辉光放电光谱法分析掺杂纳米硅薄膜的研究

介绍了利用辉光放电光谱法分析掺杂纳米硅薄膜，通过优化辉光光源激发参数、计算标准样品的溅射率，建立了掺杂纳米硅薄膜的定量表面分析方法。方法应用于实际掺杂纳米硅薄膜样品的分析，并将分析深度、剖析结果与表面形貌仪的结果进行了对照。试验结果表明，分析方法快速、准确，具有实际应用价值。     

辉光放电,阴极溅射／瞬变原子化原子吸收光谱中阴极材料的研究

辉光放电、阴极溅射／瞬变原子化原子吸收光谱中阴极材料的研究张必成（湖北大学化学系，武汉，４３００６２）关键词辉光放电，阴极溅射，阴极材料辉光放电、阴极溅射／瞬变原子化原子吸收光谱（ＴＡＣＳＧＤ／ＡＡＳ）是近年来出现的高灵敏度痕量分析技术［１］．它是通...     

辉光放电光谱法在深度分析上的应用现状

本文简单地介绍了辉光放电光谱法（GD-OES）的基本原理。分别对深度分析的定量方式、放电方式、应用领域和相关标准进行了详细地阐述。重点描述了商品化仪器中使用的SIMR深度分析定量方法。分别对三种放电方式（如直流、射频和脉冲）在深度分析中的特点进行了介绍。综述了GD-OES在金属镀层、复杂涂镀层、纳米级薄膜和样品制备领域的具体应用。最后,介绍了GD-OES在深度分析方面的标准     

辉光光谱分析中内标法的应用

辉光光谱已成功地应用于定量分析,它不但适合于各种合金的分析,且用于金属表面逐层定量分析。徐升美等提出的辉光光谱分析方法中,在恒定电压和气压的放电条件下,以纯金属为标样进行金属表面逐层定量分析,元素j的谱线强度为:Ij=kεjAqCjt(1)式中q(溅射率)一般是采用样品在溅射前后的减量来获得,由于几克重的样品经溅射后发     

稀土纳米薄膜摩擦学性能研究

用自组装方法可以在单晶硅表面获得稀土纳米薄膜，得到的薄膜通过XPS，偏振光椭圆率测量仪、角接触仪、AFM等手段表征。通过滑动摩擦实验，可以测试稀土薄膜的界面粘附力。通过DF-PM型复复摩擦磨损试验机，考察稀土纳米薄膜的摩擦磨损特性。实验结果表明，稀土纳米薄膜具有低摩擦系数和高抗磨损特性。稀土纳米薄膜具有纳米级尺度、强界面结合力和低表面能，使其成为MEMS装置固体润滑的理想选择。     

辉光放电质谱法测定高纯钛中痕量杂质元素及其相对灵敏度因子校正EI北大核心CSCD

通过选择合适的同位素及分辨率,建立了辉光放电质谱法(GDMS)测定高纯Ti中57种痕量杂质元素的方法。辉光放电过程优化条件为Ar流量500 mL/min,放电电流2.2 mA,预溅射时间30 min。利用高纯Ti标准样品获得了与基体匹配的13种元素的相对灵敏度因子(RSF)值。用建立的方法对高纯Ti溅射靶材样品进行检测,主要杂质元素为Al, Si, S, Cl, V, Cr, Mn, Fe, Ni, Cu, Zr,含量在0.051~2.470μg/g之间,相对标准偏差(RSD)<23%,杂质总量<5μg/g。其中,Ca, Nb元素的检出限为0.5μg/g,其余元素的检出限低至10 ng/g级或1 ng/g级,而且Th, U元素的检出限达到0.1 ng/g。该方法能够满足5N级高纯金属Ti溅射靶材的检测要求。     

辉光放电质谱法测定超高纯铜溅射靶材中痕量杂质元素及其相对灵敏度因子的求取北大核心CSCD

通过选择合适的同位素及分辨率,提出了辉光放电质谱法(GDMS)测定超高纯铜溅射靶材中39种痕量杂质元素的分析方法。对辉光放电过程中的参数进行了优化,条件如下:放电气体流量为450 mL·min^(-1),放电电流为2.00 mA,预溅射时间为20 min。由于高纯铜的GDMS标准样品极难获得,为提高痕量杂质元素的检测准确度,在现有的标准样品条件下,利用高纯铜标准样品只获得了与基体匹配的21种杂质元素的相对灵敏度因子(RSF),其余18种杂质元素的RSF只能按照仪器自带的标准RSF进行计算。参照美国材料与试验协会的标准ASTM F1593-08(2016)的TypeⅢ中的第2种方法计算33种杂质元素的检出限,而其他6种主要杂质元素因其含量高于仪器噪声水平而无法用此法得到检出限。用GDMS对超高纯铜溅射靶材样品进行了检测,主要杂质元素为硅、磷、硫、氯、铁、银,检出量为0.015~0.082μg·g^(-1),杂质总量小于1μg·g^(-1)。除锌、碲、金的检出限在10 ng·g^(-1)级外,其余元素的检出限能够达到ng·g^(-1)级,其中钍、铀的检出限甚至达到了0.1 ng·g^(-1)级,说明方法能够满足GB/T 26017-2010中的6N(99.9999%)超高纯铜溅射靶材的检测要求。     

辉光放电光源在铝合金发射光谱分析上的初步应用

前言辉光放电光源的稳定度高,只要有精度好的检测系统,可保证分析结果有很高的精密度。直接进行固体块样的合金组分元素分析,是这种光源的特长之一。用辉光放电光源作铝合金的分析,国外也有报导。因铝合金极易氧化,试样表面易形成氧化膜,所以试样不易产生正常的剥离,而且预燃时间往往很长又无规律,因而分析再现性不好。浅田庄太郎等认为铝合金的分析,用辉光放电光源是很困难的。他们在试验中还发现了第三元素的影响。试样中只要含有铜,溅射量就增大,使准确度变坏。Dogan研究了铜-     

强短脉冲辉光放电阴极溅射逐层分析研究

利用强短脉冲供电电源和一种新型的辉光放电灯联用进行阴极表面溅射，发现它与在直流供电下有不同的结果，扫描电镜进行观察，得到样品溅射表面的扫描图，结果表明，该技术的金属或合金样品表面的逐层分析提供了一种新方法。     

辉光放电等离子体对聚丙烯纤维的表面改性

在对电晕、介质阻挡放电、γ射线辐射接枝对化纤改性的简要介绍基础上，重点论述了辉光放电等离子体对聚丙烯纤维的改性。并按等离子体技术的发展过程，对低压和常压辉光放电等离子体对聚丙烯纤维与织物改性的特点、原理及发展前景进行了扼要综述，指出常压辉光放电等离子体是一种很有潜力的表面改性技术。     

Preparation and Characterization of Hydrophobic Nano Silver Film on Butterfly Wings as Bio-template

Hydrophobic nano silver films were fabricated on butterfly wings as bio-template. The micrometric/nano structures and hydrophobicity of the surfaces were investigated with the help of scanning electron microscope（SEM） and video-based contact angle meter. The hydrophobic mechanism of silver film was analyzed with the aid of Cas- sie＇s formula. On the nano silver films of various thicknesses（5, 10, 20, 40, 60, 80, 100 nm）, all the contact an- gles（CAs） of water were bigger than 120°. When the silver film was 5 nm, the CAs of water on it on the wing surfa- ces of Mimathyma nycteis and Speyeria aglaja were 143.2° and 139.2°, respectively. Coated with the sliver film of the same thickness, butterfly wing surface exhibited the CA remarkably bigger than glass slide surface, exhibiting its high hydrophobicity. With the increase of silver film thickness on butterfly wing surface, the hydrophobicity kept de- creasing. The micrometric/nano hierarchical structures on butterfly wing surface result in the transition of metal silver from hydrophilicity to hydrophobicity.     

Ni／丝光沸石覆盖物的特性

采用蒸气相法合成了Ｎｉ／丝光沸石覆盖物，用ＸＲＤ，ＳＥＭ，电子能谱证明了合成的材料为丝光沸石包覆于金属镍粉表面成的复合物。用二甲本异构化探针反应和ＮＨ３－ＴＰＤ考察了该包覆物的催化活性及酸性。结果表明，Ｎｉ／丝光沸石覆盖物具有良好的表面酸性，二甲苯异构化的活性均高于采用同样方法合成的Ｃｒ／丝光沸石覆盖物，间二甲苯异构化活性可以达到９７％。     

循环伏安法的电扫描方式对苯胺聚合产物形貌影响的观察

在含有0.2 mol.L-1苯胺的0.5 mol.L-1H2SO4溶液中,以扫描速度50 mV.s-1,扫描电位为-0.1~0.9 V,采用循环伏安法(CV),在金属Ti基体上,通过控制扫描方式分别得到了颗粒状、纤维状及管-片状的苯胺聚合产物,分析了形成不同形貌聚苯胺的原因,并通过扫描电子显微镜(SEM)、循环伏安法和电化学阻抗谱(EIS)对不同形貌聚苯胺的结构和性能进行了表征.结果表明,不同形貌聚苯胺的形成是由于聚苯胺的成核及生长模式不同,而无论何种形貌的聚苯胺膜都具有很大的比表面积和良好的导电性能,其中,管-片状聚苯胺的膜层阻抗最小,导电性能最好.     

The effect of glow discharge sputtering on the analysis of metal oxide films

The potential of radiofrequency glow discharge optical emission spectrometry (rf-GD-OES) for the quantification and the solid-state speciation of metal oxide films has been investigated in this work. Two types of oxide coatings, an iron oxide film deposited on silicon and a chromate conversion coating (CCC), were studied at 700 Pa of pressure and 30 W of forward power. The metal to oxygen ratios in the quantitative depth profiles (Fe/O and Cr/O, respectively) were used to evaluate the oxidation states of iron and chromium in the oxide films, demonstrating the capability of GD-OES technique for depth-resolved solid-state speciation. Furthermore, the effect of glow discharge sputtering on the samples surface in terms of modifications in the surface morphology and species transformations, were investigated by using atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The iron and chromium oxidation states were carefully studied by XPS at the original samples surface and at the bottom of GD craters, and a systematic reduction of metal elements was observed after rf-GD-OES analysis. In the case of thin oxide films, preferential sputtering can be considered as a critical factor since oxygen atoms can be preferentially sputtered, leaving a metal-enriched surface and, therefore, promoting the reduction of metal elements. In the present study preferential sputtering was found to be sample dependent, changing the proportion of the metal reduction in the oxide film with its composition. Additionally, alternative sputter-depth-profiling techniques such as secondary ion mass spectrometry (SIMS), femtosecond laser ablation (fs-LA), and XPS ion gun were used for the analysis of the CCC in order to evaluate the reduction of Cr⁶⁺ to Cr³⁺ depending on the sputtering mechanism.     

用表面增强拉曼散射研究电解法制备的纳米银膜

用一种廉价的电解方法制备了纳米银膜,并详细研究了在这种银膜上的表面增强拉曼散射效果．结晶紫为本实验的检测性分子．通过实验发现,这种银膜用便携式拉曼光谱仪测试并计算出的表面增强拉曼散射的增强因子为603,并对结晶紫的最小检出限为0．1nmol／L．     

Nano silver coated patterned silica thin film by sol–gel based soft lithography technique

We report the fabrication of nano silver coated patterned silica thin film by sol–gel based soft lithography technique. Initially, silica gel film on soda lime silica glass was prepared by dipping technique from a silica sol of moderate silica concentration. A PolydimethylSiloxane elastomeric stamp containing the negative replica of the patterns of commercially available compact disc was used for embossing the film and the embossed film was cured up to 450 °C in pure oxygen atmosphere for oxide film. Finally, a precursor solution of AgNO₃ in water containing polyvinyl alcohol as an organic binder was made and used for coating on the patterned silica film by dipping technique and cured the sample up to 450 °C in reducing gas atmosphere to obtain nano silver layer. The formation of only cubic silver (~4.0 nm) and both cubic silver (~5.2 nm) and silver oxide (~3.6 nm) crystallites at 350 and 450 °C film curing temperatures respectively were confirmed by XRD measurements. The % of nano silver metal and silver oxide were 75.4 and 24.6 respectively. The nano-structured surface feature was visualized by FESEM whereas AFM revealed the high fidelity grating structure of the films. Presence of both spherical and rectangular structure (aspect ratio, 2.37) of nano silver/silver oxide was confirmed by TEM. The films were also characterized by UV–Vis spectral study. The patterned film may find application in chemical sensor devices.     

Influence of local structure on local electric field in Island‐like silver films

The infrared absorption enhancement phenomenon in the normal configuration of vacuum‐evaporated metal films on a transparent substrate is known to depend not only on the metal film morphology but also on the local structures of metal particles. To date, however, few studies have examined the effect of local structure on the phenomenon. Size distributions of islands and gaps, along with the volume fractions of Ag in thin films, were measured using scanning electron microscopy as a function of film thickness. The local structure of Ag nano clusters deposited on silicon substrates was investigated using a total conversion electron yield X‐ray absorption fine structure (XAFS) method at the Ag K‐edge. We observed a correlation between the electromagnetic field intensity at the surface as evaluated by IR measurement and the coordination numbers evaluated by XAFS. We found that the film morphology had a greater effect on resonant and nonresonant contributions than did the local structure of a particle. Copyright © 2006 John Wiley & Sons, Ltd.     

EFFECT OF THICKNESS NON-HOMOGENEITY ON THE KINETIC BEHAVIOUR OF MICROSCOPIC FOAM FILM

The effect of thickness non-homogeneity on the drainage of microscopic horizontal foam films was studied experimentally and theoretically. Quasi-static and asymmetrical distribution of thickness irregularities over the film surface was established in the experiment. This type of dimpling was modelled theoretically and employed to derive a new equation for the film thinning. It differs from the theoretical expressions known from the literature and is in better agreement with the experimentally determined functional dependence of thinning rate on film size.     

Synthesis of Supported Bimetal Catalysts using Galvanic Deposition Method

Supported bimetallic catalysts have been studied because of their enhanced catalytic properties due to metal‐metal interactions compared with monometallic catalysts. We focused on galvanic deposition (GD) as a bimetallization method, which achieves well‐defined metal‐metal interfaces by exchanging heterogeneous metals with different ionisation tendencies. We have developed Ni@Ag/SiO₂ catalysts for CO oxidation, Co@Ru/Al₂O₃ catalysts for automotive three‐way reactions and Pd−Co/Al₂O₃ catalysts for methane combustion by using the GD method. In all cases, the catalysts prepared by the GD method showed higher catalytic activity than the corresponding monometallic and bimetallic catalysts prepared by the conventional co‐impregnation method. The GD method provides contact between noble and base metals to improve the electronic state, surface structure and reducibility of noble metals.     

Surface topography effects on glow discharge depth profiling analysis

Glow discharge optical emission spectroscopy (GD‐OES) has been shown to be of immense value in elemental depth profiling of thin or thick films on conductive or non‐conductive substrates. For aluminium, GD‐OES has been employed to examine locations of markers and tracers in anodic films, thereby assisting understanding of transport phenomena. In order to investigate the influence of surface topography on depth profiling analysis, anodic aluminium oxide films of various thicknesses, with incorporated electrolyte species, were produced on superpure aluminium substrates of controlled roughnesses. The distributions of incorporated species in the films were subsequently probed. Surface topography modifications and consequent depth resolution degradation were examined during depth profiling analysis performed by GD‐OES. The results reveal that the sputtering process leads to the roughening or smoothing of the surface topography of the specimen for a ratio of the film thickness to the amplitude of the substrate texture less, or greater, than 1 respectively. As a consequence of the surface topography dependence of the ion bombardment, analysis of thin films over rough surfaces suffers from depth resolution limitations due to sputtering‐induced topography changes, thereby limiting quantification of the resultant spectra. Copyright © 2010 John Wiley & Sons, Ltd.