微孔-介孔复合SiO2-Al2O3分子筛的水热合成研究

中国科学院山西煤炭化学研究所

Preparation, structure and luminescence of BaMAl10O17 : Eu2+ (M = Be, Mg, Ca, Zn, Cd, Mn, Co, Li) system

The BaMA(10)O(17) (M = Be, Mg, Ca, Zn, Cd, Mn, Co, Li) system has been synthesized by solid state method and characterized by XRD. The results show that when M is Mg, Zn, Mn, Co, Li, there exists the structure of beta-Al2O3 for BaMAl10O17 system, and when M indicates Cd, beta-Al2O3 structure is formed accompanying alpha-Al2O3 phase, and when M represents Be and Ca, beta-Al2O3 structure cannot be formed. This demonstrates that the condition forming beta-Al2O3 structure compounds for the system BaMAl10O17 is 0.05nm < R-M < 0.09nm (R-M represents the radius of M). The thought that if a M ion can form a stable spinel structure there exsits a corresponding magnetoplumbite and beta-alumina structure is proposed for BaMAl10O17 system according to the experimental results. When M is Li, Be, Zn, Eu2+ activator produces an emission of nearly 450 nm with half height width about 50 nm, when M is Mn, there are simultaneously the emissions of Eu2+ and Mn2+ and the excitation energy of Eu2+ can transfer to Mn2+ in the host, when M is Cd, Eu2+ displays a double-emission band, which can be explained by the Jahn-Teller's effect. It is possible for the system BaMAl10O17 with M being Li, Be, Zn to become blue-emitting component in three colour lamp through further study.

Progress in luminescent films prepared by sol-gel process

In this paper, state of the art for luminescent films prepared by sol-gel process has been reviewed. The basic process and characteristics for the synthesis of luminescent films via sol-gel method, Characterization methods for the films and the current status for the development and application of luminescent films are discussed in the context, An elucidation has been made on the luminescent films classified by composition, including inorganic luminescent films and organic/inorganic hybrid luminescent films. The sol-gel derived luminescent films have found applications in the display devices for photoluminescence, electroluminescence, cathodoluminescence and field emission etc. Finally, the future development tendency for the luminescent films are forecasted.

Luminescence of Eu2+ in sodium polyaluminates

The sodium polyaluminates were synthesized by a high temperature solid state method and the luminescence of Eu2+ in the sodium polyaluminates was studied. The results show that the structure of the system Na1+xMgxAl11-xO17 from x=0.1 to x=1.0 belongs to Na-beta-alumina and the structure of the system Na1.67-2xBaxMg0.67Al10.33O17 changes at about x equal to 0.30, when x is smaller than 0.30 the system forms the solid solution structure of Na-beta-alumina, when x is larger than 0.30 the system becomes the ordered structure of Ba-beta-alumina, correspondingly the emission peak position and the relative emission intensity of Eu2+ change with the changes of composition and structure of the system. There exist two kinds of the luminescent centers of high and low energies of Eu2+ in the matrix of Na-beta-alumina structure. New phosphor with Ba-beta-alumina structure, Na0.67Ba0.50Mg0.67Al10.33O17:Eu2+, was obtained.

Atomic force microscopy imaging of molybdenum oxide film electrodeposited on a carbon electrode

Non-stoichiometric mixed-valent molybdenum(VI, V) oxide film was grown on carbon substrates by the electrodeposition method. Responses of the prepared molybdenum oxide thin films to potential and to different solution acidities were studied by cyclic voltammetry, and the corresponding morphological changes of the film were monitored by atomic force microscopy (AFM). AFM images of the molybdenum oxide film show that the characteristic domed structure on the film surface increased during the transition from the oxidized state to the reduced state without signification change in the KMS surface roughness value. Furthermore, AFM studies show that the solution acidity has great effect on the morphology of the films, and the films undergo a homogenizing process with increasing pH of the solutions. (C) 1999 Elsevier Science S.A. All rights reserved.

The luminescence of Eu2+ in mixed phase system

The dependence of the structure of the hosts on the M ion radius in MMgAl10O17 (M = Be, Mg, Ca, Sr, Ba, Pb, Eu, Mn, Fe, Co, Ni, Zn, Cd, Sn) system was studied and the luminescence of Eu2+ the mixed phase system was discussed. When M ion radius is less than 0.10 nm, the system MMgAl10O17 constructs by the mixed phases consisting of manegtoplumbite and spinel, alpha-alumina or spinel and alpha-alumina. In the mixed phase of manegtoplumbite and spinel and alpha-alumina, Eu2+ ion preferentially occupies lattice site of the cations in manegtoplumbite well matched with the radius and charge of Eu2+. There exists only d-->f transition emission of Eu2+ and no characteristic emission of Eu3+ occurs in those hosts. In the mixed phase of spinel and alpha-alumina, Eu2+ can enter the lattice site of Mg2+ ion or Al3+ ion and the d-->f and f-->f transition of Eu2+ can been observed respectively. Meanwhile, since the radius and charge of matrix lattice ions substituted by Eu2+ do not match with those of Eu2+, the valence state of Eu2+ is unstable. Eu2+ is partly changed into Eu3+ and the emission of Eu3+ is obviously observed even under the condition of reduction atmosphere. If reaction temperature is more than 1 150 degrees C, Al2O3 forms alpha-Al2O3 structure, the f-->f transition of Eu2+ appears. If reaction temperature is less than 1 150 degrees C, a mixed phase of alpha-Al2O3 and gamma-Al2O3 is formed, the f-->f transition of Eu2+ disappears and a new band emission from d-->f transition of Eu2+ occurs.

ENHANCED AMPEROMETRIC DETECTOR FOR LOCAL-ANESTHETICS IN LIQUID-CHROMATOGRAPHY WITH METAL-OXIDE DISPERSED GLASSY-CARBON ELECTRODES

Chemically modified electrodes (CMEs) prepared by the dispersion of metal oxide particles on a glassy carbon (GC) substrate greatly enhance the voltammetric response and amperometric detection of local anesthetics following liquid chromatography (LC). The enhancement is more pronounced with the GC electrodes dispersed by the metal oxides of higher oxidation states (+3, +4) and for the species exhibiting relatively slow electrode kinetics under given conditions. With an applied potential of 1.2 V (vs. SCE), LC amperometric detection of the analytes at the alpha-alumina modified GC surface gives detection limits 2-5 times lower than those obtained at the bare electrode. The metal oxide-dispersed electrodes display significant improvement in sensitivity, and selectivity and indicate excellent preparation reproducibility and performance stability.

ROLE OF H2S IN THE REDUCTION OF MOO3/AL2O3

MoO3/Al2O3 is reduced at least partly by sulfur which is formed from H2S in sulfidation with H2S/N2 mixture. SO2 formation during TPD of MoO3/Al2O3 with presorbed H2S provides evidence for the explanation.

Enhancement of molar heat capacity of nanostructured Al2O3

The nanosized alumina prepared by the hydrolysis method with an average particle size of 20 nm was characterized by X-ray diffraction. The heat capacity measurements of the prepared sample were carried out using an adiabatic calorimeter in the temperature range from 78 to 370 K. Enhancement of heat capacity was observed in the nanostructured materials as the heat capacity data were compared with those of the corresponding coarse-grained materials. The enhanced heat capacity was discussed on the basis of experiments. Differential scanning calorimetry and thermogravimetry were used to determine the thermal stability of the nanostructured alumina.

Adsorption and interaction of H2S/SO2 on TiO2

Adsorption and interaction of H2S/SO2 on titania as well as on alumina for comparison has been studied by temperature programmed desorption (TPD), infrared (IR) spectroscopy and temperature programmed electronic conductivity (TPEC) techniques. It was found that the adsorption of both H2S acid SO2 on TiO2 is much greater than on Al2O3. The electronic conductivity of TiO2 measured by TPEC varies significantly as adsorption and desorption takes place on TiO2, showing a strong interaction between TiO2 and adsorbates. At temperature above 200 degrees C, H2S or SO2 adsorbed on TiO2 can be converted into S, H2O and SO2 or SO3. While on the hydrogen treated TiO2, H2S is decomposed into S and H-2, SO2 into S. The active sites on TiO2 surface cannot be so strongly adsorbed by SO2 that it is much more resistant to the sulfation reaction. Unlike TiO2, Al2O3 only provides surface adsorption sites, which can be readily sulfated. The data obtained support one's understanding why TiO2 exhibits a better catalytic performance than that of Al2O3 as a Claus reaction catalyst. (C) 1999 Elsevier Science B.V. All rights reserved.

Templateless synthesis of catalysts with narrow mesoporous distribution

In this study, amorphous silica-alumina nanomaterials with narrow mesoporous distribution can be obtained by two novel sol-gel processes, without the use of any templates. The results of our experiments show that the preparation method has a great influence on the precursor sol structure as well as the specific surface area and mesopore volume of the final product, but has no effect on the pore size distribution.

Genômica e proteômica de Anaplasma marginale: contribuições para o controle da riquétsia.

A anaplasmose bovina é causada pela riquétsia intra-eritrocítica Anaplasma marginale, responsável por importantes prejuízos econômicos, por causa da alta morbidade e mortalidade em rebanhos bovinos suscetíveis. A vacinação tem sido uma forma econômica e eficiente de controlar a enfermidade. No entanto, os métodos de imunização tradicionais apresentam efeitos adversos em algumas categorias de animais. Nas últimas décadas, os estudos sobre imunização contra Anaplasma concentraram-se nas proteínas de superfície MSP1a, 1b, 2, 3, 4 e 5. No entanto, até o momento, os resultados foram pouco promissores, apontando a necessidade de ampliar o conhecimento sobre o rol das proteínas de membrana da riquétsia e das relações estruturais entre elas. Nesse contexto, os estudos do genoma e do proteoma da riquétsia têm contribuído com essa finalidade. Pela análise genômica, 14 genes para novas proteínas de membrana externa foram identificados (omp 1-14), dentre os quais, omp2, 3 e 6 não são transcritos. Esses genes ostraram-se altamente conservados entre isolados da riquétsia. As proteínas OMP4, 7, 10 e 14 foram reconhecidas por soros de bovinos imunizados com membrana de A. marginale, mostrando potencial para desenvolvimento de imunógenos. Além disso, mediante análise proteômica, foi possível detectar novas proteínas de membrana, negligenciadas pela anotação genômica. Dentre elas estão AM097 - conjugal transfer protein, AM956 - PepA citosol amino peptidase, AM254 - fator de elongação Tu e quatro proteínas de função desconhecida: AM127, 197, 387 e 854, as quais também foram reconhecidas por soros de bovinos imunizados com membrana de A. marginale.

Imunização de bovinos com MSP1a e MSP2 recombinantes de Anaplasma marginale com CpG ODN 2006 como adjuvante, e desafio com isolado heterólogo.

A anaplasmose é uma importante enfermidade de bovinos de áreas tropicais e subtropicais do mundo, causada pela riquétsia intra-eritrocítica Anaplasma marginale. A vacinação tem sido a forma mais econômica e eficiente de controlar a anaplasmose bovina. Nos últimos anos, esses estudos têm se concentrado nas proteínas de membrana da riquétsia, sobretudo MSP1a e MSP2. Este trabalho teve como objetivos avaliar o grau de proteção induzido pelas proteínas de membrana MSP1a e MSP2 recombinantes de A. marginale, associadas com adjuvante CpG ODN 2006, perante desafio heterólogo e avaliar a resposta imune gerada. Novilhos da raça Aberdeen Angus foram imunizados três vezes com 200 ?g de MSP1a e/ou MSP2 recombinantes, associadas com CpG ODN 2006 e alúmen. Posteriormente, foram desafiados com 3 x 107 eritrócitos infectados com isolado heterólogo de A. marginale. Os animais experimentais apresentaram quadro clínico de anaplasmose (redução do volume globular, febre e riquetsemias detectáveis por distensões sangüíneas coradas). Não foram detectadas diferenças significativas entre os grupos imunizados e os controles quanto ao percentual de redução do volume globular, riquetsemias máximas e temperaturas retais máximas, indicando que as imunizações não foram protetoras. A despeito da significativa produção de IgG total contra MSP1a e MSP2, detectada no dia do desafio, os animais imunizados apresentaram produção significativa de IgG2 apenas contra MSP1a. As razões para as possíveis falhas de proteção são discutidas. Neste trabalho, é relatada a imunização de bovinos com MSP1a e MSP2 recombinantes de A. marginale, associadas com alúmen e CpG ODN 2006, e posterior desafio com isolado heterólogo, bem como a avaliação da resposta imune gerada.

The effect of chromium on sulfur resistance of Pd/HY-Al2O3 catalysts for aromatic hydrogenation

Sulfur is a major poison to noble metal catalysts for deep aromatic hydrogenation in the petroleum refining industry. In order to study the sulfur resistance of Pd-based catalysts, a series of Pd, Cr, and PdCr catalysts supported on HY-Al2O3 were studied by NH3-TPD, pyridine-adsorption IR, TPR, IR spectra of adsorbed CO, and toluene hydrogenation in the presence of 3000 ppm sulfur as thiophene under the following conditions: 533-573 K, 4.2 MPa, and WHSV 4.0 h(-1). Cr has no influence on the acidity of the catalysts. TPR patterns and in situ IR spectra of adsorbed CO revealed a strong interaction between Cr and Pd, and the frequency shift of linear bonded CO on Pd indicates that the electron density of Pd decreases with the increase of the Cr/Pd atomic ratio. The catalytic performance of Pd, Cr, and PdCr catalysts shows that the sulfur resistance of Pd is strongly enhanced by Cr, and the activity reaches its maximum when the Cr/Pd atomic ratio equals 8. The active phase model "Pd particles decorated by Cr2O3" is postulated to explain the behavior of PdCr catalysts. (C) 2001 Academic Press.