Estimation of detection limits in electron probe X-ray microanalysis

Different local methods of analysis are estimated with the aim of revealing the possibility for determining the minimum concentrations of chemical elements. Among all examined approaches, electron probe X-ray microanalysis (EPMA) has been chosen as the most accurate and promising technique. The dependences between the elemental detection limit and the analyzer??s technical parameters are investigated. It has been ascertained that the experimentally determined detection limits of light elements are substantially higher than those of heavy elements. The reasons leading to the less efficient EPMA of light elements, as well as possible ways of elimination thereof, are discussed. It is demonstrated that an X-ray mirror can be used to reach the theoretically predicted detection limits of B, O, and C.     

Methods for quantitative electron probe microanalysis of small particles and thin films

The application of the electron probe microanalyzer to quantitative determination of the thickness and composition of thin films and the composition of small particles is described. The key element in these applications has been the development of accurate predictive models for the depth distribution of X-ray production (θ(ϱz) curves). The sensitivity for most elements in the periodic table is less than one monolayer based on modest electron beam currents and analysis times. By measuring intensities as a function of electron energies, the determination of concentration gradients is also possible.     

X-ray microanalysis of uranium dioxide particles by using low electron beam energy

The elemental analysis results of the various size uranium dioxide fragments, performed with a scanning electron microscope (SEM) equipped by X-ray energy dispersive analyzer (INCA x-act, “Oxford Instruments”, Great Britain), are presented. The elemental composition calculation was carried out applying the pre-installed program based on the XPP matrix correction algorithm. It is shown that for the bulky UO₂ samples, measured with the varied accelerating voltage in range of 6–20 kV, the uranium concentrations slightly differ (relative uncertainties doesn’t exceed ±2%). The composition of uranium dioxide particles sized up to 0.5 μm can be defined using beam energy of 6 keV with typical for bulky sample accuracy.     

Monte Carlo calculation using a personal computer for electron probe microanalysis

Monte Carlo simulation for calculating x‐ray spectra under electron impact is carried out by a personal computer. Reduction of the CPU time by reducing the number of incident electrons for calculation is performed. One of the methods used to reduce the number of incident electrons to obtain the results within an acceptable error is provided. We limit the present report to five typical compounds: an oxide (Al₂O₃), a nitride (TiN), a carbide (Al₄C₃), a light–light element compound (BN), and a heavy–light element compound (PbS). We calculate the relative x‐ray intensity generated from the five compounds listed above with the change of the number of the incident electrons. The calculated x‐ray intensity is then converted into the mass % by the ZAF method. Comparisons are made between the calculation and experiment for Al₄C₃ and PbS. It is found that the present Monte Carlo method is useful for investigating a relationship between the number of incident electrons and the acceptable error. The results of 150 incident electrons can be applied in practical analysis, and the calculation time is less than 2 min. Copyright © 2004 John Wiley & Sons, Ltd.     

X-ray microanalysis of quaternary semiconductor solid solutions and its application to the (SnTe-SnSe):In system

A reliable technique of local chemical characterization of multicomponent semiconductor solid solutions has been developed, and the possibility of its application to the SnTe-SnSe quaternary solid solutions doped with 16 at.% In verified. The behavior of the electrical resistivity of samples of these solid solutions at low temperatures, 0.4–4.2 K, has been studied. The critical temperature T _c and the second critical magnetic field H _c2 of the superconducting transition and their dependences on the solid-solution composition have been determined. The superconducting transition at T _c≈2–3 K is due to hole filling of the In-impurity resonance states, and the observed variation of the superconducting transition parameters with increasing Se content in the solid solution is related to the extrema in the valence band and the In band of resonance states shifting with respect to one another. Fiz. Tverd. Tela (St. Petersburg) 41, 612–617 (April 1999)     

Invariant embedding approach for electron probe microanalysis. Tilt factor,atomic number and energy of the incident electrons

Electron probe microanalysis (EPMA) is a well‐established and practical technique for the microchemical analysis of materials. Although the physical processes that take place in microprobe analysis are relatively well understood, most of the commercially available approaches for data correction are still empirical or semi‐empirical or make use of numerical calculations. Recently, a so‐called Invariant Embedding Approach to Microanalysis, which is free of the disadvantage of the empirical methods, has been reported. This paper critically assesses the capabilities and limitations of this new approach when different values for the energies of the incident electrons, the atomic number and size and the sample tilt are considered. The theoretical results follow the general trends of the experimental data and Monte Carlo calculations, although a more in‐depth study of the physical parameters involved in the model is still needed. Copyright © 2005 John Wiley & Sons, Ltd.     

Resonant laser ablation of copper and its application in microanalysis

Resonant laser ablation (RLA) is a two-step process, occurring within a pulse of a tunable laser, in which the leading edge of the laser pulse ablates a solid surface to produce neutral atoms or molecules that are then resonantly ionized by the trailing edge of the same laser pulse. The sensitivity and selectivity of RLA allow detection and quantitation at very low concentrations. In our preliminary RLA research, a sub-ppm detection level has been reached for copper in a standard aluminium sample. In addition, the threshold and saturation effects of RLA have been observed.     

Kelvin probe force microscopy and its application

Kelvin probe force microscopy (KPFM) is a tool that enables nanometer-scale imaging of the surface potential on a broad range of materials. KPFM measurements require an understanding of both the details of the instruments and the physics of the measurements to obtain optimal results. The first part of this review will introduce the principles of KPFM and compare KPFM to other surface work function and potential measurement tools, including the Kelvin probe (KP), photoemission spectroscopy (PES), and scanning electron microscopy (SEM) with an electron beam induced current (EBIC) measurement system. The concept of local contact potential difference (LCPD), important for understanding atomic resolution KPFM, is discussed. The second part of this review explores three applications of KPFM: metallic nanostructures, semiconductor materials, and electrical devices.     

An upgraded external beam PIXE setup for multielemental analysis of atmospheric aerosol samples

The external beam particle‐induced X‐ray emission (PIXE) setup has been upgraded by introducing a new silicon drift detector with the aim of obtaining better minimum detection limits (MDLs) at the 2 × 1.7 MV Tandetron accelerator of the Beijing Normal University in China. The upgraded external beam PIXE setup is equipped with two silicon drift detectors for PIXE analysis of low and high Z elements. A surface barrier detector for Rutherford backscattering spectrometry monitors beam and helium flow. Two kinds of aerosol filter samples (quartz fiber filters and Teflon filters) were studied. A 200‐μm thick Mylar absorber in front of the medium‐high energy X‐rays detector was adopted, and it got the best MDLs for atmospheric aerosol samples analysis. Multielemental analysis of quartz fiber filter aerosol samples was achieved. For more accurate and better MDLs of low Z elements in PIXE analysis, it is necessary to keep sufficient helium flow behind the thin samples.     

X射线波带片的制作及其应用

波带片的低衍射效率限制其在可见光波段的使用,可是在Ｘ射线波段,波带片是唯一达到衍射极限的光学元件,因而引起人们的极大兴趣。本文介绍了当前国际上Ｘ射线波带片的主要制作方法及其应用,同时回顾了用于Ｘ射线聚焦、成像的光学元件——Ｘ射线菲涅耳波带片及近几年才出现的布拉格－菲涅耳波带片的历史背景、基本概念和主要类型。     

一种X射线聚焦光学及其在X射线通信中的应用

基于栅控脉冲发射X射线源与单光子探测技术的X射线通信已经实现了实验室语音通信验证,并对通信系统的误码率性能进行了分析,为探索未来X射线深空应用打下了坚实的基础.针对目前X射线通信面临的信号发散角大、通信距离短、难以实现工程化应用的情况,迫切需要对X射线通信天线系统进行深入研究.为了提高信号增益、增大X射线通信的距离,提出了多层嵌套式X射线聚焦光学作为X射线通信的"收发天线",理论分析了X射线聚焦光学用于X射线通信"收发天线"的可行性,分析了X射线聚焦光学的理论基础与结构设计,对"发射天线"发散角、"接收天线"有效面积与焦斑尺寸、信号增益等性能做了探讨.结果表明:在信号发射端,"天线"的发散角为3 mrad左右,发射增益23 d B;在信号接收端,"接收天线"的有效面积5700 mm2@1.5 keV,焦斑直径为4.5 mm,接收增益为25 d B,通信系统总的增益可达48 d B.     

大气颗粒物滞留时间的确定方法及初步实验验证

通过研究大气颗粒物中222Rn子体活度比与颗粒物平均寿命之间的关系,建立了基于活度比估算大气颗粒物滞留时间(residence time of atmospheric aerosol,RTAA)的方法,并在相对理想条件下进行了实验验证.当氡室浓度稳定为1.816kBq/m3时,由214Bi/214Pb活度比计算出的RTAA为112.17min,与氡室的平均换气时间(104.17min)相当,表明大气颗粒物中同一衰变链上的放射性核素活度比(如214Bi/214Pb,210Bi/210Pb或210Po/210Pb)可以用于估算RTAA.     

微波共振探针及其在等离子体诊断中的应用

介绍了能够测量稳定和时变等离子体电子密度的微波共振探针,给出了其工作原理和在测量稳定、时变和瞬态等离子体电子密度中的应用。分析了传输模式和反射模式的工作过程及对测量范围、测量精度和空间分辨率等影响因素。结果表明,选用较长的探针有利于提高电子密度的测量范围和精度;选用的微波扫频源高端频率越高,频率分辨率越高,则电子密度的测量范围越大,测量精度越高。理论分析得出系统可测量的电子密度约为1.37×10⁸~4.1×10¹¹cm^-3。     

Characterization of compositional particles in eye shadow powder by scanning electron microscope and X-ray mapping

We developed an analysis method to evaluate the size and shape of particles of eye shadow cosmetics by applying the scanning electron microscopy (SEM) combined with the energy-dispersive spectroscopy (EDS). Backscattered electron (BE) and X-ray mapping images from the SEM-EDS measurements were interpreted to identify the size and shape of powder particles according to different factors such as 9 size and 5 shape indices established in this work. By using the developed method, we could classify the inorganic and organic particles of the eye shadow powder by composition, which can contribute to improving the product quality.