Solid-state and solution structural study of acetylacetone-modified tin(IV) chloride used as a precursor of SnO2 nanoparticles prepared by a sol-gel route

被引:34
作者
Briois, V
Belin, S
Chalaça, MZ
Santos, RHA
Santilli, CV
Pulcinelli, SH
机构
[1] Univ Paris 11, LURE, F-91898 Orsay, France
[2] UNESP, Inst Quim, BR-14800970 Araraquara, SP, Brazil
[3] USP, Inst Quim Sao Carlos, BR-13560970 Sao Carlos, SP, Brazil
关键词
D O I
10.1021/cm040141q
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
The effect of addition of different amounts of acetylacetone (acacH) on the species formed at room temperature and after thermohydrolysis at 70 degreesC for 30 and 120 min of ethanolic SnCl4.5H(2)O solutions is followed by EXAFS spectroscopy at the Sn K-edge. We show that thermohydrolyzed solutions are a mixture of SnO2 nanoparticles and soluble tin polynuclear species. The complexation of the tin molecular precursors by acetylacetonate ligands is evidenced by H-1, C-13, and Sn-119 NMR spectroscopy and EXAFS for a acacH/Sn ratio higher than 2. Single crystals are isolated from solution and the structure, determined by X-ray diffraction, is built up from monomeric Cl-3(H2O)Sn(acac)-H2O units bridged together by hydrogen bonding. The acacH/Sn ratio in solution controls the polycondensation of the hydrolyzed species but not the crystallite size of the SnO2 nanoparticles (similar to2 nm). Because of the major presence of chelated tin mono- and dimeric complexes in solution for acacH/Sn > 2, the condensation is almost inhibited, meanwhile the decrease of amount of chelated complexes for the acacH/Sn < 2 gives rise to an increase of the number of nanoparticles.
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页码:3885 / 3894
页数:10
相关论文
共 41 条
  • [1] Comparative study of SnO2:Sb transparent conducting films produced by various coating and heat treatment techniques
    Aegerter, MA
    Reich, A
    Ganz, D
    Gasparro, G
    Putz, J
    Krajewski, T
    [J]. JOURNAL OF NON-CRYSTALLINE SOLIDS, 1997, 218 : 123 - 128
  • [2] [Anonymous], 1998, PROGRAMS CRYSTAL STR
  • [3] Hydrolysis-condensation behavior of acetylacetone modified tin(IV) tetra tert-amyloxide
    Armelao, L
    Ribot, FO
    Sanchez, C
    [J]. BETTER CERAMICS THROUGH CHEMISTRY VII: ORGANIC/INORGANIC HYBRID MATERIALS, 1996, 435 : 387 - 393
  • [4] Baou W. H., 1956, ACTA CRYSTALLOGR, V9, P515
  • [5] EXAFS AND XRD ANALYSES OF THE STRUCTURAL EVOLUTIONS INVOLVED DURING DRYING OF SNO2 HYDROGELS
    BRIOIS, V
    SANTILLI, CV
    PULCINELLI, SH
    BRITO, GES
    [J]. JOURNAL OF NON-CRYSTALLINE SOLIDS, 1995, 191 (1-2) : 17 - 28
  • [6] EXAFS study of niobium sites in nanocrystalline Nb-doped SnO2 oxide ceramics
    Briois, V
    Pulcinelli, SH
    Santilli, CV
    [J]. JOURNAL OF MATERIALS SCIENCE LETTERS, 2001, 20 (06) : 555 - 557
  • [7] SAXS study of formation and growth of tin oxide nanoparticles in the presence of complexing ligands
    Broussous, L
    Santilli, CV
    Pulcinelli, SH
    Craievich, AF
    [J]. JOURNAL OF PHYSICAL CHEMISTRY B, 2002, 106 (11) : 2855 - 2860
  • [8] SN119 NUCLEAR MAGNETIC RESONANCE SPECTRA
    BURKE, JJ
    LAUTERBUR, PC
    [J]. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1961, 83 (02) : 326 - &
  • [9] THE STRUCTURES OF MONO AND BIS BETA-DIKETONATE TIN(IV) ALKOXIDE COMPLEXES
    CHANDLER, CD
    FALLON, GD
    KOPLICK, AJ
    WEST, BO
    [J]. AUSTRALIAN JOURNAL OF CHEMISTRY, 1987, 40 (08) : 1427 - 1439
  • [10] Synthesis and characterization of crystalline tin oxide nanoparticles
    de Monredon, S
    Cellot, A
    Ribot, F
    Sanchez, C
    Armelao, L
    Gueneau, L
    Delattre, L
    [J]. JOURNAL OF MATERIALS CHEMISTRY, 2002, 12 (08) : 2396 - 2400