 Ni10 60 87 48
B Ti87 Ni13 60 89 79
C Ti72 Ni28 60 78 116
B1 Ti87 Ni13 15 78 72
B2 30 89 80
B3-(Ti-II) 60 89 79

II D1 Co10 (Ti87 Ni13 )90 15 88 90

D2 30 92 91
D3 60 94 93
E1 Co40 (Ti87 Ni13 )60 15 84 95
E2 30 85 94
E3 60 86 96

III F1-a Al3 (Ti87 Ni13 )97 60 89 86

F1-b (600 ◦ C—1 h) 60 86 83
F2-a Al5 (Ti87 Ni13 )95 60 88 94
F2-b (600 ◦ C—1 h) 60 84 93
Co HP Co 5 97 108
1192 S. Spriano et al. / Wear 259 (2005) 1190–1196
3. Results and discussion
3.1. Ti–Ni alloys: binary matrixes characterization
As previously mentioned, this work began from the study
of series I, i.e. Ti–Ni system, in order to select a suitable ratio
of Ti/Ni. The alloys had a Ni content ranging from 22 wt.%
(eutectic composition) to 10 wt.% (close to bcc solid solution
solvus line) (Table 2). Two methods were used in order to cal-
culate the theoretical density. As first pure element density
was employed. As second semi-quantitative XRD analysis
was employed and the density of the crystallographic phases
was used. The two methods gave quite close results, differing
for less then 4%. Optical and electron microscopy observa-
tions confirm the relative density trend and the sample with
highest Ni content (C sample −28 wt.%) shows a relevant
higher porosity level. It was reported in the literature that
non-uniform diffusion between titanium and nickel will take
place in the binary Ti–Ni system when sintered under the eu-
tectic temperature [12]. Nickel diffuses faster than titanium,
the small nickel particles experience a net loss of atoms and
porosities are created at the prior nickel sites, resulting in the
formation of a skeleton pore network in the sintered struc-
ture. At the same time it was reported that transient liquid
phase formed during sintering can cause swelling in this sys-
tem [13]. So the increment in relative density, registered in
this work, by lowering Ni content and moving away from
the eutectic point is in agreement with literature data. It is
interesting to note that the samples B and B3, which were
prepared by using different titanium powder size (B with Ti-I
and B3 with Ti-II), show the same relative density. XRD anal-
ysis (Fig. 1) shows that two crystalline phases, ␣-Ti (HCP)
and Ti2 Ni, are present in all series I samples. Their recipro-
cal quantities were investigated by semi-quantitative analysis
and the data are listed in Table 3.
Fig. 1. XRD analysis of B, D3, E3 and F2-b samples.
Table 3
Semi-quantitative XRD analysis of the Ti–Ni matrixes
Sample code Sample composition Ti (HCP) Ti2 Ni
(wt.%) (wt.%) (wt.%)
A Ti90 Ni10 65a 35a
70 b 30b
B Ti87 Ni13 55a 45a
60b 40b
C Ti72 Ni28 28a 72a
25b 75b
a Experimental values.
b Theoretical values calculated from the equilibrium phase diagram.
It is seen that the results obtained from the XRD anal-
ysis are close to theoretical values reported on the phase
diagram, which means that during sintering the system has
almost reached the equilibrium condition and that there is
a relevant increment of the intermetallic compound in the
C sample. In Fig. 2 BS-SEM image of the Ti87 Ni13 alloy
(sample B) is reported, quantitative EDS analysis was also
performed. The biphasic aspect of the alloy is evident. The
intermetallic compound is present as thin plates (about 1 ␮m
thick) or bigger irregular crystals about 10 ␮m in diameter.
EDS analysis shows that Ti is present as pure element and that
the Ti/Ni ratio in the intermetallic compound corresponds to
the Ti2 Ni phase (Ti 69%at–Ni31%at). No pure Ni particles
were detected, the Ti/intermetallic interface is continuous and
the reactive sintering process seems to be well developed. By
observing the hardness values, it can be underlined that a
linear hardness increment follows the Ti2 Ni enrichment of
the alloys. In any case the hardness value of the binary al-
loy Ti87 Ni13 , that is the best performing as relative density,
seems to be too low respect to the requested value. As an
experimental reference the hardness of the pure hot pressed
cobalt sample (Table 2) can be considered. The literature re-
ports hardness values of about 96–112 RB in the case of the
Next 300–200–100 hot pressed commercial alloys [14,15].
Fig. 2. SEM microphotograph of a Ti87 Ni13 sintered alloy (B sample). The
light phase is the Ti2 Ni intermetallic compound, the dark matrix is Ti.
 S. Spriano et al. / Wear 259 (2005) 1190–1196
At the same time the amount of intermetallic compound and
Ni content cannot be enhanced, because of porosity matters
related to a high Ni content. Therefore, the ratio of Ti/Ni equal
to 87/13 was considered as the suitable ratio for the further
study carried out. As a consequence, in series II and III and
Co or Al were added to this binary alloy.
3.2. Ti–Ni-Co alloys: ternary matrixes characterization
Because of the good sintering ability and performance
of cobalt as matrix for diamond tools, different amounts
of this metal were added to the Ti87 Ni13 alloy in order to
verify its effect on the mechanical properties and hardness
of the material. In fact no data was available in the lit-
erature about sintering ability and characteristics of these
ternary alloys. So Co10 (Ti87 Ni13 )90 (D1–D2–D3 samples)
and Co40 (Ti87 Ni13 )60 (E1–E2–E3 samples) alloys were pre-
pared. It can be observed that a significant increment both in
relative density and in hardness values is obtained by adding a
10 wt.% of cobalt (series II—D samples—Co10 (Ti78 Ni13 )90 ).
On the other hand a further cobalt increment (series II—E
samples—Co40 (Ti78 Ni13 )60 ) seems to have a detrimental ef-
fect on relative density without a significant hardness incre-
ment. It must also be considered that a 40 wt.% as Co content
is not desirable due Co toxicity. XRD analysis shows the
presence of Ti and Ti2 Ni in the D samples, while in the case
of E samples CoTi was also detected (Fig. 1). These data are
in agreement with the ternary phase diagram. Co probably
forms a Ti2 (Co,Ni) phase that is not detectable by XRD. In
fact Ti2 Ni and Ti2 Co have the same crystallographic struc-
ture and form a solid solution. SEM/EDS analysis for the
Co10 (Ti87 Ni13 )90 alloy (Fig. 3) shows the presence of a pure
Ti phase and of Co–Ti–Ni containing areas. The ratio among
Fig. 3. BS-SEM microphotograph of a Co10 (Ti87 Ni13 )90 sintered alloy
(sample D3). White areas correspond to TiCo phase, the light grey areas
are Ti2 (Co,Ni) phase and the dark grey areas are Ti matrix. Pores appear as
black.
1193
Fig. 4. BS- SEM microphotograph of a Co40 (Ti87 Ni13 )60 sintered alloy
(sample E3). White and lighter grey areas correspond to TiCo and Ti(Co,Ni)
phase, the grey areas are Ti2 (Co,Ni) phase and the dark grey areas are Ti
matrix.
the element was close to Ti 66%at + Co 19%at + Ni 15%at.
This datum confirms the formation of Ti2 (Co,Ni). Small ar-
eas containing Ti–Co in the ratio 50%at/50%at where also
detected as a minority phase. They appear as bright white
areas in the image, while Ti–Ni–Co areas are the grey ones
and the darker areas are Ti-rich zones. In the case of E sam-
ples EDS/SEM analysis reveal that the CoTi intermetallic
compound detected by XRD contains also Ni and it can be
described as a Ti(Co,Ni) phase (Fig. 4). According to this
observation, the ternary phase diagram shows that CoTi and
TiNi form a solid solution.
3.3. Solid solution hardening effect: the Ti–Ni–Al system
Although wear rate does not always correlate directly to
hardness, for many cases of abrasive wear the hardness of
the material can be used for a first selection [3]. As discussed
previously, the Ti–Ni binary system showed a low relative
density and hardness, since Ti is a soft phase and the inter-
metallic compound Ti2 Ni, although producing a significant
hardness increment, does not satisfy the request value. Cobalt
and then aluminum were used to obtain the required proper-
ties as a matrix. While cobalt forms intermetallic compounds,
aluminum is expected to form a solid solution together with
Ti. Also this ternary system was not explored before in sin-
tering literature.
Different quantity of Al were used and the Al5 (Ti87 Ni13 )95
(F2-a, F2-b samples) and Al3 (Ti87 Ni13 )97 (F1-a, F1-b sam-
ples) alloys were prepared These compositions were selected
because of, according to the ternary phase diagrams, they
are inside the biphasic Ti rich solid solution—Ti2 Ni range.
There is a significant increase of hardness for these samples,
in comparison with the binary Ti–Ni system (see Table 1).
By comparing the two Al containing alloys, the hardness is
higher in the alloy with a higher Al content (F2—5 wt.%).
XRD analysis (Fig. 1) shows only two phases in all these
1194 S. Spriano et al. / Wear 259 (2005) 1190–1196
Fig. 5. BS-SEM microphotograph of a Al5 (Ti87 Ni13 )95 alloy (F2-b sample).
Light phase is Ti2 Ni, while the grey matrix is (Ti,Al) solid solution.
samples: Ti and Ti2 Ni. SEM/EDS analysis for the F1-b and
F2-b samples confirms that the microstructure is quite similar
to the binary alloy and that Al has entered into the Ti-rich area
(Figs. 5 and 6). In this respect, the presence of an isothermal
step at 600 ◦ C seems to be relevant. In fact for the samples F1-
a and F2-a, EDS analysis shows the presence of Al both into
the Ti-rich area and into the Ti2 Ni phase. The low temper-
ature isothermal step (600 ◦ C—1 h) was introduced in order
to avoid Al melting during sintering and to enhance its solid
state diffusion before the melting temperature. It is seen that
samples prepared by introducing the isothermal step (F1-b,
F2-b) show a slightly lower relative density and hardness
compared with the samples without isothermal step (F1-a,
F2-a). A part from these slight differences, it must be consid-
ered that the presence of Al only in the Ti rich phase might
be an advantage in order to obtain the maximum hardening
of the soft titanium phase. By comparing the relative density
Fig. 6. SEM image of a fracture surface of a diamond composite (Ti87 Ni13
matrix). A diamond grit well embedded in the metal matrix without cracks.
Metal fragments are observable on it.
values of the ternary Al–Ti–Ni system it can be observed that
they are not so far from the binary Ti87 Ni13 alloy.
4. Effect of different sintering time on the matrix
properties
The effect of different sintering time e.g. 15, 30, and
60 min were carried out for samples with the same chemi-
cal composition (e.g. sample B1, B2, B). It is noted that for
the Ti87 Ni13 alloy, the matrixes sintered in 30 and 60 min (i.e.
B2, B) shows a higher relative density and hardness compared
with the sample sintered in 15 min (i.e. B1). For the D1-2-
3 and E1-2-3 samples, no significant difference was noted
among sintering in different times. XRD analysis confirmed
these data. In the case of the binary alloy, after 15 min of sin-
tering, a large amount of Ti2 Ni has been formed; the increase
in time from 30 to 60 min slightly increases its quantity. Also
by observing SEM images no significant difference in mi-
crostructure can be observed by considering different sinter-
ing times. So it can be concluded that the reaction among the
elemental powders is quite rapid and almost complete after
15 min sintering. In the case of the binary alloy the use of
30 min as sintering time can be useful in order to increase
alloy relative density.
5. Retention of diamond grits by the matrix
A metal binder for diamond tools should, first of all, have
good diamond retention capability. The bond strength at the
interface between the diamond grains and the matrix has to
withstand the stresses developed at the individual diamond
during cutting and the diamonds should not be lost perma-
nently by pull out [4]. When sintered without pressure, as in
our case, the mechanism of bonding may be mainly chemi-
cal bonding, i.e. the metal binder can solve carbon or form
carbides. In this study, the based metal was Ti and it can
form chemical strong bonds with diamond via carbide for-
mation [7]. A different case is when Co is used as metal
binder and the hot pressing process employed. In this case
the thermal coefficient mismatch between Co and diamond
causes a residual stress at the interface, that is responsible
for the retention capability [16,17]. In this study the dia-
mond retention capability and the metal-diamond interface
were evaluated by electron microscopy observations on the
fracture surfaces of composites. Fig. 6 illustrates such eval-
uations in the case of Ti87 Ni13 matrix. It shows a diamonds
grain embedded in the matrix and no fracture at the inter-
face. Metal matrix fragments were detected on the diamonds
grits and EDS analysis carried out also on smooth diamond
surfaces shows the presence of Ti element. This could be
the evidence of the formation of a chemical bond between
matrix and diamonds. Such bond was responsible for hold-
ing the diamonds grains firmly even if they are highly pro-
truding (Fig. 7). In this image it can be also seen the high
 S. Spriano et al. / Wear 259 (2005) 1190–1196
Fig. 7. Diamond grits on the fracture surface of a composite (Ti87 Ni13 ma-
trix).
number of diamond grits embedded on the fracture surface,
that is an evidence of the diamond retention capability of
the metal matrix. Similar observations were made on dia-
mond composites realized by using series II and series III ma-
trixes. No graphitization evidence on diamond particles was
observed
6. Erosion test
The results of the erosion tests are shown in Fig. 8. Tests at
20◦ and 90◦ were performed in order to investigate the erosion
mechanism, considering that vertical impact causes high ero-
sion in fragile materials, while ductile samples are faster worn
away during tests at 20◦ . All the investigated samples show
an erosion rate at 20◦ higher than that at 90◦ , so it can be con-
cluded that none shows a really fragile fracture mechanism.
The Al5 (Ti87 Ni13 )95 alloy (F2b sample) obtained interesting
good results, with an erosion speed only 20% higher than
Fig. 9. SEM images of worn surfaces. (a) Pure Co (HP Co sample); (b) Al5 (Ti87 Ni13 )95 alloy (F2b sample); (c) Ti72 Ni28 (C sample).
1195
Fig. 8. Erosion test data. All the samples were sintered for 60 min at 930 ◦ C.
Samples were ordered on X axis by considering their erosion rate at 20◦ .
that of Co. A further refining of the sintering process might
possibly give higher relative density and still better results in
terms of erosion resistance.
Among the binary components the best results are given by
the Ti87 Ni13 alloy (considering both erosion data at 20◦ and
90◦ ), in accordance with the results of the hardness and den-
sity tests. In the case of the Ti72 Ni28 sample the erosion rate
at 90◦ shows a remarkable increment. SEM observations of
the worn surfaces confirmed that this sample behaves also at
20◦ in more fragile way respect to the other samples (Fig. 9).
This can be related to the high amount of intermetallic com-
pound. This is also the case of the Co10 (Ti87 Ni13 ) alloy, which
present a similar worn surface morphology after tests at 20◦ .
In Fig. 9 the worn surfaces of pure Co and F2-b sample were
also reported. In these cases wear mechanism seams to be
pretty ductile and there is evidence of crawling of alumina
particles. Some alumina particles inserted on the worn surface
were found in the case of pure Co. The difference among F2-a
1196 S. Spriano et al. / Wear 259 (2005) 1190–1196
and -b samples, can be related to the effect of the aluminium
dissolution into the intermetallic compound. In the F2-a case
the worn surface reveals a slight more fragile mechanism.
7. Conclusions
Binary Ti–Ni and ternary Ti–Co–Ni and Ti–Al–Ni alloys
were sinterized and characterized in order to evaluate their
performance as matrix for diamond tools. Free sintering of
elemental powders allows reactive sintering and equilibrium
condition is reached. A good compromise between high hard-
ness, relative density and erosion resistance was found in
the case of a Ti–Al–Ni alloy. All the titanium based alloys
explored show good diamond retention ability and a strong
interface with diamond grits, probably due to a chemical sur-
face reaction, as suggested by Ti presence on the diamond
grits protruding on fracture surfaces.
Acknowledgements
Pro.ba. Forni is acknowledged for the vacuum sintering
furnace kindly supplied. Eurotungstene and DeBeers are ac-
knowledged for the material kindly supplied.
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