Synthesis and Characterization of Ni/Mg/Al Mixed Oxides Obtained by Co-precipitation

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.

2011 ◽  
Vol 8 (1) ◽  
pp. 113-117
Author(s):  
Presenjit Pauri ◽  
S. K. Ghoshal ◽  
H. S. Tewari

In this work, mixed (Sm1-xYx)2[C2O4]3.nH2O with x= 0.50 and 0.70 were prepared using standardized co precipitation method. All the synthesized oxalates were characterized by x-ray diffraction and differential scanning calorimeter. All the samples are homogeneous in stoichiometry. The XRD analysis of these synthesized samples reveals that a solid solution forms for these two compositions The thermal decomposition of the mixed oxalates is complex although completed a lower temperatures. This is an important result for the preparation of Sm-Y mixed oxides, because all the properties of the mixed oxides are intrinsic and depend only on their composition and thermal treatment schedules.


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.


2012 ◽  
Vol 581-582 ◽  
pp. 525-528
Author(s):  
Jia Feng Zhang ◽  
Bao Zhang ◽  
Xue Yi Guo ◽  
He Zhang Chen ◽  
Jian Long Wang ◽  
...  

The LiFe0.98Mn0.02PO4/C was synthesized by spray-drying and low temperature reduction route using FePO4•2H2O as precursor, which was prepared by a simple co-precipitation method. The LiFe0.98Mn0.02PO4/C sample was characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and electrochemical measurements. The XRD analysis and SEM images show that sample has the good ordered structure and spherical particle. The charge-discharge tests demonstrate that the powder has the better electrochemical properties, with an initial discharge capacity of 162.1 mAh•g−1 and 155.8 mAh•g−1 at current density of 0.1 C and 1C, respectively. The capacity retention reaches 99.4% after 100 cycles at 1C.


2021 ◽  
Vol 3 (1) ◽  
pp. 8-11
Author(s):  
Yelmida Azis ◽  
Cory Dian Alfarisi ◽  
Komalasari Komalasari ◽  
Khairat Khairat ◽  
Yusnimar Sahan

Hydroxyapatite (HAp, Ca10(PO4)6(OH)2) is the most stable form of calcium phosphate and widely used in various medical applications, mainly in orthopedics and dentistry due to its close similarities with the inorganic mineral component of bone and teeth. This study aims to synthesize hydroxyapatite from duck eggshell using the precipitation method. The duck eggshell was calcined, hydrated (slaking) and underwent carbonation to form Precipitated Calcium Carbonate (PCC).  Afterwards, (NH4)2HPO4 was added to produce HAp by varying the molar ratio of Ca/P by 1.67, 1.77 and 1.87 and stirring speed by 200, 250, 300rpm under basic condition (pH 10 – 11). The best results were obtained at a molar ratio of 1.77 with 200rpm stirring speed. Furthermore, the X-ray Diffraction (XRD) analysis showed that its crystals were hexagonal with sizes of 23.062nm, in the absence of other crystalline phases. Therefore, the hydroxyapatite was obtained in the agglomerates form with a specific surface area of ??55.929m2/g.


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.


2013 ◽  
Vol 664 ◽  
pp. 515-520
Author(s):  
Chih Wei Tang ◽  
Jiunn Jer Hwang ◽  
Shie Hsiung Lin ◽  
Chin Chun Chung

The NiO-ZnO binary materials had been prepared by co-precipitation method. The weight percent of nickel of NiO-ZnO materials were 5, 10 and 20; they were pretreated under air at temperature of 300, 500 and 700°C, respectively. The characterization of NiO-ZnO materials were the thermal gravity analysis(TGA), X-ray diffraction(XRD), N2 adsorption-desorption at 77K, scaning electron microscope(SEM) and temperature-programmed reduction(TPR). The results revealed that surface areas of NiO-ZnO materials order from large to small were 20NiZn(OH)x(66 m2·g-1) > 10NiZn(OH)x(34 m2·g-1) > 5NiZn(OH)x(9 m2·g-1) after being calcined at the temperature of 500°C. Further, NiO-ZnO materials had two main reductive peaks at 390-415°C and 560-657°C, respectively. In all NiO-ZnO materials, 20NiZn(OH)x-C500 material had the highest surface area and the best interaction between NiO and ZnO.


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):  
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.


2019 ◽  
Vol 37 (2) ◽  
pp. 190-195 ◽  
Author(s):  
Denis Sokol ◽  
Maksim Ivanov ◽  
Andrei N. Salak ◽  
Robertas Grigalaitis ◽  
Juras Banys ◽  
...  

AbstractMagnesium-aluminum-bismuth layered double hydroxides (Mg3Al1−xBix; LDHs) were prepared using both coprecipitation and sol-gel methods. For the preparation of Mg/Al/Bi LDH by the co-precipitation method, the appropriate amounts of dissolved starting materials (Al(NO3)3 · 9H2O, Mg(NO3)2 · 6H2O and Bi(NO3)3 · 5H2O) were mixed with a solution of NaHCO3:NaOH. In the sol-gel processing, the precursor Mg–Al–Bi–O gels were synthesized using the same starting materials and ethylene glycol as complexing agent. The mixed-metal oxides obtained by subsequent heating of Mg–Al–Bi–O gels at 650 °C were reconstructed to Mg3Al1−xBix LDHs in water at 80 °C. All the synthesized products were characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and dielectric measurements.


2011 ◽  
Vol 391-392 ◽  
pp. 835-838
Author(s):  
Gui Xin Wang ◽  
Chun Jing Liu ◽  
Yu Meng Zhang ◽  
Hui Fen Peng ◽  
Xin Wang

The citric-acid coated Mn-Zn ferrite nanocrystalline was prepared by an improved co-precipitation method. X-ray diffraction (XRD) and TEM measurements indicated that the coated samples were pure spinel Mn-Zn ferrite nanocrystalline and the particles coated after boiling circumfluence were more homogeneous than that before boiling circumfluence. Vibrating sample magnetometer (VSM) indicated that the Ms of the coated samples was higher than that without coating. Specially when the content of citric acid is 4.76wt% after boiling circumfluence, the Ms of the coated sample is 54.15 emu•g-1 which is 28.7% higher than that without coating.


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