Barium Titanium Alkoxides for Barium Titanates: Synthesis, Characterization, and Applications

1994 ◽  
Vol 351 ◽  
Author(s):  
Victor W. Day ◽  
Todd A. Eberspacher ◽  
Walter G. Klemperer ◽  
Shurong Liang
Keyword(s):  
Sol Gel ◽  
Solvent Molecule ◽  
X Ray Diffraction ◽  
Aryl Group ◽  
Barium Titanates ◽  
Acidic Conditions ◽  
Moisture Sensitive ◽  
Gel Processing ◽  
Hydrolysis Of ◽  
Alkoxide Precursors

ABSTRACTSeveral new crystalline bimetallic alkoxide precursors for barium titanates processing have been prepared: {[Ba(Solv)2]2[Ti(OAr)6]2} (1) (Solv = coordinated solvent molecule, Ar = aryl group), [Ba(CH2OHCH2OH)4(H20)][Ti(OCH2CH2O)3] (2), Ba[Ti2(OR)9]2 (3) (R = methyl, ethyl, and n-propyl), and [Ba(BzOH)Ti2O(OBz)8]2 (4) (Bz = benzyl). These precursors have been characterized by elemental analysis, IR, NMR, and single-crystal X-ray diffraction techniques. Compound 1 is well-suited for sol-gel processing of BaTiO3 powders and thin films under a variety of conditions. The facile preparation of 2 using relatively inexpensive starting materials makes it a viable alternative for the synthesis of BaTiO3 fine powders. Both compounds 3 and 4 are fairly moisture-sensitive; hydrolysis of these precursors under acidic conditions affords the formation of gels instead of precipitates. The reactivity of 3 toward hydrolysis can be tailored by varying the alkyl group.

Preparation of Multicomponent Ceramic Powders by Sol-Gel Processing

1990 ◽  
Vol 180 ◽  
Author(s):  
J.R. Bartlett ◽  
J.L. Woolfrey
Keyword(s):  
Electron Microscopy ◽  
Sol Gel ◽  
Processing Conditions ◽  
X Ray Diffraction ◽  
Ceramic Powders ◽  
X Ray ◽  
Acidic Conditions ◽  
Powder Properties ◽  
Gel Processing ◽  
Hydrolysis Of

ABSTRACTSol-gel methods have been applied to the production of the multicomponent ceramic, Synroc B. These techniques involved the hydrolysis of a mixture of Ti and Zr, alkoxides peptising to form a sol and subsequent sorption of Al3+, Ba2+ and Ca2+ cations under acidic conditions. Powder properties were examined by a variety of techniques, including electron microscopy, x-ray diffraction, N2 sorption, and differential thermal analysis. The effects of processing conditions on the physical properties of the powders are discussed.

Crystallization of barium titanate thin films synthesized via sol-gel processing

1995 ◽  
Vol 53 ◽  
pp. 258-259
Author(s):  
M. C. Gust ◽  
N. D. Evans ◽  
M. L. Mecartney
Keyword(s):  
Thin Films ◽  
Barium Titanate ◽  
Sol Gel ◽  
X Ray Diffraction ◽  
Independent Films ◽  
X Ray ◽  
Fine Grained ◽  
Diffraction Patterns ◽  
Gel Processing ◽  
Alkoxide Precursors

Sol-gel processing of oxide thin films offers the potential to generate different microstructures by varying process parameters such as water of hydrolysis, chemical precursor, or substrate. For this work, barium titanate (BaTiO3) thin films were prepared by the sol-gel method in order to try and generate different microstructures for dielectric measurements. However, for BaTiOs prepared using alkoxide precursors, the final microstructures of the films were found to be almost process independent. Films using different precursors, different substrates, and different amounts of water of hydrolysis all showed similar TEM microstructures. All the films after final heat treatment were polycrystalline, nanoporous, and randomly oriented BaTiO3; they were also fine-grained, with an average uniform grain size of 25-50 nm (Fig. 1). This fine-grained microstructure has also been observed in other studies of sol-gel derived BaTiO3 thin films. In addition to BaTiO3, electron diffraction patterns showed the presence of trace amounts of rutile TiO2 that were not observed by x-ray diffraction (XRD).

Fabrication and Characterization of Sol-Gel Derived PZT/WO3 Ceramics

2008 ◽  
Vol 55-57 ◽  
pp. 369-372 ◽  
Author(s):  
T. Sreesattabud ◽  
Anucha Watcharapasorn ◽  
Sukanda Jiansirisomboon
Keyword(s):  
Lead Zirconate Titanate ◽  
Sol Gel ◽  
Rhombohedral Phase ◽  
Lead Zirconate ◽  
X Ray Diffraction ◽  
Calcination Process ◽  
Materials Used ◽  
Phase Characterization ◽  
Gel Processing

Lead zirconate titanate/tungsten oxide (PZT/WO3) ceramics were prepared from the powders synthesized by a modified triol sol-gel processing method. In this study, the starting materials used for synthesis of PZT-sol were zirconium (IV) propoxide, titanium (IV) isopropxide, lead (II) acetate trihydrate and 1,1,1,- tris (hydroxymethyl) ethane. To prepare PZT/xWO3 powders (where x = 0, 0.5, 1 and 3 wt%), nano-sized WO3 was ultrasonically dispersed and mixed with the PZT sol, dried and calcined at 600°C for 4 h. X-ray diffraction results indicated that fully crystallized powders were obtained. Phase characterization suggested that at high WO3 concentration, the reaction between PZT and WO3 occurred during the calcination process. To prepare PZT/xWO3 ceramics, the powders were pressed and sintered at 1100°C for 6 h. Phase characterization by XRD indicated that the content of WO3 significantly affected tetragonal-to-rhombohedral phase transition. Microstructure of thermally etched samples showed that increasing the content of WO3 decreased grain size of the ceramics.

scholarly journals Preparation and morphology of porous SiO2 ceramics derived from fir flour templates

2010 ◽  
Vol 75 (3) ◽  
pp. 385-394 ◽  
Author(s):  
Li Zhong ◽  
Tiejun Shi ◽  
Liying Guo
Keyword(s):  
Amorphous Material ◽  
Sol Gel ◽  
Size Distributions ◽  
X Ray Diffraction ◽  
Ordered Structures ◽  
Porous Sio2 ◽  
Pore Size Distributions ◽  
Naoh Solution ◽  
Gel Processing ◽  
Highly Porous

The preparation of SiO2 ceramics with controllable porous structure from fir flour templates via sol-gel processing was investigated. The specific size the fir flour, which was treated with 20 % NaOH solution, was infiltrated with a low viscous silica sol and subsequently calcined in air, which resulted in the formation of highly porous SiO2 ceramics. X-Ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and field emission scanning electron microscopy (FESEM) were employed to investigate the microstructure and phase formation during processing as well as of the SiO2 ceramics. N2 adsorption measurements were used to analyze the pore size distributions (PSD) of the final ceramics. The results indicated that the surface topography was changed and the proportion of the amorphous material was increased in NaOH-treated fir flour. The final oxide products retained ordered structures of the pores and showed unique pore sizes and distributions with hierarchy on the nanoscale derived from the fir flour.

Effect of acidity on the properties of silica-aluminas synthesized by sol-gel method

2020 ◽  
Vol 63 (7) ◽  
pp. 126-132
Author(s):  
Lyubov V. Furda ◽  
◽  
Evgenia A. Tarasenko ◽  
Sofya N. Dudina ◽  
Olga E. Lebedeva ◽  
...  
Keyword(s):  
Surface Area ◽  
Sol Gel ◽  
Molar Ratio ◽  
Active Centers ◽  
Indicator Method ◽  
Synthesis Conditions ◽  
Alkaline Conditions ◽  
Acidic Conditions ◽  
Amphoteric Properties ◽  
Hydrolysis Of

In the present work amorphous silica-aluminas were synthesized by the coprecipitation method during the hydrolysis of an alcohol solution of tetraethoxysilane (with a tetraethoxysilane: alcohol mass ratio of 1: 1) and 6% aqueous solution of aluminum nitrate at pH values of 1, 3, and 10. The Si/Al molar ratio for all synthesized samples were 4.72 (± 0.29). The amorphous character of the investigated materials was confirmed by X-ray phase analysis. According to the results of scanning electron microscopy, it was found that the resulting powders have particles with a size of 1-20 μm. It was shown that the conditions of synthesis affected the specific surface area and porosity of the materials under study. By the method of low-temperature adsorption-thermodesorption of nitrogen it was established that silica-aluminas obtained under acidic conditions were microporous materials. For the sample obtained under alkaline conditions (pH = 10), the contribution of macropores is very significant. A decrease in surface area is observed as the pH of the synthesis increases. The Hammett indicator method was used to identify and quantify surface centers of different acidity. All studied silica-aluminas are characterized by the presence of both Brønsted basic (pKax from 7 to 12.8) and acidic (pKax from 0 to 7) centers, and Lewis basic (pKax from -4.4 to 0) with a pronounced maximum at pKax = 1.02. It was found that the synthesis conditions had a significant effect on the concentration of active centers. The values of the Hammett function are practically the same for the 3 studied silica-aluminas and describe the studied samples as materials of medium acidity. The variety of Lewis and Brønsted centers on the surface indicates the amphoteric properties of the materials under study. This gives the samples the properties of polyfunctional sorbents and catalysts.

XRD Study of the Influence of Heat Treatment on the Microstructure of Sol-Gel Processed ZrO2-Y2O3 Ceramics

1995 ◽  
Vol 398 ◽  
Author(s):  
C. Barrera-Solano ◽  
M. PiÑero ◽  
C. Jiménez-Solís ◽  
L. Gago-Duport
Keyword(s):  
Heat Treatment ◽  
Sol Gel ◽  
X Ray Diffraction ◽  
Profile Function ◽  
Xrd Study ◽  
Different Temperatures ◽  
Hydrolysis Of Metal Alkoxides ◽  
Induced Changes ◽  
Hydrolysis Of ◽  
Controlled Hydrolysis

ABSTRACTYSZ samples containing 5 and 10 mol% of Y203 were prepared by controlled hydrolysis of metal alkoxides. The dried powders were calcined at 800°C and then they were uniaxially pressed and sintered at different temperatures and next heated at 1400°C (∼ 5 MPa) or annealed at 1600°C for 24 h. The quantitative analysis of the experimental X-ray diffraction (XRD) spectra was performed by Whole Pattern Fitting (WPF). A Pseudo-Voigt (Thompson-Cox-Hastings) was used as shape profile function. The respective phase fractions (wt %) were fitted for both solid state solutions using the scale factor. The heat treatment induced changes are discussed.

Sol-gel processing of nanocrystalline haematite thin films

1997 ◽  
Vol 12 (6) ◽  
pp. 1441-1444 ◽  
Author(s):  
L. Armelao ◽  
A. Armigliato ◽  
R. Bozio ◽  
P. Colombo
Keyword(s):  
Electron Microscopy ◽  
Thin Films ◽  
Transmission Electron Microscopy ◽  
Raman Spectroscopy ◽  
Sol Gel ◽  
X Ray Diffraction ◽  
Single Particles ◽  
X Ray ◽  
Transmission Electron ◽  
Gel Processing

The microstructure of Fe2O3 sol-gel thin films, obtained from Fe(OCH2CH3)3, was investigated by x-ray diffraction (XRD), transmission electron microscopy (TEM), and Raman spectroscopy. Samples were nanocrystalline from 400 °C to 1000 °C, and the crystallized phase was haematite. In the coatings, the α–Fe2O3 clusters were dispersed as single particles in a network of amorphous ferric oxide.

Gel-derived amorphous cesium-aluminosilicate powders useful for formation of pollucite glass-ceramics

1991 ◽  
Vol 6 (2) ◽  
pp. 217-219 ◽  
Author(s):  
Mari A. Hogan ◽  
Subhash H. Risbud
Keyword(s):  
Electron Microscopy ◽  
Sol Gel ◽  
Glass Ceramics ◽  
Amorphous Powder ◽  
Glass Crystallization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Amorphous Powders ◽  
Gel Processing ◽  
Scanning Electron

Amorphous powders in the Cs2O–Al2O3−SiO2 system were prepared by sol-gel processing. Gels made from TEOS, Al-chelate, and Cs-acetate were dried and calcined to obtain molecularly mixed powders of analyzed compositions in the range useful for conversion to pollucite (CsAlSi2O6) glass-ceramics. X-ray diffraction (XRD), differential thermal analysis (DTA), thermogravimetry (TG), and scanning electron microscopy (SEM) were used to characterize the powders. A typical amorphous powder of analyzed chemical composition (in wt.%) = 28.05Cs2O, 37.77SiO2, and 37.96Al2O3 was found to have a glass transition temperature of 945 °C and a glass crystallization temperature of 1026 °C. Preliminary experimental results of densification and crystallization of the amorphous powders show pollucite/mullite phases to be present.

Hydrolysis of aluminium metal and sol–gel processing of nano alumina

2004 ◽  
Vol 58 (24) ◽  
pp. 3063-3066 ◽  
Author(s):  
M Thiruchitrambalam ◽  
V.R Palkar ◽  
V Gopinathan
Keyword(s):  
Sol Gel ◽  
Nano Alumina ◽  
Gel Processing ◽  
Hydrolysis Of ◽  
Aluminium Metal

Dense and optical transparent CdWO4 films by sol-gel processing for scintillation applications

2007 ◽  
Vol 22 (6) ◽  
pp. 1527-1536 ◽  
Author(s):  
H.M. Shang ◽  
M. Bliss ◽  
S. Heald ◽  
T.K. Sham ◽  
F. Heigl ◽  
...  
Keyword(s):  
Sol Gel ◽  
Tungstic Acid ◽  
Cadmium Nitrate ◽  
Sintering Process ◽  
X Ray Diffraction ◽  
X Ray ◽  
Optical Luminescence ◽  
Optically Transparent ◽  
Rapid Sintering ◽  
Gel Processing

In this paper, we report the first successful fabrication of dense and optically transparent cadmium tungstate (CWO) films by sol-gel processing and the study of their optical and x-ray scintillation properties. A new sol-gel processing method was developed using tungstic acid and cadmium nitrate as precursors and hydrogen peroxide as solvent; homogeneous and stable CWO sols were aged at room temperature and used for the preparation of CWO films. A rapid sintering process was investigated and found to be necessary to make dense and optically transparent nanocrystalline CWO films. CWO films were uniform, fully dense, and crack-free, with CWO as the only detectable crystalline phase, as determined by x-ray diffraction. The thickness, density, grain size, and crystallinity of CWO films are all found to be strongly dependent on the sintering conditions and in turn impact the optical and x-ray scintillation properties. Sol-gel-derived dense CWO films demonstrated intense photoluminescence and x-ray excited optical luminescence intensity. The relationships between sol-gel processing, nanostructures, and optical and x-ray scintillation properties are discussed in detail.

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