STRUCTURAL PROPERTIES OF NANOCRYSTALLINE Ni–Al SPINEL FERRITES

2011 ◽  
Vol 25 (08) ◽  
pp. 1121-1125 ◽  
Author(s):  
A. T. RAGHAVENDER

Ultra fine NiAl x Fe 2-x O 4(0 ≤ x ≤ 1) nanopowders were synthesized by sol-gel method and their structural properties were investigated using X-ray diffractometer (XRD) and fourier transform infrared (FTIR) spectrometer. The particle size D, lattice constant a, density dx decreased with increasing non-magnetic Al content x. The combustion reaction mechanisms were explained with the help of FTIR analysis.

2009 ◽  
Vol 23 (27) ◽  
pp. 3289-3297 ◽  
Author(s):  
LUNHONG AI ◽  
JING JIANG

CoLa x Fe 2-x O 4 (x = 0.00, 0.05 and 0.1) nanoparticles were prepared simply by a modified citrate precursor route. Effects of La -substituting level on the their magnetic properties were investigated on the basis of the structural analysis. The thermal evolution of the precursor, as well as the microstructure of as-prepared products were studied by means of a thermogravimetric analyzer (TGA), X-ray diffractometer (XRD) and Fourier transform infrared (FTIR) spectrometer. The magnetic properties of the as-prepared samples were measured using a vibrating sample magnetometer (VSM). It was found that the magnetic properties were dependent on many factors such as La -substituting level, particle size and microstructure. The observed saturation magnetization decreased with increasing La content, whereas coercivity exhibited reverse behavior.


Arena Tekstil ◽  
2013 ◽  
Vol 28 (1) ◽  
Author(s):  
Maya Komalasari ◽  
Bambang Sunendar

Partikel nano TiO2 berbasis air dengan pH basa telah berhasil disintesis dengan menggunakan metode sol-gel dan diimobilisasi pada kain kapas dengan menggunakan kitosan sebagai zat pengikat silang. Sintesis dilakukan  dengan prekursor TiCl4 pada konsentrasi 0,3 M, 0,5 M dan 1 M, dan menggunakan templat kanji dengan proses kalsinasi pada suhu 500˚C selama 2 jam. Partikel nano TiO2 diaplikasikan ke kain kapas dengan metoda pad-dry-cure dan menggunakan kitosan sebagai crosslinking agent. Berdasarkan hasil Scanning Electron Microscope (SEM),diketahui bahwa morfologi partikel TiO2 berbentuk spherical dengan ukuran nano (kurang dari 100 nm). Karakterisasi X-Ray Diffraction (XRD) menunjukkan adanya tiga tipe struktur kristal utama, yaitu (100), (101) dan (102) dengan fasa kristal yang terbentuk adalah anatase dan rutile. Pada karakterisasi menggunakan SEM terhadap serbuk dari TiO2 yang telah diaplikasikan ke permukaan kain kapas, terlihat adanya imobilisasi partikel nano TiO2 melalui ikatan hidrogen silang dengan kitosan pada kain kapas. Hasil analisa tersebut kemudian dikonfirmasi dengan FTIR (Fourier Transform Infra Red) yang hasilnya memperlihatkan puncak serapan pada bilangan gelombang 3495 cm-1, 2546 cm-1, dan 511 cm-1,  yang masing-masing diasumsikan sebagai adanya vibrasi gugus fungsi O-H, N-H dan Ti-O-Ti. Hasil SEM menunjukkan pula bahwa kristal nano yang terbentuk diantaranya adalah fasa rutile , yang berdasarkan literatur terbukti dapatberfungsi sebagai anti UV.


Molecules ◽  
2021 ◽  
Vol 26 (12) ◽  
pp. 3588
Author(s):  
Jiayi Chen ◽  
Yansong Liu ◽  
Jiayue Zhang ◽  
Yuanlin Ren ◽  
Xiaohui Liu

Lyocell fabrics are widely applied in textiles, however, its high flammability increases the risk of fire. Therefore, to resolve the issue, a novel biomass-based flame retardant with phosphorus and nitrogen elements was designed and synthesized by the reaction of arginine with phosphoric acid and urea. It was then grafted onto the lyocell fabric by a dip-dry-cure technique to prepare durable flame-retardant lyocell fabric (FR-lyocell). X-ray photoelectron spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FTIR) analysis demonstrated that the flame retardant was successfully introduced into the lyocell sample. Thermogravimetric (TG) and Raman analyses confirmed that the modified lyocell fabric featured excellent thermal stability and significantly increased char residue. Vertical combustion results indicated that FR-lyocell before and after washing formed a complete and dense char layer. Thermogravimetric Fourier-transform infrared (TG-FTIR) analysis suggested that incombustible substances (such as H2O and CO2) were produced and played a significant fire retarding role in the gas phase. The cone calorimeter test corroborated that the peak of heat release rate (PHRR) and total heat release (THR) declined by 89.4% and 56.4%, respectively. These results indicated that the flame retardancy of the lyocell fabric was observably ameliorated.


Materials ◽  
2021 ◽  
Vol 14 (14) ◽  
pp. 3876
Author(s):  
Jesús Valdés ◽  
Daniel Reséndiz ◽  
Ángeles Cuán ◽  
Rufino Nava ◽  
Bertha Aguilar ◽  
...  

The effect of microwave radiation on the hydrothermal synthesis of the double perovskite Sr2FeMoO6 has been studied based on a comparison of the particle size and structural characteristics of products from both methods. A temperature, pressure, and pH condition screening was performed, and the most representative results of these are herein presented and discussed. Radiation of microwaves in the hydrothermal synthesis method led to a decrease in crystallite size, which is an effect from the reaction temperature. The particle size ranged from 378 to 318 nm when pH was 4.5 and pressure was kept under 40 bars. According to X-ray diffraction (XRD) results coupled with the size-strain plot method, the product obtained by both synthesis methods (with and without microwave radiation) have similar crystal purity. The Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDS) techniques showed that the morphology and the distribution of metal ions are uniform. The Curie temperature obtained by thermogravimetric analysis indicates that, in the presence of microwaves, the value was higher with respect to traditional synthesis from 335 K to 342.5 K. Consequently, microwave radiation enhances the diffusion and nucleation process of ionic precursors during the synthesis, which promotes a uniform heating in the reaction mixture leading to a reduction in the particle size, but keeping good crystallinity of the double perovskite. Precursor phases and the final purity of the Sr2FeMoO6 powder can be controlled via hydrothermal microwave heating on the first stages of the Sol-Gel method.


Catalysts ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 116
Author(s):  
Gian Luca Chiarello ◽  
Ye Lu ◽  
Miren Agote-Arán ◽  
Riccardo Pellegrini ◽  
Davide Ferri

Infrared spectroscopy is typically not used to establish the oxidation state of metal-based catalysts. In this work, we show that the baseline of spectra collected in diffuse reflectance mode of a series of Pd/Al2O3 samples of increasing Pd content varies significantly and reversibly under alternate pulses of CO or H2 and O2. Moreover, these baseline changes are proportional to the Pd content in Pd/Al2O3 samples exhibiting comparable Pd particle size. Similar measurements by X-ray absorption spectroscopy on a different 2 wt.% Pd/Al2O3 confirm that the baseline changes reflect the reversible reduction-oxidation of Pd. Hence, we demonstrate that changes in oxidation state of metal-based catalysts can be determined using diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and that this behavior is part of the spectral changes that are returned by experiments under operando conditions.


2013 ◽  
Vol 756 ◽  
pp. 91-98 ◽  
Author(s):  
Ftema W. Aldbea ◽  
Noor Bahyah Ibrahim ◽  
Mustafa Hj. Abdullah

Terbium –substituted yttrium iron garnet (Tb1.5Y1.5Fe5O12) films nanoparticles were successfully prepared by a sol-gel method. The films were deposited on the quartz substrate using spin coating technique. To study effect of annealing temperature, the annealing process was executed at 700, 800 and 900 °C in air for 2 hours. The X-ray diffraction (XRD) proved that the pure phase of garnet structure was detected for the film annealed at 900 °C. The lattice parameter increased with the increment of annealing temperature and the highest value of 12.35 Å was obtained at 900 °C. Field Emission Scanning Electron Microscope (FE-SEM) results showed that the particle size increased from 43nm to 56nm as annealing temperature increased from 700 to 900°C. The film’s thickness also affected by increasing of annealing temperature and become thin at 900 °C due to densification process occurred at high annealing temperature. The elemental compositions of the Tb1.5Y1.5Fe5O12 film were detected using an Energy Dispersive X-raySpectroscopy (EDX). Magnetic properties at room temperature were measured using a Vibrating Sample Magnetometer (VSM).The saturation magnetization Ms increased with the annealingtemperature and showed a high value of 104emu/cm3, but the coercivity Hc of the film was decreased due to the increment of the particle size. Normal 0 21 false false false MS X-NONE X-NONE MicrosoftInternetExplorer4 Terbium –substituted yttrium iron garnet (Tb1.5Y1.5Fe5O12) films nanoparticles were successfully prepared by a sol-gel method. The films were deposited on the quartz substrate using spin coating technique. To study effect of annealing temperature, the annealing process was executed at 700, 800 and 900°C in air for 2 hours. The X-ray diffraction (XRD) proved that the pure phase of garnet structure was detected for the film annealed at 900 °C. The lattice parameter increased with the increment of annealing temperature and the highest value of 12.35 Å was obtained at 900 °C. Field Emission Scanning Electron Microscope (FE-SEM) results showed that the particle size increased from 43nm to 56nm as annealing temperature increased from 700 to 900 °C. The film’s thickness also affected by increasing of annealing temperature and become thin at 900 °C due to densification process occurred at high annealing temperature. The elemental compositions of the Tb1.5Y1.5Fe5O12 film were detected using an Energy Dispersive X-ray Spectroscopy (EDX). Magnetic properties at room temperature were measured using a Vibrating Sample Magnetometer (VSM).The saturation magnetization Ms increased with the annealing temperature and showed a high value of 104emu/cm3, but the coercivity Hc of the film was decreased due to the increment of the particle size. st1\:*{behavior:url(#ieooui) } /* Style Definitions */ table.MsoNormalTable {mso-style-name:"Table Normal"; mso-tstyle-rowband-size:0; mso-tstyle-colband-size:0; mso-style-noshow:yes; mso-style-priority:99; mso-style-qformat:yes; mso-style-parent:""; mso-padding-alt:0cm 5.4pt 0cm 5.4pt; mso-para-margin:0cm; mso-para-margin-bottom:.0001pt; mso-pagination:widow-orphan; font-size:11.0pt; font-family:"Calibri","sans-serif"; mso-ascii-font-family:Calibri; mso-ascii-theme-font:minor-latin; mso-fareast-font-family:"Times New Roman"; mso-fareast-theme-font:minor-fareast; mso-hansi-font-family:Calibri; mso-hansi-theme-font:minor-latin; mso-bidi-font-family:"Times New Roman"; mso-bidi-theme-font:minor-bidi;}


2012 ◽  
Vol 476-478 ◽  
pp. 2059-2062
Author(s):  
Chen Wang ◽  
Ya Dong Li ◽  
Gu Qiao Ding

Tributyl borate was first adopted for the introduction of boron in the preparation of bioactive borosilicate xerogel by sol-gel method. The xerogel reacted continuously in 0.25M K2HPO4 solution with a starting pH value of 7.0 at 37 °C for 1day. The structural, morphologies and compositional changes resulting from the conversion were characterized using X-ray diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy. The results indicated that speed of formation of HA was cut way back on the time with the addition of boron and the induction period for the HA nucleation on the surface of the borosilicate xerogel was short than 1 days. The conversion mechanism of the borosilicate xerogels to hydroxyapaptite was also discussed.


PLoS ONE ◽  
2020 ◽  
Vol 15 (12) ◽  
pp. e0244511
Author(s):  
Fernando Gordillo-Delgado ◽  
Jakeline Zuluaga-Acosta ◽  
Gonzalo Restrepo-Guerrero

In this work, the effect of the inoculation of silver-incorporated titanium dioxide nanoparticles (Ag-TiO2 NPs) in spinach seeds was evaluated on certain growth, physiology and phytotoxicity parameters of the plants. This is an important crop for human consumption with high nutritional value due to their low calorie and fat content, providing various vitamins and minerals, especially iron. These NPs were obtained by means of the sol-gel method and heat treatment; the resulting powder material was characterized using X-ray diffraction and scanning electron microscopy and the influence of these NPs on plants was measured by estimating the germination rate, monitoring morphological parameters and evaluating phytotoxicity. The photosynthetic activity of the spinach plants was estimated through the quantification of the Ratio of Oxygen Evolution (ROE) by the photoacoustic technique. Samples of TiO2 powder with particle size between 9 and 43 nm were used to quantify the germination rate, which served to determine a narrower size range between 7 and 26 nm in the experiments with Ag-TiO2 NPs; the presence of Ag in TiO2 powder samples was confirmed by energy-dispersive X-ray spectroscopy. The analysis of variance showed that the dependent variable (plant growth) could be affected by the evaluated factors (concentration and size) with significant differences. The statistical trend indicated that the application of the Ag-TiO2 NPs suspension of lowest concentration and smallest particle size could be a promoting agent of the growth and development of these plants. The inoculation with NPs of 8.3 nm size and lowest concentration was related to the highest average ROE value, 24.6 ± 0.2%, while the control group was 20.2 ± 0.2%. The positive effect of the Ag-TiO2 NPs treatment could be associated to the generation of reactive oxygen species, antimicrobial activity, increased biochemical attributes, enzymatic activity or improvements in water absorption.


2013 ◽  
Vol 448-453 ◽  
pp. 3041-3045
Author(s):  
Fei Bi ◽  
Xiang Ting Dong ◽  
Jin Xian Wang ◽  
Gui Xia Liu ◽  
Wen Sheng Yu

PVP/[Y(NO3)3+Al (NO3)3] composite nanobelts were fabricated via electrospinning combined with sol-gel process and novel structure of Y3Al5O12(denoted as YAG for short) nanobelts have been obtained after calcination of the relevant composite nanobelts. The structural properties were characterized by X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). XRD analysis indicated that the composite nanobelts were amorphous, and YAG nanobelts were cubic in structure with space group Ia3d. FTIR analysis manifested that pure YAG nanobelts were formed at 900oC. SEM analysis and histograms revealed that the width of the composite nanobelts and YAG nanobelts were 3.5 μm and 2.4 μm, and the thickness were 240 nm and 112 nm, respectively, under the 95% confidence level. The formation mechanism of YAG nanobelts was discussed in detail.


1994 ◽  
Vol 9 (8) ◽  
pp. 2102-2108 ◽  
Author(s):  
E. Haro-Poniatowski ◽  
R. Rodríguez-Talavera ◽  
Heredia M. de la Cruz ◽  
O. Cano-Corona ◽  
R. Arroyo-Murillo

Sols of titania were obtained by the sol-gel method and their size profile was followed by dynamical light scattering. In the early stages of the reaction an unstable behavior was detected. After this unstable regime the particle size reaches a steady state where the sols have a constant size while increasing in number. Once the sol concentration reaches its overlap value, the gelation regime takes place. For samples prepared in this way Raman spectra and x-ray diffractometry were used to characterize the kinetics of crystallization of the material.


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