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31.
Silicon Nitride Derived from an Organometallic Polymeric Precursor: Preparation and Characterization 总被引:1,自引:0,他引:1
Wayde R. Schmidt Vijay Sukumar William J. Hurley Jr. Roberto Garcia Robert H. Doremus Leonard V. Interrante Gary M. Renlund 《Journal of the American Ceramic Society》1990,73(8):2412-2418
Partially crystalline Si3 N4 , with nanosized crystals and a specific surface area greater than 200 m2 /g, is obtained by pyrolysis of a commercially available vinylic polysilane in a stream of anhydrous NH3 to 1000°C. This polymer does not contain N initially. Crystallization to high-purity α-Si3 N4 proceeds with additional heating above 1400°C under N2 . The changes in crystallinity, powder morphology, infrared spectra, and elemental compositions, for samples annealed from 1000° to 1600°C under N2 , are consistent with an amorphous-to-crystalline transformation. Although macroscopic consolidation and local densification occur at 1400°C, volatilization and accompanying weight loss limit bulk densification. The effect of temperature on specific surface area is examined and related to the sintering process. These results are applicable to pyrolysis, decomposition, and crystallization studies of ceramics synthesized by polymeric precursor routes. 相似文献
32.
With a combined compact difference scheme for the spatial discretization and the Crank–Nicolson scheme for the temporal discretization, respectively, a high-order alternating direction implicit method (ADI) is proposed for solving unsteady two dimensional convection–diffusion equations. The method is sixth-order accurate in space and second-order accurate in time. The resulting matrix at each ADI computation step corresponds to a triple-tridiagonal system which can be effectively solved with a considerable saving in computing time. In practice, Richardson extrapolation is exploited to increase the temporal accuracy. The unconditional stability is proved by means of Fourier analysis for two dimensional convection–diffusion problems with periodic boundary conditions. Numerical experiments are conducted to demonstrate the efficiency of the proposed method. Moreover, the present method preserves the higher order accuracy for convection-dominated problems. 相似文献
33.
A. J. Leonard M. J. Genet J. Lemaitre M. Bulens B. Delmon 《Journal of the American Ceramic Society》1979,62(9-10):529-531
34.
Preparation of Silicon Carbide/Aluminum Nitride Ceramics Using Organometallic Precursors 总被引:1,自引:0,他引:1
Corinna L. Czekaj Michael L. J. Hackney William J. Hurley Jr. Leonard V. Interrante Gary A. Sigel Paul J. Schields Glen A. Slack 《Journal of the American Ceramic Society》1990,73(2):352-357
Solid solutions of 2H -SiC/AlN can be prepared at temperatures less than 1600°C by rapid pyrolysis ("hot drop") of mixtures of [(Me3 Si)0.80 ((CH2 =CH)MeSi)1.0 (MeHSi)0.35 ] n (VPS) or [MeHSiCH2 ] n (MPCS) with [R2 AlNH2 ]3 , where R=Et, i -Bu or simply by slow pyrolysis of the precursor mixture in the case of [Et2 AlNH2 ]3 . In contrast, slow pyrolysis of mixtures of VPS or MPCS with [ i -Bu2 AlNH2 ]3 yields a composite of 2 H -AlN and 3 C -SiC at 1600°C, which transforms into a single 2 H -SiC/AlN solid solution on heating to 2000°C. The influences of the nature of the precursor and processing conditions on the structure, composition, and purity of the SiC/AlN materials are discussed. 相似文献
35.
Leonard Stoloff John Dantzman John Wegener 《Journal of the American Oil Chemists' Society》1972,49(4):264-266
A procedure has been devised for preparing lot samples of mycotoxin-contaminated nut meats so that a representative analytical
sample may be removed. The sample is rapidly reduced to coarse size. A relatively large portion (about 1/10 of total sample)
of subsample is then split out and further comminuted to a fine particle size with the aid of a fat solvent (meat-solvent,
w/v, 3:2). The analytical sample is removed from this mixture. The procedure was tested with shelled almonds and shelled walnuts
using radioactive nuts to simulate the mycotoxin contamination and provide a simple, precise measure of the contaminated nut
meat distribution. The pooled coefficient of variation was 18% for the subsamples and 4.4% for the analytical samples. Considering
the dilution factors used (1.50 and 2.14 contaminated nuts/104 nuts) and the low degree of reliability of the lot sample, the sample preparation methods tested appear to be practical and
reliable. 相似文献
36.
Y. Xu A. Goyal K.J. Leonard E.D. Specht D. Shi M. Paranthaman 《Journal of the American Ceramic Society》2006,89(3):914-920
YBa2 Cu3 O7− δ (YBCO or Y123) films on rolling-assisted biaxially textured substrates (RABiTS) were prepared via a fluorine-free metallorganic deposition (MOD) through spin coating, burnout, and high temperature anneal. The effects of substrate texture and surface energy of the CeO2 cap layer were investigated. Except for the commonly accepted key factors, such as the textures of substrate and buffer layers, we found some other factors, for example, the deposition temperature of the cap layer, are also critical to the epitaxial growth of Y123 phase. With the CeO2 cap layer deposited at relative high temperature of 700°C, a critical current density, J c , over 1 MA/cm2 has been demonstrated for the first time on Ni-RABiTS by a fluorine-free MOD method. Whereas for samples with CeO2 cap layers deposited at a lower temperature of 600°C, even though XRD data showed a better texture on these buffer layers, texture degradations of YBCO grains under the optimized processing conditions were observed and a lower oxygen partial pressure around 40 ppm was necessary for the epitaxial growth of Y123 phase. As a result, J c fell to 0.45 MA/cm2 at 77 K. The observed phenomena points to the change of surface energy and reactivity of the CeO2 cap layer with respect to the CeO2 deposition temperature. In this paper, the YBCO phase diagram was also summarized. 相似文献
37.
Plant fibers are rich in cellulose and they are a cheap, easily renewable source of fibers with the potential for polymer reinforcement. The presence of surface impurities and the large amount of hydroxyl groups make plant fibers less attractive for reinforcement of polymeric materials. Hemp, sisal, jute, and kapok fibers were subjected to alkalization by using sodium hydroxide. The thermal characteristics, crystallinity index, reactivity, and surface morphology of untreated and chemically modified fibers have been studied using differential scanning calorimetry (DSC), X‐ray diffraction (WAXRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM), respectively. Following alkalization the DSC showed a rapid degradation of the cellulose between 0.8 and 8% NaOH, beyond which degradation was found to be marginal. There was a marginal drop in the crystallinity index of hemp fiber while sisal, jute, and kapok fibers showed a slight increase in crystallinity at caustic soda concentration of 0.8–30%. FTIR showed that kapok fiber was found to be the most reactive followed by jute, sisal, and then hemp fiber. SEM showed a relatively smooth surface for all the untreated fibers; however, after alkalization, all the fibers showed uneven surfaces. These results show that alkalization modifies plant fibers promoting the development of fiber–resin adhesion, which then will result in increased interfacial energy and, hence, improvement in the mechanical and thermal stability of the composites. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 2222–2234, 2002 相似文献
38.
Haiqing?Liu S.?Kay?ObendorfEmail author Michael?J.?Leonard Timothy?J.?Young Michael?J.?Incorvia 《Journal of surfactants and detergents》2005,8(4):311-317
The adsorption of aroma chemicals on cotton fabric was studied relative to the surfactant concentration, surfactant type,
water solubility, and fiber morphology. The adsorption increased with increasing surfactant concentration to a maximum near
the critical micelle concentration, then decreased with further increases in surfactant concentration. The adsorption also
was found to be highly dependent on the fiber surface area and pore structure; dramatic differences were observed between
untreated and mercerized cotton fabric and are believed to be due to morphological differences. Cationic and anionic surfactants
increased the aroma chemical adsorption, which varied with surfactant type, with cetyltrimethylammonium chloride (CTAC)>sodium
dodecyl sulfate (SDS)>H2O. Water solubility also influenced adsorption; in most cases, adsorption increased with water solubility. In addition, adsorption
was also influenced by chemical structure and hydrophobic interactions. The adsorption of aroma chemicals on cotton fabric
can be attributed to the aqueous solution being physically held in capillaries and pore structures within the fibular structure
of cotton fiber and also to molecular interactions among the aroma chemical molecules, surfactants, and cotton substrate. 相似文献
39.
Joe Kelly Mark Leonard Chutima Tantigate Ahmad Safari 《Journal of the American Ceramic Society》1997,80(4):957-964
Ceramic lead magnesium niobate–lead titanate ((1-x)PMN-x PT) of different compositions has been prepared by the columbite precursor method. This study discusses compositions ranging from 0.94PMN–0.06PT to 0.60PM–N0.40PT, focusing on two areas of the (1-x)PMNx PT system: compositions that exhibit electrostrictive behavior, and those that show piezoelectric behavior. In electrostrictive compositions where x is in the range of 0.06–0.20, the dielectric constant and electromechanical coupling factor dependencies on the bias field are evaluated. The optimal electromechanical properties are obtained with the composition 0.82PMN–0.18PT, measured at temperature T = Tm (the temperature of maximum dielectric constant) = 80°C and with a dc bias of 5 kV/cm. X–ray diffractometry is used to show that the (1-x)PMN-x PT system has a compositionally wide two–phase region and that 0.655PMN–0.345PT is the morphotropic phase boundary (MPB) composition. Electromechanical property evaluation shows that the optimal piezoelectric properties (piezoelectric charge coefficient ( d33 ) value of 720 pC/N, dielectric constant ( K ) value of 5400, and electromechanical planar and thickness coupling coefficient ( kp and kt , respectively) values of 62% and 46%, respectively) are obtained at the MPB composition. 相似文献
40.
Cationic bulk polymerization of 1,3-dioxolan has been carried out in sealed ampoules using a high vacuum technique. The polymerization is initiated with triethyl oxonium hexafluorophosphate and the equilibrium between monomer and active polymer is attained within a few hours. Specific volumes of pure monomer and polymer in solution of its own monomer have been measured. Equilibrium measurements have been performed in the 40° to 141·4°C temperature range and the ceiling temperature is estimated to be 144° ± 2°C. The effect of short polymer chains on the equilibrium is discussed briefly. Values of ΔGlc, the free energy of polymerization of one mole of pure liquid monomer to one base-mole of amorphous polymer, are computed making allowance for the non-ideal mixing. Respective values of ?17.5 ± 0.8 kJ/mol and ?47.9 ± 2.2JK?1mol?1 are deduced for the corresponding ΔHlc and ΔSlc. ΔGlc is also computed from published data on equilibrium polymerization of 1,3-dioxolan in various solvents and the combined results for both types of polymerization yield ΔHlc = ?16.7 ± 0.5kJ/mol and ΔSlc = ?45.8 ± 1.5JK?1mol?1 for the 20° to 140°C range. 相似文献