ISSN 0036-0236, Russian Journal of Inorganic Chemistry, 2016, Vol. 61, No. 5, pp. 545–553. © Pleiades Publishing, Ltd., 2016.
Original Russian Text © V.S. Popov, P.A. Ignatov, A.V. Churakov, E.P. Simonenko, N.P. Simonenko, N.N. Ignatova, V.G. Sevast’yanov, N.T. Kuznetsov, 2016, published in Zhurnal
Neorganicheskoi Khimii, 2016, Vol. 61, No. 5, pp. 572–580.
SYNTHESIS AND PROPERTIES
OF INORGANIC COMPOUNDS
Tin Trifluoroacetylacetonate [Sn(C5H4O2F3)2]
as a Precursor of Tin Dioxide in APCVD Process
V. S. Popova, P. A. Ignatova, A. V. Churakova, E. P. Simonenkoa, b, N. P. Simonenkoa, b,
N. N. Ignatovac, V. G. Sevast’yanova, and N. T. Kuznetsova
aKurnakov Institute of General and Inorganic Chemistry,
Russian Academy of Sciences, Leninskii pr. 31, Moscow, 119991 Russia
bMoscow Institute of Physics and Technology (State University),
9 Institutskiy per., Dolgoprudny, Moscow Region, 141700 Russia
cMoscow State Technical University of Radioengeneering, Electronics, and Automation,
pr. Vernadskogo 78, Moscow, 119454 Russia
e-mail: v_sevastyanov@mail.ru
Received November 2, 2015
Abstract―A new method of synthesis of volatile complex, tin trifluoroacetylacetonate [Sn(C5H4O2F3)2], was
proposed. The prepared compound was identified by IR spectroscopy, CH analysis, X-ray powder diffrac-
tion, and DTA/TGA, the composition was confirmed by MALDI-TOF mass spectrometry, crystal structure
was established. Thin films of tin dioxide on silicon were obtained by atmospheric pressure chemical vapor
deposition using [Sn(C5H4O2F3)2] as a precursor. The morphology and composition of the films were studied
by scanning electron microscopy, EDX elemental analysis, and X-ray powder diffraction. Surface resistance
and light transmission in visible and near IR region were studied.
Keywords: precursor, SnO2, CVD, thin films
DOI: 10.1134/S003602361605017X
Tin dioxide, one of the most required semicon- This compound was obtained in [23, 24] using a com-
ducting materials for gas sensors [1, 2] and solar cell plicated procedure based on alkoxides and substituted
technology, is widely used as a transparent conducting cyclopentadienyl tins, which requires specially prepared
oxide layer [1, 3, 4]. The application of chemical vapor solvents. Using this procedure, [Sn(C5H4O2F3)2] was
deposition approach to the synthesis of tin dioxide at
atmospheric pressure requires a wide series of volatile
stable precursors. As it was shown in a series of works
[5–8], the morphology and properties of coatings
based on tin dioxide produced under identical condi-
tions are dependent on the nature of precursor com-
pound.
synthesized in the work [25], which also reported on
its use as a precursor for preparing SnO2 in O2 flow and
crystal structure of this compound. However, there is
no data in CCDC on the structural characteristics
necessary for the valuable analysis of structural infor-
mation, especially the character of packing in lattice.
Therefore, the aim of this work is to develop a new
Different metal β-diketonates are widely used as simple method for the preparation and isolation of
precursors for the preparation of metallic and oxide [Sn(C5H4O2F3)2] that requires no specially prepared
materials by CVD method [9–17], while the predic-
tion of their volatility is very promising due to analysis
and modeling of their structure [18]. The use of tin(II)
hexafluoroacetylacetonate [Sn(C5HO2F6)2] [19] and
dichloro-bis(2,4-pentadionato)tin(IV) [20–22] as
precursors for the synthesis of tin dioxide by CVD
method is reported in the literature.
solvents and moisture-sensitive initial tin compounds,
to study certain physicochemical properties of
[Sn(C5H4O2F3)2] and its approbation as a precursor
for preparing thin, transparent, and electrically con-
ducting SnO2 films by APCVD method in comparison
with the closest structural analog [Sn(C5HO2F6)2].
It is practically important and urgent task to extend
the scope of stable tin complexes capable of transfer-
ring to gas phase at atmospheric pressure. The analog
of the above mentioned hexafluoroacetylacetonate,
tin(II) trifluoroacetylacetonate, is one of promising
compounds for preparing thin films of SnO2 by atmo-
EXPERIMENTAL
Chemicals used: granulated tin (99.9%, Khimreac-
tiv) was used without additional purification, 1,1,1-tri-
fluoro-2,4-pentanedione
(trifluoroacetylacetone,
spheric pressure chemical vapor deposition (APCVD). 98%, P&M-Invest) was purified by distillation.
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