锗二次阴极-直流辉光放电质谱法测定高纯石英中9种杂质元素

锂、铍、硼、钠等作为高纯石英中的常见杂质元素,对产品的性能有重要影响,建立相应的测定方法至关重要。实验采用锗罩作为二次阴极,建立了直流辉光放电质谱法(dc-GDMS)测定高纯石英中锂、铍、硼、钠、镁、铝、硫、钛、铜等9种杂质元素的方法。所用锗罩的厚度为0.25 mm,罩上有4个尺寸为1 mm×8 mm的狭缝,每个狭缝间隔1 mm。实验还考察了放电参数对基体信号强度、信号稳定性、基体和锗罩信号比的影响。实验表明,当在1.3 mA/1 350 V的放电参数下,²⁸Si的信号强度可达1.3×10⁹ cps,放电稳定,硅、锗的信号比为1∶40。按照实验方法测定高纯石英样品中锂、铍、硼、钠、镁、铝、硫、钛、铜,结果的相对标准偏差(RSD,n=5)均在30%以内;还对比了锗罩、钽罩对高纯石英测定结果的影响,结果表明,由于钽罩中铜含量较大,导致铜测定结果差异较大以外,其余元素测定结果基本一致。采用锗罩测定高纯石英中杂质元素的检出限可达ng/g级别,低于采用钽罩的检出限。     

镀锡板镀层的辉光放电光谱法解析

利用辉光放电光谱法对镀锡板样品进行逐层剥离,根据样品由表至里的辉光放电积分图谱,分别设定公式积分计算镀锡板镀层厚度及质量、钝化层厚度及质量、基板成分、镀层中有害元素等。采用辉光放电光谱对镀锡板做深度-时间图,可知镀锡层的深度分辨率低于基板铁层。将方法应用于测定镀层质量、钝化层质量、基板成分(碳、硅、锰、磷、硫、镍、铬和铜)的测定,相对标准偏差分别不大于2.3%(n=10)、3.0%(n=10)、4.3%(n=5),分别将实验方法测定结果与X射线荧光光谱法(XRF)、光度法、电感耦合等离子体原子发射光谱法(ICP-AES)进行比对,结果基本一致。采用实验方法对镀锡板镀层中的有害元素进行了测定,可实现镀锡板多个检测项目的同时测定。     

辉光放电质谱分析技术的应用进展

简单介绍了辉光放电质谱(GDMS)的基本原理。对辉光放电质谱在块状金属、半导体、非导体、溶液、气体和深度分析方面的应用进行了综述。块状金属和半导体的痕量元素分析为GDMS主要的应用,它们的研究报道众多;对非导体材料的分析扩宽了GDMS的应用范围;同时尝试采用GDMS对溶液和气体样品进行分析;GDMS作为一种重要的深度分析方法,相关的应用迅速增加。最后展望了辉光放电质谱的发展趋势。     

Hydrogen diffusivity in aluminium measured by a glow discharge permeation method

The diffusion coefficient of hydrogen in aluminium has been determined in the temperature range between 446 and 681 K by a glow discharge permeation method which enables us to extend the temperature range of measurements by enhancement of the permeation flux in spite of the small equilibrium solubility of hydrogen in solid aluminium. The temperature dependence of the diffusion coefficient of hydrogen in aluminium shows a linear Arrhenius relationship with the pre-exponential factor (6.1 ± 0.5) × 10⁻⁵ m² s⁻¹ and with the activation energy (54.8 ± 0.4) kJmol⁻¹. These values are higher than those estimated by several previous authors with hydrogen evolution techniques in high temperature regions. However, the present values are well consistent with the results by Ishikawa and McLellan using an electrolytic permeation method around room temperature, suggesting that hydrogen atoms in aluminium diffuse by the interstitial mechanism in the whole temperature range.     

The application of a glow discharge mass spectrometer in the steel industry

With the VG 9000 glow discharge mass spectrometer (GDMS), major, minor, and trace elemental constituents in conducting and semiconducting materials can be measured directly. The instrument has been developed by a combination of two well founded and proven techniques; namely, a glow discharge cell for the production of ions and a double focussing mass spectrometer designed for high resolution and high sensitivity. The glow discharge cell offers the advantage that the sputtering action and the subsequent ionisation which occur, lead to minimal matrix dependency and a narrow range of sensitivity factors across the entire periodic table. The VG 9000 GDMS has been sucessfully employed to analyse a wide range of materials including steel. For most elements the detection limits are in the ppb range. Carbon, nitrogen and oxygen have been analysed successfully to ppm concentration levels. The glow discharge mass spectrometry has considerable potential for the steel industry, offering a high level of precision together with high speed of operation.     

Analysis of high-alloy steels: Mass spectra of glow discharge in argon

The types and concentrations of ion polyatomic clusters in glow discharge plasma are calculated in cathode sputtering of Kh13N10T stainless steel in argon. Mass spectra in the mass regions of elements used for microalloying of steels are interpreted. The calculations are performed for high gas background typical of pressured pellets of powder materials. The resolution of mass spectrometer that ensures the necessary detection limit for rare-earth and alkaline-earth elements, B, V, Zr, Nb, and Mo is discussed.     

辉光放电光谱分析技术的应用进展

简单介绍了辉光放电光谱(GD-OES)的基本原理。对2000-2015年间辉光放电光谱在冶金行业、环境与有机物领域以及材料表面分析方面的应用进行了综述。钢铁材料与有色金属样品的成分分析为GD-OES的主要应用,有众多的研究报道;对于环境与有机物领域中的粉末与颗粒样品、液体样品以及气体与挥发性样品,GD-OES分别有相关分析应用尝试;同时,GD-OES作为一种重要的深度分析方法,在金属合金镀层、工艺处理层、纳米级薄层、有机涂层等材料表面分析方面都有具体的应用。对GD-OES的国内外标准进行了介绍。最后展望了辉光放电光谱的发展趋势。