Preparation of Maghemite-Silica Nanocomposites Using Sol-Gel Technique

2010 ◽  
Vol 97-101 ◽  
pp. 2140-2143 ◽  
Author(s):  
Bee Chin Ang ◽  
Iskandar Idris Yaacob
Keyword(s):  
Crystallite Size ◽  
Sol Gel ◽  
Weight Ratio ◽  
Spherical Shape ◽  
Average Crystallite Size ◽  
Silica Matrix ◽  
Silica Xerogel ◽  
Maghemite Nanoparticles ◽  
Silica Nanocomposites ◽  
Gel Technique

Superparamagnetic maghemite nanoparticles were successfully produced using Massart’s procedure. Nanocomposites consisting of the synthesized maghemite nanoparticles and silica were produced by dispersing the as-synthesized maghemite nanoparticles into the silica xerogel, which was prepared by sol-gel technique. The system was then heated for 3 days at 140oC. A variety of weight ratios of Fe2O3/SiO2 was investigated. The nanocomposites were characterized using TGA, XRD, TEM and AGM. TGA thermogram showed one significant weight loss at around 250oC. It was caused by dehydration and evaporation of solvent from sol-gel process. XRD showed that the dispersed particles were still maghemite. TEM micrographs showed that the maghemite nanoparticles were in spherical shape and they were homogeneously incorporated in the silica matrix. The values of magnetization at 10kOe applied field were in the range of 1.79emu/g to 9.53emu/g depending of the Fe2O3/SiO2 ratio. Reduction of average crystallite size of dispersed maghemite particles was observed after encapsulation process. Increasing weight ratio of Fe2O3/SiO2 caused increase of the average crystallite size of maghemite nanoparticles.

Structure Analysis of Nanocrystalline MgO Aerogel Prepared by Sol-Gel Method

2007 ◽  
Vol 130 ◽  
pp. 203-206 ◽  
Author(s):  
Grzegorz Dercz ◽  
Lucjan Pająk ◽  
Krystian Prusik ◽  
Roman Pielaszek ◽  
Janusz J. Malinowski ◽  
...  
Keyword(s):  
Crystallite Size ◽  
Magnesium Oxide ◽  
Sol Gel ◽  
Average Crystallite Size ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Gel Technique ◽  
Microscopy Images ◽  
Nanocrystalline Mgo

Wet gel obtained by sol-gel technique was dried in supercritical CO2 to prepare hydrated form of magnesium oxide. Calcination at 723 K under vacuum yielded nanocrystalline MgO aerogel. Structure studies were performed by X-ray diffraction, scanning and transmission electron microcopies. Electron microscopy images reveal rough, unfolded and ramified structure of solid skeleton. Specific surface area SBET was equal to 238 m2/g. X-ray pattern reveals the broadened diffraction lines of periclase, the only crystalline form of magnesium oxide. The gamma crystallite size distribution was determined using FW 5 4 / 5 1 M method proposed by R. Pielaszek. The obtained values of <R> and σ (measure of polydispersity) of particle size parameters are equal to 6.5 nm and 1.8 nm, respectively, whereas the average crystallite size estimated by Williamson-Hall procedure was equal to 6.0 nm. The obtained at Rietveld refinement Rwp, and S fitting parameters equal to 6.62% and 1.77, respectively, seem to be satisfactory due to the nanosize of MgO crystallites and because of the presence of amorphous phase.

scholarly journals Investigation ofFe2O3/SiO2Nanocomposite by FESEM and TEM

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
B. C. Ang ◽  
I. I. Yaacob ◽  
Irwan Nurdin
Keyword(s):  
Iron Oxide ◽  
Silica Gel ◽  
Average Pore Size ◽  
Sol Gel ◽  
Silica Matrix ◽  
Silica Xerogel ◽  
Line Profile Analysis ◽  
Maghemite Nanoparticles ◽  
Iron Oxide Particles ◽  
Average Pore

Superparamagnetic maghemite nanoparticles were synthesized using Massart’s procedure. Nanocomposites that consist of the synthesized maghemite nanoparticles and silica were produced by dispersing the as-synthesized maghemite nanoparticles into the silica xerogel prepared by sol-gel technique. The system was then heated for 3 days at 140°C. The structure, morphology, and texture of the system were analysed by FESEM and TEM. The result from FESEM showed that the silica gel forms a network structure, which contained numerous pores, with an average pore size of 15 nm. EDX line profile analysis was carried out, and the result indicated that the embedded particles were iron oxide. EELS showed the presence of Fe-L2signal, which confirmed the presence of iron oxide particles within the silica matrix. The average diameters were 5.0 nm for as-synthesized maghemite nanoparticles and 4.4 nm for the embedded maghemite nanoparticles in silica xerogel matrix. The embedded maghemite nanoparticles in nanocomposite also showed a narrower distribution compared to as-synthesized particles. The magnetization values at 10 kOe applied field,Ms10 kOe, were 9.53 emu/g and 1.79 emu/g for as-synthesized and embedded nanoparticles, respectively. A reduction in average crystallite size was observed for the dispersed maghemite particles after formation of the nanocomposite indicating a slight dissolution of maghemite nanoparticles in silica gel.

scholarly journals Tailoring Mesoporous Titania Features by Ultrasound-Assisted Sol-Gel Technique: Effect of Surfactant/Titania Precursor Weight Ratio

Nanomaterials ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 1263
Author(s):  
Elvira Mahu ◽  
Cristina Giorgiana Coromelci ◽  
Doina Lutic ◽  
Iuliean Vasile Asaftei ◽  
Liviu Sacarescu ◽  
...  
Keyword(s):  
Photocatalytic Activity ◽  
Sol Gel ◽  
Weight Ratio ◽  
Soft Template ◽  
Synthesis Process ◽  
Mesoporous Titania ◽  
Cavitation Effect ◽  
Titania Precursor ◽  
Gel Technique ◽  
Ultrasound Assisted

A mesoporous titania structure has been prepared using the ultrasound-assisted sol-gel technique in order to find out a way to tailor its structure. The TiO2 obtained was compared to the same version of titania but synthesized by a conventional sol-gel method with the objective of understanding the effect of ultrasound in the synthesis process. All synthesis experiments were focused on the preparation of a titania photocatalyst. Thus, the anatase photocatalytic active phase of titania was proven by X-ray diffraction. Additionally, the ultrasonation treatment proved to increase the crystallinity of titania samples, being one of the requirements to having good photocatalytic activity for titania. The influence of surfactant/titania precursor weight ratio on the structural (XRD), textural (N2-sorption measurements), morphological (TEM), surface chemistry (FTIR) and optical properties (UVDR) was investigated. It was observed that the crystallite size, specific surface area, band gap energy and even photocatalytic activity was affected by the synergism occurring between cavitation effect and the surfactant/titania precursor weight ratio. The study yielded interesting great results that could be considered for further application of ultrasound to tailor mesoporous titania features via sol-gel soft template synthesis, against conventional sol-gel process.

Rapid Synthesis and Characterization of Maghemite Nanoparticles

2008 ◽  
Vol 8 (2) ◽  
pp. 861-866 ◽  
Author(s):  
Bilsen Tural ◽  
Macit Özenbaş ◽  
Selçuk Atalay ◽  
Mürvet Volkan
Keyword(s):  
Particle Size ◽  
Elevated Temperatures ◽  
Sol Gel ◽  
Volume Ratio ◽  
Silica Matrix ◽  
Superparamagnetic Nanoparticles ◽  
Maghemite Nanoparticles ◽  
Gelation Temperature ◽  
Iron Oxide Particles ◽  
Evaporation Surface

Fe2O3–SiO2 nanocomposites were prepared by a sol–gel method using various evaporation surface to volume (S/V) ratios ranging from 0.03 to 0.2. The Fe2O3–SiO2 sols were gelated at various temperatures ranging from 50 °C to 70 °C, and subsequently they were calcined in air at 400 °C for 4 hours. The structure and the magnetic properties of the prepared Fe2O3–SiO2 nanocomposites were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), differential thermal analysis (DTA), and vibrating sample magnetometer (VSM) measurements. The gelation temperature of the Fe2O3–SiO2 sols influenced strongly the particle size and crystallinity of the maghemite nanoparticles. It was observed that the particle size of maghemite nanoparticles increased with the increasing of the gelation temperature of the sols, which may be due to the agglomeration of the maghemite particles at elevated temperatures inside the microporosity of the silica matrix during the gelation process, and the subsequent calcination of these gels at 400 °C resulted in the formation of large size iron oxide particles. Magnetization studies at temperatures of 10, 195, and 300 K showed superparamagnetic behavior for all the nanocomposites prepared using the evaporation surface to volume ratio (S/V) of 0.1, 0.2, 0.09, and 0.08. The saturation magnetization, Ms, values measured at 10K were 5.5, 8.5, and 9.5 emu/g, for the samples gelated at 50, 60, and 70 °C, respectively. At the gelation temperature of 70 °C, γ-Fe2O3 crystalline superparamagnetic nanoparticles with the particle size of 9±2 nm were formed in 12 hours for the samples prepared at the S/V ratio of 0.2.

Structural and Optical Characterization of Synthesized TiO2 Nanopowder Using Sol–Gel Technique

2016 ◽  
Vol 15 (01n02) ◽  
pp. 1650002 ◽  
Author(s):  
S. Lourduraj ◽  
R. Victor Williams
Keyword(s):  
Anatase Phase ◽  
Sol Gel ◽  
Visible Spectrum ◽  
Average Crystallite Size ◽  
Xrd Analysis ◽  
Force Microscopy ◽  
Morphological Studies ◽  
Atomic Force ◽  
Gel Technique

The nanocrystalline TiO2 powder was synthesized by sol–gel method. The XRD analysis reveals that TiO2 powder was highly crystalline (anatase phase) and nanostructured with tetragonal system. The average crystallite size after calcined at 673[Formula: see text]K is found to be 7.7[Formula: see text]nm. The surface morphological studies using scanning electron microscopy (SEM) exhibit that the formation of nanosized TiO2 particles with less densification nature. Atomic force microscopy (AFM) topography exhibits the uniform distribution of spherical-shaped particles. The energy dispersive X-ray spectroscopy (EDX) confirms the presence of Titanium and Oxygen in synthesized TiO2 nanopowder. The value of optical bandgap of TiO2 nanopowder calculated from UV-Visible spectrum is 3.45[Formula: see text]eV. The presence of TiO2 particles is confirmed from the dominant fourier transform infrared (FTIR) peaks at 621[Formula: see text]cm[Formula: see text] and 412[Formula: see text]cm[Formula: see text].

AN INVESTIGATION INTO MECHANOCHEMICAL SYNTHESIS OF NANOCRYSTALLINE HEXAFERRITE POWDER

2011 ◽  
Vol 25 (07) ◽  
pp. 987-993
Author(s):  
S. SADEGHI-NIARAKI ◽  
S. A. SEYYED EBRAHIMI ◽  
SH. RAYGAN
Keyword(s):  
Crystallite Size ◽  
Single Phase ◽  
Sol Gel ◽  
Milled Powder ◽  
Particle Morphology ◽  
Average Crystallite Size ◽  
Phase Evolution ◽  
High Energy ◽  
Strontium Hexaferrite ◽  
Electron Microscopes

Nanocrystalline strontium hexaferrite powder has been prepared by a new mechanochemical method in which the single phase hexaferrite was obtained via a sol–gel autocombustion process followed by an intermediate high energy milling step and subsequent annealing. The effects of the intermediate milling on the phase evolution, crystallite size and annealing behavior of the final products were investigated using the X-ray diffraction (XRD) technique. The single phase strontium hexaferrite was obtained at an annealing temperature of 800°C, while this temperature was 1,000°C for the powder synthesized without milling. It could be seen that an intermediate milling accelerates the formation of strontium hexaferrite during the calcination process. The results showed that in the milled powder, the average crystallite size of the ferrite was about 40 nm and much smaller than that of the nonmilled powder. Magnetic properties were also measured by a vibrating sample magnetometer (VSM). The particle morphology was then studied by scanning and transmission electron microscopes (SEM and TEM).

Iron and Iron-oxide on Silica Nanocomposites Prepared by the Sol-gel Method

2002 ◽  
Vol 17 (3) ◽  
pp. 590-596 ◽  
Author(s):  
G. Ennas ◽  
M. F. Casula ◽  
G. Piccaluga ◽  
S. Solinas ◽  
M. P. Morales ◽  
...  
Keyword(s):  
Sol Gel ◽  
Silica Matrix ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Gel Method ◽  
Sol Gel Method ◽  
Silica Nanocomposites ◽  
Transmission Electron ◽  
Nanometric Particles

γ–Fe2O3/SiO2 and Fe/SiO2 nanocomposites, with a Fe/Si molar ratio of 0.25, were prepared by the sol-gel method starting from ethanolic solutions of tetraethoxysilane and iron (III) nitrate. After gelation the xerogels were oxidated or reduced. Samples were investigated by transmission electron microscopy, x-ray diffraction, differential scanning calorimetry, and thermogravimetry. Magnetic properties of the samples were investigated at room temperature (RT) and at 77 K. Nanometric particles supported in the silica matrix were obtained in all cases. Bigger particles (10 nm) were obtained in the case of Fe/SiO2 nanocomposites with respect to the γ–Fe2O3/SiO2 samples (5–8 nm). A slight effect of sol dilution on particle size was observed only in the case of γ–Fe2O3/SiO2 nanocomposites. A superparamagnetic behavior was shown at RT only by γ–Fe2O3/SiO2 nanocomposites. Iron-based composites exhibited coercivity values higher than 700 Oe at RT.

Magnetic Properties of the La0.50Ba0.50MnO3 Nanomanganites

2009 ◽  
Vol 152-153 ◽  
pp. 135-138 ◽  
Author(s):  
S.V. Trukhanov ◽  
A.V. Trukhanov ◽  
Christian E. Botez ◽  
H. Szymczak
Keyword(s):  
Magnetic Properties ◽  
Crystallite Size ◽  
Sol Gel ◽  
Exchange Interactions ◽  
Average Crystallite Size ◽  
Anomalous Behavior ◽  
Air Atmosphere ◽  
Crystallite Surface ◽  
Step Heat Treatment ◽  
Lattice Compression

Nanocrystalline La0.50Ba0.50MnO3 manganite was synthesized by an optimized sol-gel method. The initial sample was subjected to step-by-step heat treatment under air atmosphere. The ion stoichiometry, the morphology of crystallites of ceramics, and the magnetic properties were studied. It is established that the average crystallite size increases with increasing annealing temperature. All of the samples studied are characterized by a perovskite-like cubic structure, with the unit cell parameter a increasing continuously with the average crystallite size. The most significant lattice compression occurs in the sample with an average crystallite size of ~ 30 nm. The increase in the average crystallite size causes a nonmonotonic increase in the Curie temperature and in the spontaneous magnetic moment. The anomalous behavior of the magnetic properties of the La0.50Ba0.50MnO3 manganites obtained is explained by the competition between two size effects, namely, the frustration of the indirect exchange interactions Mn3+ – O – Mn4+ on the nanocrystallite surface and the crystal lattice compression due to the crystallite surface tension.

Performance Effect of ZnAl2O4 - SiO2 Thin Film for Wireless Patch Antenna Application

2014 ◽  
Vol 28 ◽  
pp. 141-150 ◽  
Author(s):  
Mohd Syafiq Zulfakar ◽  
Huda Abdullah ◽  
Mohammad Tariqul Islam ◽  
Wan Nasarudin Wan Jalal ◽  
Zalita Zainuddin ◽  
...  
Keyword(s):  
Crystallite Size ◽  
Patch Antenna ◽  
Sol Gel ◽  
Average Crystallite Size ◽  
Cubic Phase ◽  
Frequency Range ◽  
Performance Effect ◽  
X Ray ◽  
Force Microscopy ◽  
Atomic Force

Polycrystalline of (1-x)ZnAl2O4 – xSiO2 compound with compositions of x = 0.00, 0.05, 0.10, 0.15, 0.20 and 0.25 have been prepared using sol-gel method. Structural properties was investigated by atomic force microscopy (AFM) and x-ray diffractometer (XRD). The AFM images analysis showed that the surface roughness of the highest composition had rougher surface compared with other samples. XRD measurement indicated that the crystallite size also increased with average crystallite size around 18 nm with cubic phase had been found. The dielectric permittivity value were measured with frequency range of 1 Hz to 1 MHz. It is showed that the dielectric value decreased as the freqeuncy was applied to the samples. The performance of the patch antenna showed that the antenna resonated at 3.30 GHz and give-13.87 dB with frequency range about 2 – 4 GHz.

scholarly journals Oryza sativa PULP AS A TEMPLATE IN α-ALUMINA NANOCRYSTALLINE SYNTHESIS BY PRECURSOR CALCINING PROCESS

2016 ◽  
Vol 1 (01) ◽  
Author(s):  
Rifki Septawendar ◽  
Bambang Sunendar Purwasasmita ◽  
Suhanda , ◽  
Leanddas Nurdiwijayanto ◽  
Taufan Hidayat
Keyword(s):  
Oryza Sativa ◽  
Crystallite Size ◽  
Calcination Temperature ◽  
Sol Gel ◽  
Weight Ratio ◽  
Xrd Analysis ◽  
Characterization Result ◽  
Nano Powder ◽  
Temperature Scanning ◽  
Α Al2o3

Synthesis and characterization of α-alumina nano powder with Oryza sativa pulp as template by precursor calcining process have been successfully conducted. The aim of this experiment is to study the potential of Oryza sativa pulp as a template of precursor calcining process method that isrelatively cheaper than that of sol gel method in α-alumina synthesis. Weight ratio between precursor and Oryza sativa pulp was 1 : 2. The effect of calcination temperature on α-alumina synthesis in this research is set by variation of calcination temperature at 900°C, 1000°C, and 1100°C. In this research, X-Ray Diffraction (XRD) analysis is used to investigate the transformation of crystal phase, structure and size of the crystal formed by the calcinations temperature. Scanning Electron Microscope (SEM)characterization is used to identify morphology of α-Al2O3 powder. Based on XRD characterization result, synthesized alumina sample forms α-Al2O3 and γ-Al2O3 crystal phases. The formed crystallite size is in nanometer dimension for α-Al2O3 which biggest crystallite size is 46.6 nm. According to SEM characterization result, it is shown that α-Al2O3 formed rhombohedral or bar shape and planar. The particle size will increase along with the elevation of calcination temperature.Key words : nano powder, α-alumina, precursor calcining process, oryza sativa pulp ABSTRAKSintesis dan karakterisasi nanopowder α-alumina dengan menggunakan pulp merang sebagai template melalui proses kalsinasi prekursor telah berhasil dilakukan. Penelitian ini bertujuan untuk mempelajari potensi pulp merang sebagai template dari precursor calcination process yang merupakan metoda relatif lebih murah dibandingkan metode sol gel dalam mensintesis α-alumina. Perbandingan berat antara prekursor dan pulp adalah 1:2. Pengaruh temperatur kalsinasi terhadap pembentukan α-alumina ditetapkan dengan variasi temperatur kalsinasi pada 900°C, 1000°C, dan 1100°C. Analisis diffraksi Sinar-X (XRD) digunakan untuk mengetahui perubahan fasa kristal, struktur, dan ukuran kristal yangterbentuk pada suhu kalsinasi tersebut. Karakterisasi SEM dilaksanakan untuk mengetahui morfologi dari serbuk α-Al2O3. Berdasarkan karakterisasi XRD, sampel alumina yang disintesis membentuk fasa α-Al2O3 dan γ-Al 2O3. Ukuran kristal yang terbentuk berskala nanometer, yaitu untuk α-Al2O3 ukuran kristal terbesar adalah 46,6 nm. Hasil karakterisasi SEM, terlihat bahwa α-Al2O3 membentuk struktur trigonal atau bentuk batang dan planar, ukuran partikel akan semakin membesar dengan meningkatnyatemperatur kalsinasi.Kata kunci : nano powder, α-alumina, proses kalsinasi prekursor, pulp merang. 

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