Thin-film characterization by grazing incidence X-ray diffraction and multiple beam interference

An overview is given of the application of two-beam and multiple-beam approach to grazing incidence X-ray diffraction (GIXD) for single-crystal thin film characterization. Crystallographic orientation, lattice mismatch, order parameter, and phase of in-plane reflection for various thin film systems are determined by using conventional two-beam GIXD and resonance three-beam GIXD. The diffraction technique, analysis procedure, and theoretical consideration are also presented and discussed.     

Mo/Si多层膜小角X射线衍射结构表征

为了实现对Mo/Si多层膜的结构表征,测量了多层膜样品的小角X射线衍射谱。介绍了小角X射线衍射谱的分析方法,包括Bragg峰值拟合法,傅里叶变换法,反射谱拟合法。Bragg峰值拟合法和反射谱拟合法得到多层膜的周期厚度为7.09nm,两种模型的反射谱拟合法得到界面的粗糙度(扩散长度)为0.40～0.41nm(Si在Mo上),0.52～0.70nm(Mo在Si上),前者要比后者小,这与透射电镜法(TEM)得到的结果0.40nm(Si在Mo上),0.6～0.65nm(Mo在Si上)是一致的。通过基于扩散模型的反射谱拟合法得到的折射率剖面也与由高倍率透射电镜(HRTEM)积分得到的灰度值剖面在趋势上是一致的。通过X射线衍射谱和TEM图像对Mo/Si多层膜进行综合表征,得到了多层膜的精细结构信息,这对多层膜制备工艺的优化具有十分重要的意义。     

Bragg diffraction of light in synthetic opals

Three-dimensional light diffraction from the crystal structure, formed by closely packed a-SiO₂ spheres of submicron size, of samples of synthetic opals was visualized. The diffraction pattern of a monochromatic light beam was established to consist of a series of strong maxima whose number and angular position depend on the wavelength and mutual orientation of the incident beam and the crystallographic planes of the sample. The diffraction patterns were studied under oblique incidence on the (111) growth surface of the sample and with light propagated in the (111) plane in various directions perpendicular to the sample growth axis. The spectral and angular relations of diffracted intensity were studied in considerable detail in both scattering geometries. The experimental data are interpreted in terms of a model according to which the major contribution to the observed patterns is due to Bragg diffraction of light from (111)-type closely packed layers of the face-centered cubic opal lattice. The model takes into account the disorder in the alternation of the (111) layers along the sample growth axis; this disorder gives rise, in particular, to twinning of the fcc opal lattice.     

An in situ high-pressure X-ray diffraction experiment on hydroxyapophyllite

The compression behavior of a natural hydroxyapophyllite is investigated up to about 10.01 GPa at 300 K using in situ angle-dispersive X-ray diffraction and a diamond anvil cell at the High Pressure Experiment Station, Beijing Synchrotron Radiation Facility (BSRF). Over this pressure range, no phase change or disproportionation is observed. The isothermal equation of state is determined for the first time. The values of zero-pressure volume V0 , isothermal bulk modulus K0 , and K0 refined with a third-order Birch-Murnaghan equation of state are V0 = 1276.3±0.9  3 , K0 = 71±3 GPa, and K0 = 8±1. Furthermore, we confirm that the values of linear compressibility β along the a and c directions of hydroxyapophyllite are elastically anisotropic.     

Separation of enantiomers in a diol monolayer studied by fluorescence microscopy and grazing incidence X-ray diffraction

Summary Monolayers of a racemic mixture and of the pure S- and R-enantiomers of 3-hexadecyloxy-propane-1,2-diol have been investigated by fluorescence microscopy and grazing incidence X-ray diffraction. Above the transition pressureΠ _c domains with a polygonal shape appear. On compressing the monolayers shape instabilities occur. While the spirals of the S-enantiomer turn clockwise and the spirals of the R-enantiomer turn counterclockwise, the spirals from one domain of the racemate exhibit opposite handedness. This behaviour is explained by a separation of enantiomers on the molecular level. At all pressures investigated the enantiomers exhibit an oblique lattice. The tilt angle of the molecules decreases with increasing pressure. Paper presented at the I International Conference on Scaling Concepts and Complex Fluids, Copanello, Italy, July 4–8, 1994.     

Study of partial melting at high-pressure using in situ X-ray diffraction

The high-pressure melting behavior of different iron alloys was investigated using the classical synchrotron-based in situ X-ray diffraction techniques. As they offer specific advantages and disadvantages, both energy-dispersive (EDX) and angle-dispersive (ADX) X-ray diffraction methods were performed at the BL04B1 beamline of SPring8 (Japan) and at the ID27-30 beamline of the ESRF (France), respectively. High-pressure vessels and pressure ranges investigated include the Paris–Edinburgh press from 2 to 17 GPa, the SPEED-1500 multi-anvil press from 10 to 27 GPa, and the laser-heated diamond anvil cell from 15 to 60 GPa. The onset of melting (at the solidus or eutectic temperature) can be easily detected using EDX because the grains start to rotate relative to the X-ray beam, which provokes rapid and drastic changes with time of the peak growth rate. Then, the degree of melting can be determined, using both EDX and ADX, from the intensity of diffuse X-ray scattering characteristic of the liquid phase. This diffuse contribution can be easily differentiated from the Compton diffusion of the pressure medium because they have different shapes in the diffraction patterns. Information about the composition and/or about the structure of the liquid phase can then be extracted from the shape of the diffuse X-ray scattering.     

Selective control of light beams in diffraction experiments on synthetic opals

This paper reports on an experimental and theoretical investigations of the possibility of selectively controlling the intensity of {hkl} diffraction reflections in synthetic opals. The calculations of the photonic stop-band width for low-contrast multi-component photonic crystals argue for a selective pattern of the vanishing of various {hkl} stop bands (and, accordingly, of the various {hkl} diffraction reflections) under variation of the dielectric permittivity of one of the components. Optical diffraction patterns have been studied visually and recorded in various scattering geometries with bulk opal samples illuminated by white unpolarized light. The experiments have made use of immersion spectroscopy, a method reducing essentially to successive measurements of diffraction patterns under variation of the dielectric permittivity of the liquid filler of the opal matrix. The {111} and {220} Bragg reflections have been observed to weaken noticeably at the filler permittivities matching very well with the values derived earlier from an analysis of transmission spectra.     

Morphology of open films of discotic hexagonal columnar liquid crystals as probed by grazing incidence X-ray diffraction

The structure and the orientation of thermotropic hexagonal columnar liquid crystals are studied by grazing incidence X-ray diffraction (GIXD) for different discotic compounds in the geometry of open supported thin films. Whatever the film deposition mode (either spin-coating or vacuum evaporation) and the film thickness, a degenerate planar alignment with the liquid crystalline columns parallel to the substrate is found. However, if a specific thermal process is applied to the liquid crystal film, homeotropic anchoring (columns normal to the interface) can be stabilized in a metastable state.     

锐钛矿金红石的高温原位X射线衍射研究

对TiO₂粉末进行了空气和真空条件下从室温到1200℃的加热原位X射线衍射实验, 得到了空气和真空条件下微米级锐钛矿颗粒转变为金红石的起始温度分别为850℃ 和855℃; 分别修正了空气条件下锐钛矿在(27–850℃)范围和金红石在(900–1200℃) 范围内的晶胞参数和真空条件下锐钛矿在(27–850℃)范围和金红石在(950–1200℃) 范围的晶胞参数, 从而得到了晶胞参数随温度变化的关系, 得到了锐钛矿和金红石在空气中和真空中的热膨胀系数, 并总结了热膨胀系数随温度变化的规律. 室温下锐钛矿在空气条件下的热膨胀系数为 α_a=4.55063×10^-6/℃, α_c=7.7543×10^-6/℃, β=16.85836×10^-6/℃; 真空下为 α_a=4.69429×10^-6/℃, α_c=9.02850×10^-6/℃, β=18.69688×10^-6/℃. 室温下, 金红石在空气条件下的热膨胀系数为 α_a=6.81243×10^-6/℃, α_c=8.71644×10^-6/℃, β=22.22178×10^-6/℃; 真空条件下为 α_a=6.05834×10^-6/℃, α_c= 8.39280×10^-6/℃, β=20.52362×10^-6/℃. 关键词： 2')" href="#">TiO₂ 原位X射线衍射 相转变 热膨胀     

Use of grazing incidence X-ray diffraction for the study of nitrogen implanted stainless steels

The identification of Fe, Ni and Cr nitrides formed by nitrogen-ion implantation (4×10¹⁷ N⁺ cm^-2, 50 keV) in austenitic steels is performed by X-ray diffraction under very low glancing angles (0.00 ⩽ i ⩽ 1.5°). Spectra obtained with increasing angles i permit the investigation of layers with depths varying from 20 to more than 1000 Å. This non-destructive technique allows the surface to be controlled at each step of the treatments. Spectra were recorded on polished steel prior to and after implantation, with or without electrochemical attack. A 100 Å martensitic layer formed during the mechanical polishing is observed on the austenitic substrate. This layer is destroyed by an anodic attack before implantation of the samples. After implantation a CrN or carbonitride overlayer of a few tens of Å in thickness, may be observed. In the subjacent layers several iron and nickel nitrides are present, mainly ϵ-Fe₂N-Fe₃N, ς-Fe₂N and Ni₃N.     

In situ accelerated leaching of cement paste by application of electrical fields monitored by synchrotron X-ray diffraction

An external dc voltage was applied to a cured cement paste to simulate its natural degradation as a function of time. The electrical treatment was monitored in situ by simultaneous acquisition of diffraction patterns every 10 min. The analysis of the diffraction patterns has confirmed that the microstructure of the whole paste changes during the treatment, with precipitation and dissolution of several phases. This work contributes to the understanding of the fundamentals of the microstructure alterations that take place upon application of an electrical field, allowing the establishment of a first approach to the understanding of the mechanism of these changes. PACS 81.40.Cd; 82.80.Fk; 83.85.Hf     

Multiple Bragg diffraction in low-contrast photonic crystals based on synthetic opals

The phenomenon of multiple Bragg diffraction in low-contrast photonic crystals based on synthetic opals has been studied both experimentally and theoretically. The transmission and reflection spectra of opal films near the K point of the Brillouin zone of the face-centered cubic lattice in s-polarization exhibit the effect of anticrossing of dispersion curves corresponding to the (111) and ([`1]11)(\bar 111) photonic stop bands. The effect of quasi-Brewster suppression of stop bands is clearly pronounced in p-polarization. The experimental data are analyzed using the calculation of the band structure of opal with the inclusion of the polarization of incident light.     

Peculiarities of the formation of the X-ray diffraction image of a surface acoustic wave in grazing geometry

The x-ray diffraction image of a Bluestein-Gulyaev surface acoustic wave (SAW) at grazing angles of incidence is considered in the noncoplanar symmetric Laue geometry. It is assumed that the SAW propagation direction makes a small angle with the diffraction vector. It is shown that small deviations from the Bragg angle (～0.01″) due to SAWs that do not lead to a change in the reflection coefficient result in the formation of diffraction satellites for both standing and traveling SAWs. The recorded x-ray diffraction image representing the time-averaged intensity distribution has characteristic profiles for even-and odd-order satellites.