Powder Metallurgy

ISSN: 0032-5899 (Print) 1743-2901 (Online) Journal homepage: http://www.tandfonline.com/loi/ypom20

Dilatometric sintering study of titanium–titanium

nitride nano/nanocomposite powders

V. V. Dabhade, T. R. Rama Mohan & P. Ramakrishnan

To cite this article: V. V. Dabhade, T. R. Rama Mohan & P. Ramakrishnan (2007) Dilatometric
sintering study of titanium–titanium nitride nano/nanocomposite powders, Powder Metallurgy,
50:1, 33-39

To link to this article: http://dx.doi.org/10.1179/174329007X186390

Published online: 19 Jul 2013.

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 Dilatometric sintering study of titanium–
titanium nitride nano/nanocomposite
powders
V. V. Dabhade1, T. R. Rama Mohan2 and P. Ramakrishnan2
The sintering behaviour of titanium–titanium nitride nano/nanocomposite powders has been
investigated by dilatometry. The nanosized titanium powders (40 nm) were produced by the
attrition milling of micron sized titanium powders (12 mm) in Ar atmosphere while the nanosized
titanium nitride powders (50 nm) were as procured. Two compositions of the nano/nanocomposite
Downloaded by [University of Saskatchewan Library] at 06:35 26 February 2016

powders, i.e. Ti–8TiN and Ti–15TiN (wt-%) were produced by physical mixing and ultrasonifica-
tion. Dilatometry was carried out at a constant rate of 10 K min21 heating to various temperatures
in the range of 450–1250uC followed by holding for 1 h. The effect of nanoTiN reinforcement on
the sintering onset temperature, linear shrinkage, shrinkage rate, activation energy for sintering,
microstructure and grain growth has been reported and discussed.
Keywords: Nano/nanocomposite, Dilatometry, Sintering, Activation energy, Grain growth

List of symbols The development of nanocomposites and nano/

Ao frequency factor (constant)
Q activation energy for sintering, kJ mol21
r shrinkage rate, 1 s21
R universal gas constant, J mol21 K21
t time, s
T temperature, K
Tm absolute melting temperature, K
y5(Dl /lo) linear shrinkage
Introduction
Nano/nanocomposites in general are those composites
in which both the reinforcement and the matrix are in
the nanometric range (,100 nm), while nanocomposites
are those in which either the reinforcement or the matrix
is in the nanometric range (in most cases the reinforce-
ment is nanometric).1,2 The development of nanocom-
posites and nano/nanocomposite has emerged as an
important step in creating a new generation of materials.
These composites have shown improvement in strength/
hardness,3–5 creep resistance6 and fracture toughness.7
Contrary to the drop in the ductility of conventional
composites with increasing strength/hardness, certain
studies have indicated a retention/adequate level of
ductility in nanocomposites4,5,8 with improvement in
strength/hardness.
1
Eco-Materials Lab, Korea Institute of Ceramic Engineering and
Technology (KICET), Seoul, South Korea (formerly Department of
Metallurgical Engineering and Materials Science, Indian Institute of
Technology Bombay, Mumbai 400076, India)
2
Department of Metallurgical Engineering and Materials Science, Indian
Institute of Technology Bombay, Mumbai 400076, India
*Corresponding author, email vvdabhade@gmail.com
nanocomposites by the consolidation of nanocomposite
and nano/nanocomposite powders has emerged as an
important technique in the processing of these compo-
sites. The most challenging problem in nanocomposite
powder consolidation is grain coarsening which results
in the loss of the desired nanostructure, high tendency
for the nanocomposites powders to agglomerate, sig-
nificant interparticle friction, and high reactivity and
associated contamination.9
Consolidation of nano/nanocomposites powders is
even more difficult as compared with that of nanocom-
posites as both the matrix and reinforcement phase are
nanocrystalline. In nano/nanocomposites grain coarsen-
ing of both the nanocrystalline matrix and the nano-
crystalline reinforcement takes place during sintering, so
it is necessary to optimise a sintering cycle for retention
of nanocristallinity of both the matrix and reinforce-
ment. Also during sintering the densification rate of
nano/nanocomposites is not a linear function of the
densification rates of the two components and each
phase has its own densification rate. The impurity
levels in nano/nanocomposites are in general higher as
compared with nanocomposites owing to the nanocrys-
talline matrix phase (nanocrystalline powders in general
have a larger amount of impurities owing to contamina-
tion from the processing). These impurities can lead to a
deleterious effect during the sintering process and affect
the properties of the sintered composite. Interparticle
friction and the tendency for agglomeration are also
higher as both the powders are nanocrystalline.10,11
Although several studies have been conducted on the
densification of nanocomposites,7,12–21 there is scarce
work available on the densification of nano/
nanocomposite powders. The present investigation aims
at studying the sintering behaviour of titanium–titanium

ß 2007 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 24 May 2006; accepted 23 July 2006
DOI 10.1179/174329007X186390 Powder Metallurgy 2007 VOL 50 NO 1 33
 Dabhade et al. Titanium–titanium nitride nano/nanocomposite powders
1 Photograph (TEM) and selected area electron diffrac-
tion (SAED) pattern of nanoTi
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nitride nano/nanocomposite powders by dilatometry.
The effect of nanosized titanium nitride reinforcement
on the sintering onset temperature, linear shrinkage,
shrinkage rate and activation energy, microstructure
and grain growth of nanosized titanium has been
investigated.
Experimental
Raw material
Synthesis of nanosized Ti was carried out on a
laboratory scale by the attrition milling of micron sized
Ti for 40 h under high purity Argon, as reported earlier
in a separate study.22 The average particle size of the
40 h milled nanosized Ti powder produced was y40 nm
as determined from TEM (Fig. 1). The particle sizes of
over 100 particles were determined individually from the
TEM, and their average was taken as the average
particle size. A Philips (CM 200) make instrument was
used for the TEM analysis. The XRD pattern of the
nanosized Ti powder is shown in Fig. 2. A Philips make
X-pert pro XRD with X’celerator instrument was used
in the present investigation with Cu target (l51.54 Å).
Figure 3 shows the differential thermal analysis (DTA)
and thermo gravimetric (TG) curves of nanosized Ti
powder. The DTA was carried out in a Du pont
2 X-ray diffraction pattern of nanoTi
34 Powder Metallurgy 2007 VOL 50 NO 1
3 DTA and TG plots of nanoTi
instrument (9900 model) using a-alumina as the
reference, while the TG was carried out in a Shimadzu
thermal analyser (DT-40). Both DTA and TG were
carried out employing a heating rate of 10 K min21 in
high purity Ar atmosphere, passed over heated (1000uC)
titanium getter to remove the traces of oxygen. The
heating rate and the atmosphere were similar to that
employed during the dilatometry. The chemical analysis
of the powder as obtained by the inductively coupled
plasma atomic emission spectroscopy (ICPAES) showed
major impurities to be that of 0.62Fe, 0.16Cr, 0.1Ni and
0.1Mn (wt-%). A Plasmalab 8440, Labtam Ltd, instru-
ment was used for the ICPAES analysis.
In the present investigation, nanosized TiN powders
of average particle size of 50 nm were used. The particle
size was determined by TEM (Fig. 4) as explained
above. The XRD pattern of the nanosized TiN powder
is shown in Fig. 5. The chemical analysis of the powder
as obtained by ICPAES indicated no impurities in the
detectable limits (,0.01 wt-%).
Compaction and Sintering procedure
Since nanosized powders were involved, extra precau-
tions were taken during powder mixing to ensure that
proper mixing of the reinforcement powder took place
4 Photograph (TEM) and SAED pattern of nanoTiN

5 X-ray diffraction pattern of nanoTiN
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and that minimum agglomeration was present in the
powders before compaction. The two individual pow-
ders were mixed in a mortar and pestle for 5 min
followed by ultrasonic agitation in high purity propanol
followed again by mixing in a mortar and pestle for
3 min. The second mixing in the mortar and pestle was
carried out since the two powders owing to difference in
density settled differentially in the propanol after the
ultrasonic agitation. These treatments were carried out to
minimise the agglomerates in the powders and to ensure
maximum homogeneous mixing of the powders. Two
compositions of Ti–TiN nano/nanocomposites were
prepared by the above method, i.e. nanoTi–8 wt% TiN
and nanoTi–15 wt% TiN.
Cylindrical green compacts (0.4 g) of 6 mm in
diameter and 4 mm in height were prepared from the
powders by uniaxial compaction in a rigid die at a
pressure of 600 MPa. The green compacts were heated
to a fixed temperature at a constant heating rate of
10 K min21, maintained at that fixed temperature for
1 h and then were allowed to cool to ambient under
argon flow. A high purity Ar gas (XL-grade; impurities
O251 ppm, H2O51 ppm, N252 ppm; BOC, Mumbai,
India) was used, passed over heated (1000uC) titanium
getter to remove the traces of oxygen before introduc-
tion in the dilatometer. A Shimadzu (TMA-30) system
was used to perform the dilatometric analysis. The
change in length could be measured with an accuracy of
¡1 mm and the temperature of the sample could be
controlled within ¡1uC.
The nanoTi and Ti–TiN nano/nanocomposite pow-
ders were heated in two steps:
(i) the first step of heating was carried out up to
300uC without allowing any holding time and
then the furnace was switched off. The sample
was allowed to cool to room temperature in the
furnace itself
(ii) in the second step, the sample was heated to the
required sintering temperature and held for 1 h
before furnace cooling.
The first step of heating was carried out to remove the
adsorbed gases in the powders (which lead to huge
expansion during the first heat) and the stresses induced
in the specimens during compaction. The 300uC
temperature was chosen as to avoid sintering that can
take place (this temperature is below the sintering onset
Dabhade et al. Titanium–titanium nitride nano/nanocomposite powders
temperature for nanoTi and the Ti–TiN nano/nanocom-
posites). Sintering was carried out at various tempera-
tures in the range 450–1250uC.
In the subsequent sections, the samples of nanosized
Ti powders are referred to as nanoTi, nanosized TiN as
nanoTiN, nanosized Ti–8 wt-% nanoTiN as nanoTi–
8TiN, nanosized Ti–15 wt-% nanoTiN as nanoTi–
15TiN and Ti–TiN nano/nanocomposites as Ti–TiN
nnc respectively (where nnc implies nano/nanocompo-
sites) as an abbreviated form.
Results and discussion
Powder characterisation
The powder morphology of nanoTi powders was
irregular while that of nanoTiN powder was angular
as seen in the TEM photographs in Figs. 1 and 4. The
SAED of both the powders (Figs. 1 and 4) exhibited a
diffraction ring along with the diffraction spots reveal-
ing the partial amorphous nature of the powders. The
XRD pattern of nanoTi (Fig. 2) shows all major peaks
of Ti along with some minor peaks of TiO2. It is
reported23 that Ti powder particles have a thin oxide
film of the order of 100 Å on their surface. The XRD
pattern of nanoTiN (Fig. 5) shows all major peaks of
TiN along with one minor peak of Ti2N. The non-
stiochiometric Ti2N phase may be present owing to the
metastable/non-equilibrium state of the powder. The
impurity content in nanoTi as explained in the section
on ‘Raw material’ was from the milling media and the
attritor vessel.
The DTA curve for nanoTi (Fig. 3) shows two
exothermic peaks at 264 and 574uC. The peak at
264uC is most likely due to the relieving of stresses in
the milled powders. It should be noted that the attrition
milled powders were highly cold worked owing to the
milling process. The peak at 574uC in nanoTi is most
likely due to the a–b transition. The drop in the
transition temperature (from 882uC for microcrystalline
titanium) can be attributed to the impurities, especially
to Fe (0.62 wt-%), a b stabiliser. Fe was reported to
lower phase transformation temperature to 590uC at
very low concentration level.24 The other impurities, i.e.
Cr and Ni are also b stabilisers. This temperature also
corresponds to the deviation in the slope of the
shrinkage/shrinkage rate curves (Figs. 6 and 7) owing
to a–b transformation in nanoTi. The TGA of nanoTi
(Fig. 3) exhibited a slight weight loss initially, which
may be due to the evaporation of the residual stearic
acid (PCA) present in the powder as well as due to
evolution of the adsorbed gases. Stearic acid was added
in the titanium powder during the attrition milling
process as a process control agent (PCA). A small
amount of it might be present in the milled powder in
spite of the degassing treatment carried out as explained
in the earlier investigation.22 The TGA curve showed a
weight gain at y400uC which stabilised at y700uC
which may have been due to oxidation. This also
corresponds to the DTA peak observed at y700uC
which also seems to be due to oxidation.
Sintering onset temperature
The sintering onset temperature for nanoTi was found
to be 400uC (0.344Tm), that for nanoTi–8TiN to be
406uC (0.347Tm) while for nanoTi–15TiN to be 415uC
(0.352Tm) respectively. The sintering onset temperature
Powder Metallurgy 2007 VOL 50 NO 1 35
 Dabhade et al. Titanium–titanium nitride nano/nanocomposite powders
6 Variation of linear shrinkage (%) with temperature dur-
ing constant rate of heating at 10 K min21 (left side)
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and linear shrinkage (%) with time during isothermal
holding (right side) for specimens made from nanoTi
was determined from the point at which deviation from
linearity during thermal expansion occurred in the
dilatometric curves. The reported onset temperatures
are the average of all the samples heated in the
temperature range of 450–1250uC. The addition of
nanoTiN in nanoTi led to an increase in the sintering
onset temperature, which could be attributed to the
lower sinterability of the nanoTiN as compared with
that of nanosized Ti.
Linear shrinkage and shrinkage rate
During the constant rate of heating (CRH) the linear
shrinkage was determined as a function of temperature
while during isothermal holding it was determined as a
function of time. Figures 6, 8 and 9 show the dilato-
metric curves obtained for heating at a constant rate of
10 K min21 up to various sintering temperatures
followed by holding at that temperature for 1 h for
specimens of nanoTi, nanoTi–8TiN and nanoTi–15TiN
respectively. The left portion of Figs. 6, 8 and 9
represents the dilatometric data during CRH while the
7 Variation of shrinkage rate during CRH with sintering
temperature for nanoTi, nanoTi–8TiN and nanoTi–15TiN
36 Powder Metallurgy 2007 VOL 50 NO 1
8 Variation of linear shrinkage (%) with temperature dur-
ing CRH at 10 K min21 (left side) and linear shrinkage
(%) with time during isothermal holding (right side) for
specimens made from nanoTi–8TiN
right side portion represents dilatometric data during
holding at sintering temperature.
It can be noticed that during CRH, the observed
shrinkage for all the specimens showed two distinct
slopes. The slope in the first region (450–550uC)
corresponds to a-Ti where the shrinkage was lower,
and the slope in the second region (575–1250uC)
corresponding to b-Ti where the shrinkage was higher.
This is most likely due to the open structure of the b-Ti
phase (bcc) compared with the a-Ti phase (hcp) which is
close packed.
All powders, i.e. nanoTi, nanoTi–8TiN and nanoTi–
15TiN, showed considerably large amount of shrinkage
during CRH than that during isothermal holding.
Figures 6, 8 and 9 indicate that for nanoTi, nanoTi–
8TiN and nanoTi–15TiN specimens, the shrinkage rate
during CRH varied with respect to temperature and
therefore this parameter was plotted as a function of
temperature. Since the individual curves shown in
9 Variation of linear shrinkage (%) with temperature dur-
ing CRH at 10 K min21 (left side) and linear shrinkage
(%) with time during isothermal holding (right side) for
specimens made from nanoTi–15TiN

10 Variation of logarithm shrinkage rate r with inverse
absolute temperature during CRH for specimens
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made from nanoTi, nanoTi–8TiN and nanoTi–15TiN in
the a-Ti and b-Ti range
Figs. 6, 8 and 9 represent the shrinkage obtained at a
single constant heating rate of 10 K min21 ideally all
these should represent a single curve. Therefore averages
of all the shrinkage values at a given temperature were
obtained and were used to determine the shrinkage rate.
The latter is shown as a function of temperature in
Fig. 7 for nanoTi, nanoTi–8TiN and nanoTi–15TiN.
The shrinkage rate was found to decrease with the
addition of nanoTiN to nanoTi owing to the lower
sinterability of the nanoTiN as compared with nanoTi.
Activation energy
Logarithms of shrinkage rates corresponding to a-Ti
region and b-Ti regions are plotted as a function of
inverse absolute temperature as shown in Fig. 10. The
curves obey the equation
y
~r~A0 e{Q=RT (1)
t nanoTi apart from the self-diffusion of Ti, diffusion of
The values of activation energy Q obtained from the
Arrhenius plot of the ln r versus 1/T are shown in
Table 1. The addition of nanoTiN reinforcement in
a 61000; b 620 000
11 Photographs (SEM) of nanoTi–8TiN at two magnifications
Dabhade et al. Titanium–titanium nitride nano/nanocomposite powders
Table 1 Activation energy values obtained from plots of
ln r versus 1/T for nanoTi, nanoTi–8TiN and
nanoTi–15TiN
System Q (a-Ti), kJ mol21 Q (b-Ti), kJ mol21
NanoTi 69¡3 37¡4
NanoTi–8TiN 51¡3 36¡3
NanoTi–15TiN 78¡6 40¡4
nanoTi led to a decrease followed by an increase in the
activation energy.
In the case of nanoTi sintering is only between Ti–Ti
contacts while in the case of nanoTi–8TiN and nanoTi–
15TiN, it is between the Ti–Ti, Ti–TiN and TiN–TiN
contacts. The number of Ti–TiN and TiN–TiN contacts
in nanoTi–15TiN is larger than that in nanoTi–8TiN.
In nanoTi the sintering is only between the Ti–Ti
contacts while in the case of nanoTi–8TiN apart from
the Ti–Ti contacts (self-diffusion); the diffusion of
nitrogen also takes place into Ti from TiN at the Ti/
TiN interfaces. Diffusion of nitrogen is rapid (interstitial
diffusion) as compared with the Ti self-diffusion. The
diffusion of nitrogen into Ti particles from the
interfacial TiN is likely to create new Ti–Ti contacts
and enhance sinterability (lower activation energy).
TiN–TiN contacts are also present but to a lesser extent.
NanoTi–15TiN system is similar to nanoTi–8TiN
system, and the difference is that the TiN–TiN contacts
are likely to be considerable in number which lead to
lower sinterability with subsequent increase in activation
energy as observed. It is also evident that the sintering
required lesser energy in b-Ti region as compared with a-
Ti owing to the more open structure of b-Ti (bcc) as
compared with a-Ti (hcp).
Apart from the role of Ti–Ti, Ti–TiN and TiN–TiN
contacts, titanium also has a thin oxide layer on its
surface which influences sintering. It is reported23 that
titanium has a thin oxide layer (100 Å) on its surface. In
the present case, the oxide content is expected to be
larger (since the titanium powder is nanocrystalline), as
evident in the XRD pattern (Fig. 2). So in the case of
oxygen also takes place in to titanium while in the case
of Ti–TiN nnc self-diffusion of Ti and that of nitrogen
and oxygen into titanium takes place.
Powder Metallurgy 2007 VOL 50 NO 1 37
 Dabhade et al. Titanium–titanium nitride nano/nanocomposite powders
a 61000; b 620 000
12 Photographs (SEM) of nanoTi–15TiN at two magnifications
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The activation energy values, although are valuable,
cannot point out the mechanisms responsible for
sintering. The latter are studied with the help of sintering
models suggested by Johnson and co-workers in another
study by the same research group.25
Microstructure and grain growth
Figures 11 and 12 show the SEM photographs of
nanoTi–8TiN and nanoTi–15TiN compacts sintered at
1000uC respectively. The microstructure of both the
compacts at lower magnification shows a well densified
structure while that at higher magnification shows a
structure of sintered agglomerates and clusters (agglom-
erates of agglomerates). Porosity is also seen between
the agglomerates and clusters in the structure in the
form of inter agglomerate space. It was not possible to
distinguish the nanoTiN reinforcement phase in the
microstructure possibly owing to lower magnifications
involved.
Figure 13 shows the variation of grain size (obtained
from X-ray line broadening) with sintering temperature
for nanoTi, nanoTi–8TiN and nanoTi–15TiN. The
slight drop in the grain size up to 700uC may be due
to recrystallisation, as the nanoTi powder is in a highly
cold worked state owing to the attrition milling. Grain
growth takes place beyond 700uC (0.5Tm) for all the
powders and reaches a maximum of y88 nm at 1200uC.
The addition of nanoTiN reinforcement in nanoTi does
not affect the grain size of the Ti–TiN nnc. The sintered
13 Grain size variation of nanoTi, nanoTi–8TiN and
nanoTi–15TiN as function of sintering temperature
38 Powder Metallurgy 2007 VOL 50 NO 1
compacts are nanocrystalline even after the sintering
process.
Conclusions
The onset of sintering temperature for nanoTi powder
was found to decrease with the addition of nanoTiN
which has been attributed to the poorer sinterability of
the nanoTiN powder at lower temperatures. The linear
shrinkage as well as the shrinkage rate during CRH was
found to decrease with the addition of nanoTiN to
nanoTi. The addition of nanoTiN in nanoTi led to a
decrease followed by an increase in the activation
energy. The microstructure showed a structure of
sintered agglomerates and clusters (agglomerates of
agglomerates) with porosity between the agglomerates
and clusters in the form of inter agglomerate space. The
addition of nanoTiN reinforcement in nanoTi did not
affect the grain size of the nanoTi.
Acknowledgements
The author, V. V. Dabhade, wishes to acknowledge Dr
B. B. Panigrahi and Professor M. M. Godkhindi for
their help in carrying out the dilatometric experiments at
the Department of Metallurgical and Materials Engineer-
ing, Indian Institute of Technology, Kharagpur, India.
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