scholarly journals Novel Sol-Gel Synthesis of Spherical Lead Titanate Submicrometer Powders

Crystals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 484
Author(s):  
Radhouane Bel-Hadj-Tahar ◽  
Mohamed Abboud ◽  
Mohd. Shkir ◽  
Abdullah Alhanash ◽  
Ali Eisa M. Anqi ◽  
...  

In this study, a novel and simple synthetic sol-gel procedure was established to directly prepare spherical lead titanate powders without prior synthesis/usage of spherical templates such as TiO2 particles. Isotropic submicron particles with a mean diameter of 1–4 μm were prepared in this way. This synthetic process takes advantage of acetone as a stabilizing ligand and autogenous pressure generated in the autoclave during the reaction. The influence of various experimental factors (nature of the ligand, thermal treatment mode, and post-calcining temperature) as well as the formation mechanism were studied. Scanning electron microscopy and transmission electron microscopy were used to explore the particle morphology. The crystalline phases were explored and identified by X-ray diffraction analysis.

2015 ◽  
Vol 2015 ◽  
pp. 1-8 ◽  
Author(s):  
Sanja Ćulubrk ◽  
Željka Antić ◽  
Vesna Lojpur ◽  
Milena Marinović-Cincović ◽  
Miroslav D. Dramićanin

Herein we presented hydrolytic sol-gel synthesis and photoluminescent properties of Eu3+-doped Gd2Ti2O7pyrochlore nanopowders. According to Gd2Ti2O7precursor gel thermal analysis a temperature of 840°C is identified for the formation of the crystalline pyrochlore phase. Obtained samples were systematically characterized by powder X-ray diffraction, scanning and transmission electron microscopy, and photoluminescence spectroscopy. The powders consist of well-crystalline cubic nanocrystallites of approximately 20 nm in size as evidenced from X-ray diffraction. The scanning and transmission electron microscopy shows that investigated Eu3+-doped Gd2Ti2O7nanopowders consist of compact, dense aggregates composed entirely of nanoparticles with variable both shape and dimension. The influence of Eu3+ions concentration on the optical properties, namely, photoluminescence emission and decay time, is measured and discussed. Emission intensity as a function of Eu3+ions concentration shows that Gd2Ti2O7host can accept Eu3+ions in concentrations up to 10 at.%. On the other hand, lifetime values are similar up to 3 at.% (~2.7 ms) and experience decrease at higher concentrations (2.4 ms for 10 at.% Eu3+). Moreover, photoluminescent spectra and lifetime values clearly revealed presence of structural defects in sol-gel derived materials proposing photoluminescent spectroscopy as a sensitive tool for monitoring structural changes in both steady state and lifetime domains.


2004 ◽  
Vol 848 ◽  
Author(s):  
Lidia Armelao ◽  
Davide Barreca ◽  
Gregorio Bottaro ◽  
Andrea Caneschi ◽  
Claudio Sangregorio ◽  
...  

ABSTRACTThis work is focused on the sol-gel synthesis of pure and Ca-doped LaCoO3 nanopowders. The samples were prepared starting from methanolic solutions of cobalt (II) acetate (Co(CH3COO)2·4H2O), lanthanum (III) nitrate (La(NO3)3·6H2O) and calcium (II) acetate (Ca(CH3COO)2·H2O). After solvent evaporation, the obtained powders were dried under vacuum and subsequently treated in air up to 1273 K. The system evolution under thermal annealing was studied by X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM), while the chemical composition was analyzed by X-ray Photoelectron (XPS) and X-ray Excited Auger electron (XE-AES) spectroscopies. The temperature and field dependence of the magnetic properties of the Ca-doped samples were investigated, and compared to those of the corresponding pure LaCoO3 powders.


2013 ◽  
Vol 389 ◽  
pp. 53-56
Author(s):  
Shu Guo ◽  
Sheng Xu Lu ◽  
Hui Ding ◽  
Zai Feng Shi

The mesoporous TiO2 particles was conveniently prepared in a room temperature ionic liquid (RTILs) of 1, 3-di-(3-propionyloxy) imdazolium tetrafluoroborate [DiprCOOBF4 system. The obtained materials were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and N2 adsorptiondesorption analysis. XRD patterns revealed that only rutile phase is formed in the RTILs. The TEM micrographs as well as N2 adsorptiondesorption measurements show that the prepared products exhibited wormlike pore structures. The FTIR (Fourier Transform Infrared Spectra) demonstrate the carboxylate groups attach via bidentate or bridging coordination to the TiO2 surface.


Author(s):  
Abubakar Hamisu ◽  
Umar Ibrahim Gaya ◽  
Abdul Halim Abdullah

Sol-gel mesoporous titanium dioxide powders have been synthesized from chitosan and/or hexadecyltrimethylammonium bromide (HDTMA) and characterized using x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) spectroscopy, thermogravimetric analysis (TGA), differential thermal analysis (DTA) and N2 adsorption-desorption measurements. The photocatalytic performance of the synthesized meso-TiO2 powders was optimized based on the central composite design (CCD) of methyl orange (MO) degradation under UV light irradiation. The maximum MO degradation was 62.3% over a period of 60 min. Oxides produced using the binary chitosan and HDTMA template (C,H-TiO2) exhibited the relatively higher surface area (99.5 m2/g), smaller crystal size (12.78 nm), narrower band-gap energy (2.92 eV) and higher photocatalytic rate constant (0.0112 min–1) than as those from chitosan (C/TiO2) or HDTMA (H/TiO2) as the template.


2021 ◽  
Vol 19 (1) ◽  
pp. 745-754
Author(s):  
Khoirina Dwi Nugrahaningtyas ◽  
Eddy Heraldy ◽  
Rachmadani ◽  
Yuniawan Hidayat ◽  
Indriana Kartini

Abstract The properties of three types of CoMo/USY catalysts with different synthesized methods have been studied. The sequential and co-impregnation methods followed by activation using calcination and reduction process have been conducted. The properties of the catalysts were examined using Fourier-transform-infrared (FTIR) spectroscopy, X-ray diffraction (XRD) with refinement, and surface area analyzer (SAA). The FTIR spectrum study revealed the enhanced intensity of its Bronsted acid site, and the XRD diffractogram pattern verified the composition of pure metals, oxides, and alloys in the catalyst. The SAA demonstrated the mesoporous features of the catalyst. Scanning electron microscopy showed an irregular particle morphology. Additional analysis using the transmission electron microscopy indicated that the metal has successfully impregnated without damaging the USY structure.


Author(s):  
G. S. Zakharova ◽  
E. Thauer ◽  
A. N. Enyashin ◽  
L. F. Deeg ◽  
Q. Zhu ◽  
...  

AbstractThe potential battery electrode material V2O3/C has been prepared using a sol–gel thermolysis technique, employing vanadyl hydroxide as precursor and different organic acids as both chelating agents and carbon sources. Composition and morphology of resultant materials were characterized by X-ray diffraction, Raman spectroscopy, scanning and transmission electron microscopies, physical sorption, and elemental analysis. Stability and electronic properties of model composites with chemically and physically integrated carbon were studied by means of quantum-chemical calculations. All fabricated composites are hierarchically structured and consist of carbon-covered microparticles assembled of polyhedral V2O3 nanograins with intrusions of amorphous carbon at the grain boundaries. Such V2O3/C phase separation is thermodynamically favored while formation of vanadium (oxy)carbides or heavily doped V2O3 is highly unlikely. When used as anode for lithium-ion batteries, the nanocomposite V2O3/C fabricated with citric acid exhibits superior electrochemical performance with an excellent cycle stability and a specific charge capacity of 335 mAh g−1 in cycle 95 at 100 mA g−1. We also find that the used carbon source has only minor effects on the materials’ electrochemical performance.


2010 ◽  
Vol 148-149 ◽  
pp. 893-896 ◽  
Author(s):  
Ze Yang Zhang ◽  
Xiang Xuan Liu ◽  
You Peng Wu

M-typical SrFe12O19 ferrites and FeNi3 nanoplatelets were successfully prepared by the sol-gel method and solution phase reduction method, respectively. The crystalline and morphology of particles were studied by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The composite coatings with SrFe12O19 ferrites and FeNi3 nanoplatelets in polyvinylchloride matrix were prepared. The microwave absorption properties of these coatings were investigated in 2-18GHz frequency range. The results showed that the M-typical SrFe12O19 ferrites and FeNi3 nanoplatelets were obtained and they presented irregular sheet shapes. With the increase of the coating thickness, the absorbing peak value moves to the lower frequency. The absorbing peak values of the wave increase along with the increasing of the content of FeNi3 nanoplatelets filling fraction. When 40% SrFe12O19 ferrites is doped with 20% mass fraction FeNi3 nanoplatelets to prepare composite with 1.5mm thickness, the maximum reflection loss is -24.8 dB at 7.9GHz and the -10 dB bandwidth reaches 3.2GHz.


2018 ◽  
Vol 41 (3-4) ◽  
pp. 53-62 ◽  
Author(s):  
Behnaz Lahijani ◽  
Kambiz Hedayati ◽  
Mojtaba Goodarzi

Abstract In this work, the PbFe12O19 nanoparticles were prepared by the simple and optimized precipitation method with different organic surfactants and capping agents. In the next step, the TiO2 nanoparticles were synthesized using the sol-gel method. At the final step, the PbFe12O19-TiO2 nanocomposites were prepared via the sol-gel method. The effect of the precipitating agent on the morphology and particle size of the products was investigated. The prepared products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and Fourier transform infrared spectroscopy. The results obtained by the vibrating sample magnetometer show the magnetic properties of the ferrite nanostructures. The photocatalytic effect of the PbFe12O19-TiO2 nanocomposite on the elimination of the azo dyes (acid black, acid violet and acid blue) under ultraviolet light irradiation was evaluated. The results indicate that the prepared nanocomposites have acceptable magnetic and photocatalytic performance.


1999 ◽  
Vol 14 (12) ◽  
pp. 4570-4580 ◽  
Author(s):  
M. Alguerá ◽  
M. L. Calzada ◽  
L. Pardo ◽  
E. Snoeck

Transmission electron microscopy has shown that the grain size of sol-gel-prepared lanthanum-modified lead titanate films increases from ∼100 to ∼1 μm when the excess of PbO in the precursor solution is reduced from 20 to 10 mol%. Switchable polarization is higher in the films with a smaller grain size. Profilometry and the temperature dependence of the dielectric permittivity indicate that films are tensile stressed by the substrate. The grain-size effect on polarization switching is explainedby taking into account this tensile stress, which is thought to induce some a-domain orientation and 90° domain wall clamping in the grains attached to the substrate.


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