Synthesis and characterization of surface-protected nanocrystalline titania particles

被引:230
作者
Scolan, E [1 ]
Sanchez, C [1 ]
机构
[1] Univ Paris 06, UMR CNRS 7574, Lab Chim Mat Condensee, F-75252 Paris 05, France
关键词
D O I
10.1021/cm980322q
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
Monodisperse nonaggregated nanoparticles of titania are obtained through hydrolysis at 60 degrees C of titanium butoxide in the presence of acetylacetone and para-toluenesulfonic acid. After the particles are dried, the resulting xerosols can be dispersed without aggregation in water-alcoholic or alcoholic solutions at concentrations higher than 1 M. The characterizations of the nanoparticles were carried out in solution by using quasi-elastic light scattering (QELS); FTIR; C-13, O-17, and H-1 NMR and in solid state by X-ray diffraction, transmission electron microscopy (TEM), FTIR, thermogravimetry-dynamic thermal analysis (TCT-DTA), C-13 cross-polarization-magic angle spinning (CP-NIAS) NMR. The mean size of the anatase oxide core can be adjusted in the 1-5 nm range by a careful tuning of the synthetic conditions. The protection of these particles toward aggregation is ensured through the complexation of the surface by acetylacetonato ligands and through an adsorbed hybrid organic-inorganic layer made with acetylacetone, para-toluenesulfonic acid, and water.
引用
收藏
页码:3217 / 3223
页数:7
相关论文
共 33 条
[1]   CROSS POLARIZATION AND MAGIC ANGLE SAMPLE SPINNING NMR-SPECTRA OF MODEL ORGANIC-COMPOUNDS .3. EFFECT OF THE C-13-H-1 DIPOLAR INTERACTION ON CROSS POLARIZATION AND CARBON-PROTON DEPHASING [J].
ALEMANY, LB ;
GRANT, DM ;
ALGER, TD ;
PUGMIRE, RJ .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1983, 105 (22) :6697-6704
[2]   SYNTHESIS OF HEXAGONALLY PACKED MESOPOROUS TIO2 BY A MODIFIED SOL-GEL METHOD [J].
ANTONELLI, DM ;
YING, JY .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION IN ENGLISH, 1995, 34 (18) :2014-2017
[3]   Si-29 and C-13 NMR investigation of the polysilane-to-poly(carbosilane) conversion of poly(methylchlorosilanes) using cross/polarization and inversion recovery cross-polarization techniques [J].
Babonneau, F ;
Maquet, J ;
Bonhomme, C ;
Richter, R ;
Roewer, G ;
Bahloul, D .
CHEMISTRY OF MATERIALS, 1996, 8 (07) :1415-1428
[4]   O-17 NMR IN SIMPLE OXIDES [J].
BASTOW, TJ ;
STUART, SN .
CHEMICAL PHYSICS, 1990, 143 (03) :459-467
[5]  
BLANCHARD J, 1995, NEW J CHEM, V19, P929
[6]   Characterisation of sol-gel derived titanium oxopolymers:: first evidence of Ti-OH groups through 1H-17O CP NMR experiments [J].
Blanchard, J ;
Bonhomme, C ;
Maquet, J ;
Sanchez, C .
JOURNAL OF MATERIALS CHEMISTRY, 1998, 8 (04) :985-989
[7]  
BRINKER CJ, 1990, SOL GEL SCI PHYSICS
[8]   The Role of Complexing Ligands in the Formation of Non-Aggregated Nanoparticles of Zirconia [J].
Chatry, M. ;
Henry, M. ;
In, M. ;
Sanchez, C. ;
Livage, J. .
JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY, 1994, 1 (03) :233-240
[9]   SOLUTION STRUCTURE ELUCIDATION OF EARLY-TRANSITION-METAL POLYOXOALKOXIDES USING O-17 NUCLEAR-MAGNETIC-RESONANCE SPECTROSCOPY [J].
DAY, VW ;
EBERSPACHER, TA ;
KLEMPERER, WG ;
PARK, CW ;
ROSENBERG, FS .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1991, 113 (21) :8190-8192
[10]   DODECATITANATES - A NEW FAMILY OF STABLE POLYOXOTITANATES [J].
DAY, VW ;
EBERSPACHER, TA ;
KLEMPERER, WG ;
PARK, CW .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1993, 115 (18) :8469-8470