Microstructure Characterization of Metal Mixed Oxides

MRS Advances ◽  
2017 ◽  
Vol 2 (64) ◽  
pp. 4025-4030 ◽  
Author(s):  
T. Kryshtab ◽  
H. A. Calderon ◽  
A. Kryvko

ABSTRACTThe microstructure of Ni-Mg-Al mixed oxides obtained by thermal decomposition of hydrotalcite-like compounds synthesized by a co-precipitation method has been studied by using X-ray diffraction (XRD) and atomic resolution transmission electron microscopy (TEM). XRD patterns revealed the formation of NixMg1-xO (x=0÷1), α-Al2O3 and traces of MgAl2O4 and NiAl2O4 phases. The peaks profile analysis indicated a small grain size, microdeformations and partial overlapping of peaks due to phases with different, but similar interplanar spacings. The microdeformations point out the presence of dislocations and the peaks shift associated with the presence of excess vacancies. The use of atomic resolution TEM made it possible to identify the phases, directly observe dislocations and demonstrate the vacancies excess. Atomic resolution TEM is achieved by applying an Exit Wave Reconstruction procedure with 40 low dose images taken at different defocus. The current results suggest that vacancies of metals are predominant in MgO (NiO) crystals and that vacancies of Oxygen are predominant in Al2O3 crystals.

2014 ◽  
Vol 70 (6) ◽  
pp. 1004-1010 ◽  
Author(s):  
Th. I. Shalaby ◽  
N. M. Fikrt ◽  
M. M. Mohamed ◽  
M. F. El Kady

This study investigated the applicability of magnetite Fe3O4 nanoparticles coated with chitosan (CMNs) for the removal of some toxic heavy metals from simulated wastewater. Magnetic nanomaterials were synthesized using the co-precipitation method and characterized by transmission electron microscope, scanning electron microscope, X-ray diffraction, and Fourier transformer infrared spectroscopy. The magnetic properties of the prepared magnetic nanoparticles were determined by a vibrating-sample magnetometer. Batch experiments were carried out to determine the adsorption kinetics of Cr(VI) and Cd(II) by magnetic nanoparticles. It is noteworthy that CMNs show a highly efficient adsorption capacity for low concentration Cr(VI) and Cd(II) ions solution, which can reach 98% within 10 min.


2016 ◽  
Vol 25 (6) ◽  
pp. 096369351602500 ◽  
Author(s):  
Ruimin Fu ◽  
Mingfu Zhu

Nowadays, the hummers method for preparation of graphene oxide (GO) was improved. The grapheme oxide @ Fe3O4 magnetic nanocomposites were synthesized by co-precipitation method. After analysing the morphology and structure of obtained nanocomposites by X-ray diffraction (XRD), transmission electron microscope (TEM) and Fourier transform infrared (FT-IR) spectroscopy, the result was shown as follows. The particle size of Fe3O4 in nanocomposites is 30 nm. Many functional groups are found in grapheme oxide, and such groups could be used to bind with the drug. In the test for magnetic properties, the nanocomposites gathered rapidly in the vicinity of the permanent magnet. The nanocomposites, with high superparamagnetism, can be used in the following applications: drug targeting transports, drug carrier, and diagnosis assistant system.


2014 ◽  
Vol 896 ◽  
pp. 104-107 ◽  
Author(s):  
Poedji Loekitowati Hariani ◽  
Fahma Riyanti

CuFe2O4 nanoparticles were synthesized by co-precipitation method from the solution of CuCl2 and FeCl3 in alkaline condition. The prepared magnetic CuFe2O4 can be used to adsorb Cr (VI) ions from aqueous solution and separated from medium by magnetic technique. The characterization of CuFe2O4 with X-Ray diffraction (XRD) showed cubic units shells with diameter in the range 15-20 nm which obtained by Transmission Electron Microscope (TEM). The saturation of magnetization is around 13 emu g-1 measured with Vibrating Sample Magnetometer (VSM). Batch adsorption studies were carried out to optimize adsorption condition. Effective conditions for adsorption of Cr (VI) were found at the weight of CuFe2O4 was 1.0 g with contact time of 60 minutes and pH 3 with adsorption capacity 9.20 mg g-1.


2011 ◽  
Vol 80-81 ◽  
pp. 405-408
Author(s):  
Li Li Zhang ◽  
Hong Wei Zhang ◽  
Xiang Hua Yao ◽  
Can Bang Zhang ◽  
Jia Jin Tian ◽  
...  

A new type of magnetic polymer microspheres with super paramagnetic properties were prepared by a co-precipitation method. Atomic absorption spectroscopy (AAS), X-ray diffraction (XRD), transmission electron microscope (TEM) and scanning electron microscopy (SEM) were used to analyze Fe content, micro morphology, particle size and phase structure of the products. Results indicate that the content of Fe in the microspheres is up to 5.25 *105ug/g. The main phase of the product is Fe3O4. The average particle sizes of the products are ~30nm.


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.


2012 ◽  
Vol 1372 ◽  
Author(s):  
G. Martínez-Lozano ◽  
T. Kryshtab ◽  
M. Hesiquio Garduño ◽  
A. Kryvko

ABSTRACTNi/Mg/Al mixed oxides were obtained from hydrotalcite-like precursors by thermal decomposition at 400º, 600º and 800ºC using co-precipitation method at pH 7. The mixed oxides were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), and Energy-dispersive X-ray spectroscopy (EDS) techniques. XRD analysis revealed the formation of NixMg1-xO (x = 0 - 1), α-Al2O3 and traces of MgAl2O4 (NiAl2O4) phases. The diffraction peak positions for MgO or NiO oxides were shifted towards 2θ values higher than simulated for pure bulk oxides that can be attributed to the possible presence of lattice vacancies or surface compressive stress. The evaluated grain size by XRD technique was about 8 -10 nm. It was also detected the presence of microstrains that can be associated with the presence of extended defects in the grains. SEM observations showed that the particles of oxides are formed as agglomerates with the particle sizes of 50 nm up to 200 nm. EDS detected the presence of Mg2+, Ni2+, and Al3+ cations and oxygen in all particles independently on their size. The obtained results revealed the presence of mixture of Ni/Mg/Al oxides in each particle obtained. The oxides calcined at temperatures of 400º and 600ºC were unstable and under air storage they revert to the precursor. The incorporation of Ni2+ in Mg-Al mixed oxides leads to stability of the compounds calcined at 800ºC.


Author(s):  
Ali A. Ati ◽  
Zulkafli Othaman ◽  
Shadab Dabagh ◽  
R. M. Rosnan ◽  
Samad Zare

Nano crystalline powders of Co-Ni ferrite compounds having the chemical formula Co(x)Ni(1-x) Fe2O4( x = 0.0, 0.2 and 1.0) have been successfully synthesized by co-precipitation technique. These synthesized compounds are characterized by X-ray diffraction (XRD), field emission scan electron microscopy (FESEM), fourier transformed infrared (FTIR) spectrum, energy dispersive X-ray diffraction (EDX) and TGA-DTA. The XRD analyses of the samples sintered at 600 °C clearly show the formation of single cubic spinel structure. XRD patterns are further analyzed to calculate the lattice constant and jump length of charge carriers. Average crystalline sizes for ferrite powders are determined from XRD line using Debye-Scherrer's formula is found to be in the range of 16 to 19 nm with narrow size distribution. The Fourier transformed infrared (FTIR) spectrum characterization of the  spinel ferrite structure sintered at 600 °C shows two fundamental strong band in the range 385-600 cm-1, which is attributed to different main metal-oxygen bands.


2015 ◽  
Vol 7 (2) ◽  
pp. 1393-1403
Author(s):  
Dr R.P VIJAYALAKSHMI ◽  
N. Manjula ◽  
S. Ramu ◽  
Amaranatha Reddy

Single crystalline nano-sized multiferroic BiFeO3 (BFO) powders were synthesized through simple chemical co-precipitation method using polyethylene glycol (PEG) as capping agent. We obtained pure phase BiFeO3 powder by controlling pHand calcination temperature. From X-ray diffraction studies the nanoparticles were unambiguously identified to have a rhombohedrally distorted perovskite structure belonging to the space group of R3c. No secondary phases were detected. It indicates single phase structure. EDX spectra indicated the appearance of three elements Bi, Fe, O in 1:1:3. From the UV-Vis diffuse reflectance spectrum, the absorption cut-off wavelength of the BFO sample is around 558nm corresponding to the energy band gap of 2.2 eV. The size (60-70 nm) and morphology of the nanoparticles have been analyzed using transmission electron microscopy (TEM).   Linear M−H behaviour and slight hysteresis at lower magnetic field is observed for BiFeO3 nanoparticles from Vibrating sample magnetometer studies. It indicates weak ferromagnetic behaviour at room temperature. From dielectric studies, the conductivity value is calculated from the relation s = L/RbA Sm-1 and it is around 7.2 x 10-9 S/m.


2011 ◽  
Vol 311-313 ◽  
pp. 1713-1716 ◽  
Author(s):  
Yan Rong Sun ◽  
Tao Fan ◽  
Chang An Wang ◽  
Li Guo Ma ◽  
Feng Liu

Nano-hydroxyapatite with different morphology was synthesized by the co-precipitation method coupled with biomineralization using Ca(NO3)2•4H2O and (NH4)2HPO4 as reagents, adding chondroitin sulfate, agarose and aspartic acid as template. The structure and morphology of the prepared powders were characterized by X-ray diffraction (XRD) and transmission electron microscope (TEM).


2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Beata Zielińska ◽  
Ewa Mijowska ◽  
Ryszard J. Kalenczuk

K-Ta mixed oxides photocatalysts have been prepared by impregnation followed by calcination. The influence of the reaction temperature (450°C–900°C) on the phase formation, crystal morphology, and photocatalytic activity in hydrogen generation of the produced materials was investigated. The detailed analysis has revealed that all products exhibit high crystallinity and irregular structure. Moreover, two different crystal structures of potassium tantalates such as KTaO3and K2Ta4O11were obtained. It was also found that the sample composed of KTaO3and traces of unreacted Ta2O5(annealed at 600°C) exhibits the highest activity in the reaction of photocatalytic hydrogen generation. The crystallographic phases, optical and vibronic properties were examined by X-ray diffraction (XRD) and diffuse reflectance (DR) UV-vis and resonance Raman spectroscopic methods, respectively. Morphology and chemical composition of the produced samples were studied using a high-resolution transmission electron microscope (HR-TEM) and an energy dispersive X-ray spectrometer (EDX) as its mode.


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