扫描电镜—X射线能谱法测定镀金饰品的镀层结构

介绍一种测定镀金饰品镀层结构的方法。该法可测定厚度为几十纳米的镀层成分。     

半导体光生电荷分离及迁移原位X射线光电子能谱仪表征分析系统的研制

在确保X射线光电子能谱仪（XPS）原有超高真空系统及性能指标的基础上,设计并研制出一套适用于半导体光生电荷分离及迁移的原位XPS分析测试系统.将XPS与半导体光照体系相结合,实现了外载激发光源与X射线同步照射于半导体表面,观测并记录样品中特征元素结合能峰位数据.通过对比光照前后结合能峰位变化,判定光致激发半导体材料光生电荷分离及迁移的方向及确定其量化数据.     

电子探针X射线能谱法测定黄金饰品的成色

本文介绍电子探针能谱法测定含金量５０％～９９％黄金饰品的成色，该法无损、快速、准确，对束流稳定性要求不高且操作简便。     

基于扫描电镜和能谱仪的薄膜表面形貌和厚度同时测量研究

扫描电子显微镜通过电子束轰击样品产生的二次电子、背散射电子等实现对样品表面形貌的观测,通过对样品横断面的观测来获得薄膜厚度信息,但难以实现对薄膜表面形貌和厚度的同时观测。通过能谱仪研究各种厚度的薄膜同其激发的特征X射线计数率之间的关系,实现了通过特征X射线计数率来测量薄膜厚度的方法。对于激光吹气系统所需的钨薄膜而言,结果表明,计数率随薄膜厚度的增加先线性增加后趋于稳定,利用该曲线的直线部分作为刻度曲线,可实现对5～19μm范围内钨薄膜表面形貌和厚度的同时测量,精度约为10%,通过增加电子能量可实现对更厚样品的测量。该方法可推广到其他种类的薄膜研究,有助于推动薄膜物理研究的开展。     

X射线光电子能谱仪的开放使用与管理

X射线光电子能谱仪(XPS)是材料表面元素定性和半定量分析的重要手段之一,是表面分析科研工作的必备仪器.为提高测试效率,实施了大型仪器设备开放共享优化,总结了在推动XPS开放过程中管理的经验和体会.     

SDD探测X射线中BP网络全谱定量分析技术研究

针对能量色散X荧光分析技术中面临的能谱复杂、标样难于制备、基体效应难于校正等问题,建立了基于BP神经网络的特征X射线全谱分析模型,对SDD探测器测量获得的Ti-V-Fe伪三元系样品特征X射线荧光谱进行定量分析,对含量较高的Fe元素的分析误差范围在0.06%～2.5%内,含量较低的Ti和V元素分析误差范围在0.33%～8.4%内,基本克服了由于谱峰重叠和基体效应对解谱带来的复杂性。     

田口方法在X射线荧光分析时曲线校正中的应用

根据田口玄一博士在测量工程学中提出的信噪比概念,计算了X荧光分析中某一标准曲线极限信噪比。当日常测试中系统的信噪比大于极限值时,不需要对曲线进行校正;当日常测试中系统的信噪比小于极限值时,应对曲线进行校正．以保证该测量系统工作的稳定性。     

模拟空间原子氧辐照下X射线光电子能谱仪的原位表征功能开发

对现有的X射线光电子能谱仪进行功能开发,在不改变仪器工作原理、不影响现有功能的前提下,将研制的空间交变温度原子氧辐照装置集成到其快速进样室,重点解决集群结构的匹配和性能兼容问题,实现模拟空间交变温度原子氧辐照环境下材料的原位表征功能.采用Kapton膜的质量损失方法测试空间交变温度原子氧辐照装置的原子氧通量密度,氧气流量、偏压和微波电流均对原子氧通量密度有较大影响.系统测试表明,原子氧辐照使WS 2薄膜表面发生了严重氧化,影响了薄膜的化学组成.不同温度原子氧辐照导致了不可忽略的化学组成与结构的差异.     

X射线荧光法测定氧化铁皮中硅锰磷

氧化铁皮是轧钢生产的一种产物，为了回收利用这些产物，其一般用于烧结矿生产、铁水的预处理和炼钢脱磷。氧化铁皮中的主要成分为铁、硅、磷、锰的氧化物和碳化物，直接用酸无法将其溶解。其分析方法一般均采用碱熔法分解样品，光度法测定硅、锰、磷的含量。该方法分析周期长，工作量大。本法用X射线荧光法测定氧化铁皮中硅、锰、磷，成本低、周期短、准确度高，完全能满足需要。     

Characterization of Paint by Fourier-Transform Infrared Spectroscopy,Raman Microscopy,and Scanning Electron Microscopy-Energy Dispersive X-ray Spectroscopy

The identification of automotive coatings has become important for forensic scientists to trace suspects. Popular automotive coatings include acrylic, amino, alkyd, nitro, and polyurethane paints. Various pigments and additives are added to the coatings, which may create difficulty in characterization of paint evidence. In this study, Fourier-transform infrared spectroscopy, Raman spectroscopy and scanning electron microscopy-energy dispersive X-ray spectroscopy were used to characterize an eleven-layer paint sample. Most layers were only a few micrometers thick. Infrared spectroscopy has several advantages in identifying resins and additives, while Raman is more effective in characterizing additives and inorganic pigments. Scanning electron microscopy-energy dispersive X-ray spectroscopy provides elemental analysis information. The results reveal that the combination of these techniques provides more accurate paint identification than using them separately.     

Assessment of Inorganic Fibre Burden in Biological Samples by Scanning Electron Microscopy – Energy Dispersive Spectroscopy

A method based on cloud point extraction (CPE) separation/preconcentration of trace cadmium as a prior step to its determination by graphite furnace atomic absorption spectrometry (GFAAS) has been developed. If the system temperature is higher than the cloud point temperature (CPT) of the nonionic surfactant of p-octyl polyethyleneglycolphenyether (Triton X-100), the complex of Cd²⁺ with 1-(2-pyridylazo)-2-naphthol (PAN) could be extracted into surfactant-rich phase. The chemical variables affecting CPE were evaluated and optimized. Under the optimum conditions, preconcentrating 10.0 mL of water samples permitted a limit of detection of 5.9 ng · L⁻¹ (3σ) for cadmium with an enhancement factor of 50 and a relative standard deviation of 2.1% (n = 11, c = 2.0 ng · mL⁻¹). The method was applied to the determination of cadmium in reference material and water samples with satisfactory results.     

扫描电子显微镜与扫描隧道显微镜联用装置

在ＫＹＫＹ－１０００Ｂ型扫描电子显微镜上所开发的与其联用的袖珍型扫描隧道显微镜主要有四个部分：（１）减震阻尼装置,（２）隧道探针,（３）探针扫描与逼近装置,（４）电子控制与图象采集系统。它的分辨率约为１ｎｍ,并用它观察了半导体光栅与硅上金膜的细微结构。     

单一颗粒物扫描电镜能谱定量分析方法研究

采用实测标准样品、实际样品与模拟样品相结合的方法,对文献中报导的用于定量分析单一颗粒物化学组成的Casino和Quanta计算程序进行了考察和比较。计算结果表明,在校正颗粒物粒径效应时,Casino程序显示了良好效果。Quanta程序在计算沙尘颗粒物中常见的Na、Mg、A l、S i、P、S、K、Ca、Ti、Fe等元素含量时,取得和Casino程序基本一致结果。     

扫描电子显微镜-能谱联用在鉴别药包材上的应用

开发了一种以扫描电子显微镜-能谱联用为主的药用包装材料鉴别手段. 通过扫描电子显微镜-能谱联用,联合红外分光光度计和差示扫描量热仪,对未知成分的胶塞和复合膜进行了分析鉴别,并对厚度进行了测定. 通过分析鉴别,胶塞为覆有乙烯-四氟乙烯共聚物膜的溴化丁基胶塞,覆膜厚度约为24 μm,复合膜为聚对苯二甲酸乙二醇酯/低密度聚乙烯/铝/低密度聚乙烯复合膜,厚度分别约为38、19、13、14 μm. 扫描电子显微镜-能谱联用技术可以确定未知化合物的元素组成和比例,可以解决传统鉴别手段在鉴别未知物时所遇到的瓶颈,极大地提高了鉴别效率和准确度,为鉴别药用包装材料提供了一种全新的思路.     

扫描电子显微镜在缓释微球制剂表征中的应用进展

综述扫描电子显微镜在缓释微球制剂表征中的重要应用. 采用扫描电子显微镜法对缓控释微球制剂进行表征, 采用自动颗粒粒形、粒径图像识别法对微球进行统计学分析, 对扫描电子显微镜在控释微球制剂研发过程中的4个广泛应用场景进行论证和总结. 缓控释微球制剂学是高度依赖结构学的制剂类型, 其性能和治疗功效很大程度上取决于微球的微观特性, 如结构、孔径等. 微球颗粒的尺寸及粒度分布、形状对药物释放起决定性作用. 扫描电子显微镜具有所见即所得的优势, 可以很直观的对微球颗粒的粒径、粒形以及表面粗糙情况进行快速评估. 由于微球制剂高药物载量的特点, 其批间一致性尤为重要, 科学的图像识别分析方法对批间一致性的评估具有重要应用价值. 结果表明, 扫描电子显微镜在微球的研发与生产控制中具有广泛的应用价值, 为此类型制剂的研发提供了先进的表征工具.     

Phase Recognition in AlN-Ti System by Energy Dispersive Spectroscopy and Electron Backscatter Diffraction

 The combination of energy dispersive spectroscopy (EDS) and electron backscatter diffraction (EBSD) techniques in scanning electron microscope was employed to characterize the reacted interface between Ti matrix and AlN particles. Due to the high localization of EDS and EBSD, representative measurements of chemical composition and reliable determination of the crystal structure were possible for each phase in the reaction zone with complex morphology. The TiN_1−x (cubic, NaCl type), Ti₃AlN (cubic, perovskite type) and Ti-rich Ti₃ Al (hexagonal, Ni₃Sn type) phases were identified in the reaction zone after annealing at 1100 °C. EDS+EBSD combination is an efficient tool for phase analysis at the interface in reactive multicomponent systems. Received August 21, 1999. Revision November 21, 1999.     

扫描电子显微镜和能谱分析高性能热塑性板材

高性能热塑性板材在汽车、电器、医药、建材等方面具有广泛的应用,常常添加一些功能性元素如Ti、Sb等用来提升其性能,如何快速检测其成分及含量对研究热塑性板材至关重要. 利用扫描电子显微镜/能谱仪（SEM/EDS）对高性能热塑性板材的形貌和成分进行分析,分别研究了导电处理前后对其形貌和成分测定的影响. 利用热分析技术分析了高性能热塑性板材的热力学特征. 研究结果表明,不做导电处理的高性能热塑性板材在能谱分析时被分解和升华,功能性元素消失,无法准确检测其成分及含量. 高性能热塑性板材能谱分析时做适当的导电处理为其准确地检测提供了方法和指导.     

Molecular and elemental characterisation of mineral particles by means of parallel micro-Raman spectrometry and Scanning Electron Microscopy/Energy Dispersive X-ray Analysis

The “fingerprinting” of a molecular structure obtained by micro-Raman spectroscopy (MRS) can be successfully complemented by means of X-ray spot analysis through the application of scanning electron microscopy equipped with an X-ray detector (SEM/EDX). The elemental composition revealed by SEM/EDX is essential for a correct interpretation of the collected Raman spectra. The results presented here illustrate how the two techniques can be combined to characterize geological samples, especially in the case of individual particles. The samples involved in the experiments were Zr- and Ti-bearing sand from South Africa (with major minerals such as zircon and rutile) and U mine tailings from Hungary (rich with feldspars, quartz and sulphate minerals). Mineral phases detected by MRS were identified according to their respective main Raman shifts, with a spatial resolution up to 1 μm, depending on the parameters set. Some unusual and sometimes inexplicable Raman activity was observed, which was ascribed to and rationalized by the presence of accompanying elements as detected with EDX. The relocation of a particle by means of the two instruments was facilitated with TEM grids. Although the limitations of the sequential use of SEM/EDX and MRS, such as different beam sizes, probing depth and surface topography, should be considered in their application to the analysis of individual geological particles, the two methods appeared to be complementary. Not only do they provide correlated chemical information about the sample, but also enable chemical characterization that would be otherwise incomplete when analyzed on a stand-alone basis.     

扫描电子显微镜对样品的要求及样品的制备

扫描电子显微镜对样品的要求很严,要求样品必须是固体,且做到五无:无毒、无放射性、无污染、无磁、无水分,成分稳定,块状样品大小要适中,粉末样品要进行特殊处理,对不导电和导电性能差的样品要进行镀膜,且要选择适当的镀膜仪,方能达到理想的分析效果.