Z衬度扫描透射电子显微术的前沿进展

文章介绍了Z衬度扫描透射电子显微术(Z-scanning transmission electron microscopy，Z-STEM，Z为原子序数)的最新进展：Z-STEM可以直接“观察”到晶体中原子的真实位置，Z衬度图像的分辨率在经过球差校正后可达0．6A；在利用Z衬度成像技术对材料的阴极荧光(cathodoluminescence，CL)性质的研究中，首次观察到了“死层”(dead layer)的存在．然后，文章以半导体与结晶氧化物界面结构、Al72Ni20Co8十角形准晶结构以及SrTiO3晶界结构为例，具体介绍了Z衬度成像在测定物质结构与化学组成方面独特的优势。     

碳掺杂BaTiO3的电子结构和磁性研究

基于密度泛函理论,从头计算了C间隙和替位氧掺杂立方结构BaTiO3的电子结构和磁学性质．结果表明C掺杂BaTiO3在自旋极化状态下的总能量比自旋非极化状态下的总能量小,说明C掺杂BaTiO3的基态具有铁磁性．从态密度和自旋电子密度分布可知,C位于BaTiO3间隙的磁性机理和过渡金属掺杂半导体产生磁性的机理类似：C替位掺杂BaTiO3体系磁性源于未配对的C2p电子．     

衍射增强成像原理

研究了衍射增强成像过程中X射线与样品和晶体的相互作用,重点分析了小角散射对衍射增强成像的影响,为衍射增强成像方程补充了小角散射噪声项,建立了更普遍的衍射增强成像方程.根据新的衍射增强成像方程,推导出峰位像和腰位像的吸收衬度,消光衬度和折射衬度的数学表达,并讨论了两种合成像(表观吸收像和折射像)的衬度问题. 关键词： 相位衬度成像 同步辐射 晶体衍射 X射线照相术     

La2／3—xYxCa1／3MnO3系统中Y掺杂效应研究

实验上探讨了Ｙ３＋离子掺杂对Ｌａ２／３－ｘＹｘＣａ１／３ＭｎＯ３（０＜ｘ＜０．２）单相样品的结构及其输运性质的影响．结果表明，随着Ｙ的掺杂，晶胞参数收缩，从顺磁性半导体到铁磁性金属的转变温度Ｔｃ明显降低，而巨磁阻效应却大大提高．为了探讨其物理起因，我们对Ｔｃ温度以上的导电机理通过定量分析电阻随温度的变化而得以研究，结果表明，载流子的迁移遵从跳跃方式而不是热激活形式，在此基础上对Ｙ掺杂作用进行了讨论．     

测定微小晶体结构的电子晶体学图像处理技术

介绍了2005年国家自然科学奖二等奖获奖项目“微小晶体结构测定的电子晶体学研究”，研究目的是建立一种借助高分辨电子显微像测定晶体结构的新方法．为此提出了高分辨电子显微学与衍射晶体学相结合的思想，在实现此思想的过程中，研究了像衬的规律，得出实用的像衬公式和理论，阐明了不同种类原子像衬与晶体厚度的关系，而且用理论指导实验，观察到晶体中锂原子的像衬，以此理论为依据，把衍射晶体学中的多种分析方法特包是直接法引入到高分辨电子显微学中，建立了一套全新的电子晶体学图像处理技术，开发了相应的可视化专用软件包，并应用于测定多个未知晶体结构．文中逐一介绍了研究工作全过程的关键问题和研究结果。     

优化X射线同轴相位衬度成像的理论研究

采用同轴相位衬度成像方法，基于PGW理论获得的频域相位衬度传递函数，对于理想光源和多色X射线源，用计算机模拟分析了如何选择物像距离和空间频率以获取最佳相位衬度像。实际应用中要综合考虑具体成像实验装置对于物像距离的可调范围以及成像分辨率的要求。对于具有一定谱宽的X射线源，应选择谱宽尽量小的源，以获得含信息量丰富、分辨率高的图像。     

调控硼硫掺杂比实现金刚石n型转变的研究

金刚石半导体由于其特殊的机械性能使其在极端环境下有较广的应用前景. 虽然通过硼(B)元素掺杂较易得到p型金刚石半导体,但具有优异电学性能的n型半导体却鲜见报道. 硼、硫（S）原子因半径及外层电子互补,其协同掺杂易合成p型或n型半导体,但其物理机理尚不清晰.在课题组已有实验报道基础上,借助第一性原理探究了B-S不同比例单掺杂及共掺杂金刚石的形成能、晶体内的存在形式及电子结构,从原子尺度揭示了金刚石由p型向n型半导体转变的阈值掺杂比例. 通过实验与理论的对比发现B在晶格内趋向团聚,而过量的S掺杂则发生析出.     

溶胶凝胶合成锰掺杂ZnO的室温磁性行为

通过溶胶凝胶自燃法合成锰掺杂氧化锌纳米晶体, 研究了Mn掺杂ZnO稀磁半导体(简称DMS)的性质．X射线衍射光谱表明,锰掺杂氧化锌保留纤锌矿型状氧化锌六角晶体结构．采用能量色散X射线能谱和扫描电子显微镜分别对成分和形态进行研究．温度依赖的电阻率显示了DMS的半导体材料行为．振动样品磁强计测定的室温磁性行为,揭示了锰掺杂氧化锌的铁磁性和反磁性特性.     

同步辐射计算机断层技术衬度误差机理分析

基于同步辐射X射线的优越特性及计算机断层重建技术对材料无损检测等优点，同步辐射计算机断层重建技术已被广泛应用.对该技术衬度误差的形成机理及形式进行了分析研究，并给出了四种基本误差形式.数值模拟结果证实了分析的正确性. 关键词： 同步辐射 计算机断层 衬度误差     

磁衬度的高压扫描电子显微镜观测

在磁性材料的研究中,磁畴的电镜观测是人们很感兴趣的问题[1]. 利用扫描电镜可以观测到磁性材料的两种磁衬度(图1).第一种磁衬度首先由Joy和Jakubovics利用二次电子信号观测到[3].引起这种磁树度的原因是磁性材料存在着漏磁场.漏磁场引起试样表面发射的二次电子轨道的改变,由于从磁性相反的磁畴中探测到二次电子的效率不同,从而引起磁衬度.由单轴各向异性的磁性材料(如钻和磁泡材料)可得到这种磁衬度[见图1(a)]. 第二种磁衬度首先由Philibert和Tixier[3]利用试样电流得到.以后,更多的研究工作者用背散射电子观测到这种磁树度.这种磁衬度产…     

Formation of cations and anions upon electron interaction with (doped) helium droplets

Superfluid helium droplets have provided a new perspective for studying electron induced chemistry at extremely low temperatures. Helium droplets represent an ideal environment for the formation of novel and exotic agglomerates of atoms and molecules. Mass spectrometry can be used to detect the resulting ions formed upon electron ionization and electron attachment to doped droplets. In the case of electron ionization a helium atom of the droplet is ionized initially and after few resonant charge transfer reactions between helium atoms the charge finally localises on the dopant. An alternative process is Penning ionization of the dopant, where the scattered electron first electronically excites a helium atom on the surface of the droplet. The attachment of a low energy electron leads to formation of an electron bubble inside the droplet which decays by autodetachment or localization on a dopant, if present in the droplet. In the present minireview a general overview about the field of electron scattering with doped helium droplets is given and a presentation of important recent results related to these electron collision studies is given as well.     

Some aspects of scanning electron microscopy

The main components of the SEM are the signal generation and the signal detection and display systems. A finely focussed electron beam scans the specimen surface. Due to the interaction between electrons and solid, signals such as secondary emission, light, X-radiation and currents are generated. Depending on the selected detection system the displayed images provide a variety of information, such as topography, element distribution, surface voltage, luminescence, conductivity, etc. The useful application of the SEM ranges from surface study to bulk analysis to device fabrication.     

Dopant profiling in silicon nanowires measured by scanning capacitance microscopy

Silicon nanowires (SiNWs) with axial doping junctions were synthesized via the Au‐catalyzed vapor–liquid–solid growth method with the use of HCl. In this work, dopant profiling from three axially doped SiNWs with p–i, p–n and n–i–p junctions were investigated using both scanning electron microscopy (SEM) and scanning capacitance microscopy (SCM). It turns out that observed doping contrasts in SEM are also affected by the surface roughness and sample charging. In contrast, SCM allows us to delineate with sub‐10 nm resolution the electrical junctions and provides a relative value of the doping concentration in each segment of the NW. SCM clearly evidences the expected doping regions within these SiNWs thanks to the addition of HCl during the growth that strongly prevents shell overgrowth. (© 2014 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Control of morphology and dopant distribution in yttrium-doped ceria nanoparticles

The morphology and distribution of dopant in yttrium-doped ceria (YDC) nanoparticles prepared by spray pyrolysis were characterised by transmission electron microscopy and X-ray energy dispersive spectroscopy (XEDS), respectively. By combining the XEDS analysis and concentration distribution modelling, accurate yttrium dopant concentration variation from the particle center to the surface can be determined. It is shown that by appropriately selecting cerium precursors, the yttrium dopant distribution in YDC nanoparticles can be controlled. Uniform yttrium distribution in the YDC particles has been achieved, which is important to decrease probability of yttrium cluster segregation to improve oxygen ion conductivity in solid oxide fuel cell electrolytes. This control is based on the suggested mechanism of dopant distribution which proposes that hydration energies influence diffusion rates of the precursors during preparation process. In addition, the morphology (solid spherical, hollow spherical and hollow concave) formation mechanisms of the YDC particles from different cerium precursors are discussed.     

Improving dopant incorporation during femtosecond-laser doping of Si with a Se thin-film dopant precursor

We study the dopant incorporation processes during thin-film fs-laser doping of Si and tailor the dopant distribution through optimization of the fs-laser irradiation conditions. Scanning electron microscopy, transmission electron microscopy, and profilometry are used to study the interrelated dopant incorporation and surface texturing mechanisms during fs-laser irradiation of Si coated with a Se thin-film dopant precursor. We show that the crystallization of Se-doped Si and micrometer-scale surface texturing are closely coupled and produce a doped surface that is not conducive to device fabrication. Next, we use this understanding of the dopant incorporation process to decouple dopant crystallization from surface texturing by tailoring the irradiation conditions. A low-fluence regime is identified in which a continuous surface layer of doped crystalline material forms in parallel with laser-induced periodic surface structures over many laser pulses. This investigation demonstrates the ability to tailor the dopant distribution through a systematic investigation of the relationship between fs-laser irradiation conditions, microstructure, and dopant distribution.     

Inelastic electron tunneling spectroscopy: Intensity as a function of surface coverage

Inelastic election tunneling spectroscopy (IETS) is a sensitive technique for obtaining vibrational spectra of molecules adsorbed on an oxide surface and incorporated into a metal-oxide-metal tunnel junction. IETS energy data are used routinely. However, IETS intensities contain additional information which, for theoretical and experimental reasons, has not been used systematically. This paper examines the variation of IETS intensity with surface coverage of dopant molecules in the junction, a relationship of practical and theoretical importance. IET spectra are taken using standard experimental techniques and a liquid doping technique which allows the surface coverage to be determined independently. From an analysis of a large number of modes of benzoic acid on alumina, it is found that IETS intensity, defined in the usual way as the normalized change in conductance, $\text{Δ σ}\text{σ}$, is a nonlinear function of surface coverage. A physical model is presented which attributes this behavior to a difference in elastic tunneling conductances through empty or filled regions of the dopant layer in a junction with a fraction of a monolayer coverage. In addition, the liquid and vapor doping techniques in common use in IETS are discussed in terms of statistical mechanics and are shown to be manifestations of the same basic phenomenon.     

Confocal laser scanning microscopy and scanning electron microscopy of tissue Ti-implant interfaces.

Microscopic inspection of heterogenous three-dimensional (3D) objects such as oral implants, or implants in general, is conventionally performed either on ground sections of methyl-metacrylate-embedded material, at the cellular level by histologic analysis of the peri-implant tissue by light microscopy (LM), or at the supramolecular level by transmission electron microscopy (TEM). Alternatively, the architecture of the tissue/implant interface is visualized by scanning electron microscopy (SEM). The two approaches exclude each other because of the sample preparation.We elaborate conditions for the non-invasive analysis of tissue/implant interfaces by confocal laser scanning microscopy (CLSM) in buffer, hoping to obtain a 3D view of fluorescently labeled tissue constituents at the tissue implant interface and, through subsequent SEM, of the metal surface. The use of water-immersion objectives, originally developed for high LM under physiological conditions is essential.In an exploratory approach, the tissue/Ti-interfaces of two retrieved dental implants were analyzed. One was a step-cylinder used for orthodontic anchoring and the other was an endosseous step-screw implant retrieved after infection-related loosening prior to load. The adhering tissue fragments were fluorescently triple-labeled for actin, fibronectin, and sm-alpha-actin. Optical sections for fluorescent images and for the laser reflection map were registered concomitantly. This approach allowed the labeled structures to be located on the metal surface. Subsequently, the same implants were prepared for SEM of the tissue/implant interface, and upon removal of the adhering structures, of the underlying metal surface. Thus, specific proteins can be identified and their spatial architecture as well as that of the underlying metal surface can be visualized for one and the same implant. The immediate visualization after fluorescence labeling in buffer by means of water immersion objective lenses proved most critical.     

Study of temperature effects on the conduction and trapping of charges in the alkali-silicate glass under electron beam irradiation

A scanning electron microscope (SEM) is employed to investigate the temperature effect on the charging behaviour of alkali-silicate glasses under electron beam irradiation using electrostatic influence method (EIM). A modified special arrangement adapted to the SEM allows to study charging mechanisms and charge transport characteristics of these glasses using the simultaneous measurement of displacement and leakage currents. The trapping process during continuous electron irradiation can be directly determined by the EIM. The experimental results reveal that the charging ability of glasses decreases with increasing temperature. The variation of charge process has been confirmed by measuring the surface potential in response to the sample temperature. In this report, we introduce also the secondary electron emission (SEE) yield. It was found the strong dependence of the SEE yield on the temperature variation. The higher is the temperature and the lower is the SEE yield. The trapping ability is analyzed taking into account the regulation mechanisms involved under electron irradiation.     

High resolution quantitative SIMS analysis of shallow boron implants in silicon using a bevel and image approach

Secondary ion mass spectrometry (SIMS) is frequently used as the preferred tool for dopant profiling due to its sensitivity and depth resolution. However, as dopant profiles become shallower most, if not all of the implant profile lies in the pre-equilibrium or transient region of an SIMS depth profile. In this region sputter yield and ionisation rate vary making accurate quantification of the implant profile very difficult. These problems can be reduced through the use of much lower beam energies or oxygen flooding of the sample. However, most SIMS instruments do not have these capabilities. In this paper an alternative technique for producing an accurate depth profile of a shallow implant, using existing SIMS technology is presented.Through the fabrication of bevels with very small slope angles on a shallow boron implanted silicon via a chemical etch, SIMS ion imaging is performed on the exposed surface. Ion image data is then summed, and in conjunction with accurate measurement of the bevel morphology, a shallow boron implant profile produced. The ‘bevel-image’ profile compares very well with a profile obtained using a 1 keV oxygen beam. To ensure a good dynamic range on the ‘bevel-image’ profile it is important to clean the bevel with a HF etch, prior to imaging.     

Defects in III–V semiconductor surfaces

This work reports the measurement of the nano-scale physical properties of surface vacancies and the extraction of the types and concentrations of dopant atoms and point defects inside compound semiconductors, primarily by cross-sectional scanning tunneling microscopy on cleavage surfaces of III–V semiconductors. The results provide the basis to determine the physical mechanisms governing the interactions, the formation, the electronic properties, and the compensation effects of surface as well as bulk point defects and dopant atoms. Received: 10 May 2001 / Accepted: 23 July 2001 / Published online: 3 April 2002