Characterization of Nanocrystalline γ–Fe2O3Prepared by Wet Chemical Method

1999 ◽  
Vol 14 (4) ◽  
pp. 1570-1575 ◽  
Author(s):  
G. Ennas ◽  
G. Marongiu ◽  
A. Musinu ◽  
A. Falqui ◽  
P. Ballirano ◽  
...  

Homogeneous maghemite (γ–Fe2O3) nanoparticles with an average crystal size around 5 nm were synthesized by successive hydrolysis, oxidation, and dehydration of tetrapyridino-ferrous chloride. Morphological, thermal, and structural properties were investigated by transmission electron microscopy (TEM), differential scanning calorimetry (DSC), and x-ray diffraction (XRD) techniques. Rietveld refinement indicated a cubic cell. The superstructure reflections, related to the ordering of cation lattice vacancies, were not detected in the diffraction pattern. Kinetics of the solid-state phase transition of nanocrystalline maghemite to hematite (α–Fe2O3), investigated by energy dispersive x-ray diffraction (EDXRD), indicates that direct transformation from nanocrystalline maghemite to microcrystalline hematite takes place during isothermal treatment at 385 °C. This temperature is lower than that observed both for microcrystalline maghemite and for nanocrystalline maghemite supported on silica.

2012 ◽  
Vol 600 ◽  
pp. 174-177 ◽  
Author(s):  
Jian Fei Xia ◽  
Zong Hua Wang ◽  
Yan Zhi Xia ◽  
Fei Fei Zhang ◽  
Fu Qiang Zhu ◽  
...  

Zirconia-graphene composite (ZrO2-G) has been successfully synthesized via decomposition of ZrOCl2•6H2O in a water-isopropanol system with dispersed graphene oxide (GO) utilizing Na2S as a precursor could enable the occurrence of the deposition of Zr4+ and the deoxygenation of GO at the same time. Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) techniques were used to characterize the samples. It was found that graphene were fully coated with ZrO2, and the ZrO2 existing in tetragonal phase, which resulted in the formation of two-dimensional composite.


2011 ◽  
Vol 311-313 ◽  
pp. 1638-1641
Author(s):  
Jun Hua Wang ◽  
Xiang Biao Cheng ◽  
Gang Huang ◽  
Feng Chun Dong ◽  
Yong Tang Jia

PCL/PVP blend membrane was prepared by casting solution method. Scanning electron microscopy (SEM), diffraction scanning calorimetry (DSC), and X-ray diffraction (XRD) techniques were employed to characterize membrane structure and morphology. Moreover, the hydrophilicity, mechanical property and biodegradability of membranes were investigated. Due to introducing PVP, the crystallinity and mechanical property of PCL altered to some extent. The hydrophilicity of the blend membrane improved remarkably with increasing PVP content, which was expressed by the contact angle declining and the rate of water absorption increasing. Lipase accelerated the degradation rate of PCL/PVP membrane.


1999 ◽  
Vol 14 (3) ◽  
pp. 771-779 ◽  
Author(s):  
K. Lu ◽  
M. L. Sui ◽  
J. H. Perepezko ◽  
B. Lanning

The reaction kinetics in vapor-deposited indium/amorphous-selenium (a-Se) multilayer thin films were studied using differential scanning calorimetry (DSC), x-ray diffraction (XRD), and transmission electron microscopy (TEM). A number of reactions were observed upon heating with characteristic temperatures which were found to be independent of the multilayer modulation wavelength. The initial interface reaction between In and a-Se is the formation of an In2Se phase. Kinetic analyses of the In2Se formation process combined with TEM observations indicated that interface reaction is characterized by the two-dimensional growth of pre-existing In2Se regions formed during deposition to impingement in the plane of the original In/a-Se interface. The change of the density of In2Se grains with temperature was analyzed in terms of the derived kinetic parameters, which is consistent with TEM observations and the heat release measurements.


2014 ◽  
Vol 798-799 ◽  
pp. 85-89 ◽  
Author(s):  
E.S.G. Junior ◽  
P.M . Jardim

Al2(WO4)3was synthesized by co-precipitation using Na2WO4and Al (NO3)3as precursors. After drying the precipitate, it was calcined at different temperatures between 500°C and 800°C. The crystallization and degradation temperatures of the samples were evaluated by means of Differential Scanning Calorimetry (DSC), Thermogravimetry (TG) and X-Ray Diffraction (XRD). It was observed that the crystallization starts at around 600°C, however Transmission Electron Microscopy (TEM) analysis showed that at this temperature the sample is partially amorphous. The degradation of the material starts at around 1200°C and at 1400°C the tungsten oxide has almost completely evaporated and the material is transformed mainly in alpha-alumina.


Author(s):  
R. E. Herfert

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.


Author(s):  
D. Nagasamy Venkatesh ◽  
S. Karthick ◽  
M. Umesh ◽  
G. Vivek ◽  
R.M. Valliappan ◽  
...  

Roxythromycin/ β-cyclodextrin (Roxy/ β-CD) dispersions were prepared with a view to study the influence of β-CD on the solubility and dissolution rate of this poorly soluble drug. Phase-solubility profile indicated that the solubility of roxythromycin was significantly increased in the presence of β-cyclodextrin and was classified as AL-type, indicating the 1:1 stoichiometric inclusion complexes. Physical characterization of the prepared systems was carried out by differential scanning calorimetry (DSC), X-ray diffraction studies (XRD) and IR studies. Solid state characterization of the drug β-CD binary system using XRD, FTIR and DSC revealed distinct loss of drug crystallinity in the formulation, ostensibly accounting for enhancement of dissolution rate.


Metals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 218
Author(s):  
Xianjie Yuan ◽  
Xuanhui Qu ◽  
Haiqing Yin ◽  
Zaiqiang Feng ◽  
Mingqi Tang ◽  
...  

This present work investigates the effects of sintering temperature on densification, mechanical properties and microstructure of Al-based alloy pressed by high-velocity compaction. The green samples were heated under the flow of high pure (99.99 wt%) N2. The heating rate was 4 °C/min before 315 °C. For reducing the residual stress, the samples were isothermally held for one h. Then, the specimens were respectively heated at the rate of 10 °C/min to the temperature between 540 °C and 700 °C, held for one h, and then furnace-cooled to the room temperature. Results indicate that when the sintered temperature was 640 °C, both the sintered density and mechanical properties was optimum. Differential Scanning Calorimetry, X-ray diffraction of sintered samples, Scanning Electron Microscopy, Energy Dispersive Spectroscopy, and Transmission Electron Microscope were used to analyse the microstructure and phases.


1995 ◽  
Vol 418 ◽  
Author(s):  
J. Forbes ◽  
J. Davis ◽  
C. Wong

AbstractThe detonation of explosives typically creates 100's of kbar pressures and 1000's K temperatures. These pressures and temperatures last for only a fraction of a microsecond as the products expand. Nucleation and growth of crystalline materials can occur under these conditions. Recovery of these materials is difficult but can occur in some circumstances. This paper describes the detonation synthesis facility, recovery of nano-size diamond, and plans to synthesize other nano-size materials by modifying the chemical composition of explosive compounds. The characterization of nano-size diamonds by transmission electron microscopy and electron diffraction, X-ray diffraction and Raman spectroscopy will also be reported.


2012 ◽  
Vol 174-177 ◽  
pp. 508-511
Author(s):  
Lin Lin Yang ◽  
Yong Gang Wang ◽  
Yu Jiang Wang ◽  
Xiao Feng Wang

BiFeO3 polyhedrons had been successfully synthesized via a hydrothermal method. The as-prepared products were characterized by power X-ray diffraction (XRD) pattern, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The possible mechanisms for the formation of BiFeO3 polyhedrons were discussed. Though comparison experiments, it was found that the kind of precursor played a key role on the morphology control of BiFeO3 crystals.


2017 ◽  
Vol 8 ◽  
pp. 1257-1265 ◽  
Author(s):  
Urszula Klekotka ◽  
Magdalena Rogowska ◽  
Dariusz Satuła ◽  
Beata Kalska-Szostko

Ferrite nanoparticles with nominal composition Me0.5Fe2.5O4 (Me = Co, Fe, Ni or Mn) have been successfully prepared by the wet chemical method. The obtained particles have a mean diameter of 11–16 ± 2 nm and were modified to improve their magnetic properties and chemical activity. The surface of the pristine nanoparticles was functionalized afterwards with –COOH and –NH2 groups to obtain a bioactive layer. To achieve our goal, two different modification approaches were realized. In the first one, glutaraldehyde was attached to the nanoparticles as a linker. In the second one, direct bonding of such nanoparticles with a bioparticle was studied. In subsequent steps, the nanoparticles were immobilized with enzymes such as albumin, glucose oxidase, lipase and trypsin as a test bioparticles. The characterization of the nanoparticles was acheived by transmission electron microscopy, X-ray diffraction, energy dispersive X-ray and Mössbauer spectroscopy. The effect of the obtained biocomposites was monitored by Fourier transform infrared spectroscopy. The obtained results show that in some cases the use of glutaraldehyde was crucial (albumin).


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