FT-Raman Spectroscopic Investigations of Titanium Alkoxides with Polymerizable Organic Ligands

2000 ◽  
Vol 54 (3) ◽  
pp. 390-395 ◽  
Author(s):  
A. Gbureck ◽  
U. Gbureck ◽  
W. Kiefer ◽  
U. Posset ◽  
R. Thull

Chelating agents are frequently used in sol-gel chemistry to decrease hydrolytic reactivity and uncontrolled precipitation of titanium alkoxides. The use of polymerizable organic compounds as chelating agents allows for the formation of copolymers consisting of hybrid inorganic/organic networks. The main task of this study was the analytical characterization of new molecular precursors and organically modified titanium oxide films. Methacrylic acid, itaconic anhydride, isoeugenol, and 2-acrylamido-2-methylpropane sulfonic acid were reacted with titanium isopropoxide and titanium ethoxide to form the corresponding chelated alkoxide sols. Thin sol-gel films of these compounds on metal substrates were prepared by dip-coating and studied by Fourier transform (FT) Raman spectroscopy. The spectra were compared to those of the precursors. By means of their characteristic vibrational bands, the presence of polymerizable groups was detected in the coatings. The systems investigated are capable of acting as adhesive promoters in dental applications.

1998 ◽  
Vol 519 ◽  
Author(s):  
M. Hoffmann ◽  
S. Amberg-Schwab ◽  
B. Claflin ◽  
G. Lucovsky

AbstractThe oxygen barrier properties of sol-gel derived inorganic-organic polymer coatings were investigated. By systematic variation of the ratios of the starting compounds and of the curing conditions, materials with different inorganic and organic network densities were obtained. The network densities were characterized using 29Si solid-state NMR and FT-Raman spectroscopy. It was found that the oxygen transmission rates decrease with increasing inorganic as well as organic network density.


1994 ◽  
Vol 341 ◽  
Author(s):  
Nelcy Della ◽  
Santina Mohallem

AbstractThin films of pure barium titanate have been prepared by the sol-gel process from organomettalic sols containing titanium alkoxides and barium acetate (molar ratio [Ba]/[Ti]=l). It leads to transparent, homogeneous and adherent coatings. The influence of various parameters such as chemical concentration, viscosity, withdrawal speed and temperature of densification on film thickness is described. The films were characterized by X-ray diffraction during their heat treatment. Their crystallization temperature was observed to be around 450°C. No variations in the optical properties were observed during the crystallization, and it occurred without the appearance of cracks or pinholes. Tetragonal BaTiO3 structure was observed, and the ferroeletric properties were investigated as functions of thickness and grain size.


2009 ◽  
Vol 609 ◽  
pp. 221-224 ◽  
Author(s):  
S. Kermadi ◽  
N. Agoudjil ◽  
Samira Sali ◽  
R. Tala-Ighil ◽  
M. Boumaour

Application of thin films of SiO2 and TiO2 using the sol-gel process were utilized as antireflection coating on monocrystalline silicon wafers. The aim of this study is to validate this process as a procedure to prepare antireflective films for monocrystalline silicon by dip-coating. The coating was carried out by dip-coating process using tetraethoxysilane (TEOS) as precursor for SiO2 and titanium isopropoxide (TIPT) as precursor for TiO2. In order to study the influence of the thickness on the reflectance and the optical parameters, several coatings with different thickness were deposited onto silicon wafers. The refractive index and the thickness were adjusted by controlling the number of dipping. The refractive index increases from 2.10 up to 2.22 by increasing the film thickness from 36 to 137 nm. It was found that the sample coated with two layers exhibits a lower reflection (1.86 % at λ = 602 nm). This result was improved by a single sub-layer of SiO2 (36.75 nm) to reach 1.08 % at λ = 674 nm). Furthermore, the low values of the extinction coefficient (k) (approach to Zero at λ = 632.8 nm) indicate that TiO2 and SiO2 films deposited by sol-gel method can be used as ARC for Si solar cells.


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.


2008 ◽  
Vol 8 (2) ◽  
pp. 685-688 ◽  
Author(s):  
Hasan Okuyucu ◽  
Paul Inge Dahl ◽  
Mari Ann Einarsrud

LaCoO3 thin film was coated on Al2O3 single crystal by sol–gel route. Appropriate composition of precursors, chelating agents and the solvent put together into a flask and magnetically stirred on a magnetic stirrer. After having the red transparent solution, it was stirred for 12 hours before coating. Ultrasonically cleaned substrate is dipped into the solution and taken immediately into vertical furnace which is preheated at 550 °C. A dense amorphous film is coated on the substrate. Fired amorphous films are annealed at temperature between 900 °C and 1000 °C for 20 minutes in the air. Then coated film was characterized by means of XRD, AFM, and SEM. Conductivity of the film was measured to be −0.1819 for 881 °C for the log σ value by assuming the thickness as 1 μm.


1990 ◽  
Vol 180 ◽  
Author(s):  
S.I. Aoki ◽  
S. C. Choi ◽  
D.A. Payne ◽  
H. Yanagida

ABSTRACTLead titanate fibers were formed from lead acetate and titanium isopropoxide by sol-gel methods. Additions of acids and chelating agents were used to influence hydrolysis and condensation reactions. A variety of solvents were examined, and the effect of conditioning treatments at elevated temperatures were investigated. Data are reported for the rheological behavior of viscous sols, fiber drawing ability, pyrolysis and crystallization of gels and fibers. Features of the ceramic microstructure are reported. A pyroelectric effect was measured for PbTiO3 fibers.


2021 ◽  
Vol 31 ◽  
pp. 25-33
Author(s):  
Affa Rozana Abdul Rashid ◽  
Hani Khaliesah Tazri

We report a fabrication and characterization of ZnO, TiO2 and ZnO:TiO2 composite thin films. The films were prepared on glass substrates by using the dip coating sol-gel method. ZnO was synthesized by using Zinc acetate dehydrated, glacial acetic acid and ethanol. Meanwhile, TiO2 was prepared by using titanium isopropoxide, acetic acid, isopropyl alcohol and methanol. The single sols were mixed with fixed molarity of 0.2 mol to obtain ZnO:TiO2 composite films. The optical properties of metal oxide, such as transmittance, absorbance and band gap were determined using UV-Vis spectrometer. FTIR was used to determine the chemical bonds of the materials. ZnO has the highest transmittance spectra (91%), followed by TiO2 (70%) and ZnO:TiO2 (35%) composite films. The absorbance edge shifted to the longer wavelength for ZnO:TiO2 composite film. The energy band gap of ZnO, TiO2 and ZnO: TiO2 composite were 3.8 eV, 3.6 eV and 3.5 eV, respectively.


2003 ◽  
Vol 18 (3) ◽  
pp. 594-603 ◽  
Author(s):  
Francis J. Allison ◽  
David M. Grant ◽  
Karen McKinlay ◽  
Craig Bailey ◽  
Philip G. Harrison

Sol-gel materials of TiO2 and vanadium-modified TiO2 of nominal composition 4, 8, and 16 wt.% vanadium were prepared by evaporation of aqueous colloidal sols obtained by the hydrolysis of aqueous solutions of titanium(IV) chloride with the appropriate amount of vanadyl oxalate using aqueous ammonia followed by peptization of the resulting hydrated solids using nitric acid. The nature of the sol-gel materials and their behavior on calcinations at temperatures up to 1273 K were investigated using x-ray fluorescence, powder x-ray diffraction, transmission electron microscopy, and electron diffraction and FT-Raman spectroscopy. At 333 K, all the gels comprised small (about 5 ± 1 nm) particles of anatase together with traces of brookite. The particle size changed little on thermal treatment at 573 K, but increased significantly at higher temperatures and was accompanied by transformation to rutile. Incorporation of vanadium in the gels reduced the temperature at which rutile began to appear from 923 K in pure TiO2 to 773 K in the V/TiO2 gels. Only rutile was present at high temperatures, except for the 16 V/TiO2 gel, when small amounts of phase-separated vanadia were also observed. A 2–3% substitutional incorporation of V4+ ions in the tetragonal rutile lattice occurred at high temperatures, but the majority of the vanadium was present in an amorphous, highly dispersed fashion.


1994 ◽  
Vol 346 ◽  
Author(s):  
Olivier Poncelet ◽  
Jean Guilment ◽  
Sylvie Truchet

ABSTRACTHalogenoalkoxides are promising molecular precursors useable in sol-gel technology. They exhibit a lower sensitivity towards hydrolysis than common alkoxides and so appear to be easier to handle. Some data about the structure of titanium chloroalkoxides, pure and with the addition of a controlled amount of water, were obtained using FT-Raman, while the effect of thermal treatment under nitrogen or oxygen was studied using TGA-IR coupling. Finally the oxide products were characterized by Raman and by ED-XRMA, proving mat chloroalkoxides could be used as molecular precursors of oxide by sol-gel process. We showed that TGA-FTIR coupling is a powerful tool in order to study a thermal treatment and could be used to optimize it.


2001 ◽  
Vol 7 (S2) ◽  
pp. 1276-1277
Author(s):  
Y. Akin ◽  
R.E. Goddard ◽  
W. Sigmund ◽  
Y.S. Hascicek

Deposition of highly textured ReBa2Cu3O7−δ (RBCO) films on metallic substrates requires a buffer layer to prevent chemical reactions, reduce lattice mismatch between metallic substrate and superconducting film layer, and to prevent diffusion of metal atoms into the superconductor film. Nickel tapes are bi-axially textured by cold rolling and annealing at appropriate temperature (RABiTS) for epitaxial growth of YBa2Cu3O7−δ (YBCO) films. As buffer layers, several oxide thin films and then YBCO were coated on bi-axially textured nickel tapes by dip coating sol-gel process. Biaxially oriented NiO on the cube-textured nickel tape by a process named Surface-Oxidation- Epitaxy (SEO) has been introduced as an alternative buffer layer. in this work we have studied in situ growth of nickel oxide by ESEM and hot stage.Representative cold rolled nickel tape (99.999%) was annealed in an electric furnace under 4% hydrogen-96% argon gas mixture at 1050°C to get bi-axially textured nickel tape.


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