Synthesis of V2O5 Powders by EDTA Assistance Ultrasound Sol-Gel Process

2012 ◽  
Vol 512-515 ◽  
pp. 207-210
Author(s):  
Quan Wen ◽  
Jian Feng Huang ◽  
Li Yun Cao ◽  
Jian Peng Wu

V2O5 powders were successfully synthesized by the EDTA assistanced ultrasound sol-gel process using NH4VO3 and EDTA, NH3•H2O as raw materials. The synthesized activation energy and the influence of pH values and the calcination temperatures on the phases and microstructures of powders were particularly investigated. The precursor powders and the V2O5 powders were characterized by X-ray diffraction (XRD), fourier transform inelectron microscopy (FT-IR), scanning electron microscopy (SEM) and differential scanning calorimetry-thermal gravimetric (DSC-TG). Results show that the obtained products exhibit good crystallization under the conditions of pH=4, calcination temperature 400~500 °C and calcination time 0.5 h during the synthesizing process. The as-prepared V2O5 powders show preferred growth orientation along (001) plane at the pH=4. By DSC analysis, the ultrasonic cavitation result in the decrease in synthesized activation energy obviously than that was prepared without ultrasonic irradiation.

2017 ◽  
Vol 748 ◽  
pp. 413-417
Author(s):  
Chun Yu Long ◽  
Fang Fang Peng ◽  
Min Min Jin ◽  
Pei Song Tang ◽  
Hai Feng Chen

Using Pr (NO3)3, butyl titanate, ethylene glycol and citric acid as main raw materials, praseodymium titanate (Pr2Ti2O7) was prepared by the sol-gel process. The samples were characterized by means of X-ray diffraction (XRD), scanning electron microscope (SEM), thermal gravity-differential thermal analysis (TG-DTA), diffuse-reflection spectra (DRS) and Fourier transform infrared (FT-IR). The effect of different calcination temperature and illumination time on the photocatalytic properties of Pr2Ti2O7 was investigated. It was found that the single phase Pr2Ti2O7 could be obtained through sol-gel process and calcination at 1000 °C. The Pr2Ti2O7 samples calcination at 1000 °C were uniform , and the resulting product had a particle size of 200 nm and an optical band gap of 3.26 eV. Under ultraviolet light, the degradation of methyl orange arrived to 80.11% after 180 min of photocatalytic reaction. The Pr2Ti2O7 samples showed good photocatalytic activity for decomposition of methyl orange.


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.


2019 ◽  
Vol 07 (01n02) ◽  
pp. 1950002
Author(s):  
Nadir Lalou ◽  
Ahmed Kadari

This work proposes the synthesis of nanocrystalline calcium oxide (CaO) pure and doped with different concentrations of lithium (Li[Formula: see text]) ions by sol–gel process. Calcium nitrate (Ca(NO[Formula: see text]4H2O; 99.99%) and lithium nitrate (LiNO3; 99.99%) were used as precursors. The synthesized powders were characterized by several techniques such as: UV-Vis transmission spectroscopy, Fourier Transform Infra-red spectroscopy (FT-IR) and X-ray diffraction (XRD). The main objective of this paper is to study the influence of lithium (Li[Formula: see text] ratio) on the structural and optical properties of synthesized powders. The band gap values decreased with the increasing of Li[Formula: see text] ions in CaO lattice; the slight change in the band gap was directly related to the energy transfer between the CaO excited states and the 2s levels of Li[Formula: see text] ions. The influence of Li[Formula: see text] doping on the physical properties of CaO nanocrystalline will be studied for the first time in this work; no literature has previously published this kind of impurities.


2011 ◽  
Vol 412 ◽  
pp. 271-274
Author(s):  
Ying Li ◽  
Qiang Xu ◽  
Ling Dai

In order to prepare ultrafine La3NbO7 powder, a potential material for thermal barrier coatings, the calcination process of La3NbO7 was studied in this paper.The precursor of La3NbO7 was synthesized by using a citric acid complex method. A calcination process had been systematically investigated. The reaction temperature was determined by differential scanning calorimetry (DSC). The phase composition of powders was characterized by X-ray diffraction (XRD), and the morphology was obtained by scanning electron microscope (SEM). The results revealed that the single-phase La3NbO7 powder could be successfully prepared while the calcination temperature exceeded 800°C and a better morphology could be maintained at 800°C for 4 hours. Considering all above, an optimum calcination scheme was adopted at 800°C for 4 hours. The as-prepared La3NbO7 powders had a grain size of about 50nm and an average particle size of about 300nm.


2016 ◽  
Vol 852 ◽  
pp. 585-590
Author(s):  
Lin Sang ◽  
Ning Pan ◽  
Jing Su ◽  
Xiao Mei Tan ◽  
Hang Li ◽  
...  

3at. % Eu3+ doped (Y, Gd)2O3 precursor powders with various compositions were synthesized via a sol-gel process, and the precursors were sintered at different temperatures. XRD, FT-IR, Raman and photoluminescence spectroscopy were used to study the phase, microstructure and luminescent properties of the precursors and the sintered powders. The results show that pure (Y, Gd)2O3 polycrystalline phase can be obtained from sintering the precursors at 700°C. The influences of the host compositions on the microstructures and fluorescence properties were analyzed, and the optimized composition was obtained for 3at. % Eu3+ doped (Y, Gd)2O3 powders.


2006 ◽  
Vol 45 ◽  
pp. 260-265 ◽  
Author(s):  
Antônio Hortêncio Munhoz Jr. ◽  
Leila Figueiredo de Miranda ◽  
G.N. Uehara

A pseudoboehmite was obtained by sol-gel synthesis using aluminum nitrate as precursor. It was used a 2n full factorial design for studying the effect of the temperature of synthesis, the concentration of ammonium hydroxide, and the radiation dose in the product of sol-gel synthesis. The product of the synthesis was analyzed by scanning electron microscopy, x-ray diffraction of the product (after firing the pseudoboehmite at different temperatures), and it was also analyzed the temperature of endothermic and exothermic transformations using the thermo gravimetric analysis (TG) and differential scanning calorimetry (DSC). The X-ray diffraction data show that α-alumina was obtained at 1100o C.


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.


2008 ◽  
Vol 396-398 ◽  
pp. 481-484
Author(s):  
Rodrigo Jiménez-Gallegos ◽  
L. Téllez-Jurado ◽  
Luis M. Rodríguez-Lorenzo ◽  
Julio San Román

This paper focuses on the preparation of siloxane-polyurethane hybrid materials using a sol-gel method. The global aim of the project is to tailor mechanical properties, degradability rate, bioactivity and biocompatibility to design scaffolds for musculoskeletal applications. A series of seven hybrid materials were synthesized with varying the proportion of polydimethylsiloxane (PDMS), and Polyurethane (PU). The organic part ratios (by weight) employed were (% PDMS:% PU) 30:0, 35:5, 20:10, 15:15, 10:20, 5:25, and 0:30. The organic part was reacted with constant 70 % TEOS to obtain the hybrid materials. A sol-gel process was selected for the synthesis of the hybrids. The characterization of materials was carried out by the fourier-infrared spectroscopy (FT-IR), x-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electronic microscopy (SEM) and proton nuclear magnetic resonance (1H-NMR) techniques in order to analyze the structure, microstructure and chemical composition of the hybrid materials. Gelification time depends on the proportion of PU used. When no PU is employed, the gel time is 8 hours but it rises up to 18 days for 30 % of polyurethane. Materials range from opaque to translucent but with a greater fragility for greater amounts of polyurethane. No differences in the bonding of materials could be appreciated.


2011 ◽  
Vol 1326 ◽  
Author(s):  
Rene Fabian Cienfuegos ◽  
Leonardo Chávez Guerrero ◽  
Sugeheidy Carranza ◽  
Laurie Jouanin ◽  
Guillaume Marie ◽  
...  

ABSTRACTThe goal in this study was to synthesize a lanthanum - nickel phase (Ruddlesden-Popper phases) La4Ni3O10. This material was prepared using a polymeric route. An easy synthesis method is presented in order to obtain an economical cathode material, which can be used in Solid Oxide Fuel Cells (SOFC). The polymeric precursors were prepared following the Castillo method. The originality of this work was to optimize the ratio HMTA/ metallic salts from 1 to 6. The obtained powders were characterized by thermal analysis; Differential Scanning Calorimetry (DSC Q10 Instrument TA), Thermogravimetric Analysis (TGA - Q50 Instrument TA-) and X-ray diffractometer (Bruker, D8 Advance diffractometer), in order to determine the crystallized phase. Experiments 5 and 6 did not present coagulation but after few days, solution 5 was transformed into a gel. Gels 2 to 5 were heated in order to obtain a solid material. These powders are characterized by thermogravimetric and thermo-differential methods. The powders obtained at 800, 900 and 1000°C were analyzed by X-ray diffraction and it was found that the temperature to get to the La4Ni3O10 phase was 1000ºC.


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.


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