Nickel–tungsten bimetallic sulfide nanostructures of fullerene type

2004 ◽  
Vol 19 (7) ◽  
pp. 2176-2184 ◽  
Author(s):  
A. Olivas ◽  
A. Camacho ◽  
M.J. Yacamán ◽  
S. Fuentes

Bimetallic NiW sulfide nanostructures of the inorganic fullerene-like (IF-like) type were prepared by a chemical method employing ammonium thiotungstate and nickel nitrate as metal-sulfide precursors followed by sulfidation in H2S/H2 at 400 °C. The nanostructures were grown with a Ni excess, at an atomic ratio R = 0.85 (R = Ni/Ni + W). The x-ray diffraction patterns showed poorly crystalline WS2, WO2, NiS, and Ni9S8 phases. High-resolution electron microscopy micrographs revealed the formation of two fullerene-like nanostructures, nickel sulfide nanoparticles and long nanotubes filled with tungsten suboxide, both coated by several WS2 layers. The surface area of 18 m2/g measured by nitrogen adsorption (BET surface-area) revealed that these materials contained micropororosity.

Author(s):  
N. Uyeda ◽  
E. J. Kirkland ◽  
B. M. Siegel

The direct observation of structural change by high resolution electron microscopy will be essential for the better understanding of the damage process and its mechanism. However, this approach still involves some difficulty in quantitative interpretation mostly being due to the quality of obtained images. Electron diffraction, using crystalline specimens, has been the method most frequently applied to obtain a comparison of radiation sensitivity of various materials on the quantitative base. If a series of single crystal patterns are obtained the fading rate of reflections during the damage process give good comparative measures. The electron diffraction patterns also render useful information concerning the structural changes in the crystal. In the present work, the radiation damage of potassium tetracyano-platinate was dealt with on the basis two dimensional observation of fading rates of diffraction spots. KCP is known as an ionic crystal which possesses “one dimensional” electronic properties and it would be of great interest to know if radiation damage proceeds in a strongly asymmetric manner.


2009 ◽  
Vol 24 (2) ◽  
pp. 448-451 ◽  
Author(s):  
Boyan Yuan ◽  
Mei Yang ◽  
Hongmin Zhu

Titanium nitride nanopowders were synthesized through a chemical reduction of titanium tetrachloride by sodium in liquid ammonia. The products of the reaction were the mixture of sodium chloride and titanium nitride nanopowders. The mixture was then separated by ammonia extraction. The nanopowders were heated under vacuum up to 1200 °C and were characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), Brunauer-Emmet-Teller (BET) surface area measurement, and chemical analysis. The results show that the product is nanocrystalline cubic phase TiN with Ti/N atomic ratio performed 1:1, and the surface area is from 20 to 50 m2 ·g−1 depending on the heating temperature. The particle sizes estimated by the TEM analysis correspond well with the results of the surface area measurements. The XRD pattern indicates that the crystal size grows with an increase in heating temperature.


1983 ◽  
Vol 219 (1215) ◽  
pp. 111-117 ◽  

The calcite coccoliths from the alga Emiliania huxleyi (Lohmann) Hay and Mohler have been studied by ultra-high resolution electron microscopy. This paper describes the two different types of structure observed, one in the upper elements, the other in the basal plate, or lower element. The former consisted of small, microdomain structures of 300-500 Å (1 Å = 10 -10 m) in length with no strong orientation. At places along these elements, and particularly in the junction between stem and head pieces, triangular patterns of lattice fringes were observed indicating multiple nucleation sites in the structure. In contrast, the lower element consisted of a very thin single crystalline sheet of calcite which could be resolved into a two dimensional lattice image, shown by a computer program that is capable of simulating electron diffraction patterns and lattice images to be a [421] zone of calcite. A possible mechanism for these growth patterns in the formation of coccoliths is discussed, together with the relevance of such mechanisms to biomineralization generally.


2016 ◽  
Vol 2016 ◽  
pp. 1-12 ◽  
Author(s):  
Václav Štengl ◽  
Jiří Henych ◽  
Michaela Slušná

h-BN-TiO2nanocomposites were synthesized by the thermal hydrolysis of titanium peroxo-complexes in the presence of exfoliated h-BN. The bulk h-BN was prepared by annealing mixture of boric acid and urea, and high intensity ultrasound was used for its exfoliation. The prepared samples were characterized by X-ray powder diffraction (XRD), infrared spectroscopy, Raman spectroscopy, electron spin resonance (ESR), high resolution electron microscopy, BET surface area, and BJH porosity measurement. The UV-Vis diffuse reflectance spectroscopy was employed to estimate band-gap energies. The photoinduced charge on the surface of h-BN-TiO2nanocomposites was visualized using electric force microscopy (EFM). The photocatalytic activity was determined by azo dyes Orange II and Reactive Black 5 photobleaching. The highest rate constantk= 0.0762 min−1and 0.0164 min−1, under UV and visible light irradiation, respectively, showed sample denoted TiP050BN with moderate concentration of h-BN.


2001 ◽  
Vol 16 (1) ◽  
pp. 101-107 ◽  
Author(s):  
Takeo Oku ◽  
Jan-Olov Bovin ◽  
Iwami Higashi ◽  
Takaho Tanaka ◽  
Yoshio Ishizawa

Atomic positions for Y atoms were determined by using high-resolution electron microscopy and electron diffraction. A slow-scan charge-coupled device camera which had high linearity and electron sensitivity was used to record high-resolution images and electron diffraction patterns digitally. Crystallographic image processing was applied for image analysis, which provided more accurate, averaged Y atom positions. In addition, atomic disordering positions in YB56 were detected from the differential images between observed and simulated images based on x-ray data, which were B24 clusters around the Y-holes. The present work indicates that the structure analysis combined with digital high-resolution electron microscopy, electron diffraction, and differential images is useful for the evaluation of atomic positions and disordering in the boron-based crystals.


Author(s):  
Sven Hovmöller ◽  
Linus Hovmöller Zou ◽  
Xiaodong Zou ◽  
Benjamin Grushko

Quasi-crystals shocked the crystallographic world when they were reported in 1984. We now know that they are not a rare exception, and can be found in many alloy systems. One of the richer systems for quasi-crystals and their approximants is Al−Co−Ni. A large series of pseudo-decagonal (PD) approximants have been found. Only two of them, PD4 and PD8, have been solved by X-ray crystallography. We report here the structures of PD1, PD2, PD3 and PD5, solved from the limited information that is provided by electron diffraction patterns, unit cell dimensions and high-resolution electron microscopy images.


2013 ◽  
Vol 834-836 ◽  
pp. 476-480
Author(s):  
Hai Rong Zhang ◽  
Hong Yan Liu ◽  
Yu Jiang ◽  
Xiao Hua Chang ◽  
Kai Yuan ◽  
...  

A series of Mo-ZSM-5 zeolites have been synthesized by in site hydrothermal method and their catalytic performance for methanol conversion to propylene was tested in a fixed bed reaction at WHSV=4 h-1, pressure of 1 atm, and MeOH/H2O (mol) ratio of 1. The effect of Mo and Al content on the structure and acidity of Mo-ZSM-5 zeolites were characterized by nitrogen adsorption and NH3-TPD. The results showed that Mo incorporation gradually decreased the BET surface area and weaken the strong acidity on the surface of the zeolites. At 470 °C, the maximum selectivity of propylene and the P/E (Propylene to Ethane) ratio were achieved 45.04 % and 7.30, which were higher than those over Mo free HZSM-5 by 4.12% and 3.47, respectively. Mo-ZSM-5 zeolites are promising catalysts for methanol conversion to propylene with a high P/E.


2017 ◽  
Vol 733 ◽  
pp. 36-41
Author(s):  
Edidiong Okon ◽  
Habiba Shehu ◽  
Edward Gobina

In this study, esterification of lactic acid and ethanol to produce ethyl lactate using different cation-exchange resin catalysts was performed at 100 °C. The catalysts used for the esterification process were amberlyst 16 and dowex 50W8x cation-exchange resins. Two simplified mechanisms based on Langmuir-Hinshelwood model were employed to describe the components that adsorbed most on the surface of the catalysts. Fourier Transform Infrared (Nicolet iS10 FTIR) was employed to verify the rationality of the mechanisms. FTIR of the esterification product reflected C=O, H=O and C=C bonds on the spectra confirming water and ethanol as the most adsorbed components. The kinetic study of the retention time and the peak areas of the esterification produced with the different catalysts were compared using an autosampler gas chromatography/mass spectrometry (autosampler GC-MS). The chromatogram of the esterification product catalysed by amberlyst 16 showed a faster elution at 1.503 mins with the peak area of 1229816403 m2 in contrast to the dowex 50W8x. The BET surface area and BJH pore size distribution of the resin catalysts were determined using liquid nitrogen adsorption (Quantachrome, 2013) at 77 K. The BET surface area results of amberlyst 16 resin catalysts was found to be 1.659m2/g compared to 0.1m2/g for the dowex 50W8x. The BJH results of the catalysts exhibited a type IV isotherm with hysteresis confirming that the materials were mesoporous with pore size in the region of 2 – 50 nm.


1987 ◽  
Vol 4 (1-2) ◽  
pp. 87-104 ◽  
Author(s):  
Bruce D Adkins ◽  
Jill B. Heink ◽  
Burtron H. Davis

Scanning electron microscopic data, X-ray diffraction patterns and porosity measurements are consistent with a structure for an Mo-A12O3 catalyst series containing a single surface layer of Mo up to the point where the Mo loadings exceed the amount required for a monolayer. For greater Mo loadings than required for a monolayer, three dimensional orthorhombic MoO3 is also present. The cumulative pore volume, on an alumina basis, does not appear to be significantly altered by MoO3 loadings up to about 15 wt.%. The BET surface area, on an alumina basis, remains constant with Mo loading. However, the apparent surface area calculated from mercury penetration data decreases with Mo loading. For these materials with cylindrical pores, the Broekhoff-deBoer model for the calculation of pore size distributions produced closer agreement to the mercury penetration pore size distribution. This is in contrast to materials composed of nonporous spheres where the Broekhoff-deBoer model provided poorer agreement to mercury penetration results than either the Cohan or a packed sphere model. The results show that, within a factor of two the pore size distributions calculated from nitrogen adsorption and mercury penetration data are comparable.


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