SELF-PROPAGATING HIGH-TEMPERATURE SYNTHESIS
OF ZIRCONIUM NITRIDE FROM THE ELEMENTS
V. V. Zakorzhevskii,
V. É. Loryan,
I. P. Borovinskaya,
A. V. Kirillov,
and S. N. Sannikova
Translated from Novye Ogneupory, No. 9, pp. 56 – 58, September, 2016.
Original article submitted July 25, 2016.
Research results from the preparation of zirconium nitride powders from the elements via combustion in a lab
oratory reactor are presented. The optimal synthetic conditions for zirconium nitride with respect to charge
composition and initial N
pressure are determined. Test samples of zirconium nitride of purity up to 99.5%
Keywords: self-propagating high-temperature synthesis (SHS), zirconium nitride powder, import
Zirconium nitride powder is widely used as a component
for preparing metal-ceramics and creating protective
wear-resistant or decorative coatings on metal and graphite
and for other purposes because of its unique properties (high
hardness, wear-resistance, heat resistance). Currently, most
zirconium nitride powders are manufactured in furnaces.
This method is energy-intensive and has a lengthy processing
cycle. Increasing requirements for ceramics have tightened
requirements on the quality of the starting powders that, in
turn, required the improvement of existing methods and the
development of new production methods.
Self-propagating high-temperature synthesis (SHS) of
inorganic compounds is a promising direction in technology
development for the production of ceramic powders [1, 2].
SHS is more economical than existing methods because of
the high throughput, flexible production, and simple process
ing cycle. SHS allows syntheses to be carried out over broad
temperature and pressure ranges.
Herein, results of research on the import-replacement
program for the preparation of zirconium nitride powder by
SHS from the elements in an 8-L reactor are presented.
Experiments were performed in an SVS-8 laboratory re-
actor. Starting zirconium (Zr) powders were dried at
50 – 70°C for 24 h. Charge components were weighed using
an electronic balance (±2 g accuracy) and mixed in a 3-L
stainless-steel drum without using grinding spheres.
The reaction boat was covered with a layer of zirconium
nitride that acted as a thermal insulator and barrier protecting
the charge from coming into direct contact with the graphite.
The charge was loaded into the boat and spread into an even
layer 20 – 30 mm thick. Then, the boat with the charge was
placed into the reactor, which was sealed, purged with N
displace oxygen from the reactor, and filled with N
to the re
quired pressure before initiation of the synthesis. The com
bustion time and pressure change in the reactor were moni
tored during the synthesis. After cooling, the sinter was re
moved from the reactor, cleaned, fractured, and milled in a
stainless-steel drum using tungsten carbide spheres.
The morphologies of the zirconium nitride powders were
studied using a LEO 1450 scanning electron microscope
(Carl Zeiss SMT AG Co.). X-ray phase analysis (XPA) was
conducted using a DRON-3M diffractometer and Cu K
diation. Particle-size distributions were determined using a
MicroSizer 201 laser particle-size analyzer.
Refractories and Industrial Ceramics Vol. 57, No. 5, January, 2017
1083-4877/17/05705-0513 © 2017 Springer Science+Business Media New York
Institute of Structural Macrokinetics and Materials Science Prob
lems of the Russian Academy of Sciences, Chernogolovka, Rus