Revision of the model of a fibril with amorphous nodules for oriented soft-chain semicrystalline polymers

A critical analysis of literature data about calculations of small-angle x-ray scattering (SAXS) from a model of a fibril with amorphous nodules (FAN) is made. Changes in the SAXS patterns are reviewed for the effect of stretching the FAN. Possibilities of using the calculation results for interpretation of microdeformational behavior of oriented, flexible chain semicrystalline polymers are analyzed. Invoking the FAN model, a retrospective analysis of some literature data and also analysis of new experimental results obtained by SAXS and wide-angle x-ray scattering methods for oriented samples of cellulose triacetate, poly(vinylidene fluoride-co-hexafluoropropylene), and poly(vinyl alcohol) are carried out.     

Quantitative analysis of electron diffraction data from epitaxially grown crystals

Epitaxial growth produces oriented crystal projections where a long unit cell axis is parallel to the major crystal face rather than perpendicular to it and thus provides a favorable condition for electron diffraction data collection which minimizes perturbations due to elastic crystal bending. Even though the crystals are not so perfect as those produced by solution growth, the intensity data from them have been useful for the quantitative crystal structure analysis of several molecular organic compounds and linear polymers as discussed in this review.     

Structure determination of Pt‐coated Au dumbbells via fluctuation X‐ray scattering

A fluctuation X‐ray scattering experiment has been carried out on platinum‐coated gold nanoparticles randomly oriented on a substrate. A complete algorithm for determining the electron density of an individual particle from diffraction patterns of many particles randomly oriented about a single axis is demonstrated. This algorithm operates on angular correlations among the measured intensity distributions and recovers the angular correlation functions of a single particle from measured diffraction patterns. Taking advantage of the cylindrical symmetry of the nanoparticles, a cylindrical slice model is proposed to reconstruct the structure of the nanoparticles by fitting the experimental ring angular auto‐correlation and small‐angle scattering data obtained from many scattering patterns. The physical meaning of the refined structure is discussed in terms of their statistical distributions of the shape and electron density profile.     

Mechanisms of reversible thermal deformation of oriented polymers

Reversible thermal deformation coefficients (TDCs) of oriented samples of a flexible-chain polymer (polyethylene) and of a number of rigid-chain polymers were measured in the longitudinal and transverse directions near room temperature. The same samples were used to measure the TDCs of crystallites by x-ray diffraction. The magnitudes of the TDCs of macroscopic oriented samples and of constituting crystallites and the characteristics of the thermal deformation of flexible-chain and rigid-chain polymers are compared. A conclusion is made that the mechanisms that determine thermal deformation in the longitudinal and transverse directions for the flexible-chain and rigid-chain polymers are different.     

Determination of the chain inclination angle of isothermally crystallized bulk polyethylene

The crystal lamella is well established as a basic structural unit of most semicrystalline polymers. It is also accepted that the chain axis is generally not parallel to the normal to the large flat lamella surfaces, but inclined at some angle θ to it. Due to the random orientation of lamellae in bulk polymers where spherulitic growth predominates, no direct method exists for determining θ. However, the angle has been determined by acid etching bulk samples and then using electron microscopy techniques on fragments. An alternative approach is utilized in this work. The etched fragments, after suitable washing procedures, were sedimented to form an oriented mat. An x-ray diffraction technique was employed in which the regions of high pole density for several crystallographic planes were determined. From these results, the inclination angle was determined to be 40.4°, with a standard deviation of 1.5°. This study represents the first time that an x-ray pole figure technique has been used to determine chain inclination in isotherm-ally crystallized PE.     

Local surface skimming longitudinal wave velocity and residual stress mapping

Local variation in surface skimming longitudinal wave (SSLW) velocity has been measured using a scanning acoustic microscope. A very narrow width electrical impulse has been used to excite the transducer of the acoustic lens. This permits the separation of the SSLW signal from the direct reflected signal in the time domain. A simple method of measuring the time delay between the directly reflected signal and the SSLW signal at two defocuses has been utilized for the local measurement of SSLW velocity. The variation in the SSLW velocity measured over an area of the sample is scaled and presented as an image. The method has been implemented to image the variation of the SSLW velocity around a crack tip in a sample of Ti-6Al-4V. Since the SSLW velocity is known to change linearly with the stress, the SSLW velocity image is considered as a representation of the image of stress around the crack tip. Local stress variation in the same region of the crack tip is directly measured using x-ray diffraction. The SSLW velocity image is compared with the x-ray diffraction stress image. The contrast in the two images, spatial resolution, and the penetration depth into the sample of acoustic waves and x rays are discussed.     

Measurement of lattice damage caused by ion-implantation doping of semiconductors†

Two new techniques have been used to measure the lattice damage produced in gallium arsenide by the implantation of 60 keV cadmium ions. In one of these methods, optical reflection spectra of the ion-implanted samples were measured in the wavelength range from 2000 to 4600Å. The decrease in reflectivity resulting from ion- implantation was used to determine the relative amount of lattice damage as a function of ion dose. The second technique employed the scanning electron microscope. Patterns very similar in appearance to Kikuchi electron diffraction patterns are obtained when the secondary and/or backscattered electron intensity is displayed in the scanning electron microscope as a function of the angle of incidence of the electron beam on a single crystal surface. The degradation of these ‘Coates-Kikuchi’ patterns resulting from ion implantation was used to obtain a quantitative measure of the lattice damage caused by the implantation process. The results of measurements made by both of the methods described have been compared with each other, and with data obtained by the more established method of measuring lattice damage by Rutherford scattering of 1 MeV helium ions.     

Determination of the orientational order parameter of the homologous series of 4-cyanophenyl 4-alkylbenzoate (n.CN) by different methods

The orientational order parameters of a homologous series of 4-cyanophenyl 4-alkylbenzoates have been determined at different temperatures from (13)C-NMR, x-ray diffraction, optical birefringence, high resolution density and diamagnetic susceptibility anisotropy measurements. To determine the temperature dependence of the orientational order parameter from the (13)C chemical shift values, the two-dimensional polarization inversion spin exchange at the magic angle (PISEMA) method was also used for the measurement of (13)C-(1)H dipolar couplings at different sites in the oriented phase. The nematic order parameters determined from each of these methods have been compared. Apart from a slight shift in their values their trends with temperature are very similar. The differences among the results obtained by these five different methods have been discussed. From the high resolution density data, the values of the critical exponents near the T(N-I) transition are found to lie between the Ising model and tricritical behaviour.     

Helical signature motif in the fibre diffraction patterns of random-walk chains

Helical geometry is one of the most dominant structural features in polypeptides, nucleic acids, carbohydrates and long-chain polymers in general. Structures of a large number of helical biomolecules and important non-biological polymers have been determined by fibre diffraction and helical diffraction theory. This paper reports on a study of fibre diffraction patterns calculated for two different on-lattice random-walk models of polymers, with no built-in helical features. It is noted that such on-lattice random walks are natural models for polymers with fixed monomer geometries and inter-monomer angles. The presence of layer-line intensities is observed, characteristic of fibre diffraction patterns from helices with an integral number of units per turn. It is shown that under certain circumstances, fibre diffraction patterns of helical objects may be difficult to distinguish from cylindrically-averaged fibre diffraction patterns of random walks on lattices with fixed angles. A simple correspondence is demonstrated between the parameters of a helix and a random-walk chain with equivalent fibre diffraction patterns. These results call for a critical examination of the way the helical diffraction theory is typically used: certain structures that have been modelled as helical might, under some circumstances, be more naturally described as random-walk chains with no preferred conformation even on the shortest length-scale and in the context of a fibre.     

Atomic structure of cadmium sulfide nanoparticles

A method for calculating the x-ray diffraction patterns of cadmium sulfide nanoparticles with a disordered internal structure, a real surface, shape, and size is proposed within the kinematic theory of scattering. A computer analysis has revealed that the characteristic shape of the experimental x-ray diffraction patterns of cadmium sulfide films and powders is determined by a specific disordered nanoparticle structure differing from the crystal structures of wurtzite and sphalerite. According to the computer simulation, cadmium sulfide nanoparticles synthesized through chemical deposition have a shape similar to a hexagonal prism with a characteristic size of approximately 5 nm.     

A study of symmetrical LLL X-Ray polylithic interferometers on the basis of the Takagi equations

The Takagi approach to the dynamical theory of x-ray diffraction has been used to study LLL x-ray polylithic interferometers. A computational tool has been implemented to solve the Takagi equations with boundary conditions of the Cauchy type. The mean intensity, visibility and initial phase of the x-ray fringes generated by displacing the analyzer have been calculated for any wavefront, absorption of the incident radiation and for the most common geometric arrangements. Geometric aberrations of different kinds, introduced during interferometer preparation, are considered. The curve relevant to the calculated difference between the reflected and transmitted x-ray fringes as a function of analyzer rotation is in agreement with the experimental curve.     

Direct observation of azimuthal correlations between DNA in hydrated aggregates

This study revisits the classical x-ray diffraction patterns from hydrated, noncrystalline fibers originally used to establish the helical structure of DNA. We argue that changes in these diffraction patterns with DNA packing density reveal strong azimuthally dependent interactions between adjacent molecules up to approximately 40 A interaxial or approximately 20 A surface-to-surface separations. These interactions appear to force significant torsional "straightening" of DNA and strong azimuthal alignment of nearest neighbor molecules. The results are in good agreement with the predictions of recent theoretical models relating DNA-DNA interactions to the helical symmetry of their surface charge patterns.     

硅衬底上Zn1-xMgxO薄膜的结构与光学性质

采用脉冲激光法（PLD）在Si衬底上沉积Zn1-xMgxO薄膜.x射线衍射(XRD)表明薄膜为c轴取向，（002）峰的半高宽仅为0.211°，且没有MgO的相偏析.透射电子显微镜可以清楚看到Zn1-xMgxO薄膜的c轴择优取向.在选区电子衍射图中可以看到Zn1-xMgxO结晶薄膜整齐的衍射斑点.室温下对Zn1-xMgxO薄膜进行了光致荧光光谱分析，发现其带边发射峰相对ZnO晶体有0.4eV的蓝移，带边发射峰与杂质发射峰的强度之比高达159.Zn1-xMgxO结晶薄膜质量良好，显示了应用于光电器件的潜力. 关键词： Zn1-xMgxO合金薄膜 硅衬底 脉冲激光沉积法 c轴取向 光致荧光光谱     

Calculation of the Band Intensities of the IR Spectra of Oriented Polymers

An attempt has been made to extend the theory of IR spectra of polymers to oriented polymers. Formulas for the absorption-band intensities in polarization IR spectra of oriented polymers reflecting the dependence of the polarized absorption-band intensity on the structural and orientation characteristics of polymers have been obtained. These formulas permit calculating the intensity of polarized absorption bands at different degrees of orientation of the polymer.     

Precession photography of fibres: Prediction of patterns

The Buerger precession method of recording x-ray diffraction patterns can also be used for fibres. This method has some advantages over the conventional flat plate method. Since the fibre has inherent cylindrical symmetry, the precession photograph of the fibre is equivalent to the ‘rotation-precession’ photograph of a single crystal. An analytical prediction of diffraction patterns of the rotation-precession photography is discussed. Also, experimental data are provided to confirm the validity of the equations derived.     

基于径向剪切干涉仪的三维位移测量技术

本文提出一种基于双圆光栅径向剪切干涉仪的三维位移测量方法,其测量原理是径向剪切干涉仪所形成的莫尔条纹不仅由二维平面内位移决定,轴向位移会在+1和–1级莫尔条纹之间产生一个特定的相移.首先,基于标量衍射理论对双圆光栅径向剪切干涉仪的+1和–1级莫尔条纹强度分布进行推导,建立了三维位移量与莫尔条纹强度分布的精确解析关系;其次,在频谱分析的基础上,利用半圆环滤波器进行空间滤波,实现+1和–1级莫尔条纹的同时成像;然后,提出了从莫尔条纹图中定量提取三维位移的算法,并通过数值模拟进行验证;最后,实验结果验证了该方法测量平面内位移的最大绝对误差为4.8×10^–3 mm,平均误差为2.0×10^–4 mm,轴向位移的最大绝对误差为0.25 mm,平均误差为8.6×10^–3 mm.该方法具有装置简单、测量精度高、非接触、瞬时测量等特点,可实现三维位移的同时测量.     

Energy resolution of the CdTe‐XPAD detector: calibration and potential for Laue diffraction measurements on protein crystals

The XPAD3S‐CdTe, a CdTe photon‐counting pixel array detector, has been used to measure the energy and the intensity of the white‐beam diffraction from a lysozyme crystal. A method was developed to calibrate the detector in terms of energy, allowing incident photon energy measurement to high resolution (approximately 140 eV), opening up new possibilities in energy‐resolved X‐ray diffraction. In order to demonstrate this, Laue diffraction experiments were performed on the bending‐magnet beamline METROLOGIE at Synchrotron SOLEIL. The X‐ray energy spectra of diffracted spots were deduced from the indexed Laue patterns collected with an imaging‐plate detector and then measured with both the XPAD3S‐CdTe and the XPAD3S‐Si, a silicon photon‐counting pixel array detector. The predicted and measured energy of selected diffraction spots are in good agreement, demonstrating the reliability of the calibration method. These results open up the way to direct unit‐cell parameter determination and the measurement of high‐quality Laue data even at low resolution. Based on the success of these measurements, potential applications in X‐ray diffraction opened up by this type of technology are discussed.     

Interference Patterns of three-fiber Mach-Zehnder Interferometer and its Numerical Simulation

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Pulsed TV-holography recording for vibration analysis applications

TV-holography is a well-known tool for vibration analysis. Using the so-called time-average method, this technique allows to record interferograms showing the mode shapes of a structure submitted to vibration excitation and is currently used for modal identification.Within the frames of a BRITE-EURAM program called vibration intensity processing using full-field multi-pulse laser technique (VIP), a TV-holography equipment has been developed, working with a 25 Hz pulsed laser and allowing easy on-site measurements. A measurement procedure has been defined and a specific data processing has been developed for the determination of structural intensity fields, which give transfer path of the vibration energy within a structure.The measurement of these quantities is possible the using classical means (accelerometers, stress gauges, etc.) but the data processing is complex and require a lot of accurate sensors because it is based on spatial derivatives of high order. The optical techniques (laser vibrometry, holography, etc.) are more suited for that purpose because of the high density of measuring points and because of the well-known advantages of these methods: reduced measurement time and no modification of the mass parameters of the structure as it is the case when using contact sensors.Different kinds of output data are then given: operational deflection shape, amplitude and phase, structural intensity field and its divergence through a further step of data processing. The complete procedure with the associated data processing has been tested (for various configurations of excitation and damping) first on a clamped plate, then on a cylinder and at the end on several industrial components.This paper describes the general measurement procedure and the equipment used. The data processing is also presented and various measurement results are shown. The conclusion gives the main advantages and limitations of the method and evaluates the application possibilities.