scholarly journals Hybrid Xerogels: Study of the Sol-Gel Process and Local Structure by Vibrational Spectroscopy

Polymers ◽  
2021 ◽  
Vol 13 (13) ◽  
pp. 2082
Author(s):  
Guillermo Cruz-Quesada ◽  
Maialen Espinal-Viguri ◽  
María Victoria López-Ramón ◽  
Julián J. Garrido

The properties of hybrid silica xerogels obtained by the sol-gel method are highly dependent on the precursor and the synthesis conditions. This study examines the influence of organic substituents of the precursor on the sol-gel process and determines the structure of the final materials in xerogels containing tetraethyl orthosilicate (TEOS) and alkyltriethoxysilane or chloroalkyltriethoxysilane at different molar percentages (RTEOS and ClRTEOS, R = methyl [M], ethyl [E], or propyl [P]). The intermolecular forces exerted by the organic moiety and the chlorine atom of the precursors were elucidated by comparing the sol-gel process between alkyl and chloroalkyl series. The microstructure of the resulting xerogels was explored in a structural theoretical study using Fourier transformed infrared spectroscopy and deconvolution methods, revealing the distribution of (SiO)4 and (SiO)6 rings in the silicon matrix of the hybrid xerogels. The results demonstrate that the alkyl chain and the chlorine atom of the precursor in these materials determines their inductive and steric effects on the sol-gel process and, therefore, their gelation times. Furthermore, the distribution of (SiO)4 and (SiO)6 rings was found to be consistent with the data from the X-Ray diffraction spectra, which confirm that the local periodicity associated with four-fold rings increases with higher percentage of precursor. Both the sol-gel process and the ordered domains formed determine the final structure of these hybrid materials and, therefore, their properties and potential applications.

2007 ◽  
Vol 350 ◽  
pp. 31-34 ◽  
Author(s):  
Teruhisa Makino ◽  
Masashi Arimura ◽  
Kunitaka Fujiyoshi ◽  
Yoko Yamashita ◽  
Makoto Kuwabara

We synthesized barium titanate (BaTiO3) nanoparticles by sol-gel process and investigated their crystallization behavior using differential scanning calorimetry and X-ray diffraction. BaTiO3 nanoparticles with various degrees of crystallinity were obtained by adjusting synthesis conditions. Under aging conditions that do not allow dealcholization reaction to complete, many hydroxyl ligands remain in as-synthesized BaTiO3 nanoparticles, resulting in the formation of voids or defects in the nanoparticles after calcination. It is essential to use high concentration alkoxides precursor solutions for producing BaTiO3 nanoparticles with high crystallinity at low temperature.


1994 ◽  
Vol 346 ◽  
Author(s):  
E. Mouchon ◽  
L. C. Klein ◽  
V. Picard ◽  
M. Greenblatt

ABSTRACTFor more than a decade, the sol-gel process has been used to prepare lithium silicate gels that have potential applications as solid electrolytes in lithium batteries and electrochromic windows. The interest in these Li2O-SiC2 materials is their fast and stable ionic conductivity from room temperature up to 350°C. Typically these materials have been prepared with 15 mole % Li2O in bulk samples, but rarely in thin films. This work was undertaken to prepare chemically stable lithium silicate thin films with up to 30 mole % Li2O. Lithium nitrate was used as the lithium precursor. Solutions were evaluated for gelling time and homogeneity. Thin films were made by dip coating. After heat treatment at 200, 250 and 300°C, films were characterized for surface quality, thickness and microstructure using electron microscopy, x-ray diffraction analysis and profilometry. Transparency was investigated in the visible range (350–800 nm).


2012 ◽  
Vol 217-219 ◽  
pp. 733-736
Author(s):  
Xiu Mei Han ◽  
Shu Ai Hao ◽  
Ying Ling Wang ◽  
Gui Fang Sun ◽  
Xi Wei Qi

Zn2SiO4:Eu3+, Dy3+ phosphors have been prepared through the sol-gel process. X-ray diffraction (XRD), thermogravimetric and ddifferential thermal analysis (TG-DTA), FT-IR spectra and photoluminescence spectra were used to characterize the resulting phosphors. The results of XRD indicated that the phosphors crystallized completely at 1000oC. In Zn2SiO4:Eu3+,Dy3+ phosphors, the Eu3+ and Dy3+ show their characteristic red(613nm, 5D0-7F2), blue (481nm, 4F9/2–6H15/2) and yellow (577nm, 4F9/2–6H13/2) emissions.


2010 ◽  
Vol 97-101 ◽  
pp. 1611-1615 ◽  
Author(s):  
Qing Wang ◽  
Xin Li Li ◽  
Wei Nie ◽  
Yong Mei Xia ◽  
Jian Feng Dai

The ZnO/TiO2 composite films were deposited over glass using spin coating technique by sol-gel process. Single-walled carbon nanotubes (SWNTs) were used to modify the ZnO/TiO2 films successfully in this paper. The structure and composition of the ZnO/TiO2 composite and SWNTs doped ZnO/TiO2 composite were characterized by X-ray diffraction (XRD). The morphology of samples was characterized by scanning electron microscopy (SEM). The photocatalytic activity was investigated by photocatalytic degradation of aqueous methyl orange under ultraviolet (UV) radiation. The UV-vis absorption spectra of the ZnO/TiO2 films and SWNTs doped ZnO/TiO2 films in the wavelength region 200~800 nm were obtained. The results indicate that the SWNTs addition can decrease the grain size of ZnO/TiO2, which can enhance the photocatalytic activity. UV-vis absorption spectra of SWNTs-ZnO/TiO2 showed obvious blue shifts compared with ZnO/TiO2. The optimal amount of doping SWNTs is 1% according to this research. The enhanced mechanism of the SWNTs for the photocatalytic activity in ZnO/TiO2 films was analyzed in this article.


2002 ◽  
Vol 737 ◽  
Author(s):  
R.E. Melgarejo ◽  
M.S. Tomar ◽  
A. Hidalgo ◽  
R.S. Katiyar

ABSTRACTNd substituted bismuth titanate Bi4-xNdxTi3O12 were synthesized by sol-gel process and thin films were deposited on Pt substrate (Pt/TiO2/SiO2/Si) by spin coating. Thin films, characterized by X-ray diffraction and Raman spectroscopy, shows complete solid solution up to the composition x < 1. Initial results indicate that the ferroelectric polarization increases with increasing Nd content in the film with 2Pr = 50μC/cm2 for x = 0.46, which may have application in non-volatile ferroelectric memory devices.


2011 ◽  
Vol 399-401 ◽  
pp. 1447-1450
Author(s):  
Zhi Yong Yu ◽  
Han Xing Liu

The layered LiNi1/2Mn1/2O2 cathode materials were synthesized by a sol gel method. The effects of calcination temperature and time on the structural and electrochemical properties of the LiNi1/2Mn1/2O2 were investigated. The prepared samples were characterized by X-ray diffraction (XRD) and electrochemical analysis. The results revealed that the layered LiNi1/2Mn1/2O2 material could be optimal synthesized at temperature of 900°C for 10h. The sample prepared under the above conditions has the highest initial discharge capacity of 151 mAh/g and showed no dramatic capacity fading during 20 cycles between 2.5-4.5V at a current rate of 20mA/g.


2010 ◽  
Vol 93-94 ◽  
pp. 231-234
Author(s):  
B. Hongthong ◽  
Satreerat K. Hodak ◽  
Sukkaneste Tungasmita

Strontium substituted hydroxyapatite(SrHAp) were fabricated both in the form of powder as reference and thin film by using inorganic precursor reaction. The sol-gel process has been used for the deposition of SrHAp layer on stainless steal 316L substrate by spin coating technique, after that the films were annealed in air at various temperatures. The chemical composition of SrHAp is represented (SrxCa1-x)5(PO4)3OH, where x is equal to 0, 0.5 and 1.0. Investigations of the phase structure of SrHAp were carried out by using X-ray diffraction technique (XRD). The results showed that strontium is incorporated into hydroxyapatite where its substitution for calcium increases in the lattice parameters, and Sr3(PO4)2 can be detected at 900°C. The SEM micrographs showed that SrHAp films exhibited porous structure before develop to a cross-linking structure.


2014 ◽  
Vol 543-547 ◽  
pp. 3741-3744
Author(s):  
Quan Jing Mei ◽  
Cong Ying Li ◽  
Jing Dong Guo ◽  
Gui Wang ◽  
Hai Tao Wu

The ecandrewsite-type ZnTiO3was successfully synthesized by the aqueous sol-gel method using TiO2dioxide and zinc nitrate as starting materials instead of expensive organic solvent and metal alkoxides. The as-prepared nanopowders were characterized by X-ray diffraction (XRD), differential thermal analysis (DTA) and transmission electron microscopy (TEM), respectively. The results showed that the calcination process of gel consisted of a series of oxidation and combustion reactions, accompanied by significantly exothermal effects. Highly reactive nanosized ZnTiO3powders were successfully obtained at 850 °C with particle size ~50 nm. By comparison, the aqueous sol-gel process was the most effective and least expensive technique used for the preparation of ZnTiO3nanopowders.


2007 ◽  
Vol 546-549 ◽  
pp. 2007-2010
Author(s):  
Gao Yang Zhao ◽  
Huang Li Zhang ◽  
Ren Zhong Xue ◽  
Yuan Qing Chen ◽  
Li Lei

precursor solution was prepared using barium trifluoroacetae (Ba-TFA) and non-fluorine yttrium (Y) and copper (Cu) organic salts. The precursor solution was modified by benzalacetone (BzAcH), in which the Cu2+ were chelated with BzAcH, which preventing the loss of Cu in the pyrolysis process. Dense YBCO superconducting films with smooth surface, which confirmed by scanning electron microscopy (SEM), were repeatedly obtained through sol-gel process. X-ray diffraction (XRD) 2θ scanning and φ scanning indicated that the as-prepared YBCO films had good c-axis texture. YBCO films with superconducting transition temperature (TC) above 89K were obtained.


2018 ◽  
Vol 762 ◽  
pp. 408-412
Author(s):  
Raivis Eglītis ◽  
Gundars Mežinskis

In this work two different hydrosols were used to impregnate a commercially available cotton fabric with anatase nanoparticles to give it photocatalytic activity. To increase the activity, different pre-treatment methods were applied. The nanoparticle size was determined using dynamic light scattering and x-ray diffraction and the fabrics were examined using scanning electron microscopy. Photocatalytic activity was measured using the degradation of methyl-orange while irradiating the samples with UV light. The synthesis method allowed to produce anatase with an average particle size of 32 to 37 nm depending on the synthesis method used.


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