Comparison of Titanium Precursors in the Sol-Gel Synthesis of Pb0.5Ba0.5TiO3 Powders and Thin Films

2003 ◽  
Vol 784 ◽  
Author(s):  
Stacey W. Boland ◽  
Sossina M. Haile

ABSTRACTTwo sol-gel processes for producing Pb1-xBaxTiO3 (PBT), a ferroelectric material of interest for sensor and actuator applications, are investigated. Each system incorporates lead nitrate and barium acetate as metal sources and ethylene glycol as a solvent. Diethanolamine is used as a chelating agent for titanium isopropoxide or titanium butoxide. Precursor chemistry was systematically varied and the resulting sols and powders were studied using TGA/DSC, FTIR, and XRD. Thin films were prepared using both precursor sources by spin coating onto single crystal (100) MgO. Spin speed and pyrolysis temperature were optimized to produce oriented thin films with thicknesses of up to approximately 500nm. Sols incorporating titanium isopropoxide and a large excess of diethanolamine were particularly stable against hydrolysis.

2004 ◽  
Vol 19 (5) ◽  
pp. 1492-1498 ◽  
Author(s):  
Stacey W. Boland ◽  
Suresh C. Pillai ◽  
Wein-Duo Yang ◽  
Sossina M. Haile

Solid solution Pb1-xBaxTiO3, with particular emphasis on Pb0.5Ba0.5TiO3, was prepared using a sol-gel process incorporating lead acetate trihydrate, barium acetate, and titanium isopropoxide as precursors, acetylacetone (2,4 pentanedione) as a chelating agent, and ethylene glycol as a solvent. The synthesis procedure was optimized by systematically varying acetylacetone: Ti and H2O:Ti molar ratios and calcination temperature. The resulting effects on sol and powder properties were studied using thermogravimetric analysis/differential scanning calorimetry, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller analysis, and x-ray diffraction (XRD). Crystallization of the perovskite structure occurred at a temperature as low as 450 °C. Thin films were prepared by spin coating on (100) MgO. Pyrolysis temperature and heating rate were varied, and the resultant film properties investigated using field-emission scanning electron microscopy, atomic force microscopy, and XRD. Under optimized conditions, highly oriented films were obtained at a crystallization temperature of 600 °C.


2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Piotr Dulian ◽  
Jan Zajic ◽  
Witold Żukowski

AbstractTiO2 thin films with different surface structure have been prepared from alkoxide solutions by the sol-gel method using different cationic precursors and heat treatment techniques. The effect of using titanium isopropoxide as well as titanium butoxide as a titanium source on the surface structure and photocatalytic activity of the resultant thin films was studied. Significant differences in the rate of hydrolysis and condensation reactions during the sol-gel synthesis were observed for these titanium precursors. This had a direct influence on the morphology of the as-prepared TiO2 films. Higher quality oxide coatings were obtained from titanium isopropoxide. They were characterized by a smaller grain size, improved surface roughness and uniform coverage of the glass substrate. A beneficial effect of calcination process after each sol application cycle in contrast to single step calcination after all dip-coating cycles was observed. Photocatalytic degradation tests showed that methyl orange was decolorized in the presence of all prepared TiO2 films by exposing their aqueous solutions to UV light (λ = 254 nm). The highest photocatalytic activity had the TiO2 layer produced using titanium isopropoxide.


2002 ◽  
Vol 748 ◽  
Author(s):  
Wein-Duo Yang ◽  
Suresh C. Pillai ◽  
Stacey W. Boland ◽  
Sossina M. Haile

ABSTRACTA sol-gel process incorporating lead acetate trihydrate, barium acetate and titanium isopropoxide as precursors, acetylacetone as a chelating agent, and ethylene glycol as a solvent was used to prepare solid solution (Pb0.5,Ba0.5)TiO3. Water content, annealing temperature and heating rate were varied and the resulting effects on material properties were studied using TGA/DSC, FTIR, FESEM and X-ray diffraction. Crystallization of the perovskite structure occurred at a temperature as low as 450°C. Thin films were prepared by spin coating on (100) MgO using the optimized precursor sol. Pyrolysis and anneal temperatures were varied and the resultant film properties investigated. The pyrolysis temperature used to dry the film was found to strongly affect orientation. Under optimized conditions, highly oriented films were obtained at a crystallization temperature of 600°C.


2012 ◽  
Vol 581-582 ◽  
pp. 514-518
Author(s):  
Hong Zhu ◽  
Zhi Jun Guo ◽  
Wein Duo Yang ◽  
Wein Feng Chang

This study investigated the structure, microstructure and optical properties of the highly-oriented lead barium titanate (Pb1-xBaxTiO3, PBT) thin films prepared on MgO (100) substrate by a nonaqueous sol-gel process. The film precursor was synthesized by the modified sol-gel processing from lead acetate, barium acetate, and titanium isopropoxide, acetylacetone as chelating agent, and ethylene glycol as solvent. This stable precursor was formed by acetylacetone chelating with titanium isopropoxide and then mixing the solution of the acetates. The spin-coating technique was used to deposit the PBT films on MgO (100) substrate with different barium contents and various spin-coating numbers, respectively. X-ray diffraction was employed to study the crystal structure of the thin film and field emission scanning electron microscopy was used to characterize the microstructure of the films. Optical properties of the thin films were investigated by Ultraviolet-visible spectrophotometer. All films exhibited a (100) preferred orientation, especially the PB0.5T (3-coating layers) thin film. In the optical properties, the adsorption wavelength shifted to the ultraviolet region with increasing barium.


2003 ◽  
Vol 18 (2) ◽  
pp. 357-362 ◽  
Author(s):  
Mary M. Sandstrom ◽  
Paul Fuierer

Control over crystallographic orientation in thin films is important, particularly with highly anisotropic structures. Because of its ferroelectric nature, the layered perovskite La2Ti2O7 has interesting piezoelectric and electrooptic properties that may be exploited when films are highly textured. Sol-gel films with an orientation factor of greater than 95% were fabricated without relying on epitaxial (lattice-matching) growth from the substrate. Film orientation and crystallization were confirmed by x-ray diffraction, scanning electron microscopy, atomic force microscopy, and optical measurements. The particle sizes in all precursor solutions were measured by dynamic light scattering experiments. Experimental results indicate that film orientation is a function of precursor solution concentration, size of the molecular clusters in the solution, and film thickness.


2003 ◽  
Vol 13 (6) ◽  
pp. 1413-1419 ◽  
Author(s):  
M. Yu ◽  
J. Lin ◽  
J. Fu ◽  
H. J. Zhang ◽  
Y. C. Han

2017 ◽  
Vol 41 (12) ◽  
pp. 4771-4775 ◽  
Author(s):  
Maria R. Catalano ◽  
Anna L. Pellegrino ◽  
Patrizia Rossi ◽  
Paola Paoli ◽  
Paolo Cortelletti ◽  
...  

A new Na(hfa)·tetraglyme adduct has been synthesized and successfully applied, together with the RE(hfa)3·diglyme (RE = Y, Yb, Er) complexes, in the sol–gel synthesis of upconverting hexagonal NaYF4:Yb3+,Er3+ films.


2017 ◽  
Vol 1 (8) ◽  
pp. 1830-1846 ◽  
Author(s):  
Martin Rohloff ◽  
Björn Anke ◽  
Siyuan Zhang ◽  
Ulrich Gernert ◽  
Christina Scheu ◽  
...  

Facile sol–gel synthesis of Mo:BiVO4 thin films with optimized morphology results in reduced surface recombination and enhanced hole transfer efficiency.


2013 ◽  
Vol 832 ◽  
pp. 128-131
Author(s):  
Sharipah Nadzirah ◽  
Uda Hashim

Titania or titanium dioxide (TiO2) thin film has been synthesized via sol-gel method with monoethanolamine (MEA) as a catalyst. The mixing of titanium butoxide as a precursor, ethanol as a solvent and MEA were stirred using magnetic stirrer under ambient temperature [. The TiO2solution prepared then was deposited on SiO2substrates using spin-coater and the coated films were annealed at 600°C. Finally, both before and after annealed TiO2thin films were characterized using Field Emission Scanning Electron Microscopy (FESEM). The obtained results show the different TiO2particles formation before and after annealed.


2009 ◽  
Vol 24 (8) ◽  
pp. 2541-2546 ◽  
Author(s):  
Eisuke Yokoyama ◽  
Hironobu Sakata ◽  
Moriaki Wakaki

ZrO2 thin films containing silver nanoparticles were prepared using the sol-gel method with Ag to Zr molar ratios [Ag]/[Zr] = 0.11, 0.25, 0.43, 0.67, 1.00, 1.50, and 2.33. After dip coating on glass substrate, coated films were annealed at 200 and 300 °C in air. X-ray diffraction peaks corresponding to crystalline Ag were observed, but a specific peak corresponding to ZrO2 was not observed. At the molar ratio [Ag]/[Zr] = 0.25, the particle size of Ag distributed broadly centered at 17 nm for an annealing temperature of 200 °C and at 25 nm for 300 °C. The films annealed in air at 200 °C showed an absorption band centered at 450 nm because of the silver surface plasmon resonance, whereas films heated at 300 °C in air caused a red shift of the absorption to 500 nm. The absorption peak was analyzed using the effective dielectric function of Ag-ZrO2 composite films modeled with the Maxwell-Garnett expression.


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