Characterization of cordierite-based glass-ceramics produced from fly ash

The cordierite-based glass-ceramics have been developed using fly ash as one of the starting raw materials. On the basis of DTA analysis, nucleation experiments were carried out at 840 °C for 2 h and crystallization experiments were performed at 1020 °C for 2 h. X-ray diffraction analysis revealed that the major phase of the synthesized glass-ceramics was cordierite along with a trace of anorthite and iron cordierite. The properties of the synthesized cordierite-based glass-ceramics compared well with the values of industrial cordierite. Results indicate an interesting potential for fly ash to produce useful materials.     

Thermal analysis of bulk amorphous arsenic triselenide

Through the use of differential scanning calorimetry, the heat capacity and crystallization parameters of amorphous As₂Se₃ have been studied. It is found that the heat capacity above the glass transition temperature (T_g) exceeds, by a factor of 1.6, the Dulong-Petit limiting value found below T_g. The crystallization process is found to obey first-order kinetics with an activation enthalpy of 1.24 eV and an enthalpy of crystallization of 0.36 eV · molecule^?1. The effect of sample age on the rate constant is also reported.     

Influence of cluster defects of variable composition on the optical and radiative characteristics of oxide crystals

It is shown that oxide crystals contain cluster defects of variable composition, which cause absorption of light in the transparency region of crystals. The model based on the presence of cluster defects in oxide crystals explains well the experimental data on the thermal and radiative coloring of these crystals. It is noted that cluster defects accumulate oxygen in oxide crystals. These defects are responsible also for the photochromic effect in them. Application of the noted model made it possible to fabricate lead tungstate scintillators at North Crystals Company for the ALICE project (CERN) with almost 100% reproducibility of their operating characteristics.     

Investigations on the homogeneity of single crystals of materials with variable composition grown by chemical transport reactions

To investigate the problem of homogeneity in crystals grown by chemical transport reactions (CTR) solid solutions Fe_1-yCo_yS, Fe_1-yNi_yS, and Zn_1-yCo_yO were choosen as model substances. Relative concentration profiles of Co and Ni, respectively, were measured by electron-probe microanalysis and light absorption (in Zn_1-yCo_yO only). No significant deviations from homogeneity were found for Fe_1-yMe_yS, whereas in Zn_1-yCo_yO the Co contents increase in the growth direction. A qualitative explanation due to different diffusivities in the solids can be given.     

Methods of chemical and phase composition analysis of gallstones

This review presents the instrumental methods used for chemical and phase composition investigation of gallstones. A great body of data has been collected in the literature on the presence of elements and their concentrations, obtained by fluorescence microscopy, X-ray fluorescence spectroscopy, neutron activation analysis, proton (particle) induced X-ray emission, atomic absorption spectroscopy, high-resolution gamma-ray spectrometry, electron paramagnetic resonance. Structural methods—powder X-ray diffraction, infrared spectroscopy, Raman spectroscopy—provide information about organic and inorganic phases in gallstones. Stone morphology was studied at the macrolevel with optical microscopy. Results obtained by analytical scanning and transmission electron microscopy with X-ray energy dispersive spectrometry are discussed. The chemical composition and structure of gallstones determine the strategy of removing stone from the body and treatment of patients: surgery or dissolution in the body. Therefore one chapter of the review describes the potential of dissolution methods. Early diagnosis and appropriate treatment of the disease depend on the development of clinical methods for in vivo investigation, which gave grounds to present the main characteristics and potential of ultrasonography (ultrasound scanning), magnetic resonance imaging, and X-ray computed tomography.     

Cost-effective synthesis of silica aerogels from fly ash via ambient pressure drying

Silica aerogels were synthesized from the industrial fly ash by ambient pressure drying method. The process consists of two stages, preparation of sodium silicate solution from fly ash by hydrothermal reaction with sodium hydroxide, and synthesis of porous silica aerogels from the obtained sodium silicate solution. Silica wet gels were formed by vitriol-catalysis or resin-exchange-alkali-catalysis of the obtained sodium silicate solution. The trimethylchlorosilane(TMCS)/ethanol(EtOH)/hexane mixed solution was used for solvent exchange/surface modification of the wet gel so as to obtain porous silica aerogels via ambient pressure drying. The results indicated that the synthesized silica aerogels were lightweight and hydrophobic. The BET specific surface area, pore volume and average pore diameter were 362.2-907.9 m² g^− 1, 0.738-4.875 cm³ g^− 1, and 7.69-24.09 nm respectively. Particularly, the synthesized silica aerogels by resin-exchange-alkali-catalysis method showed uniform mesoporous structure, and had much higher specific surface area (907.9 m² g^− 1) and pore volume (4.875 cm³ g^− 1) than that of by vitriol-catalysis process.     

Thermal analysis of non-isothermal crystallization kinetics in glass forming liquids

A brief review is given of previously suggested methods for analysis of experimental data of non-isothermal crystallization kinetics based on the Johnson-Mehl-Avrami transformation rate equation. Conditions for applicability are outlined and an estimate of error is made. A method of non-isothermal analysis is presented which facilitates rapid data evaluation over large temperature ranges and which justifies the previous applications in the literature of Kissinger's method to the analysis of crystallizations kinetics. An extension of these methods is made to the case of growth rates which obey a Vogel-Further temperature relation.     

Thermal analysis, fragility and viscosity of Au-based metallic glasses

Metallic glasses based on Au of composition Au₄₉Cu_26.9Ag_5.5Pd_2.3Si_16.3 and (Au₄₉Cu_26.9Ag_5.5Pd_2.3Si_16.3)₉₉X₁ where X = Ti and In, have been produced and characterized in ribbon form. They show a glass transition and a rather wide undercooled liquid region before crystallisation.The fragility index (m) of the alloys was investigated with two methods involving differential scanning calorimetry (DSC) measurements. In one method the glass transition temperature was determined at different scanning rates in the range 0.3-100 °C/min and its trend fitted to give m. In the other m was obtained from the temperature span of the glass transition range at the scanning rate of 20 °C/min. Implications for viscosity in the undercooled liquid are derived and thoroughly discussed ending with a VFT (Vogel-Fulcher-Tammann) expression for it.     

Microstructure and composition analysis of group III nitrides by X-ray scattering

The importance of Group III-nitride structures for both light-emitting devices and high-power field effect transistors is well known (J.W. Orton, C.T. Foxon, Rep. Prog. Phys. 61 (1998) 1). In both cases, different alloy composition and doping levels or type are utilised and the device performance also depends critically on the interface quality and defect density. We have used high resolution X-ray scattering to measure the state of strain in the individual layers on an absolute scale to derive the alloy composition, i.e. we have avoided the conventional method of using the substrate as an internal reference since it could be strained. The composition and individual layer thickness are derived through simulation of the profile with this additional strain information and the best-fit profile is obtained with an automatic procedure. These structures are laterally inhomogeneous arising from defects breaking up the structure into narrow vertical columns of nearly perfect material and this produces significant broadening of the diffraction pattern. This broadening in the diffraction pattern has been modelled using an extended dynamical scattering model (P.F. Fewster, X-Ray Scattering from Semiconductors, Imperial College Press, World Scientific, Singapore, 2000) to yield the size distribution of perfect crystal regions. The measurement of the rotation about an axis defined by the growth direction of the GaN with respect to the sapphire is determined and is found to be small. However, a poor quality sample indicates that a large range of rotations is possible in these structures.     

Dislocation density in InxGa1–xAs films grown on GaAs substrates with intermediate buffer layer InGaAsP of variable composition

In_xGa_1–xAs films with x = 0.03 and 0.05 were grown from an In Ga As P liquid phase. Because of high value of distribution coefficient of P we have heterojunction GaAs In_yGa_1–yP_zAs_1–x–In_xGa_1–xAs. The influence of Phosphorus atom fraction (X_p) in liquid phase on dislocation density in the top In_xGa_1–xAs layer was studied. It was found that dislocation density (N_d) as a function of X_p is a curve with some minima. The minima of N_d for substrates of (111) A and (111) B orientations are observed in the different intervals of X_p axis. — The width of N_d minimum is decreased if the substrate is misoriented from the (111) plane. — It was supposed that the clusters exist in the liquid phase. On the basis of this assumption one can explain the influence of substrate position over or under the melt on the film perfection. The diameter of these clusters is estimated to be about 500 Å.     

Crystallization properties of zeolite A synthesized from coal fly ash using a fusion/hydrothermal method

Abstract

Zeolitic materials were synthesized from coal fly ash (CFA) using the fusion/hydrothermal method. The effect of NaOH/CFA ratio and particle size on the morphological structure of the zeolitic material crystals prepared was investigated by analyzing crystals morphology and crystallinity. The chemical composition, morphology, and crystallinity of the synthesized materials were characterized by SEM, XRD, and XRF. It was possible to synthesize chamfered-edged cubic crystals at NaOH/CFA ratio of 0.9. The particle size of the zeolite crystals tended to decrease with increasing the alkali content of NaOH/CFA from 0.9 to 1.8. The morphological structure of the crystalline particles was similar to that of zeolite A synthesized from the CFA. This study has shown that the fusion/hydrothermal method is a very effective technique for synthesizing the zeolitic materials from the CFA and provides a potential application for obtaining commercial products.     

用煤系高岭土制备轻质隔热材料的研究

以煤系高岭土、紫木节粘土为主要原料,以木屑和聚苯乙烯球为造孔剂,制备了体积密度为0.74 g/cm3、抗压强度为2.84 MPa,导热系数0.15 W/m.K的莫来石质轻质隔热耐高温材料。优化的工艺条件为:配料中煤系高岭土用量达到了90 wt%,添加木屑和聚苯乙烯球总加入量为12 wt%作为复合造孔剂,最终烧成温度为1300℃。通过XRD、SEM等分析的得到:轻质隔热材料的物相组成为莫来石、刚玉和少量方石英。材料内部的孔结构特征为1~2 mm的相对孤立的较大孔和微米级的小孔。     

The application of differential thermal analysis to the study of isothermal and non-isothermal crystallization kinetics of coal fly ash based glasses

The crystallization kinetics of glasses obtained from coal fly ash was investigated by both isothermal and non-isothermal methods using differential thermal analysis (DTA) data. In DTA experiments, glass samples having coarse (800-1000 μm) and fine (<180 μm) particle sizes were used and the results were compared. The Avrami exponent (n) was calculated by means of Johnson-Mehl-Avrami (JMA) and Ozawa equations. Calculated kinetic parameters indicated that the appropriate crystallization mechanisms were bulk and surface crystallization for coarse and fine particles, respectively. Isothermal and non-isothermal DTA experiments showed that the crystallization activation energies of coarse glasses are changed in the range of 444-578 kJ/mol, while the crystallization activation energies of fine glasses are changed in the range of 610-662 kJ/mol. It was found that crystallization activation energies of fine glasses are higher than those of the coarse glasses. Results showed that isothermal and non-isothermal crystallization kinetics of glasses produced from coal fly ash is in agreement within the experimental error.     

Development of methods of X-ray diffraction analysis for determining the composition and structure of sillenite-family crystals

A methodology for refining the crystal structure of sillenites of nominal composition Bi₂₄ M ₂O₄₀ based on the choice of the correct initial model and thermal atomic parameters is reported. The validity of the approach proposed is demonstrated by examples of crystals with M = Si, Fe, or V, for which the real composition is found with allowance for the composition of each structural site. Individual structural details are confirmed by IR and Raman spectroscopy data.     

The structure and phase composition of sinters obtained from siderite concentrate containing BaSO4

To obtain a full diagnostic characteristic of mineral components of investigated sinters, microscopic methods used to supplement X-ray diffraction studies and X-ray spectral analysis in microvolume. All obtained results provide an adequate basis for phase identification. In silicate phase of the siderite sinters occur the following minerals with Ba admixture: in acid sinters: olivines and pyroxenes. in basic sinters: α′ – Ca₂SiO₄, melilites and 3 CaO · SiO₂. In no sinter occurs β – Ca₂SiO₄.     

Thermal treatment-dependent chemical composition of ternary CdS1−xSex nanocrystals grown in borosilicate glass

Variation of the chemical composition of ternary CdS_1−xSe_x nanocrystals grown in borosilicate glass depending on the thermal treatment is studied by resonant Raman spectroscopy. It is shown that only for the nanocrystals with roughly equal content of substitutive S and Se chalcogen atoms (0.4<x<0.6) the nanocrystal composition is independent of the thermal treatment parameters. In other cases an increase of the thermal treatment temperature (625–700 °C) and duration (2–12 h) results in a considerable increase of the predominant chalcogen content in the nanocrystals.     

Empirical methods for estimating the linear coefficient of expansion of oxide glasses from their composition

Empirical methods for estimating the linear coefficient of expansion (α) of oxide glasses have been derived. New parameters (β_i) are define for the glass modifiers. The β_i are calculated from the ionic radius R, charge Z, and the electronegativity EN of the modifiers. β_i parameters and their normalized values (γ_i) with respect to a standard modifier, classify the modifiers according to their contribution to the thermal expansion. Two semi-emperical relations were derived for the calculation of α. Calculated expansion coefficient for over 500 glass compositions are within ± 15% of the measured values. The application of the methods to ternary, quaternary and multicomponent industrial glasses is treated.     

Effect of composition on the glass-forming tendency of barium aluminosilicate gels derived from metal alkoxides

The effect of composition on the glass-forming tendency of barium aluminosilicate gels derived from metal alkoxides with compositions near the theoretical composition of barium feldspar was studied. Results indicated that, in the experimental range, larger SiO₂ content and larger BaO/Al₂O₃ ratio were advantageous to glass formation. A criterion for glass formation in the studied system was established as (b+3−4y)/(2y+s(1+b)/(100−s))<J_c, where b is the BaO/Al₂O₃ ratio, s the mol percentage of SiO₂, y the fraction of four-coordinated aluminum over the total amount of aluminum, and J_c is a constant for a definite experimental condition. The criterion showed good fitness with the experimental results.