Synthesis and Structural Characterization of Mo-Ni-W Oxide Nanostructures

2008 ◽  
Vol 8 (6) ◽  
pp. 2983-2989 ◽  
Author(s):  
F. Paraguay-Delgado ◽  
R. Huirache-Acuña ◽  
M. Jose-Yacaman ◽  
G. Alonso-Nuñez

In this work, we report the synthesis and characterization of Mo-Ni-W oxides. The precursor was prepared from an aqueous solution of ammonium heptamolibdate, ammonium metatungstate, and nickel nitrate with an atomic ratio of 1:1:1 (Mo:W:Ni). The solution was then transferred to a Teflon-lined stainless steel autoclave and heated to 200 °C and left at this temperature for 48 h. The resulting material was then washed and dried. The morphology and elemental composition were studied by scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction. The porosity was studied by the Brunauer, Emmett, and Teller method. The materials synthesized at 200 °C remained amorphous and had a specific surface area of 114 m2/g with pore size of 34 Å. The average length was 1 μm and the average diameter was 60 nm. The crystalline phase of synthesized material corresponded to W0.4Mo0.6O3 and WO3. After annealing at 550 °C for two hours, the material was polycrystalline with a segregated structure of MoO3, WO3; NiMoO4 was observed. The sublimation of the molybdenum oxide was evident when annealed at 900 °C for two hours and finally two crystalline phases of material remained; roundish WO3 and elongated particles of NiWO4.

2011 ◽  
Vol 110-116 ◽  
pp. 1411-1416
Author(s):  
Elham Motyeian ◽  
Hamid Reza Aghabozorg ◽  
Hossein Aghabozorg

A series of crystalline Ce1-xZrxO2 nanoparticles (where x = 0, 0.25, 0.5, 0.75 and 1.0) have been prepared by (i) hydrothermal (ii) polymer based metal-complex precursor solution reactions. Hydrothermal method was performed with diethanol amine as hydrolysis catalyst. The effect of reaction conditions on the size of particles and their morphology were investigated. In the polymer based method, by calcination of suitable polymer precursor solutions at a temperature range between 300 and 450 °C along with variation in the period of time, the metal oxide powders were subsequently obtained. The prepared powders have been characterized by powder X-ray diffraction (XRD), X-ray Fluorescence (XRF) .These studies reveled that zirconium is a good host for insertion into Cerium oxide in fluorite structure. The as-prepared samples were further characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The average diameter of the nanoparticles were calculated from line broadening of XRD peaks and confirmed by SEM and TEM studies.


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.


2012 ◽  
Vol 186 ◽  
pp. 212-215
Author(s):  
Jacek Krawczyk ◽  
Włodzimierz Bogdanowicz ◽  
Grzegorz Dercz ◽  
Wojciech Gurdziel

Microstructure of terminal area of Al65Cu32.9Co2.1ingots (numbers indicate at.%), obtained via directional solidification was studied. Scanning Electron Microscopy, Transmission Electron Microscopy and X-ray powder diffraction were applied. Point microanalysis by Scanning Electron Microscope was used for examination of chemical compositions of alloy phases. It was found that tetragonal θ phase of Al2Cu stoichiometric formula was the dominate phase (matrix). Additionally the alloy contained orthogonal set of nanofibres of Al7Cu2Co T phase with the average diameter of 50-500 nm and oval areas of hexagonal Al3(Cu,Co)2H-phase, surrounded by monoclinic AlCu η1phase rim. Inside some areas of H-phase cores of decagonal quasicrystalline D phase were observed.


2012 ◽  
Vol 583 ◽  
pp. 86-90 ◽  
Author(s):  
Hai Bin Li ◽  
Xin Yong Li ◽  
Yan De Song ◽  
Shu Guang Chen ◽  
Ying Wang ◽  
...  

TiO2nanotubes were prepared via a hydrothermal route. CeO2nanoparticles with diameters around 5nm were loaded onto the surface of TiO2nanotubes via a deposition approach followed by a calcination process. Transmission electron microscopy (TEM), X-ray diffraction (XRD), and UV-vis diffuse reflectance spectroscopy (UV-vis) were applied for the characterization of the as-prepared CeO2/TiO2nanotubes composites. The results show that CeO2particles are highly dispersed on the surface of TiO2nanotubes. The TiO2 nanotubes are modified to response to the visible light due to the combination with CeO2. The CeO2/TiO2nanotubes composites with a CeO2/TiO2atomic ratio of 2.5% show a further improvement on the photocatalytic activity for degradation of Rhodamine B in water. The presence of CeO2improves the light absorption of TiO2nanotubes and inhibits the electron-hole recombination.


2000 ◽  
Vol 15 (10) ◽  
pp. 2076-2079
Author(s):  
Chika Nozaki ◽  
Takashi Yamada ◽  
Kenji Tabata ◽  
Eiji Suzuki

Synthesis of a rutile-type lead-substituted tin oxide with (110) face was investigated. The characterization was performed by x-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive x-ray spectroscopy, infrared spectroscopy, x-ray photoelectron spectroscopy, and Brunauer–Emmett–Teller surface area measurements. The homogeneous rutile-type lead-substituted tin oxide was obtained until 4.1 mol% of tin was substituted with lead. The surface of obtained oxide had a homogeneously lead-substituted (110) face.


1999 ◽  
Vol 14 (5) ◽  
pp. 1782-1790 ◽  
Author(s):  
X. L. Dong ◽  
Z. D. Zhang ◽  
S. R. Jin ◽  
W. M. Sun ◽  
X. G. Zhao ◽  
...  

Ultrafine Fe–Ni(C) particles of various compositions were prepared by arc discharge synthesis in a methane atmosphere. The particles were characterized by x-ray diffraction, transmission electron microscopy, energy disperse spectroscopy, chemical analysis, x-ray photoelectron spectroscopy, Mössbauer spectroscopy, and magnetization measurement. The carbon atoms solubilizing at interstitial sites in γ–(Fe, Ni, C) solution particles have the effects of forming austenite structure and changing microstructures as well as magnetic properties. A carbon layer covers the surface of Fe–Ni(C) particles to form the nanocapsules and protect them from oxidization. The mechanism of forming Fe–Ni(C) nanocapsules in the methane atmosphere was analyzed.


Materials ◽  
2019 ◽  
Vol 12 (3) ◽  
pp. 537
Author(s):  
Jishuo Han ◽  
Guohua Li ◽  
Lin Yuan

Nanostructured hollow MgO microspheres were prepared by the template method. First, D-Anhydrous glucose was polymerized by the hydrothermal method to form a template. Second, a colorless solution was obtained by mixing magnesite with hydrochloric acid in a 1:2 proportion and heating in an 80 °C water bath for 2 h. Finally, the template from the first step was placed in the colorless solution, and the resulting precipitate was calcined at 550 °C for 2 h. The phase composition and microstructure of the calcined samples were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The XRD results indicated that the main crystal is periclase. The SEM results indicates that the template carbon microsphere surface is smooth, and the its size is uniform and concentrated in the range of 100–200 nm. The diameters of the samples range from 60 to 90 nm, which is smaller than the size of the carbon microsphere. The TEM results indicates that the sample is hollow with a shell thickness of about 6–10 nm. The specific surface area of the calcined hollow sphere is 59.5 m²·g−1.


2019 ◽  
Vol 2019 ◽  
pp. 1-17 ◽  
Author(s):  
M. S. Pudovkin ◽  
D. A. Koryakovtseva ◽  
E. V. Lukinova ◽  
S. L. Korableva ◽  
R. Sh. Khusnutdinova ◽  
...  

A set of Pr3+:LaF3 nanoparticles (NPs) were synthesized via coprecipitation method at three stoichiometric proportions of La(NO3)3, Pr(NO3)3, and NaF (1 : 0.8, 1 : 1, and 1 : 6, respectively). Two ways of mixing of the La(NO3)3, Pr(NO3)3, and NaF solutions (dropwise and swift addition) were used. One sample was subjected to microwave (MW) treatment for 30, 90, and 180 min. All the samples were characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). For all the samples, optical spectroscopy experiments were carried out. The XRD data were analyzed via the Debye-Scherrer and Williamson-Hall methods. It was revealed that the way of mixing of the La(NO3)3, Pr(NO3)3, and NaF solutions strongly affects the shape of the NPs. The slow dropwise addition of the NaF solution leads to the plate-like NP (PLNP) formation; otherwise, the swift addition of the NaF solution leads to the formation of more sphere-like NPs (SLNPs). The size and regularity in shape of the NP increase with the increasing stoichiometric proportion of La(NO3)3, Pr(NO3)3, and NaF from 1 : 0.8 to 1 : 6. The size and regularity in shape of the SLNPs increase with the increasing time of MW treatment. The Debye-Scherrer and Williamson-Hall methods confirmed the anisotropic shape of the PLNPs. The Williamson-Hall method showed that the values of strain are almost similar for all the samples (around 14∗10-4). Optical spectroscopy experiments revealed that although all the samples have an equal chemical composition, the luminescence lifetimes for different samples differ between each other. The luminescence lifetime of the PLNPs is less than that of the SLNPs having an equal stoichiometric proportion of La(NO3)3, Pr(NO3)3, and NaF. The luminescence lifetime of the 1 : 1 SLNPs increases with the increasing time of MW treatment.


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