Spectroscopic characterization of alkaline earth uranyl carbonates

A series of alkaline uranyl carbonates, M[UO₂(CO₃)₃]·nH₂O (M=Mg₂, Ca₂, Sr₂, Ba₂, Na₂Ca, and CaMg) was synthesized and characterized by inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectrometry (AAS) after nitric acid digestion, X-ray powder diffraction (XRD), and thermal analysis (TGA/DTA). The molecular structure of these compounds was characterized by extended X-ray absorption fine-structure (EXAFS) spectroscopy and X-ray photoelectron spectroscopy (XPS). Crystalline Ba₂[UO₂(CO₃)₃]·6H₂O was obtained for the first time. The EXAFS analysis showed that this compound consists of (UO₂)(CO₃)₃ clusters similar to the other alkaline earth uranyl carbonates. The average U-Ba distance is 3.90±0.02 Å.Fluorescence wavelengths and life times were measured using time-resolved laser-induced fluorescence spectroscopy (TRLFS). The U-O bond distances determined by EXAFS, TRLFS, XPS, and Raman spectroscopy agree within the experimental uncertainties. The spectroscopic signatures observed could be useful for identifying uranyl carbonate species adsorbed on mineral surfaces.     

Behaviors and mechanisms of copper adsorption on hydrolyzed polyacrylonitrile fibers

Polyacrylonitrile fiber (PANF) was hydrolyzed in a solution of sodium hydroxide and the hydrolyzed polyacrylonitrile fiber (HPANF) was used as an adsorbent to remove copper ions from aqueous solution. Scanning electron microscopy (SEM) showed that the hydrolysis process made the surface of HPANF rougher than that of PANF. Fourier transform infrared (FTIR) spectroscopy revealed that the HPANF contained conjugated imine (-Cz=Nz-) sequences. Batch adsorption results indicated that the HPANF was very effective in adsorbing copper, and the adsorption equilibrium could be reached within 10-20 min. Atomic force microscopy (AFM) showed that some aggregates formed on the surface of the HPANF after copper ion adsorption and the average surface roughness (R(a)) value of the HPANF changed from 0.363 to 3.763 nm due to copper adsorption. FTIR analysis indicated that copper adsorption caused a decrease of the light adsorption intensity of the imine (-Cz=Nz-) groups at 1573 and 1406 cm(-1) wavenumbers, and X-ray photoelectron spectroscopy (XPS) showed that the binding energy (BE) of some of the nitrogen atoms in the HPANF increased to a greater value due to copper adsorption. The FTIR and XPS results suggest that the adsorption of copper ions to the HPANF is attributed to the imine groups on the surface of the HPANF.     

XPS characterization of wood chemical composition after heat‐treatment

XPS was used to characterize the chemical changes occurring after drying or applying a heat‐treatment to beech wood samples. Our results indicate that the surface of this air‐exposed material could be strongly affected either by the ambient atmosphere during storage or by the complex atmosphere in the oven during drying or heat‐treatment. However, the O/C ratio measured after removal of a thin slice of a few millimetres of an untreated sample is in reasonable agreement with that calculated from the well‐established chemical composition of beech. Through this methodology (equivalent to scraping for hard materials) it is expected to get a realistic characterization of the wood. The reliability and repeatability of the XPS measurements have been checked and the method applied to the study of the chemical changes of the beech samples subjected to heat‐treatment. Heating at 240 °C induces a significant decrease of the O/C ratio from 0.55 before to 0.44 after the treatment. Heat‐treatment induces also a decrease of the C₂ carbon contribution (carbon atom bound to a single non‐carbonyl oxygen) associated with an increase of the C₁ carbon contribution (carbon atoms bound only to carbon or hydrogen atoms), in agreement with chemical modifications reported previously in the literature. Thanks to the small analysed area of the equipment used in this study, different spots were analysed to demonstrate the presence or absence of a gradient of chemical composition due to thermal degradation or migration of extractives from within the wood structure to its surface. At the scale of our observations, the different wood samples investigated (dried or heat treated) appear to be homogeneous. Copyright © 2006 John Wiley & Sons, Ltd.     

Influence of the aggregation state in solution on the supramolecular organization of adsorbed type I collagen layers

In the last years, adsorbed collagen was shown to form layers with a supramolecular organization depending on the substrate surface properties and on the preparation procedure. If the concentration of collagen and the duration of adsorption are sufficient, fibrillar collagen structures are formed, corresponding to assemblies of a few molecules. This occurs more readily on hydrophobic compared to hydrophilic surfaces. This study aims at understanding the origin of such fibrillar structures and in particular at determining whether they result from the deposition of fibrils formed in solution or from the building of assemblies at the interface. Therefore, type I collagen solutions with an increasing degree of aggregation were prepared, using the “neutral-start” approach, by ageing pH 5.8 solutions at 37 °C for 15 min, 2 or 7 days. The obtained solutions were used to investigate the influence of collagen aggregation in solution on the supramolecular organization of adsorbed collagen layers, which was characterized by X-ray photoelectron spectroscopy and atomic force microscopy. Polystyrene and plasma-oxidized polystyrene were chosen as substrates for the adsorption. The size and the density of collagen fibrils at the interface decreased upon increasing the degree of aggregation of collagen in solution. This is explained by a competitive adsorption process between monomers and aggregates of the solution, turning at the advantage of the monomers. More aggregated solutions, which are thus depleted in free monomers, behave like less concentrated solutions, i.e. lead to a lower adsorbed amount and less fibril formation at the interface. This study shows that the supramolecular fibrils observed in adsorbed collagen layers, especially on hydrophobic substrates, are not formed in the solution, prior to adsorption, but are built at the interface, through the assembly of free segments of adsorbed molecules.     

XPS研究多壁碳纳米管的阳极氧化处理效果

采用阳极氧化法对多壁碳纳米管（MWNTs）进行表面处理以提高其表面极性官能团含量。研究了不同电解参数对MWNTs处理结果的影响，采用X射线光电子能谱对处理前后的MWNTs的表面特征进行了分析。结果表明，经阳极氧化处理后，MWNTs表面氧原子摩尔分数与极性官能团总量均有不同程度增加。通电量和碱性电解质的电导率（物质的量浓度）是阳极氧化处理过程的主要影响因素，MWNTs表面极性官能团总量的增加可以归结为羟基的增加和羰基的减少，另外还探讨了可能的氧化反应机理。     

钒系催化剂表面结构及活性微区模型的研究

运用ＸＲＳ，ＩＲ和ＬＲＳ等手段，对萘氧化制苯酐钒系催化剂的表面组成和结构的联合分析结果表明：催化剂表面各元素以Ｖ：Ｋ：Ｓ：Ｏ＝１：２：２：１０的比例存在；催化剂以Ｖ２Ｏ５为基本骨架，形成了ＶＯ（ＳＯ４）＾２－及Ｓ２Ｏ７＾２－的配位形式，组成了［Ｋ２ＶＯ３ＳＯ４ＳＯ３］ｎ型的表面活性微区。     

聚N-乙烯基甲酰胺碱性水解反应的XPS研究

用X-射线光电子能谱仪(XPS)和胶体滴定法研究了聚N-乙烯基甲酰胺(PNVF)的碱性水解反应.结果表明PNVF水解产物的胺化度随着体系中碱浓度的增大而增大.在PNVF中含有约10%的非甲酰胺基团,由XPS谱图推论这些基团存在C O C结构.PNVF水解产物的高解像度C 1s XPS谱图中,存在5种不同结合能的碳,各峰的变化与PNVF水解过程中的官能团变化规律一致.在285.5 eV处的峰为-CHNH2结构中的碳,归因于PNVF的-NHCHO水解为-NH2;胶体滴定和XPS谱图分析结果的比较表明:采用胶体滴定法测定氨基含量时,如果不考虑PNVF的纯度,将存在较大的误差.     

纳米晶LaFeO3 薄膜的制备与不同气氛处理后的光电子能谱

利用sol\|gel工艺, 在硅衬底上制备了纳米晶LaFeO₃薄膜. 测试了在乙醇蒸气和NO₂气氛下处理后的光电子能谱(XPS), 结果表明, 纳米晶LaFeO₃ 薄膜吸附乙醇后, 表面吸附氧含量明显降低, 铁含量略有下降; 吸附氧化性气体NO₂后, 表面吸附氧和铁含量明显增高, 且存在三价铁离子向四价铁离子转化的趋势. 通过测试和分析表明, LaFeO₃ 的敏感机理不仅与表面吸附氧相关, 还与表面三价铁离子的变价有关.     

Surface modification of poly（vinyl chloride） by long-distance and direct argon RF plasma

AS AN ELECTRICALLY NEUTRAL, HIGHLY IONIZED GAS COM- POSED OF IONS, ELECTRONS, AND NEUTRAL PARTICLES, PLASMA IS A PHASE OF MATTER DISTINCT FROM SOLIDS, LIQUIDS, AND NOR- MAL GASES,KNOWN AS THE FOURTH STATE OF MATTER[1]. RECENT YEARS SEE GREAT PROGRESS IN P…     

A Study on the Surface Structures of Viscose-based Activated Carbon Fiber by FT-IR Spectroscopy and XPS

Using viscose fiber (VF) as starting material and common steam as activating agent, formation of oxygen structures in activated carbon fiber is investigated. In the preparation of samples, VF was first heated at temperatures between 450℃ and 900℃ in N_2 artmosphere. Then, in a successive activation stage, the product carbonized at 600℃ was activated in steam at 450-900℃ for 30 min, and at 600℃ for 5-30 min. The other carbonization products were activated at 600 and 900℃ for 30 min respectively. The products activated at 900℃ were then activated at 450℃ for 30 min again. The starting materiah carbonized products and all activation products were examined by FT-IR spectroscopy and some products were examined by X-ray photoelectron spectroscope (XPS). And the yields of the carbonized and activated products were calculated. By analysing these spectra, the amount of oxygen-containing functional groups of the activated products attained under various activation time, various activation temperature and