0020-1685/03/3903- $25.00 © 2003 MAIK “Nauka /Interperiodica” 0271
Inorganic Materials, Vol. 39, No. 3, 2003, pp. 271–275. Translated from Neorganicheskie Materialy, Vol. 39, No. 3, 2003, pp. 337–341.
Original Russian Text Copyright © 2003 by Ushakov, Red’kin, Zharkov, Solov’ev.
INTRODUCTION
There is considerable technological interest in tita-
nium nitride because it offers a high heat resistance,
superior high-temperature strength, and good corrosion
and wear resistance. However, the use of titanium
nitride is limited because of its high sintering tempera-
ture. One effective way of activating the sintering pro-
cess is by using fine powders [1]. For this reason, ever
increasing attention has recently been paid to the syn-
thesis of ultrafine powders. The most widely used tech-
nique for producing titanium nitride ultrafine powders
is plasma synthesis [2]. Very recently there has been
intense interest in the synthesis of ultrafine powders of
refractory compounds, including titanium nitride, via
evaporation of bulk materials and subsequent deposi-
tion [3]. To evaporate materials, use is made of laser
heating, electron beams, electric flashing of wire, and
other techniques. The ultrafine titanium nitride powders
prepared by such techniques are in a nonequilibrium,
high-energy state. The enhanced activity of such pow-
ders in compaction and sintering processes is due to the
high excess energy associated with the large specific
surface area and high density of structural defects. The
relaxation processes at defects provide an additional
energy and increase the mobility of metal atoms. The
chief drawback of such approaches is poor control over
the deposition process in supersaturated vapor flows
[4]. This reduces the fraction of ultrafine particles,
thereby raising the cost of the final product and affect-
ing the engineering performance of the articles pro-
duced from such powders. The formation of multicom-
ponent compounds upon rapid evaporation of materials
in reactive atmospheres has not yet been studied in suf-
ficient detail.
Low-pressure arc discharges are used mainly to gen-
erate highly ionized plasma consisting of ions supplied
by the electrode material being sputtered [5]. A serious
impediment to wide application of low-pressure arc
discharges for producing ultrafine powders is the for-
mation of large, more than 1 μm in size, particles as a
result of electrode erosion. Nevskii [6] showed that
high-current low-pressure arc discharges have consid-
erable potential for the preparation of ultrafine metal
powders. Heating a mixture of an evaporant and plasma
gas, followed by rapid quenching, allows one to obtain
ultrafine powder with a much narrower particle-size
distribution. Among the many parameters influencing
the properties of ultrafine powders (porosity, nonmetal
inclusions in the cathode, cathode temperature, nature
of the plasma gas, magnetic field, and others), the resid-
ual gas pressure in the vacuum system was shown to be
of prime importance [7]. Increasing the gas pressure in
the system reduces the mean energy of the forming par-
ticles, which allows one to produce materials with dif-
ferent structures, from amorphous to crystalline, and to
control the particle size and shape.
The purpose of this work was to investigate the
effect of gas pressure on the properties of ultrafine tita-
nium nitride powders produced by low-pressure arc-
discharge synthesis.
EXPERIMENTAL AND RESULTS
We used the experimental setup described in detail
previously [8]. The discharge current through the arc
evaporator was 500 A. The longitudinal magnetic field
generated by the focusing coil on the cathode surface
was 0.1 T. As the cathode material, we used commercial
titanium. The chamber was pumped down to 1 mPa and
Effect of Gas Pressure
on the Properties of Electric-Arc Titanium Nitride Powders
A. V. Ushakov*, V. E. Red’kin*, S. M. Zharkov**, and L. A. Solov’ev***
* Krasnoyarsk State Technical University, ul. Akademika Kirenskogo 26, Krasnoyarsk, 660074 Russia
** Kirensky Institute of Physics, Siberian Division, Russian Academy of Sciences,
Akademgorodok, Krasnoyarsk, 660036 Russia
*** Institute of Chemistry and Chemical Technology, Siberian Division, Russian Academy of Sciences,
ul. Karla Marksa 42, Krasnoyarsk, 660049 Russia
e-mail: ushackov@mail.ru
Received November 22, 2001; in final form, March 14, 2002
Abstract—Ultrafine titanium nitride powder is prepared by evaporating titanium in a high-current low-pressure
arc discharge in a mixture of 20% N
2
and 80% Ar. It is shown that increasing the gas pressure to 32 Pa sharply
reduces the particle size and improves the uniformity of the powder in particle size. The possible reasons for
the markedly reduced lattice parameter of ultrafine titanium nitride are discussed.