大角度会聚束电子衍射的新方法

会聚束电子衍射是测定晶体点群、空间群的有效方法。要清楚地判断会聚束电子衍射图样的对称性,电子束的会聚角要大,但衍射盘不能重叠。本文提出了一种新方法来获得不重叠的大角度会聚束电子衍射。新方法是使电子束离焦,固定样品,从而保留了样品的同心倾动位置,作大角度倾动时不会失去原来感兴趣的区域。新方法在原理上和田中等人提出的方法相同,但优越性更大。同时也研究了大束斑(≥2μm)大角度会聚束电子衍射。 关键词：     

On the temperature dependence of positron lifetimes in tin and the transition from theβ- to theα-phase

The N₂, O₂, H₂O, and CO₂ molecules that have condensed on the surface of a pyroelectric tourmaline crystal were degassed successively by means of electron bombardment. The temperature dependence of the electrostatic field strength on the specimen surface was observed by electron diffraction; it decreased as the degassing advanced. The tourmaline surface behaved as a gas Chromatographic adsorbent.     

Enhancement of second harmonic generation efficiency: Growth and characterization of magnesium(II)-doped tetrakis(thiourea)nickel(II) chloride crystals

The influence of magnesium doping on the properties of tetrakis(thiourea)nickel(II) chloride crystals has been described. The reduction in the intensity observed in powder X-ray diffraction of doped specimen and slight shifts in vibrational frequencies confirm the lattice stress as a result of doping. Surface morphological changes due to doping of the alkaline earth metal are observed by scanning electron microscopy. The incorporation of Mg(II) into the crystal lattice was confirmed by energy dispersive X-ray spectroscopy. Lattice parameters are determined by single crystal XRD analysis. The thermogravimetric and differential thermal analysis studies reveal the purity of the materials and no decomposition is observed up to the melting point. The crystal is further characterized by Kurtz powder technique and dielectric studies.     

Transmission electron microscopy of fine aromatic hydrocarbon particles

Fine perylene and pyrene particles were produced by evaporation in helium gas. The particles were sensitive to electron beam radiation. The pyrene particles sublimed under observation. These difficulties were cleared up by reducing electron beam exposure and sandwiching a specimen between two Formvar films. The fine perylene particles were rectangular or hexagonal plates about 50nm thick. The size was about 200-2000nm. The fine pyrene particles were polymorphic with a size of about 300-2000nm. The crystal forms of the perylene and pyrene particles were determined from the electron diffraction patterns to be alpha-perylene and pyrene I, respectively.     

Mesoscale strain measurement in deformed crystals: A comparison of X-ray microdiffraction with electron backscatter diffraction

Mapping of residual stresses at the mesoscale is increasingly practical thanks to technological developments in electron backscatter diffraction (EBSD) and X-ray microdiffraction using high brilliance synchrotron sources. An analysis is presented of a Cu single crystal deformed in compression to about 10% macroscopic strain. Local orientation measurements were made on sectioned and polished specimens using EBSD and X-ray microdiffraction. In broad strokes, the results are similar to each other with orientations being observed that are on the order of 5° misoriented from that of the original crystallite. At the fine scale it is apparent that the X-ray technique can distinguish features in the structure that are much finer in detail than those observed using EBSD even though the spatial resolution of EBSD is superior to that of X-ray diffraction by approximately two orders of magnitude. The results are explained by the sensitivity of the EBSD technique to the specimen surface condition. Dislocation dynamics simulations show that there is a relaxation of the dislocation structure near the free surface of the specimen that extends approximately 650 Å into the specimen. The high spatial resolution of the EBSD technique is detrimental in this respect as the information volume extends only 200 Å or so into the specimen. The X-rays probe a volume on the order of 2 µm in diameter, thus measuring the structure that is relatively unaffected by the near-surface relaxation.     

Ultra-precision machining induced phase decomposition at surface of Zn-Al based alloy

The microstructural changes and phase transformation of an ultra-precision machined Zn-Al based alloy were examined using X-ray diffraction and back-scattered electron microscopy techniques. Decomposition of the Zn-rich η phase and the related changes in crystal orientation was detected at the surface of the ultra-precision machined alloy specimen. The effects of the machining parameters, such as cutting speed and depth of cut, on the phase decomposition were discussed in comparison with the tensile and rolling induced microstrucutural changes and phase decomposition.     

Magnetostriction of a single crystal of nickel observed with an X-ray four-circle goniometer

We proposed a technique to observe magnetostrictive coefficients of a single crystal specimen with X-ray diffraction. An angle between a direction of crystallographic orientation and a direction of magnetic field could be estimated with two kinds of diffraction peaks which were found with an X-ray four-circle goniometer. The magnetostriction was measured by a shift of Bragg angle. This technique was suitable for a case to observe the magnetostrictive coefficient which varied as a function of the magnetic field direction. We applied the technique to a single crystal specimen of nickel and showed dependences of the magnetostriction on the magnetic field strength and its direction around an axis of easy magnetization at room temperature.     

静电场作用下α-LiIO3单晶的光衍射增强现象的弛豫行为和“低温冻结”

在以前工作的基础上,利用在频率平面上进行空间滤波的方法,研究了α-LiIO₃单晶在静电场作用下,空间电荷分布引起的衍射光强变化的弛豫行为。得出了弛豫过程的唯象表达式,发现其中的弛豫参数依赖于温度和电压的大小以及所加电压为同号或异号电压,且随样品的不同而变化。在低温下,衍射会被“冻结”:即在“冻结”温度(～-25℃)以下加电压,衍射增强不显著;在“冻结”温度以上加电压,然后降至“冻结”温度以下,衍射光强度仍保持高温时增强后的数值;撤去电压,因加电压所增加的衍射并不消失。 关键词：     

Anomalously large changes in diffracted X-ray intensity from silicon single crystals produced by microwave fields

Results of a high resolution X-ray diffraction study of effects produced by microwave fields of frequency 2.45 GHz in silicon single crystals are reported. Microwaves travelled along a strip line evaporated along a diameter of the specimen crystal disc, which was aligned for diffraction from a desired set of lattice planes. Diffraction curves and high resolution traverse topographs were recorded and curvature measurements were made before, during and after application of the microwave field. An anamalously large increase in diffracted X-ray intensity from a large volume of the specimen was observed on application of the microwave field. The peak intensity in some cases increased by more than ten times. Integrated intensity also showed similar large changes. No significant change in the shape of the diffraction curves was observed upto microwave powers of ～10W. Some regions of the crystals showed a large decrease in intensity. High resolution traverse topographs directly showed the changes in intensity. Also, dot like defects were observed. Most of these changes were reversible. However, some irreversible effects were observed which suggest the possible use of this method in microwave field/power measurement as well as dosimetry. The observed effect could be due to influence of the field on the dispersion surface or due to strong interaction of the field with electron cloud of silicon atoms.     

Analysis of thermal effects accompanying the interaction of electron beams with ferroelectric crystals

A spatial nonstationary temperature distribution in a model ferroelectric specimen exposed to electron beams of a scanning electron microscope (SEM) is simulated. A solution to the problem on the effect of focused heat sources having different configurations on a single ferroelectric crystal and crystal with electrodes deposited on its faces is presented. The model is based on the finite-difference method. A program for calculating temperature fields and maximum overheating temperature for preset specimen characteristics and experimental parameters of different scanning electron microscopes is suggested.     

On the oxidation of CaF2 in transmission electron microscope

Electron stimulated oxidation of CaF₂ in transmission electron microscope has been thoroughly studied using various electron microscopy techniques, including imaging, electron diffraction and electron energy-loss spectroscopy. It found that the electron irradiation induced CaO locate on the edge of specimen. The oxidation process is associated with desorption of F by electron irradiation, and originates from O impurities in the specimen. Driven by electric field produced by electron irradiation, the O ions inside bulk diffuse to the edge region, occupying the interstitials of metallized Ca lattice. Therefore, the accumulation of O along the edge of specimen results in forming CaO.     

二维X射线衍射及其应用研究进展

介绍了三维、一维和二维X射线衍射的有关概念,给出二维X射线衍射的定义:在X射线衍射实验中使用二维探测器,并对由二维探测器记录的二维象、二维衍射花样的数据进行处理分析和解释的X射线衍射方法称为二维X射线衍射术。之后,分四部分综述二维X射线衍射(2D-XRD)和散射及其应用的进展。1)单晶样品的二维衍射包括经典的劳厄法定向和用二维探测器(带衰减底片组件、CCD和IP等)的劳厄法测定晶体结构的单晶样品现代二维衍射术;2)随后,评述多晶样品二维衍射的衍射几何、实验装置,以及在物相鉴定、应力测定和织构测定方面应用的方法和基本公式;3)二维小角散射(2D-SAXS)也作了简介。4)把一维和二维衍射术作了较全面的比较和综合评论。     

二维X射线衍射及其应用研究进展

介绍了三维、一维和二维X射线衍射的有关概念,给出二维X射线衍射的定义:在X射线衍射实验中使用二维探测器,并对由二维探测器记录的二维象、二维衍射花样的数据进行处理分析和解释的X射线衍射方法称为二维X射线衍射术。之后,分四部分综述二维X射线衍射(2D-XRD)和散射及其应用的进展。1)单晶样品的二维衍射包括经典的劳厄法定向和用二维探测器(带衰减底片组件、CCD和IP等)的劳厄法测定晶体结构的单晶样品现代二维衍射术;2)随后,评述多晶样品二维衍射的衍射几何、实验装置,以及在物相鉴定、应力测定和织构测定方面应用的方法和基本公式;3)二维小角散射(2D-SAXS)也作了简介。4)把一维和二维衍射术作了较全面的比较和综合评论。     

Studies on the optical and dielectric properties of a zinc thiourea chloride NLO single crystal

Single crystals of a nonlinear optical material, zinc thiourea chloride were grown by the slow evaporation technique. The crystal structure and lattice parameters of the grown crystal were determined by the single crystal X-ray diffraction studies. The single crystal XRD revealed that the material crystallized in a orthorhombic crystal system. Optical studies were carried out and it was found that the tendency of transmission observed from the specimen, with respect to the wavelength of light, is practically more suitable for opto-electronic applications. The optical band gap is found to be 4.30 eV. Optical constants such as the band gap, refractive index, reflectance, extinction coefficient and real (?_r) and imaginary (?_i) components of the dielectric constant and electric susceptibility were determined from the UV–vis–NIR spectrum. The dielectric constant and dielectric loss of zinc thiourea chloride were measured in the different frequency range from 50 Hz to 5 MHz at different temperatures. Further, electronic properties, such as valence electron plasma energy, Penn gap, Fermi energy and electronic polarizability of the grown crystal have been estimated.     

Messung der Elektronenbeugungsintensitäten polykristalliner Aluminiumschichten bei tiefer Temperatur und Vergleich mit der dynamischen Theorie

By means of a retarding field apparatus the electron diffraction intensities of a polycrystalline Aluminium-foil have been measured for different electron energies between 17 and 50 kev. The specimen was kept at 154 °K and the thickness of the crystallites was about 280 Å. It has been shown that the high index reflections behave kinematically, while the first order reflections [e.g. (111), (200)] are much influenced by dynamical extinction effects which can be explained very well by the dynamical two beam approximation. Also the intensities of the higher orders [e.g. (222), (400)] of the strong reflections show marked deviations from the kinematical values. This intensity deficit can be interpreted by multiple scattering processes due to systematic interactions. The experimental results are compared with the second Bethe approximation (introduction of dynamic potentials) as well as with the second Born approximation where double scattering processes within the crystal are taken into account.     

Measurement of orientation crystallization rates of linear polymers by means of dynamic X-ray diffraction technique. II. Frequency dispersion of strain-induced crystallization coefficient of natural rubber vulcanizates in subsonic range

The orientation crystallization behavior of natural rubber vulcanizates was investigated by means of a dynamic X-ray diffraction technique utilizing the half-circle sector technique. The frequency dependence of dynamic diffraction intensities from diatropic and paratropic crystal planes, (002) and (200) planes, was observed over a frequency range from 10^?3 to 10¹ Hz as a function of temperature, degree of cross-linking, static extension ratio, and dynamic strain amplitude.

The frequency dependence of the dynamic X-ray diffraction gives two dispersion regions around 10^?2 and 10^?1 Hz. The phase angle between the dynamic X-ray diffraction and dynamic strain of a bulk specimen is definitely positive; i.e., the dynamic strain of the specimen is always behind the dynamic orientation crystallization.

The frequency dispersion at low frequencies, around 1WZ Hz is very obvious for the (200) crystal plane and shifts somewhat to higher frequencies under those conditions that increase the mobility of self-diffusion of rubber molecules, i.e., increase of temperature and decreases of extension ratio and degree of cross-linking. The frequency dispersion at high frequencies, around 10¹ Hz, is rather obvious for the (002) crystal plane and does not shift appreciably under the experimental conditions.     

纳米云纹法条纹倍增技术研究

提出了一种纳米云纹法的条纹倍增技术，可用于单晶材料纳米级变形测量.在测量中，单晶材料的晶格结构由透射电镜（TEM）采集并记录在感光胶片上作为试件栅，几何光栅作为参考栅.对纳米云纹条纹的形成原理，透射电镜放大倍数与试件栅的频率关系，条纹倍增技术，位移、应变测量方法等进行了详细讨论.该方法不仅能够测量连续力学参量，如应变和位移，而且能够表征纳观非连续参量，如位错、夹杂.     

On a new technique of small angle electron diffraction

The article deals with a new arrangement of the optical system of a transmission electron microscope used for small angle diffraction. The technique is based on a strong underfocussing of the objective lens and the focussing of a demagnified image of the cross-over in the object plane of the objective lens. An electron image of the specimen area from which the diffraction pattern is formed can be obtained together with the selection of the area. The attainable results are discussed using the Tesla BS 413 electron microscope as an example.     

A modified Marton-type electron interferometer

It is shown that the original Marton-type electron interferometer is based on the Fresnel diffraction of two coherent beams by a crystal. The modified Marton-type electron interferometer presented here is based on the Fraunhofer diffraction. The advantages of the proposed interferometer are given in the text along with a simplified sketch of the major components.     

用高分辨电子显微镜测定晶体结构

本文提出一个把高分辨电子显微图和相应的选区电子衍射图结合起来以测定晶体结构的方法。此法可解决从电子衍射数据求解结构振幅绝对值的问题,亦可解决各种衍射分析所共有的相角问题。所得结构图像的分辨本领将优于电子显微图,而有可能接近于衍射分辨极限。