用铜物理显影的多级放大成像过程Ⅲ.影像中铜和银的分布及明胶对Au3+的还原

本文研究了铜物理显影后影像中铜和银的分布以及在非影像区明胶对Au³⁺的还原作用。铜含量随着影像深度的增加而增加,银含量却随着深度的增加而减少。Ag3d结合能向低值位移说明影像内部的银处于单原子和多原子的混合状态,但是影像表面的银却为单原子状态,如果铜物理显影进行得足够长,铜最终会将银全部遮盖。在这以后的铜物理显影是铜的自催化过程,样片浸入氯金酸溶液中后,非影像区中吸收的氯金酸量大大高于影像区,因而铜的沉积速度在非影像区也比影像区大得多。明胶能还原Au³⁺.还原过程可分为两步:第一步由Au³⁺还原成Au⁺,这一步在室温下是快反应;第二步由Au⁺还原成金,这个反应比较慢,Au⁺和Au在物理显影中可作为催化核,使铜在非影像区沉积。     

新试剂HBPCF用于生物样品及铝合金中微量铜的测定

研究了新试剂 1 ,5-二 ( 2 -羟基 - 5-溴苯 ) - 3-氰基甲 ( HBPCF)与铜的显色反应 ,在p H=3.6的乙酸 -乙酸钠介质中 ,Cu( )与 HBPCF反应生成蓝色配合物 ,在 630 nm处有最大吸收 ,表观摩尔吸光系数为 2 .8× 1 0 4 L· mol- 1· cm- 1,Cu( )浓度在 0～ 2 5μg/2 5m L范围中皆服从比耳定律。该试剂在此条件下选择性很好 ,可应用于茶叶、绿豆及铝合金中微量铜的直接测定 ,结果令人满意。     

X射线荧光光谱法测定铝合金中铜元素的测量不确定度评定

利用X射线荧光光谱法(XRF)对硬铝合金中铜元素进行测定,分析了测量不确定度来源,并对不确定度分量进行评定,经计算得出合成标准不确定度和扩展不确定度。当硬铝合金中铜的质量分数为4.33%时,扩展不确定度为0.17%(k=2)。     

示波滴定法测定铝合金中铜的含量

研究了铝合金中铜含量的示波滴定法。在酸性溶液中抗坏血酸将铜（Ⅱ）还原为铜（Ⅰ）,用过量四苯硼钠沉淀铜（Ⅰ）,过量的四苯硼钠用氯化四乙基铵标准溶液返滴定,以四苯硼钠切口消失为终点,计算出铜含量。方法终点变化敏锐,不外加指示剂,与标准分析方法相比较,操作简便、快速,所用分析试剂无毒,测定结果的RSD小于0．19％,标准加入回收率为98．7％～102．0％。     

ZrO2氧空位显微结构的高分辨电镜研究

基于透射电镜X射线能谱仪得到的微区成分信息及高分辨电子显微结构信息,构建具有氧空位缺陷的ZrO2晶体结构模型,用200 kV透射电子显微镜的参数进行高分辨实验像的多片层法模拟计算,观察分析了ZrO2多晶材料样品的晶格缺陷.沿[001]方向的二维晶格像及相应的傅立叶变换像显示出ZrO2样品的晶格缺陷.将计算机模拟结果与高分辨实验像进行比较,结果表明计算机模拟像的衬度及周期性与实验像之间符合良好.根据晶体结构的缺陷模型和模拟计算,阐明了氧空位缺陷引起的实验像衬度的变化.通过高分辨电子显微观察结果及计算机模拟结果,揭示了陶瓷ZrO2多晶材料样品晶格中氧空位的存在.     

电子能谱线形分析研究碳物种的化学状态

利用ＸＰＳ的ＣＩｓ携上峰,Ｘ射线激发供歇线形,ＸＰＳ价带谱以及俄歇电子能谱的ＣＫＬＬ线形研究了几处碳材料的化学状态和电子结构。研究结果表明：ＸＰＳ的携上效应可以鉴别不同结构的碳材料。ＸＡＥＳＲ 化学位移和线形也可以有效地研究中不同的碳材料的成像方式。ＸＰＳ的价带谱电子结构的一种有效方法,对碳材料的研究也很有效。ＡＥＳ的ＣＫＬＬ俄歇线形非常适合金属碳化物的鉴别。     

铜在碱性溶液中阳极过程的研究

用慢电势扫描和恒电流法研究铜在浓碱中的阳极过程,并用角分辨X射线光电子能谱测试了铜表面二次钝化膜。结果表明,该膜由内层Cu₂O和外层CuO-Cu(OH)₂组成,越靠近膜的表面,CuO/Cu(OH)₂含量比越小,吸附水越多。据此提出成膜的电化学氧化-表面转化历程。     

铝合金建材的X射线荧光分析

用高性能飞利浦PW2424型X射线荧光光谱仪,测定铝合金建材中的Si、Fe、Cu、Mn、Mg、Zn、Ti、Cr、Ni等9个化学元素的含量.给出各元素的干扰校正系数和基体效应校正系数.方法准确、灵敏,稳定性好,速度快.     

多嵌段聚醚氨酯脲类固态离子导体的X光电子能谱研究

固态离子导体作为一种高能密度电池中的电解质在传感器中的实际应用受到了普遍关注。聚氧化乙烯与碱金属盐的复合物是其中研究得最早、最多的一类。但它在室温下电导率较低、力学性能不理想,人们正着力于研制综合性能优良的高分子固态离子导     

Non-invasive surface analysis of ancient bronze arrowheads with scanning electron microscopy and X-ray powder diffractometry

In this research, surfaces of eight ancient metal arrowheads were investigated regarding chemical composition, homogeneity, and products of corrosion. To perform that, two nondestructive techniques were applied: Scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS), and X-ray powder diffractometry (XRPD). Importantly, both methods did not require sampling, cutting, nor significant cleaning of the historical artifacts, which made the measurements not only nondestructive but noninvasive too. SEM-EDS measurements provided information on the morphology and elemental composition of the surfaces of the studied objects as well as the distribution of chemical elements on the surfaces and supported crystalline phase analysis. It was revealed that the arrowheads were cast of tin bronze, but some of them contained high amounts of lead and admixtures of antimony and arsenic while copper and tin oxides and lead carbonates were found as the major corrosion products. In some cases, distribution of elements in the surface exhibited serious nonhomogeneity, probably resulting from limited solubility of the casting metals and degradation processes. Based on the obtained results, authenticity and declared provenience of the arrowheads were assessed in reference to the characteristics of similar objects described in literature.     

Chromatographic,Microscopic, and Spectroscopic Characterization of a Wooden Architectural Painting from the Summer Palace,Beijing, China

The wooden construction painting is a type of an ancient decorative art on Chinese ancient structures. Comprehensive reports concerning the composition of these materials are rather limited. Here multiple analytical methods were applied to systematically explore the morphology and materials. Several paintings were characterized using a morphological microscope. Scanning electron microscopy–energy dispersive spectrometry (SEM-EDS), X-ray fluorescence (XRF), and X-ray diffraction (XRD) detected emerald green and ultramarine in the paint layers. Gas chromatography–mass spectrometry (GC-MS) indicated that the binding medium in the first layer was composed of blood. Our study helps to comprehensively understand the preparation of the wooden construction paintings in the renowned Summer Palace and provide a scientific basis for its restoration and related archeology work.     

Nickel-containing nanophases as the carriers of catalytic active sites in the ethylene oligomerization in the presence of systems based on Ni(acac)2 and organoaluminum compounds

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Magnetite nanoparticle mediated catalytic aquathermolysis of Omani heavy crude oil

The worldwide demand for energy continues to grow and the production of heavy crude is escalating due to shortage of conventional light crude. The transportation of heavy crude oil from the head-well to the refinery is a challenging task due to its high viscosity and low API gravity. Catalytic aquathermolysis is one of the most significant and cost-effective viscosity reduction techniques employed in the up gradation of the crude oil at elevated temperatures and hence to enhance oil extraction process. In this study, catalytic aquathermolysis of Omani heavy crude oil was performed using magnetite nanoparticles (NPs). The NPs were synthesised by reverse co-precipitation method using iron salts in alkaline medium. The synthesised NPs were characterized using Scanning Electron Microscopy (SEM), X-Ray Powder Diffraction (XRD), Energy Dispersive X- Ray analysis (EDX) and Fourier Transform Infrared Spectroscopy (FTIR). The XRD results exhibited a characteristic peak confirming the high purity of iron oxide nanoparticles. The FTIR spectral analysis designated two well-defined peaks corresponding to wave numbers of 500 ?cm^?1 and 630 ?cm^?1, endorses the presence of Fe–O. The catalytic aquathermolysis experiments were carried out in a Parr high temperature-high pressure batch reactor at different experimental conditions. The processing parameters in temperature range of 250 ?°C - 300 ?°C, 0.1% to 0.3% catalyst loading, water to oil ratio of 1:7 to 3:7 with 24–72 ?h of reaction time. The initial pressure in the reactor was maintained at 32 ?bars and the optimization was performed using the Taguchi method to maximize the level of heavy oil. An orthogonal array was employed to analyse the effects of mean response and mean signal-to-noise ratio (S/N) to upgrade the heavy oil. The regression analysis was used to establish a relationship between the viscosity and experimental parameters. The experimental outcomes indicates that the maximum reduction in viscosity occurred at a processing temperature of 300 ?°C, 1:7 ?W/O ratio, 0.1 ?wt% of catalyst concentration and 48 ?h of reaction time. Similarly, the optimum conditions for the reduction in API gravity were obtained at 280 ?°C temperature, 3:7 ?W/O ratio, 0.2 ?wt% of catalyst concentration and a reaction time of 24 ?h.     

唐代彩绘陶俑中无机颜料的化学组成

采用X射线粉末衍射（XRD）、X射线荧光光谱（XRF）和扫描电子显微镜-能谱（SEM-EDS）等测试技术对西安西曹M16唐墓出土的2尊唐代彩绘陶俑颜料进行了化学组成分析。结果表明,陶俑中含有丰富的无机颜料,其中红色颜料的显色成分为铅丹（Pb₃O₄）;白色颜料的显色成分为铅白（PbCO₃）和石灰石（CaCO₃）;粉色颜料的主要显色成分为铅丹和铅白的混合物;青色颜料为铜绿（Cu₂（OH）₂CO₃）和青石（Cu₃（OH）₂（CO₃）₂）混合物。     

Analytical Electron Microscopy Study of a ZnO-NiO Solid Solution

 Results of an analytical electron microscopy study of a binary ZnO-NiO system are reported and discussed. Emphasis was placed on the determination of Ni concentration (solubility) in the ZnO grains using quantitative TEM-EDXS. The influence on the results of beam diameter, foil thickness and corrections used are described and discussed. During the study small precipitates, presumably NiO, were found in the ZnO grains of the ZnO-NiO samples with different ZnO/NiO ratios. In TEM, the precipitates exhibited image contrast only at certain orientations and were normally invisible during the EDXS analysis. The presence of the precipitates too small to be seen using scanning electron microscopy could explain erroneous results for the Ni concentration in a ZnO solid-solution phase obtained previously using SEM-EDXS. Quantitative EDXS analyses were performed on ZnO grains using different electron beam diameters. In each sample, the spread of the results was correlated to the beam diameter (analysed volume). It was found that when the average number of precipitates was less than one per analysed volume the measured points that included precipitates could easily be identified on the basis of their deviation from the mean value of the Ni content.     

Al5Fe2合金熔体中程有序结构的研究

采用紧束缚原子间作用势，利用分子动力学模拟(MD)的方法研究了Al5Fe2合金熔体的微观结构，发现在结构因子的小角部分(Q=15.7nm^-^1)出现了一个明显的预峰(FSDP)，并得到X射线衍射实验的进一步印证，在实验测得的合金衍射图样中，液态衍射曲线与固态衍射曲线间存在着很好的对应关系，它们在小角部分都存在峰位，这表明Al5Fe2合金熔体与其固态在结构上存在着很大的相似性。通过对化学短程序参数α及Bhatis-Thornton(BT)结构因子的分析计算，发现熔体中存在较强的化学序，并认为正是这种化学序导致了中程有序结构(MRO)的产生。Faber-Ziman(FZ)偏结构因子的SFe-Fe(Q)和SAl-Fe(Q)在Q=15.7nm^-^1处分别存在最大值与最小值，也是熔体中存在着超结构的表征。同时，我们还给出了体系的配位数及代表中程有序的原子团簇的结构模型。     

Structural Stability of LiCoO2 at 400°C

The relative stability of the lithiated-spinel structure, Li₂[Co₂]O₄, at 400°C to the layered LiCoO₂ structure has been investigated. “Low-temperature” LT-LiCoO₂ samples were synthesized at 400°C by the solid-state reaction of Li₂CO₃ with CoCO₃ (or Co₃O₄) for various times between 10 min and 232 days. Least-squares refinements of X-ray powder diffraction patterns were used to determine the fractions of lithiated-spinel Li₂[Co₂]O₄ and layered LiCoO₂ in the samples. X-ray powder diffraction and transmission electron microscope data show that Li₂[Co₂]O₄ nucleates from an intermediate Li_xCo_1−x[Co₂]O₄ spinel product before transforming very slowly to layered LiCoO₂. The experimental data confirm the theoretical prediction that layered LiCoO₂ is thermodynamically more stable than the lithiated-spinel structure at 400°C and support the arguments that a non-ideal cation distribution in Li₂[Co₂]O₄, non-stoichiometry and kinetic factors restrict the transformation of the lithiated-spinel structure to layered LiCoO₂ at this temperature.     

Combined analysis methods for investigating titanium and nickel surface contamination after plasma deep etching

Plasma etching techniques can result in damage and contamination of materials, which, if not removed, can interfere with further processing. Therefore, characterisation of the etched surface is necessary to understand the basic mechanisms involved in the etching process and enable process control and cleaning procedures to be developed. A detailed investigation by means of the combined use of scanning electron microscopy coupled with energy-dispersive X-ray spectrometry (SEM/EDS), X-ray photoelectron spectroscopy (XPS) and optical microscopy (OM) has been carried out on deep titanium trenches etched by plasma. This innovative approach has provided a further insight into the microchemical structure of the surface contamination layer on both the titanium and the nickel hard mask surfaces. The described experiments were conducted on 25 to 100-μm wide trenches, first etched in bulk titanium by an optimised Cl₂/SF₆/O₂-based inductively coupled plasma process, through an electroplated nickel hard mask. The results allow to identify chlorine, fluorine and carbon as the main contaminating agents of the nickel mask and to associate three oxidation states around the etched trenches highlighting certain specific aspects related to the passivation mechanism. These observations reinforce the scientific relevance of the combined use of complementary optical and imaging analytical techniques.     

Structural characteristics and cyclic voltammetric behaviour of Sonogel-Carbon tyrosinase biosensors. A detailed comparative study of three immobilization matrixes

Structural characteristics an cyclic voltammetry of three amperommetric biosensors based on immobilization of tyrosinase on a Sonogel-Carbon electrode for detection of phenols are described. Cyclic voltammetry was applied to study the electrochemical behaviour of the electrode and the electrochemical reaction on the electrode surface. Scanning electron microscopy, X-ray energy dispersive spectroscopy and atomic force microscopy were used for the structure characterization of the electrode surface, enzyme film and polymers coatings. The influence of additive-protective polymers, such as polyethylene glycol and perfluorinated-Nafion ion-exchanger on the surface of the biosensor were explored.