SYNTHESIS OF NANO-SIZED TITANIUM DIBORIDE
821
TiFe and LaNi , its operation principle is described in
All subsequent work with the titanium diboride thus
obtained was carried out in an argon atmosphere,
including sampling for analysis.
5
detail in [20, 21]. The commercially available fine
crystalline boron of chemically pure grade with
particle size 10–20 μm was preliminary evacuated to a
REFERENCES
–
1
residual pressure of 1.3×10 Pa at 573 K. The
anhydrous borax was prepared by evacuation of
commercial Na B O ·5H O of chemically pure grade
1
2
. Kobayashi, N., Introduction to Nanotechnology,
Moscow: Binom, Laboratoriya Znanii, 2005.
. Nanomaterials Handbook, Gogotsi, T., Ed., USA: CRC
2
4
7
2
–
1
in a vacuum of 1.3×10 Pa at 623 K.
Press, 2006.
Methods of analysis. X-ray studies were perf-
ormed on an automated complex consisting of ADP-2
diffractometer (monochromatic CuK -radiation) The
3
4
. Andrievskii, R.A., Usp. Khim., 2005, vol. 74, no. 12, p. 1163.
. Andrievskii, R.A., Kravchenko, S.E., and Shilkin, S.P.,
α
.
Neorg. Materialy, 1995, vol. 31, no. 8, p. 1048.
error in determining the TiB crystal lattice periods did
2
5
6
7
8
9
. Kravchenko, S.E., Torbov, V.I., and Shilkin, S.P.,
Neorg. Materialy, 2010, vol. 46, no. 6, p. 691.
. Kravchenko, S.E., Torbov, V.I., and Shilkin, S.P., Zh.
Neorg. Khim., 2011, vol. 56, no. 4, p. 1.
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met. Chem., 1993, vol. 444, no. 1, p. 21.
not exceed 0.0003 nm. The coherent scattering region
(
CSR) Dhkl of hexagonal titanium diboride in the
direction perpendicular to the hkl plane was estimated
from the powder diffraction pattern with the Scherrer
formula Dhkl = kλ/βhkl cos θ , where k is the
hkl
anisotropy factor, which in this case was taken equal to
0
.9, λ is X-ray wavelength, λ(CuK = 1.54178 Å, θ is
α
the diffraction angle, and β is the half-width of the
diffraction peak (in radians).
. Rice, G.W., Woodin, R.L., Cho, Y.W., Kim, J.H., and
Oh, K.H, J. Am. Chem. Soc., 1988, vol. 71, no. 4, p. 181.
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Electron microscopic studies were performed on an
autoemission scanning electron microscope Supra 25.
The IR spectra were recorded in the range of 4000–
–
1
6
75 cm on a FT-IR spectrometer Perkin-Elmer Spec-
trum 100 with an ATR attachment. The content of
hydrogen, nitrogen, and oxygen was determined on a
CHNSO-analyzer, content of titanium was determined
by complexometric titration in the presence of xylenol
orange, and boron, by potentiometric titration of mannite-
boric acid with alkali after the deposition of titanium
from the sample solution using conventional technique.
1
1
4. Chen, L.,Gu, Y., Chi, L., Yang, Z., and Ma, J., J. Alloys
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Inorganic and Coordination Compounds, Moscow: Mir,
Experimental procedure. Equimolar amounts of
Ti and B powders were mixed with an excess of
anhydrous borax (Na B O ) in a vibratory mill (drum
1
966.
2
4
7
1
1
6. Lundstrom, T., Arkiv Kemi, 1969, vol. 31, p. 227.
capacity 50 ml, titanium balls, load 1:1, vibration
amplitude 10 mm, frequency 28 Hz) under argon at
7. Ilyushchenko, N.G., Anfinogenov, A.I., and Shurov, N.I.,
Vzaimodeistvie metallov v ionnykh rasplavakh (Interac-
tion of Metals in Ionic Solutions), Moscow: Nauka, 1991.
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Volkova, L.S., Govorkova, L.V., and Mozgina, N.G.,
Zh. Obshch. Khim., 1984, vol. 54, no. 3, p. 491.
2
93 K for 8 h to complete homogenization of the
mixture. Then a sample of the mixture in a corundum
crucible was placed in a quartz reactor of 50 mm
diameter and 500 mm length. The reactor was
1
–
1
evacuated to a residual pressure of 1.3×10 Pa, filled
with argon and heated for a desired time in the
temperature range 973–1088 K. Then the reactor
temperature was brought to room temperature, and the
reaction mixture was ground and successively treated
with distilled water at 343 K, ethyl alcohol and
acetone, and then evacuated to a residual pressure of
1
2
9. Fokin, V.N., Fokina, E.E., and Shilkin, S.P., Zh.
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Volkova, L.S., and Mozgina, N.G., Zh. Obshch. Khim.,
1987, vol. 57, no. 4, p. 729.
2
–
1
1
.3×10 Pa and filled with argon.
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 82 No. 5 2012