Characterization of Nanoscaled TiO2 Produced by Simplified Sol–Gel Method Using Organometallic Precursor

This work is concerned with development of sol–gel method for preparation of nanoscaled TiO2 using organometallic precursor—titanium tetraisopropoxide (TTIP) and determination of the present crystalline phases depending on the temperature of further thermal treatment. The characteristic processes and transformations during the thermal treatment were determined by means of thermal gravimetric analysis and/or differential thermal analysis (TGA/DTA) method. The crystalline structure and size of the TiO2 crystallites were analyzed by means of Raman spectroscopy and X-ray powder diffraction (XRPD) method. At 250 °C, cryptocrystalline structure was detected, where amorphous TiO2 is accompanied with crystalline anatase. The anatase crystallite phase is stable up to 650 °C, whereas at higher temperature rutile transformation begins. It was observed that at 800 °C, almost the whole TiO2 is transformed to rutile phase. According to XRPD analysis, the increase of the temperature influences on the increase of the size of the crystalline particles ranging from 6 nm at 250 °C to less than 100 nm at 800 °C. The size and shape of the TiO2 crystalline particles were observed by transmission electron microscopy (TEM). The shape of the studied samples changes from nanospheres (250, 380, and 550 °C) to nanorods (650 and 800 °C). Morphology of the formed TiO2 aggregates was observed by scanning electron microscopy (SEM).

Download Full-text

Magnetic PbFe12O19-TiO2 nanocomposites and their photocatalytic performance in the removal of toxic pollutants

Main Group Metal Chemistry ◽

10.1515/mgmc-2017-0055 ◽

2018 ◽

Vol 41 (3-4) ◽

pp. 53-62 ◽

Cited By ~ 2

Author(s):

Behnaz Lahijani ◽

Kambiz Hedayati ◽

Mojtaba Goodarzi

Keyword(s):

Electron Microscopy ◽

Photocatalytic Performance ◽

Sol Gel ◽

Precipitation Method ◽

X Ray Diffraction ◽

Gel Method ◽

Sol Gel Method ◽

Photocatalytic Effect ◽

Transmission Electron ◽

Ultraviolet Light Irradiation

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.

Download Full-text

Growth and Characterizations of Relaxor-Based Pb(Mg1/3Nb2/3)O3-PbTiO3 Thin Films by Sol-Gel Method

Key Engineering Materials ◽

10.4028/www.scientific.net/kem.280-283.839 ◽

2007 ◽

Vol 280-283 ◽

pp. 839-844

Author(s):

Hui Qing Fan

Keyword(s):

Electron Microscopy ◽

Thin Films ◽

Sol Gel ◽

Silicon Substrates ◽

Final Annealing ◽

Gel Method ◽

Sol Gel Method ◽

Phase Development ◽

Transmission Electron ◽

Pt Films

Relaxor-based 0.7Pb(Mg1/3Nb2/3)O3-0.3PbTiO3 (PMN-PT) thin films were grown epitaxially on silicon substrates by sol-gel method and PbO cover coat technique, and investigated by x-ray diffraction, auger electron spectroscopy, scanning electron microscopy, and transmission electron microscopy. The phase development and microstrure evolution of the PMN-PT film were significantly affected by the final annealing temperature and time. A perovskite PMN-PT film was obtained after annealing at 850oC for 1 min. Then, highly <100>-oriented and textured PMN-PT films could be achieved by using a LaNiO3 perovskite template.

Download Full-text

Effects of Varying Alx Moles on the Structure and Luminescence Properties of ZnAlxO1.5x + 1:0.1% Tb3+ Nano Phosphor Prepared using Citrate sol-gel Method

10.21203/rs.3.rs-348042/v1 ◽

2021 ◽

Author(s):

V Maphiri ◽

L Melato ◽

Mhlongo ◽

TT Hlatshwayo ◽

TE Motaung ◽

...

Keyword(s):

Crystal Structure ◽

Electron Microscopy ◽

Single Phase ◽

Sol Gel ◽

Gel Method ◽

X Ray ◽

Sol Gel Method ◽

Transmission Electron ◽

Nano Phosphor ◽

Scanning Electron

Abstract Un-doped and ZnAlxO(1.5x + 1):0.1% Tb3+ (ZAOT) nano-powders were synthesized via citrate sol-gel method. The Alx moles were varied in the range of 0.25 ≤ x ≤ 5.0. The X-ray powder diffraction (XRD) data revealed that for the x < 1.5, the prepared samples crystal structure consists of mixed phases of the cubic ZnAl2O4 and hexagonal ZnO phases, while for the x ≥ 1.5 the structure consists of single phase of cubic ZnAl2O4. This was confirmed by the Raman and Fourier-Transform Infrared (FTIR) vibrational spectroscopy. Scanning electron microscopy (SEM) showed that varying Alx moles influences the morphology while Transmission electron microscopy (TEM) shows the dual morphology at x < 1.5. The photoluminescence (PL) revealed intense and distinct emissions attributed to both the host and Tb3+ transitions. The emission intensity highly depends on the Alx moles. The International Commission on Illumination (CIE) colour chromaticity showed that the emission colour could be tuned by varying the Alx moles.

Download Full-text

Synthesis of SnO2 by Sol-Gel Method

Solid State Phenomena ◽

10.4028/www.scientific.net/ssp.254.200 ◽

2016 ◽

Vol 254 ◽

pp. 200-206 ◽

Cited By ~ 1

Author(s):

Catalina Nuțescu Duduman ◽

María Isabel Barrena Pérez ◽

José Maria Gómez de Salazar ◽

Ioan Carcea ◽

Daniela Lucia Chicet ◽

...

Keyword(s):

Electron Microscopy ◽

Chemical Composition ◽

Diffraction Pattern ◽

Sol Gel ◽

X Ray Diffraction ◽

Gel Method ◽

X Ray ◽

Sol Gel Method ◽

Transmission Electron ◽

Sol Gel Process

Nanostructured SnO2 was prepared based on the sol-gel method used in the preparation of crystalline metal oxides. Sol-gel process can be described as a forming network of oxide polycondensation reaction of a molecular precursor in a liquid. Six experiments were carried out. Morphological structures and chemical composition were examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) after calcination. It is noted that TEM images show that the spheres consist from nanocrystals, quantitative EDS analysis of the chemical composition shows an absence of the chlorine, which is a desired fact. For structural characterization of the material we used X-Ray Diffraction (XRD). The X-ray diffraction pattern for all samples indicates peaks which are agreeable with standard diffraction pattern of SnO2. The particle size of all samples was in the range of 28-92 nm calculated according to Scherrer equation.

Download Full-text

Preparation of Nano-Ceramics via Aqueous Sol-Gel Method Modified with Surfactants: An Overview

Materials Science Forum ◽

10.4028/www.scientific.net/msf.644.79 ◽

2010 ◽

Vol 644 ◽

pp. 79-84

Author(s):

Yibran Perera

Keyword(s):

Electron Microscopy ◽

Sol Gel ◽

Calcium Nitrate ◽

Calcium Nitrate Tetrahydrate ◽

Gravimetric Analysis ◽

Nano Materials ◽

Scanning Calorimetry ◽

Gel Method ◽

Sol Gel Method ◽

Silica Alumina

The present paper shows an overview related to the preparation and characterization of different nano-materials such as: silica, alumina, di- and tri-calcium silicates and a composite in the ternary CaO-SiO2-Al2O3 system. These nano-materials are related to the construction area so some basic tests are carried out to evaluate their cementitious and/or pozzolanic behavior. The nano-ceramics have been synthesized via hydrolysis and condensation of aqueous sol-gel method modified with surfactants using different precursors such as: tetraethyl orthosilicate (TEOS), calcium nitrate tetrahydrate (Ca(NO3)2.4H2O), sodium silicate (Na2O.SiO2), aluminum nitrate nonahydrate (Al(NO3)3•9H2O) and an industrial aluminum hydroxide (gibbsite). The synthesis parameters such as: pH, temperature, kind of surfactants, etc., are reported. To characterize the structural, chemical composition, particle size and morphology of the nanoparticles, different techniques such as: Fourier transform infrared (FTIR), thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), field emission electron microscopy (FESEM) and high-resolution transmission electron microscopy (HR-TEM) are used.

Download Full-text

Synthesis of Mn(II)-Loaded TixSi1-xO4 Composite Acting as a Visible-Light Driven Photocatalyst

Indonesian Journal of Chemistry ◽

10.22146/ijc.21222 ◽

2015 ◽

Vol 15 (1) ◽

pp. 43-49 ◽

Cited By ~ 2

Author(s):

Misriyani Misriyani ◽

Eko Sri Kunarti ◽

Masahide Yasuda

Keyword(s):

Thermal Treatment ◽

Visible Light ◽

Sol Gel ◽

Ion Concentration ◽

Molar Ratio ◽

Titanium Tetraisopropoxide ◽

Gel Method ◽

Sol Gel Method ◽

Visible Light Driven ◽

Diffuse Reflectance Spectrometry

The synthesis and characterization of Mn-loaded TixSi1-xO4 (x= 0.4-0.8) composites and a preliminary study of an activity testing their ability to work as photocatalysts for the degradation of methylene blue (MB) have been studied. Synthesis was conducted by the sol-gel method at room temperature using tetraethyl orthosilicate, titanium tetraisopropoxide, and manganese(II) chloride as precursors followed by thermal treatment at 500 °C. The characterizations were performed by X-ray diffraction, FT-IR spectrometry, UV-Vis diffuse reflectance spectrometry and a surface area analyzer. The photocatalytic activity test of composites for degradation of MB was carried out in a closed reactor equipped with UV and visible lights. In this test, the effects of ratio of Ti/Si composites, Mn2+ ion concentration, pH, and time of irradiation on the effectiveness of photodegradation of MB were studied. The results indicated that Mn-Ti0.6Si0.4O4 composite could be synthesized through the sol-gel method followed by thermal treatment with a molar ratio of Ti/Si=60/40 and the optimum concentration of manganese was 2.5 wt%. The Mn-Ti0.6Si0.4O4 composite significantly increased the photodegradation of MB at pH 10, with a percent degradation of 84.41% for 30 min under irradiation of visible light. The percent degradation of Ti0.6Si0.4O4 was only 18.23% under irradiation of visible light.

Download Full-text

Structural and magnetic properties of nanostructured Li–Ni–Co ferrite prepared by sol–gel method

International Journal of Modern Physics B ◽

10.1142/s0217979217500837 ◽

2017 ◽

Vol 31 (12) ◽

pp. 1750083 ◽

Cited By ~ 1

Author(s):

Nandeibam Nilima ◽

Mamata Maisnam ◽

Sumitra Phanjoubam

Keyword(s):

Electron Microscopy ◽

Sol Gel ◽

Xrd Analysis ◽

Initial Permeability ◽

X Ray Diffraction ◽

Gel Method ◽

Sol Gel Method ◽

Increase With Increase ◽

Transmission Electron ◽

Frequency Variations

Li–Ni–Co ferrite samples with compositional formula Li[Formula: see text]Ni[Formula: see text]Co[Formula: see text]Fe[Formula: see text]O4 with [Formula: see text] ranging from 0.00 to 0.1 in steps of 0.02 were prepared by sol–gel method. X-ray diffraction (XRD) analysis confirmed the formation of single phase with spinel structure in all the samples. The lattice constant evaluated from XRD data was found to increase with increase of Co[Formula: see text] substitution and crystallite size was observed in the range of 30–59 nm. The microstructure of the samples was studied by using scanning electron microscopy (SEM). Nanocrystalline nature of ferrites was also confirmed by transmission electron microscopy (TEM). [Formula: see text]–[Formula: see text] measurements were made using a vibrating sample magnetometer and hysteresis parameters such as saturation magnetization and coercivity were obtained for all compositions. The frequency variations of initial permeability and permeability loss showed a dispersive behavior for all compositions and an increase in initial permeability is observed with increase of Co[Formula: see text] substitution. The results obtained and mechanisms involved are discussed in the paper.

Download Full-text

Fabrication of Mesoporous Bioactive Glass Nanoparticles by Sol-Gel Method

Key Engineering Materials ◽

10.4028/www.scientific.net/kem.765.136 ◽

2018 ◽

Vol 765 ◽

pp. 136-139

Author(s):

Wei Wen Lin ◽

Wei Fang ◽

I Hao Chen ◽

Tze Yo Hung ◽

Chih Ling Huang

Keyword(s):

Electron Microscopy ◽

Bioactive Glass ◽

Sol Gel ◽

Tumor Resection ◽

Gel Method ◽

Sol Gel Method ◽

Ph Values ◽

Transmission Electron ◽

Mesoporous Bioactive Glass

Bioactive glass (BG) is characteristic of its great biocompatibility as well as osteoconductivity. Application of BG after surgery (e.g., tumor resection) aids rehabilitation of previously traumatized area, promotes bone regeneration, and prevents aggravation of wounds. In this in vitro study, bioglass nanoparticles (BGN) were successfully produced via sol-gel method. We observed the morphology of BGN through Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). Particle size was measured by Dynamic Light Scattering (DLS): 182.9 nm ± 37.7 nm in diameter, which corresponds to images obtained by SEM and TEM. We then synthesized BGs containing different proportions of Ca and P ions. Under different pH values, gels with various morphologies were formed.

Download Full-text

Synthesis, characterization and in vitro cytotoxicity study of Co and Ni ferrite nanoparticles prepared by sol-gel method

SN Applied Sciences ◽

10.1007/s42452-021-04709-y ◽

2021 ◽

Vol 3 (7) ◽

Author(s):

Alexandre Pancotti ◽

Dener Pereira Santos ◽

Dielly Oliveira Morais ◽

Mauro Vinícius de Barros Souza ◽

Débora R. Lima ◽

...

Keyword(s):

Photoelectron Spectroscopy ◽

Sol Gel ◽

Test Sample ◽

In Vitro Cytotoxicity ◽

Gel Method ◽

X Ray ◽

Sol Gel Method ◽

Transmission Electron ◽

Crystallite Sizes

AbstractIn this study, we report the synthesis and characterization of NiFe2O4 and CoFe2O4 nanoparticles (NPs) which are widely used in the biomedical area. There is still limited knowledge how the properties of these materials are influenced by different chemical routes. In this work, we investigated the effect of heat treatment over cytotoxicity of cobalt and niquel ferrites NPs synthesized by sol-gel method. Then the samples were studied using transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), vibrating sample magnetometer (VSM), Fourier Transform Infrared Spectroscopy Analysis (FTIR), and X-ray fluorescence (XRF). The average crystallite sizes of the particles were found to be in the range of 20–35 nm. The hemocompatibility (erythrocytes and leukocytes) was checked. Cytotoxicity results were similar to those of the control test sample, therefore suggesting hemocompatibility of the tested materials.

Download Full-text