Small angle scattering of partially oriented polymers

Summary A general method for the calculation of the small angle scattering pattern of partially oriented polymers with rotational symmetry about the fiber axis is explained. The method can be used with widely varying models for the basic scattering unit.

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Zusammenfassung Es wird eine allgemeine Methode zur Berechnung des Kleinwinkelstreudiagramms von partiell orientierten Polymeren mit Rotationssymmetrie bezüglich der Faserachse angegeben. Als Modell für die streuende Grundeinheit können die verschiedensten Strukturen verwendet werden.

     

Conformational analysis of oriented non-crystalline polymers using wide angle X-ray scattering

A procedure is presented for obtaining conformational parameters from oriented but non-crystalline polymers. This is achieved by comparison of the experimental wide angle X-ray scattering with that calculated from models but in such a way that foreknowledge of the orientation distribution function is not required. X-ray scattering intensity values for glassy isotactic poly(methylmethacrylate) are analysed by these techniques. The method could be usefully applied to other oriented molecular systems such as liquid crystalline materials.     

Small-angle scattering of partially oriented polymers: model calculations

Three-dimensional small-angle intensity plots are calculated and discussed for a structure consisting of a linear paracrystalline lattice built up by finite lamellar or cylindrical crystallites, tilted with respect to the lattice direction. The lattice directions are distributed with respect to the fiber axis. The effects of different parameters (orientation, tilt angle, crystallite size, etc.) on the diffraction pattern are studied.     

Small angle neutron scattering from steels

Summary By small angle neutron scattering from steels valuable quantitative parameters of the microstructure can be obtained in a non-destructive way. Various features of this method are discussed. Microstructural results are presented which were obtained from neutron scattering experiments with neutron-irradiated pressure vessel steel, with a creep-tested super alloy and transformer sheets.

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Zusammenfassung Wertvolle quantitative Parameter der Mikrostruktur können durch Neutronen-Kleinwinkelstreuung an Stählen gewonnen werden. Die Methode ist dabei zerstörungsfrei. Weitere Charakteristika werden erläutert. Beispielhaft werden Ergebnisse zur Mikrostruktur vorgestellt, die aus Neutronen-Streuexperimenten mit neutronen-bestrahltem Druckwasserstahl, mit Superlegierungen aus Zeitstandversuchen und mit Transformator-Blechen erhalten wurden.

     

Small angle neutron scattering and its application in battery systems

Small angle neutron scattering is a powerful, non-destructive technique that can provide both structural and compositional information. Recently, it has been applied to the field of battery research and has helped elucidate some of the phenomena that are traditionally difficult to probe, including lithiation mechanisms, solid electrolyte interface formation/composition, and electrode microstructure. Specific components of interest can be selectively probed through the application of targeted experiments, contrast variation, and specific composition/structural models gained from complementary data from other analytical techniques.     

Analysis of orientation fluctuation in fluids by small angle X-ray scattering

The small angle X-ray scattering of molecular fluids contains information on particular aspects of their orientational order. Examples are given for the case of the isotropic, nematic and cholesteric phases of mesogenic molecules. It is shown that the distribution of the molecular centers relative to the direction defined by the molecular long axes can be analysed by means of small angle X-ray scattering. An approximate expression for the circulation correlation function is given.     

小角X射线散射法研究CH2Cl2,CHCl3和CCl4对PE液晶结构的影响

采用小角X射线散射法研究了CH_2Cl_2、CHCl_3和CCl_4对磷脂酰乙醇胺(PE)液晶结构影响的机理.CH_3Cl_2、CHCl_3和CCl_4对PE液晶结构影响的差别主要是其空间旋转电子云密度分布形状不同所致.空间旋转电子云密度分布呈椭球状的物质有使PE液晶形成六角形H_1相的趋向;呈圆锥状的物质有诱发PE液晶形成立方六角相的趋向;呈球状的物质有使PE液晶形成片层立方相的趋向.     

聚乙烯片晶辐照破坏机理的电子显微镜研究

用透射电子显微镜观察了高密度辐照聚乙烯的形态结构,并通过统计方法定量地分析了其结构与辐照剂量的关系。发现室温辐照聚乙烯的片晶形态不随辐照剂量而变化。若将室温辐照聚乙烯重新熔融,然后再于125℃下等温结晶4h后,其片晶厚度则随辐照剂量的增加而变薄,长周期亦随之变短。小角X射线散射的测试结果与上述结果符合得很好。室温辐照聚乙烯及其125℃重结晶试样的电子显微镜数据从又一直观角度验证了辐照聚乙烯“片晶内部破坏机理”的正确性。     

Poisson ratios and upper bounds of intrinsic birefringence from brillouin scattering of oriented polymers

To overcome the difficulties in measuring high-frequency shear constants of polymeric materials by ultrasonic or Brillouin scattering technques, we extrapolate results from oriented materials to zero birefringence. Shear constants C₄₄ in the high-frequency limit (GHz) are determined for polyethylene, poly(ethylene terephthalate), poly(vinyl chloride), poly(methyl methacrylate), and polycarbonate using Brillouin scattering. Accurate values of Poisson's ratio are derived. The extrapolation to full orientation using an amended Moseley relation gives upper bounds for the “intrinsic birefringence.” Changes in the character of the orientation process are easily detected by monitoring the mode numbers, which are defined by analogy to Poisson's ratio. Extrapolation of these ratios to their upper bound 0.5 gives an independent check of the maximum intrinsic birefringence. © 1993 John Wiley & Sons, Inc.     

Small angle X-ray scattering investigations of thermodynamic properties of fluid mixtures

Absolute small angle X-ray studies of concentration fluctuations were performed in order to determine thermodynamic properties of a model blend, consisting ofn-hexane and perfluoro-n-hexane. The quantities which we determined were the second derivate of the Gibbs free energy of mixing with respect to the concentration of the components, the location of the spinodal, interaction and solubility parameters, the energy gradient density coefficient as well as the correlation length of the fluctuations at various compositions and temperatures, particularly in the neighbourhood of the spinodal and the critical point. The data obtained were compared with those obtainable from the well known location of the binodal, to test the reliability of the scattering method.     

聚合物对硫化铅钠米微粒的稳定作用

以含铅聚合物微凝胶与Ｈ２Ｓ气体反应制得ＰｂＳ纳米微粒／聚合物复合体系，利用小角Ｘ光散射方法对复合在聚合物中的ＰｂＳ纳米微粒的粒度及分布进行了表征，研究了不同反应条件对其粒度及复合体系稳定性的影响。     

Simultaneous small-angle X-ray scattering and wide-angle X-ray diffraction

The simultaneous SAXS/WAXD technique is shown to provide an unambiguous method for following structural changes taking place during the programmed heating of a range of multiphase polymeric materials. Results are given for polyethylene, block copolyurethanes and block copolyesters containing liquid crystalline hard segments. UK Thermal methods Group Award Lecture     

Small angle x-ray scattering study of ultra-high molecular weight poly(ethylene oxide) gamma irradiated in bulk

The effect of gamma irradiation on the structure of ultra-high molecular weight poly(ethylene oxide) (UHMWPEO) has been investigated by small-angle x-ray scattering (SAXS). The pressed and irradiated polymer possesses quite strong diffuse scattering. That fact makes the direct determination of the main structural parameters very difficult. To solve the problem a modification of the standard evaluating methods is suggested. Thus, the separation of the porous scattering from that of structural formations of PEO becomes possible. The application of a collimation correction according to Schmidt's method enables to separate diffuse and discrete parts in the scattering. Dependences of the long period, the gyration radii, and the difference between densities of crystalline and amorphous phases on the irradiation dose show that the irradiation increases the density of amorphous areas. A packing of the lamellar aggregates and increase of the porous sizes are observed.     

Tetraalkylammonium bromides in methanol: Small angle neutron scattering and vapor pressure measurements

Vapor pressure measurements and small angle scattering (SANS) experiments are reported and discussed for bispiperidinium (BP) bromide and n-tetrapentylammonium bromide solutions in methanol at 25°C. The BP⁺ ion which may be considered as a tetraalkylammonium (TAA) ion with pairwise connected alkyl chains, is used for the study of the effects due to flexible TAA alkyl chains. SANS intensities are calibrated with the help of the precise osmotic coefficients from the vapor pressure measurements.     

预氧化过程中张力对聚丙烯腈预氧化纤维微缺陷结构的影响

本文报道用同步辐射二维小角X射线散射(2D|SAXS)研究预氧化过程中张力对PAN纤维缺陷的影响.     

A small angle neutron scattering and electrochemical impedance spectroscopy study of the nanostructure of the iron chalcogenide glass ion-selective electrode

This paper presents a preliminary structural and interfacial study of the iron chalcogenide glass [i.e., Fe_x(Ge₂₈Sb₁₂Se₆₀)_100−x] ion-selective electrode (ISE) using small angle neutron scattering (SANS) and electrochemical impedance spectroscopy (EIS). SANS detected variations in the neutron scattering as a function of iron content in the chalcogenide glass. Furthermore, a change in the chalcogenide glass structure was observed at elevated iron dopant levels. Conversely, EIS was used to show that the iron chalcogenide membrane comprises various time constants, and the interfacial charge transfer reaction depends on the membrane iron content. Equivalent circuit modeling revealed that the charge transfer resistance decreases at elevated iron levels, and this may be related to the presence of iron defects in the glass. It is proposed that the iron chalcogenide membrane comprises an iron nanostructural network embedded in the amorphous matrix, and this directly influences the electrical conductivity and concomitant electrochemical reactivity of the glass.     

Small Angle X-ray Scattering Study of PS Conformation in Tetrahydrofuran Solvent with Gas Anti-solvent

Compressed gases or supercritical fluids (SCFs) are highly soluble in some liquid solvents, and thus reduces the solvent strength of the liquids1. As a result, precipitation of the dissolved solutes occurs, which is called as gas anti-solvent (GAS) process. Recently, this new technique has been used to produce fine particles of different compounds, such as polymers2. Effect of the dissolved gases on the conformation of polymer molecules is a very interesting topic. In this work, we report t…     

聚丙烯腈基碳纤维及其原丝中的微孔尺寸分布

利用二维小角X射线散射技术(SAXS)研究了聚丙烯腈基碳纤维及其原丝的微孔结构。结合逐级切线法、对数正态分布及麦克斯韦分布函数对2类实验样品内部微孔的尺寸分布进行了分析。结果表明,2类样品中的孔结构具有显著差别,原丝微孔在4~8 nm范围内分布比较集中,碳纤维中微孔的分布区域则移向1.3~1.8 nm。散射数据显示出明显的分形特征,碳纤维与其原丝的孔分形维数分别为1.33和1.55,表明原丝中具有较大的孔隙缺陷。相对于原丝,碳纤维微孔尺寸分布走向均匀和集中,前者则表现出比后者更宽的尺寸分布。就拟合方法而言,逐级切线法的解析手段容易引入误差,低角区的纤维表面散射和高角区的噪音容易对其结果造成影响。正态分布得到了比较窄的尺寸分布,但对于低尺寸区域孔隙的拟合不理想。麦氏分布在一定程度上弥补了以上不足,能够较好地拟合两类纤维样品中微孔的分布状况。     

Crystalline and supermolecular structure evolution of poly(ethylene terephthalate) during isothermal crystallization and annealing treatment by means of wide and small angle X-ray investigations

Small-angle X-ray scattering, wide-angle X-ray diffraction and differential scanning calorimetry analysis were carried out to evaluate the evolution of the supermolecular structure of poly(ethylene terephthalate) (PET) during isothermal crystallization and annealing process. PET was crystallized from the melt by isothermal treatments at 226 °C. Partially crystallized samples were prepared interrupting the crystallization by quenching, while prolonged treatments were performed to prepare annealed samples. The adopted crystallization procedures allowed to form crystals which developed during primary and secondary crystallization, and the annealing process. On the basis of X-ray data, the lamellar and amorphous phases were unambiguously attributed. The lamellar thickness and the crystallinity progressively enhance with increasing the time of thermal treatment; on the contrary, the long period decreases and this effect is mainly due to the contraction of the amorphous phase. The melting behaviour of the annealed samples indicates that the heating-induced crystal reorganization phenomena are inconsistent. The interdependency between the melting temperature and the crystal thickness allowed to extrapolate the equilibrium melting temperature.