High temperature reactions between molybdenum and metal halides

Good colour rendering properties, high intensity and efficacy are of vital importance for high-end lighting applications. These requirements can be achieved by high intensity discharge lamps doped with different metal halide additives (metal halide lamps). To improve their reliability, it is very important to understand the different failure processes of the lamps. In this paper, the corrosion reactions between different metal halides and the molybdenum electrical feed-through electrode are discussed. The reactions were studied in the feed-through of real lamps and on model samples too. X-ray photoelectron spectroscopy (XPS) was used to establish the chemical states. In case of the model samples we have also used atomic absorption spectroscopy (AAS) to measure the reaction product amounts. Based on the measurement results we were able to determine the most corrosive metal halide components and to understand the mechanism of the reactions.     

X光光电子能谱法测定胶片中氟,硅和铝的研究

应用Ｘ光光电子能谱法测定了几种彩色胶片表面层中氟的１ｓ能级的结合能；分别比较了水处理前后、溅蚀前后胶片护膜层氟的变化，表明氟化物分布在护膜最表层，是一种易溶于水的氟化物；测定了彩色片护膜层所含硅２ｐ能级的结合能，与自制彩色片护膜层测定结果比较，优质片含一种较多负电性，用与自制片的无机硅不同的硅化物作毛面剂；对溅蚀前后优质片和自产彩色片中的硅铝比变化进行比较，提出优质彩色片Ｆ－４００的护膜层可能是双     

Surface analytical studies of Ar-plasma etching of thin heptadecafluoro-1-decene plasma polymer films

An audio-frequency plasma polymerization set-up with a planar plasma source was used to deposit thin heptadecafluoro-1-decene (HDFD) plasma polymer films. The morphology and chemical structure of the films after deposition were compared with the state of the film after a subsequent Ar-plasma treatment by means of in situ Fourier transform infrared reflection absorbance spectroscopy (FT-IRRAS), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and atomic force microscopy (AFM) as well as contact angle measurements. The results revealed the correlation of wettability of the model Teflon-like films with change of surface chemistry and surface topography as a result of Ar-plasma treatment.     

X-ray photoelectron spectroscopy characterization of stain-etched luminescent porous silicon films

The surface and in-depth chemical nature of the photoluminescent stained Si layer obtained with a novel procedure based on HF/HNO₃ is presented. Oxide-free porous Si surfaces result from controlled preparation, storing and handling of samples, as revealed by parallel X-ray photoelectron spectroscopy and X-ray-induced Auger electron spectroscopy measurements, coupled with Ar⁺ ion sputtering. The present findings support the model for the porous layer of oxidized samples of Si grains embedded in a silica gel matrix.     

同步辐射软X射线近边吸收谱方法研究长期施肥对黑土有机碳官能团的影响

以定位20年的黑土肥料试验为平台,利用同步辐射软X射线近边吸收谱(C-1s NEXAFS)方法,研究了长期施用化肥以及化肥配施玉米秸秆对土壤有机碳官能团的影响。结果表明：与不施肥的空白处理(CK)相比,单施化肥(N,NPK)后土壤的芳香C和羧基C含量增加,脂族C和羰基C含量下降,脂族C/芳香C比值降低;与单施化肥处理相比,化肥配施玉米秸秆后芳香C含量下降而脂族C含量增加,脂族C/芳香C比值增加,并随玉米秸秆用量增加表现的更为明显;无论配施玉米秸秆与否,NPK肥混施处理的芳香C、脂族C以及脂族C/芳香C比值均高于单施N肥处理。上述结果说明,单施化肥比不施肥使土壤有机碳官能团中芳香类化合物的相对比例增加,而脂肪烃类化合物的相对比例下降;化肥配施玉米秸秆则比单施化肥增加了脂肪烃类化合物的相对比例,配施高量比低量玉米秸秆的增加趋势更为明显,同时NPK肥混施比单施N肥有利于提高脂肪烃类化合物的相对比例。C-1s NEXAFS方法能够原位表征长期定位施肥条件下土壤有机碳官能团组成的变化。     

Spectroscopic ellipsometric properties and resistance switching behavior in Si_x（ZrO_2）_（100-x） films

We prepare Si x (ZrO 2 ) 100 x composite films using the co-sputtering method. The chemical structures of the films which are prepared under different conditions are analyzed with X-ray photoemission spectroscopy. Thermal treatment influences on optical property and resistance switching characteristics of these composite films are investigated by spectroscopic ellipsometry and semiconductor parameter ana- lyzer, respectively. With the proper Si-doped Si x (ZrO 2 ) 100 x interlayer, the Al/ Si x (ZrO 2) 100 x /Al device cell samples present very reliable and reproducible switching behaviors. It provides a feasible solution for easy multilevel storage and better fault tolerance in nonvolatile memory application.     

Influence of atmospheric pressure plasma treatment time on penetration depth of surface modification into fabric

In order to determine the relationship between the treatment duration of atmospheric pressure plasma jet (APPJ) and the penetration depth of the surface modification into textile structures, a four-layer stack of polyester woven fabrics was exposed to helium/oxygen APPJ for different treatment durations. The water-absorption time for the top and the bottom sides of each fabric layer was reduced from 200 s to almost 0 s. The capillary flow height for all fabric layers in the stack increased linearly with the treatment duration but the rate of increasing reduced linearly with the fabric layer number. A model for the capillary flow height as a function of treatment duration and the layer number was established based on the experimental data and the maximum penetration depth of the APPJ was predicted for the polyester fabric. The improved wettability of the fabrics was attributed to the enhanced surface roughness due to plasma etching and the surface chemical composition change due to plasma-induced chemical reaction as detected by scanning electron microscopy and X-ray photoelectron spectroscopy, respectively. The surface roughness and the surface chemical composition change diminished as the fabric layer number increased.     

Morphological and surface compositional changes in poly(lactide-co-glycolide) tissue engineering scaffolds upon radio frequency glow discharge plasma treatment

Chemical functionalisation of polymeric scaffolds with functional groups such as amine could provide optimal conditions for loading of signalling biomolecules over the entire volume of the porous scaffolds. Three-dimensional (both surface and bulk) functionlisation of large volume scaffolds is highly desirable, but preferably without any change to the basic morphological, structural and bulk chemical properties of the scaffolds. In this work, we have carried out and compared treatments of poly(lactide-co-glycolide) tissue engineering scaffolds by two methods, that is, a wet chemical method using ethylenediamine and a glow discharge plasma method using heptylamine as a precursor. The samples thus prepared were analysed by scanning electron microscopy and X-ray photoelectron spectroscopy. The plasma treatment generated amide and protonated amine (NH⁺) groups which were present in the bulk and on the surface of the scaffold. Amination also occurred for the wet chemical treatments but the structural and chemical integrity were adversely affected.     

Aqueous electrochemical insertion of Na into the tungsten oxide hybrid WO3(4,4′-bipyridyl)0.5

Aqueous electrochemical insertion of M⁺ (Na⁺ and H⁺) species into WO₃(4,4′-bipyridyl)_0.5 has been carried out. The chemical states and structure of the resulting product were analysed by X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). XPS showed the presence of W⁶⁺ as well as the usual reduced W species (W⁵⁺) which is responsible for a change in colour. Moreover, the presence of these intercalates correlates with the evolution of the reduced W species. The bulk structure of the layered hybrid, as determined by powder X-ray diffraction, showed no alteration after electrochemistry, in contrast to the same measurements on tungsten trioxide (WO₃). This however concurs with single-crystal X-ray studies, which show little change in lattice parameters with Na⁺ insertion. Four-probe resistance measurements of the layered hybrid coated film display a drop in resistance after electrochemistry, which can be attributed to the injection of charge-carriers into the conduction band.     

翡翠成分、结构和矿物组成的无损分析

利用便携式能量色散型X射线荧光(portable energy-dispersive X-ray fluorescence,PXRF)、外束质子激发X射线(external beam proton induced X-ray emission,PIXE)、X射线衍射(X-ray diffraction,XRD)和激光拉...     

Physicochemical characterization of thermally aged Egyptian linen dyed with organic natural dyestuffs

A number of organic natural dyestuffs used in dyeing in ancient times, i.e. indigo, madder, turmeric, henna, cochineal, saffron and safflower, have been used to colour Egyptian fabrics based on linen. Their physicochemical properties have been evaluated on thermally aged linen samples. The aged dyed linen samples were thoroughly examined by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), X-ray diffraction (XRD) and tensile strength and elongation measurements. It was found that, in the molecular level, dyes interact mainly with the cellulose compounds of the aged linen while in the macroscopic level tensile and elongation parameters are altered. Tensile strength is positively related to the dye treatment while elongation depends specifically on the type of the dye used. Results converge that the dyed textiles did indeed play a role as protecting agents affecting strength and reducing thermal deterioration.     

Study of the combined carbonization of poly(vinylidene fluoride) by X-Ray photoelectron spectroscopy

The surface composition of two samples synthesized by the combined carbonization of poly(vinylidene fluoride) (PVDF) films is studied by X-ray photoelectron spectroscopy. One of them is successively exposed only to chemical and radiation impacts, and the treatment of the other includes chemical, heat, and radiation exposure. The chemical preparation of both samples is the same. It is shown that the magnitude and direction of the gradient of the residual fluorine concentration in the surface layer of PVDF carbonization products can be controlled. Since dehydrofluorination decreases the surface electrical resistance of the material, a combination of chemical, heat, and radiation treatments can be used to create a predetermined sequence of heterolayers with different fluorine concentration on a flexible and transparent polymer base and, therefore, with different conductivities.     

Complex elemental analysis of heterogeneous objects

A complex method of local microanalysis of samples, in which the analysis conditions depend on the orientation of the boundaries of heterogeneous objects, has been considered. X-ray and electron spectroscopy methods are simultaneously used. Application of special instrumental methods for recording X-ray and electron spectra makes it possible to determine the elemental composition of samples in cuts and near interphase boundaries with a high accuracy. Such a possibility is realized due to the development of a method and equipment providing simultaneous recording secondary radiations in two mutually opposite directions with a change in the azimuthal direction with respect to the point of analysis, without loss of the beam positioning point, through application of microtomography.     

Cadmium colours: composition and properties

The composition and the properties of cadmium aquarelle colours are discussed. The examined colours were 24 different aquarelle cadmium colours from six different manufacturers. The colours ranged from light, bright yellows to dark, deep-red tones. The aim of this research was to find out if the pigments contain cadmium salts: sulphides and/or selenides. This information will help in choosing watercolours in conservation processes. Today, aquarelle colours not containing cadmium pigments are being sold as cadmium colours; thus their properties might be different from actual cadmium colours. The aim of the research was to verify that the colour samples contained cadmium pigments and to estimate their compositions and ageing properties. Element analyses were performed from colour samples using micro-chemical tests and X-ray fluorescence measurements. Thin-layer chromatography was used for analysing gum Arabic as a possible binding medium in the chosen colour samples. Through ageing tests, the resistance of the colour samples to the exposure to light, heat and humidity was studied. Visible-light spectroscopy was used in determining the hues and hue changes of the aquarelle colour samples. The spectrophotometer used the CIE L^*a^*b^* tone colour measuring system. From the colour measurements the changes in the lightness/darkness, the redness, the yellowness and the saturation of the samples were examined. PACS 32.30.Rj; 32.30.Jc; 33.20.Kf     

NEXAFS spectromicroscopy of polymers: overview and quantitative analysis of polyurethane polymers

The successful application of X-ray spectromicroscopy to chemical analysis of polymers is reviewed and a detailed application to quantitative analysis of polyurethanes is presented. Near Edge X-ray Absorption Fine Structure (NEXAFS) spectroscopy is the basis of chemical sensitive X-ray imaging, as well as qualitative and quantitative micro-spectroscopy. These capabilities are demonstrated by a review of recent work, and by presentation of new results outlining a methodology for quantitative speciation of polyurethane polymers. C 1s inner-shell excitation spectra of a series of molecular and polymeric model compounds, recorded by gas phase inelastic electron scattering (ISEELS) and solid phase NEXAFS techniques, are used to understand the spectroscopic basis for chemical analysis of polyurethanes. These model species contain the aromatic urea, aromatic urethane (carbamate) and aliphatic ether functionalities that are the main constituents of polyurethane polymers. Ab initio calculations of several of the model molecular compounds are used to support spectral assignments and give insight into the origin and relative intensities of characteristic spectral features. The model polymer spectra provide reference standards for qualitative identification and quantitative analysis of polyurethane polymers. The chemical compositions of three polyurethane test polymers with systematic variation in urea/urethane content are measured using the spectra of model toluene diisocyanate (TDI) urea, TDI-carbamate, and poly(propylene oxide) polymers as reference standards.     

Sulfur speciation in two typical soil samples using X-ray absorption near-edge structure spectroscopy and chemical fractionation

Sulfur K-edge X-ray absorption near-edge structure spectroscopy and chemical sequential extraction was respectively used to study the speciation of sulfur in two sulfur-rich soils samples. Sulfur K-edge X-ray absorption near-edge structure spectroscopy analysis obtained a variety of spectra. Spectral fitting of the X-ray absorption near-edge structure spectra utilizing a large set of model compounds showed great differences between these two sulfur-rich soil samples. It was found that both of the soil samples had high sulfur content (8.40 and 11.57?g?kg^?1, respectively). Chemical extraction results suggested that sulfur mainly existed as organic in the ancient paddy soil (7.37?g?kg^?1) and more reduced sulfur was identified in it. X-ray absorption near-edge structure spectroscopy also got similar results. These organic forms of sulfur existed in organic matter across a range of oxidation states. There was high proportion of oxidized sulfur in the sulfuric acid plant that mainly existed as sulfate.     

Reactivity of lithium exposed graphite surface

Lithium as a plasma-facing component has many attractive features in fusion devices. We investigated chemical properties of the lithiated graphite surfaces during deposition using X-ray photoelectron spectroscopy and low-energy ion scattering spectroscopy. In this study we try to address some of the known issues during lithium deposition, viz., the chemical state of lithium on graphite substrate, oxide layer formation mechanisms, Li passivation effects over time, and chemical change during exposure of the sample to ambient air. X-ray photoelectron studies indicate changes in the chemical composition with various thickness of lithium on graphite during deposition. An oxide layer formation is noticed during lithium deposition even though all the experiments were performed in ultrahigh vacuum. The metal oxide is immediately transformed into carbonate when the deposited sample is exposed to air.     

庙底沟遗址出土仰韶文化彩陶的科学研究

彩陶文化作为新石器时期的重大发明,改变了远古先民的审美方式,而著名的仰韶文化以其彩陶的优美造型、绚丽色彩和丰富的纹饰揭示了原始的艺术特征,承载了史前时期重要的社会文化信息。而利用现代光谱分析技术准确、无损和微损的特点,可以为文物保护的研究提供更科学的技术支撑。研究应用相位辅助光学三维扫描、多光谱成像、X射线荧光、激光拉曼光谱分析技术,对河南省陕县庙底沟遗址出土的新石器时代晚期仰韶文化彩陶碗进行面、点相结合的综合分析,获得了较为完整的文物物理和化学信息。利用三维扫描技术所构建的彩陶碗数字化模型对样品进行了几何尺寸的非接触测量和虚拟修复,利用多光谱成像技术所获得的灰度图像对样品表面化学特征相似区域进行了区分,结合X射线荧光和激光拉曼光谱分析技术对彩陶残片的分析结果,确定了所分析彩陶样品的主要化学成分特征和颜料物相组成。综合研究结果,提出了建立彩陶文物多源信息数字化模型的构想,为这类文物的数字化保护和展示提供了基础科学信息。     

现代仪器在胆结石研究中的运用

对胆结石组分和元素进行准确的分析可为治疗胆结石和预防其复发提供重要的参考。文章综述了现代仪器在胆结石研究中运用的研究进展,这些技术包括拉曼光谱、能谱(EDX)、傅里叶红外光谱(FTIR)及其二阶导数谱、热重分析(TG)、差示扫描量热法(DSC)、原子吸收光谱、电感耦合等离子发射光谱、高效液相色谱(HPLC)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)等。     

Preparation of visible light responsive N doped TiO2 via a reduction-nitridation procedure by nonthermal plasma treatment

A visible light responsive N-doped TiO₂ was prepared via a reduction-nitridation procedure by nonthermal plasma treatment. X-ray diffraction, N₂ adsorption, UV-vis spectroscopy, photoluminescence, and X-ray photoelectron spectroscopy were used to characterize the prepared TiO₂ samples. The plasma treatment did not change the phase composition and particle sizes of TiO₂ samples, but extended its absorption edges to the visible light region. The photocatalytic activities were tested in the degradation of an aqueous solution of a reactive dyestuff, methylene blue, under visible light. The photocatalytic activities of TiO₂ prepared by reduction-nitridation procedure were much higher than that of samples prepared by simple nitridation treatment. The enhanced activity was ascribed to the substitutional N-doping and appropriate concentration of oxygen vacancies. TOHN10 prepared by reduction-nitridation procedure exhibited excellent photocatalytic stability. A possible mechanism for the photocatalysis was proposed.