Hydroxylation-induced modifications of the Al2O3/NiAl(0 0 1) surface at low water vapour pressure

STM, STS, LEED and XPS data for crystalline θ-Al₂O₃ and non-crystalline Al₂O₃ ultra-thin films grown on NiAl(0 0 1) at 1025 K and exposed to water vapour at low pressure (1 × 10⁻⁷-1 × 10⁻⁵ mbar) and room temperature are reported. Water dissociation is observed at low pressure. This reactivity is assigned to the presence of a high density of coordinatively unsaturated cationic sites at the surface of the oxide film. The hydroxyl/hydroxide groups cannot be directly identify by their XPS binding energy, which is interpreted as resulting from the high BE positions of the oxide anions (O_1s signal at 532.5-532.8 eV). However the XPS intensities give evidence of an uptake of oxygen accompanied by an increase of the surface coverage by Al³⁺ cations, and a decrease of the concentration in metallic Al at the alloy interface. A value of ∼2 for the oxygen to aluminium ions surface concentration ratio indicates the formation of an oxy-hydroxide (AlO_xOH_y with x + y ∼ 2) hydroxylation product. STM and LEED show the amorphisation and roughening of the oxide film. At P(H₂O) = 1 × 10⁻⁷ mbar, only the surface of the oxide film is modified, with formation of nodules of ∼2 nm lateral size covering homogeneously the surface. STS shows that essentially the valence band is modified with an increase of the density of states at the band edge. With increasing pressure, hydroxylation is amplified, leading to an increased coverage of the alloy by oxy-hydroxide products and to the formation of larger nodules (∼7 nm) of amorphous oxy-hydroxide. Roughening and loss of the nanostructure indicate a propagation of the reaction that modifies the bulk structure of the oxide film. Amorphisation can be reverted to crystallization by annealing under UHV at 1025 K when the surface of the oxide film has been modified, but not when the bulk structure has been modified.     

平台石墨炉原子吸收测磷的方法研究

研究了平台石墨炉原子吸收测定磷的方法,表明以氯化钯和硝酸钙的混合液作为基体改进剂测定生物样品中的磷效果最好,方法特征量为8×10~(-9)g,工作曲线线性范围为0～0.400吸光度,精密度好,抗干扰能力强,方法简单,利用标准曲线即可测定生物样品中磷。     

Preparation and microwave absorption properties of electroless Co-Ni-P coated strontium ferrite powder

A new type of Co-Ni-P coated strontium ferrite nanocomposite was prepared with electroless plating enhanced by ultrasonic wave at room temperature. The plating process was studied carefully. The morphology, crystal structure and microwave absorption properties of the Co-Ni-P coated powder were studied with field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), energy dispersive analysis of X-rays (EDX) and vector network analyzer. The results show that the strontium ferrite powder was successfully coated with Co-Ni-P alloy and possesses excellent microwave absorption properties. The maximum microwave loss of the composite powder reaches −44.12 dB. The bandwidth with the loss above −10 dB exceeds 13.8 GHz.     

应变Si1-xGex层中p型杂质电离常温和低温特性

本文采用解析的方法计算了应变Si1-xGex层中p型杂质电离度与Ge组分x、温度T以及掺杂浓度N的关系.发现常温时,在同一Ge组分下,随着掺杂浓度的升高,杂质的电离度的先变小,而后又迅速上升到1.在同一掺杂浓度下,轻掺杂时,杂质的电离度随Ge组分的增加先变大,而后几乎不变;重掺杂时,杂质电离能变为0后,杂质电离度为1.低温下,轻掺杂时,载流子低温冻析效应较为明显,杂质的电离度普遍较小,当掺杂浓度大于Mott转换点时,载流子冻析效应不再明显,电离率迅速上升到1.在同一Ge组分下,随着掺杂浓度的升高,杂质的电离度先变小,后变大,而后又迅速上升到1.在同一掺杂浓度下,轻掺杂时,杂质的电离度随Ge组分的增加变大;重掺杂时,杂质电离能变为0后,杂质电离度为1.     

基于痕量联苯胺阻尼作用的荧光光度分析

在HCl介质中，联苯胺的存在对KBrO3氧化吡咯红反应有抑制作用，据此建立了测定痕量联苯胺的荧光动力学新方法。对方法的介质条件、试剂用量、干扰物质影响进行了系统研究。在最佳实验条件下，方法的线性范围为30～400ng／mL，检出限为14．4ng／mL，对11份浓度为80ng／mL，300ng／mL的联苯胺标准溶液进行平行测定，相对标准偏差分别为2．1％和1．2％。本法用于塑料和雨水中联苯胺的测定，回收率为97．8％～102．1％。     

硅钙合金中钙含量的测定

研究了用一氧化二氮-乙炔火焰原子吸收光谱法测定硅钙合金中钙,并对样品消化处理条件和干扰因素进行了综合考虑.该法灵敏度高、步骤简单,操作容易掌握,干扰少等特点.其相对标准偏差均小于1.0%(n=6).加标回收率均为97.0%-100.0%范围内,本法完全达到了仪器分析质量与质量控制要求.     

STM/AFM studies of the evolution of morphology of electroplated Ni/W alloys

The surface morphology evolution of Ni/W alloys was studied, as a function of the alloy composition. Using the modified plating baths developed in our laboratory recently, electroplated Ni/W alloys with different W content, in the range of 7–67 atom percent (a/o), can be obtained. This was found to lead to different structures, ranging from polycrystalline fcc-Ni type structure to amorphous, followed by orthorhombic with increasing W content in the alloy. Powder XRD was studied to determine the crystal structures. Ex situ STM, AFM and SEM were used to study in detail the surface morphologies of the different alloys, and their evolution with increasing W content.

The important findings are that a mixture of two crystalline forms can give rise to an amorphous structure. Hillocks that are usually a characteristic of epitaxial growth can also exist in the amorphous alloys. Oriented scratches caused by stress can also be formed.

Up to 20 a/o of W is deposited in the alloys in crystalline form, with the fcc-Ni type structure. Between 20 and about 40 a/o an amorphous structure is observed, and above that an orthorhombic crystal structure is seen, which is characteristic of the NiW binary alloy. Careful choice of the composition of the plating bath allowed us to deposit an alloy containing 67 a/o W, which corresponds to the composition NiW₂.     

New methodologies in trace analysis of volatile organic compounds

Two methods for sampling and concentration of volatile organic compounds are reported. In the first method, traps coated with a very thick film (ca. 100 μm) of cross-linked silicone stationary phase are employed. Such thick films can be prepared with a modified dynamic coating procedure, which is briefly described. The low phase ratio traps can be utilized for enrichment of volatiles from gaseous as well as aqueous matrices. The second technique is based on chromatographic evaporation of a solvent in a capillary tube, where the process is sustained by a repeated sample injection and a cyclic flow reversal. In this way, large solvent volumes can be handled by a small volume system. Under optimal conditions, when using a solvent barrier, quantitative recovery is possible even for compounds of comparatively high volatility. Another important application of the technique is extraction of trace components from gases such as headspace samples, polluted air, etc.     

Separation of Monovinyl and Divinyl Protochlorophyllides Using C30 Reverse Phase High Performance Liquid Chromatography Column: Analytical and Preparative Applications

A new, high performance liquid chromatography method has been developed for the separation of monovinyl- and divinyl-protochlorophyllides, using commercially available, C₃₀ reverse phase column and isocratic elution. This method can be used both for analytical applications and preparative scale purification of monovinyl- and divinyl-protochlorophyllides using the same column where submilimolar concentrations of the crude protochlorophyllide extract can be separated in one run. The purity of the obtained protochlorophyllides was demonstrated by spectroscopic methods, as well by the formation of aggregates in toluene.     

Hypothesis testing for the generalized multivariate modified Bessel model

In this paper, we consider hypothesis testing problems in which the involved samples are drawn from generalized multivariate modified Bessel populations. This is a much more general distribution that includes both the multivariate normal and multivariate-t distributions as special cases. We derive the distribution of the Hotelling's T²-statistic for both the one- and two-sample problems, as well as the distribution of the Scheffe's T²-statistic for the Behrens–Fisher problem. In all cases, the non-null distribution of the corresponding F-statistic follows a new distribution which we introduce as the non-central F-Bessel distribution. Some statistical properties of this distribution are studied. Furthermore, this distribution was utilized to perform some power calculations for tests of means for different models which are special cases of the generalized multivariate modified Bessel distribution, and the results compared with those obtained under the multivariate normal case. Under the null hypothesis, however, the non-central F-Bessel distribution reduces to the central F-distribution obtained under the classical normal model.