C-410树脂分离富集-电感耦合等离子体质谱法测定地质样品中的金、铂、钯

研究了地质样品中超痕量Au、Pt和Pd的测定方法。采用C 4 1 0阴离子交换树脂在 1 .5mol LHCl条件下对Au、Pt、Pd的吸附率分别为 91 .2 %、1 0 0 .0 %、95 .7%。共存离子除Ge4+ 、Cr6 + 、Ti4+ 外 ,无显著性干扰。用ICP MS测定Au、Pt、Pd的检出限分别为 0 .2 7、0 .4 0和 0 .1 9μg L。当n =8时 ,Au的RSD为 1 9.2 % ;Pt的RSD为 2 8.1 % ;Pd的RSD为 1 5 .6%。

主链含六元氮杂环聚酰亚胺的合成及性能

聚酰亚胺是一类综合性能优异的耐热高分子材料，不仅具有很高的热性能，机械性能，和化学稳定性，还具有较低的介电常数和热膨胀系数，使它在航空，航天工业，微电子工业等诸多领域获得了广泛的应用。研究发现芳杂环的引入能为聚酰亚胺带来一定特殊的性能，因而由芳杂环单体合成的聚酰亚胺一直备受关注。近年来由含氮杂环的单体合成的聚酰亚胺及其性能不断被报道，这些聚合物具有很优异的性能。研究表明这些优异的性能与酰亚胺环的对称性，芳香性和杂原子带来的极性有关。吡啶、嘧啶等芳杂环是刚性的芳杂环分子，具有很好的耐热性能及化学稳定性能，而且杂环中的N 原子又可与金属离子配位和质子化。因而，含吡啶(或嘧啶)环聚合物在具有很好的热稳定性及化学稳定性同时，还会具有较好的可加工性。本论文以硝基取代的vinamidinium salts，amidine salts和易烯醇化的羰基化合物为原料，通过在碱性条件下的环化反应得到得含吡啶环(或嘧啶环)的硝基化合物；硝基化合物用Pd/C和水合肼还原得到棒状含氮芳杂环二胺：2,5-二(4-氨基苯基)嘧啶，2-氨基-5-(4-氨基苯基)嘧啶，2-(4-氨基苯基)-5-氨基嘧啶，2,5-二(4-氨基苯基)吡啶，和2-(4-氨基苯基)-5-氨基吡啶。通过1H-NMR、13C-NMR、IR、MS及元素分析确证了含氮芳杂环二胺及其中间产物的结构。这种二胺或加一定量对苯二胺与均苯二酐(PMDA)或联苯二酐(BPDA)通过两步法聚合获得一系列聚酰亚胺，通过红外、动态力学、静态力学、热重分析、广角X-Ray衍射等实验测试了该类聚合物的结构、热性能、机械性能及结晶性能。研究表明，所得聚酰亚胺的分子链有很高的规整性，表现出很好的化学稳定性，优异的热性能和机械性能。当PPD的含量为50%时，由相同二酐单体所得的聚合物具有最好的综合性能，其中杂环中氮原子的极性对维持聚合物的热稳定性和聚合物在高温条件下的机械性能性起着很重要的作用。并将PPD的含量为50%的聚酰胺酸胶液通过干-湿纺，热亚胺化，和高温牵伸获得聚酰亚胺纤维，并研究了亚胺化条件和牵伸条件对聚酰亚胺纤维性能的影响。

芳香型螺双内酯衍生物的合成和性能研究

芳香型螺双内酯是一类含双内酯环和螺碳原子这一特定结构的化合物，它是一类具有面不对称性手性化合物。由于这类化合物具有强的刚性使得它们的熔点非常高，而且含有这类结构的聚合物也同样具有良好的热稳定性。另外，螺双内酯化合物由于具有与酸酐相类似的性质，它的衍生化既容易又多样化，有可能从它衍生得到含氮、含磷、含硫等的衍生物。本文通过有机合成、手性拆分和聚合反应讨论了芳香性螺双内酯在这几方面的性质。1. 以对硝基甲苯和多聚甲醛为原料，探索了两种途径合成了二硝基芳香型螺双内酯，并发现在酸性体系中氧化反应可高收率地直接得到二硝基螺双内酯。2. 探索了两种途径合成了二氨基芳香型螺双内酯。经过一系列的对照试验，优化了还原反应条件，发现在低极性溶剂和使用5% Pd/C催化剂的还原条件下，生成一种稳定的芳香型二羟胺类化合物；而在强极性溶剂中和使用10% Pd/C催化剂的还原条件下，发生还原开环反应。通过对二氨基螺双内酯及其中间产物的结构解析，给出了可能的还原机理。3. 以芳香型螺双内酯的三种衍生物为原料，通过内酰胺化反应，合成了五种芳香型螺双内酯内酰胺化合物和二硝基芳香型螺双内酰胺。发现芳香型螺双内酯化合物易于在一个环上发生内酰胺化反应，生成稳定的螺双内酯内酰胺化合物，而芳香型螺双内酰胺则需要在很高的温度下得到且产率较低、不易分离。4. 对螺双内酯化合物的化学拆分进行了探索，找到了芳香型螺双内酯四酸的拆分体系。5. 通过常温溶液聚合得到了一系列含有芳香螺双内酯结构的聚酰胺和聚酰亚胺，其结构由红外光谱和元素分析得到了验证。同时发现它们具有很高的热稳定性、抗氧化性和溶解性。

Carbon-supported Pd–Ir catalyst as anodic catalyst in direct formic acid fuel cell

It was reported for the first time that the electrocatalytic activity of the Carbon-supported Pd-Ir (Pd-Ir/C) catalyst with the suitable atomic ratio of Pd and Ir for the oxidation of formic acid in the direct formic acid fuel cell (DFAFC) is better than that of the Carbon-supported Pd (Pd/C) catalyst, although Ir has no electrocatalytic activity for the oxidation of formic acid. The potential of the anodic peak of formic acid at the Pd-Ir/C catalyst electrode with the atomic ratio of Pd and Ir = 5:1 is 50 mV more negative than that and the peak current density is 13% higher than that at the Pd/C catalyst electrode.

Highly Active Carbon-supported PdSn Catalysts for Formic Acid Electrooxidation

PdSn/C catalysts with different atomic ratios of Pd to Sn were synthesised by a NaBH4 reduction method. Electrochemical tests show that the alloy catalysts exhibit significantly higher catalytic activity and stability for formic acid electrooxidation (FAEO) than the Pd/C catalyst prepared with the same method. XRD and TEM indicate that a particle-size effect is not the main cause for the high performance. XPS confirms that Pd is modified by Sn through an electronic effect which can decrease the adsorption strength of poisonous intermediates on Pd and thus promote the FAEO greatly.

基于2,5-二(4-氨基苯)嘧啶聚酰亚胺的合成及性能表征

1,5-二氮杂戊二烯盐(vinamidium salts)与4-硝基苯甲脒盐在碱性物质的存在下发生成环反应得含嘧啶环的硝基化合物;硝基化合物用Pd/C和水合肼还原得到棒状含氮芳杂环二胺——2,5-二(4-氨基苯基)嘧啶.通过1H-NMR,13C-NMR,IR,MS及元素分析确证了含氮芳杂环二胺及其中间产物的结构.这种二胺或加一定量对苯二胺与均苯二酐(PMDA)或联苯二酐(BPDA)通过两步法聚合获得一系列聚酰亚胺,通过红外、动态力学、静态力学、热重分析、广角X射线衍射等实验测试了该类聚合物的结构、热性能、机械性能及结晶性能.

H-酸合成新工艺-硝基T-酸催化加氢制取氨基T-酸

利用催化技术对现有H-酸生产工艺中的硝基T-酸加氢制取氨基T-酸进行改进.通过对贵金属Pd/C催化剂的研究,讨论了非贵金属镍催化剂用于催化加氢制取氨基T-酸的可能性.

High-quality hydrogen from the catalyzed decomposition of formic acid by Pd-Au/C and Pd-Ag/C

Pd-Au/C and Pd-Ag/C were found to have a unique characteristic of evolving high-quality hydrogen dramatically and steadily from the catalyzed decomposition of liquid formic acid at convenient temperature, and further this was improved by the addition of CeO2(H2O)(x).

Preparation and optical properties of silicate glasses containing Pd nanoparticles

We report the space selective precipitation of Pd nanoparticles in Pd2+ -doped silicate glass by ultrashort laser pulses irradiation and further annealing. Absorption spectra, transmission electron microscopy, refractive index measurement and Z-scan technique demonstrated that metallic Pd nanoparticles were precipitated in the glass sample after irradiation by an 800-nm femtosecond laser and subsequent annealing at 600 degrees C. We discuss a refractive index change and nonlinear absorption that combines the precipitation of Pd nanoparticles. Crown Copyright (c) 2005 Published by Elsevier B.V. All rights reserved.

Long-wavelength SiGe/Si MQW resonant-cavity-enhanced photodiodes (RCE-PD)

Si1-xGex/Si optoelectronic devices are promising for the monolithic integration with silicon-based microelectronics. SiGe/Si MQW RCE-PD (Resonant-Cavity-Enhanced photodiodes) with different structures were investigated in this work. Design and fabrication of top- and bottom-incident RCE-PD, such as growth of SiGe MQW (Multiple Quantum Wells) on Si and SOI (Si on insulator) wafers, bonding between SiGe epitaxial wafer and SOR (Surface Optical Reflector) consisting Of SiO2/Si DBR (Distributed Bragg Reflector) films on Si, and performances of RCE-PD, were presented. The responsivity of 44mA/W at 1.314 mum and the FWHM of 6nm were obtained at bias of 10V. The highest external quantum efficiency measured in the investigation is 4.2%.

Luminescence properties of multi-layer InGaN quantum dots grown on C- and R-plane sapphire substrates

In this study, we report comparative luminescence properties of multi-layer InGaN quantum dots grown on C- and R-plane sapphire substrates by metal organic chemical vapor deposition (MOCVD). High-density InGaN quantum dots (QDs) are formed on GaN templates by decreasing the growth temperature and increasing the adatom hopping-barrier through surface passivation. Atomic force microscopy (AFM) has been employed to estimate the size and height of these dots. Photoluminescence (PL) spectra recorded from (1120) InGaN QDs/(1102) sapphire show much stronger emission intensity compared to spectra recorded from (0001) InGaN QDs/(0001) sapphire. Due to the absence of strong spontaneous polarization and piezoelectric field, such (1150) InGaN QDs in the active layers would lead to high efficiency light emitting devices. (c) 2005 Elsevier B.V. All rights reserved.

Polarity dependence of hexagonal GaN films on two opposite c faces of Al2O3 substrate

GaN films were grown in pairs on two opposite c faces of Al2O3 substrate by low-pressure metal-organic vapor phase epitaxy, and studied by scanning electron microscopy and converged beam electron diffraction. It is found that GaN film on the c-Al2O3 whose c face is forward to its crystal seed has [0001] polarity, and the other film on the C-Al2O3 whose c face is backward to its crystal seed has [000 (1) over bar] polarity. (C) 2001 American Institute of Physics.