Beobachtungen von Stapelfehlordnungen bei der Oxydation der zweiten zur ersten Stufe des Graphithydrogensulfats / Observation of stacking disorder during the oxidation of second stage to first stage graphite hydrogensulfate

1984 ◽  
Vol 39 (8) ◽  
pp. 768-777 ◽  
Author(s):  
Ko Young Shin ◽  
Hanns-Peter Boehm

Graphite has been oxidized to graphite hydrogensulfate with (NH4)2S2Og in concentrated H2SO4. The stage 2 compound formed very rapidly, but further oxidation to stage 1 could be followed conveniently. X-ray diffraction of the intermediate phases showed nonintegral (00l)-reflections indicative of partial interstratification disorder. The interlayer spacing of the stage 1 compound increased with continued oxidation. The degree of oxidation as function of oxidation time has been determined from the position of the minima in the reflectance spectra. The density of the compounds and the ratio of acid molecules to anions in the intercalated layers has been estimated using these data and those of buoyancy measurements. There is a minimum in packing density early in the formation of the first stage. The kinetics of intercalation seems to be first order with respect to the free interlayer spaces.

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Mohamed S. Yahia ◽  
Ahmed S. Elzaref ◽  
Magdy B. Awad ◽  
Ahmed M. Tony ◽  
Ahmed S. Elfeky

Abstract Commercial Granulated Active Carbon (GAC) has been modified using 10 Gy dose Gamma irradiation (GAC10 Gy) for increasing its ability of air purification. Both, the raw and treated samples were applied for removing Chlorpyrifos pesticide (CPF) from ambient midair. Physicochemical properties of the two materials were characterized by Fourier Transform Infrared (FT-IR) and Raman spectroscopy. The phase formation and microstructure were monitored using X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), supported with Energy-Dispersive X-ray (EDX). The Surface area measurement was detected using BET particle size prosometry. Obtained outcomes showed that, the maximum adsorption capacity, given by Langmuir equations, was greatly increased from 172.712 to 272.480 mg/g for GAC and GAC10 Gy, respectively, with high selectivity. The overall removal efficiency of GAC10 Gy was notably comparable to that of the original GAC-sorbent. The present study indicated that, gamma irradiation could be a promising technique for treating GAC and turned it more active in eliminating the pesticides pollutants from surrounding air. The data of equilibrium has been analyzed by Langmuir and Freundlich models, that were considerably better suited for the investigated materials than other models. The process kinetics of CPF adsorbed onto both tested carbon versions were found to obey the pseudo first order at all concentrations with an exception at 70 mg/l using GAC, where, the spontaneous exothermic adsorption of Chlorpyrifos is a strong function for the pseudo-first order (PFO) and pseudo second order (PSO) kinetics.


1992 ◽  
Vol 45 (12) ◽  
pp. 1943 ◽  
Author(s):  
SJ Dunne ◽  
RC Burns ◽  
GA Lawrance

Oxidation of Ni2+,aq, by S2O82- to nickel(IV) in the presence of molybdate ion, as in the analogous manganese system, involves the formation of the soluble heteropolymolybdate anion [MMogO32]2- (M = Ni, Mn ). The nickel(IV) product crystallized as (NH4)6 [NiMogO32].6H2O from the reaction mixture in the rhombohedra1 space group R3, a 15.922(1), c 12.406(1) � ; the structure was determined by X-ray diffraction methods, and refined to a residual of 0.025 for 1741 independent 'observed' reflections. The kinetics of the oxidation were examined at 80 C over the pH range 3.0-5.2; a linear dependence on [S2O82-] and a non-linear dependence on l/[H+] were observed. The influence of variation of the Ni/Mo ratio between 1:10 and 1:25 on the observed rate constant was very small at pH 4.5, a result supporting the view that the precursor exists as the known [NiMo6O24H6]4- or a close analogue in solution. The pH dependence of the observed rate constant at a fixed oxidant concentration (0.025 mol dm-3) fits dequately to the expression kobs = kH [H+]/(Ka+[H+]) where kH = 0.0013 dm3 mol-1 s-1 and Ka = 4-0x10-5. The first-order dependence on peroxodisulfate subsequently yields a second-order rate constant of 0.042 dm3 mol-1 s-1. Under analogous conditions, oxidation of manganese(II) occurs eightfold more slowly than oxidation of nickel(II), whereas oxidation of manganese(II) by peroxomonosulfuric acid is 16-fold faster than oxidation by peroxodisulfate under similar conditions.


1998 ◽  
Vol 62 (5) ◽  
pp. 647-656 ◽  
Author(s):  
Helen J. Bray ◽  
Simon A. T. Redfern ◽  
Simon M. Clark

AbstractThe thermal dehydration of naturally occurring Ca-montmorillonite has been studied by in situ X-ray diffraction at temperatures between 60–120°C. The time-temperature-dependence of the position of the basal (001) reflection reveals that interlayer water loss on isothermal dehydration occurs in two stages. After an initial rapid decrease in interlayer spacing (on shock heating to an isothermal soak temperature) the reaction proceeds towards equilibrium more slowly. Furthermore, the width of the (001) reflection changes with time, reflecting transformation-dependent changes in homogeneity perpendicular to (001) with a maximum in peak width at the point where the rate of the reaction appears to change. This suggests that, as the interlayer spacing collapses, a local change is induced in the structure, affecting the means of movement of the water from the interlayer.


2011 ◽  
Vol 197-198 ◽  
pp. 281-284 ◽  
Author(s):  
Yan Hong Zhao ◽  
Li Chun Hou ◽  
Xiang Li ◽  
Xiaodong Yang ◽  
Xiao Jing Wang

Tungsten doped tantalum oxide (W-Ta2O5) particles were synthesized by a low temperature hydrothermal method. The phase structure of W-Ta2O5particles was characterized by X-ray diffraction (XRD). The XRD results indicated that the samples belonged to orthorhombic crystal. The photocatalytic activity of samples was investigated with degradation methylene blue (MB) under ultraviolet light. The degradation efficiency of MB under the catalysis of W-Ta2O5particles attained 91% when the reaction time was 7 h. The kinetics of MB degradation was respect to the first-order in the presence of the photocatalysts.


2010 ◽  
Vol 156-157 ◽  
pp. 1440-1443
Author(s):  
Yan Hong Zhao ◽  
Min Sun ◽  
Shu Wei Wang ◽  
Wen Ming Tong ◽  
Xiao Jing Wang

The Ba doped tantalum oxide (Ba-Ta2O5) particles were synthesized using low temperature hydrothermal method. The phase structure of samples was characterized by X-ray diffraction (XRD). The result showed that Ba-Ta2O5 had still good crystallinity and belonged to rhombic crystal. The catalytic activity of samples was investigated with the degradation methylene blue (MB) under visible light. The degradation efficiency attained 82% when the reaction time was 12 h. The kinetics of MB degradation was respect to the first-order.


Author(s):  
A. R. Landa Canovas ◽  
L.C. Otero Diaz ◽  
T. White ◽  
B.G. Hyde

X-Ray diffraction revealed two intermediate phases in the system MnS+Er2S3,:MnEr2S4= MnS.Er2S3, and MnEr4S7= MnS.2Er2S3. Their structures may be described as NaCl type, chemically twinned at the unit cell level, and isostructural with CaTi2O4, and Y5S7 respectively; i.e. {l13} NaCl twin band widths are (4,4) and (4,3).The present study was to search for structurally-related (twinned B.) structures and or possible disorder, using the more sensitive and appropiate technigue of electron microscopy/diffraction.A sample with nominal composition MnEr2S4 was made by heating Mn3O4 and Er2O3 in a graphite crucible and a 5% H2S in Ar gas flow at 1500°C for 4 hours. A small amount of this material was thenannealed, in an alumina crucible, contained in sealed evacuated silica tube, for 24 days at 1100°C. Both samples were studied by X-ray powder diffraction, and in JEOL 2000 FX and 4000 EX microscopes.


Author(s):  
A. Leineweber ◽  
M. Löffler ◽  
S. Martin

Abstract Cu6Sn5 intermetallic occurs in the form of differently ordered phases η, η′ and η′′. In solder joints, this intermetallic can undergo changes in composition and the state of order without or while interacting with excess Cu and excess Sn in the system, potentially giving rise to detrimental changes in the mechanical properties of the solder. In order to study such processes in fundamental detail and to get more detailed information about the metastable and stable phase equilibria, model alloys consisting of Cu3Sn + Cu6Sn5 as well as Cu6Sn5 + Sn-rich melt were heat treated. Powder x-ray diffraction and scanning electron microscopy supplemented by electron backscatter diffraction were used to investigate the structural and microstructural changes. It was shown that Sn-poor η can increase its Sn content by Cu3Sn precipitation at grain boundaries or by uptake of Sn from the Sn-rich melt. From the kinetics of the former process at 513 K and the grain size of the η phase, we obtained an interdiffusion coefficient in η of (3 ± 1) × 10−16 m2 s−1. Comparison of this value with literature data implies that this value reflects pure volume (inter)diffusion, while Cu6Sn5 growth at low temperature is typically strongly influenced by grain-boundary diffusion. These investigations also confirm that η′′ forming below a composition-dependent transus temperature gradually enriches in Sn content, confirming that Sn-poor η′′ is metastable against decomposition into Cu3Sn and more Sn-rich η or (at lower temperatures) η′. Graphic Abstract


2013 ◽  
Vol 834-836 ◽  
pp. 531-535
Author(s):  
Li Yan Yang ◽  
Yi Hui Guo ◽  
Li Li Yu ◽  
Jing You

A type of cross-linking starch microsphere (CSMs) has been synthesized via reversed phase suspension method. Crosslinked starch microsphere has good adsorption performance to metal ions in water. The adsorption kinetics of Co (II) on the CSMs, selectivity of adsorption CSMs towards Co (II),Cu (II),Pb (II),Cd (II) and adsorption effects of media towards Co (II) were investigated. The CSMs and its adsorption product were comparatively characterized by X-ray diffraction (XRD). The results showed that The adsorption rate is mainly controlled by liquid film diffusion, and the constant of adsorption rate is 0.0686min-1 at 308K. The crystal structure of the CSMs decreased greatly after the incorporation of Co (II). Co (II) has better adsorption selectivity on CSMs. Ions coexist and other substances in the solution have certain impact on adsorption. Those data are helpful for treatment of the wastewater containing heavy ions.


Materials ◽  
2021 ◽  
Vol 14 (11) ◽  
pp. 3103
Author(s):  
Laurent Gremillard ◽  
Agnès Mattlet ◽  
Alexandre Mathevon ◽  
Damien Fabrègue ◽  
Bruno Zberg ◽  
...  

Due to growing demand for metal-free dental restorations, dental ceramics, especially dental zirconia, represent an increasing share of the dental implants market. They may offer mechanical performances of the same range as titanium ones. However, their use is still restricted by a lack of confidence in their durability and, in particular, in their ability to resist hydrothermal ageing. In the present study, the ageing kinetics of commercial zirconia dental implants are characterized by X-ray diffraction after accelerated ageing in an autoclave at different temperatures, enabling their extrapolation to body temperature. Measurements of the fracture loads show no effect of hydrothermal ageing even after ageing treatments simulated a 90-year implantation.


Author(s):  
Ke Guo ◽  
Shaoyan Wang ◽  
Renfeng Song ◽  
Zhiqiang Zhang

AbstractLeaching titaniferous magnetite concentrate with alkali solution of high concentration under high temperature and high pressure was utilized to improve the grade of iron in iron concentrate and the grade of TiO2 in titanium tailings. The titaniferous magnetite concentrate in use contained 12.67% TiO2 and 54.01% Fe. The thermodynamics of the possible reactions and the kinetics of leaching process were analyzed. It was found that decomposing FeTiO3 with NaOH aqueous solution could be carried out spontaneously and the reaction rate was mainly controlled by internal diffusion. The effects of water usage, alkali concentration, reaction time, and temperature on the leaching procedure were inspected, and the products were characterized by X-ray diffraction, scanning electron microscope, and energy dispersive spectroscopy, respectively. After NaOH leaching and magnetic separation, the concentrate, with Fe purity of 65.98% and Fe recovery of 82.46%, and the tailings, with TiO2 purity of 32.09% and TiO2 recovery of 80.79%, were obtained, respectively.


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