Modification of Classical SPM for Slightly Rough Surface Scattering with Low Grazing Angle Incidence

Based on the impedance/admittance rough boundaries, the reflection coefficients and the scattering cross section with low grazing angle incidence are obtained for both VV and HH polarizations. The error of the classical perturbation method at grazing angle is overcome for the vertical polarization at a rough Neumann boundary of infinite extent. The derivation of the formulae and the numerical results show that the backscattering cross section depends on the grazing angle to the fourth power for both Neumann and Dirichlet boundary conditions with low grazing angle incidence. Our results can reduce to that of the classical small perturbation method by neglecting the Neumann and Dirichlet boundary conditions.

Small angle X-ray scattering beamline at SSRF

Beamline BL16B1 at Shanghai Synchrotron Radiation Facility(SSRF) is dedicated to studying the microstructure and dynamic processes of polymers, nanomaterials, mesoporous materials, colloids, liquid crystals,metal materials, etc. At present, SAXS, wide angle X-ray scattering(WAXS), simultaneous SAXS/WAXS,grazing incident SAXS, and anomalous SAXS techniques are available for end user to conduct diverse experiments at this beamline. The sample-to-detector distance is adjustable from 0.2 m to 5 m. The practicable q-range is 0.03–3.6 nm-1at incident X-ray of 10 ke V for conventional SAXS whilst a continuous q-region of0.06–33 nm-1can be achieved in simultaneous SAXS/WAXS mode. Time-resolved SAXS measurements in sub-second level was achieved by the beamline upgrating in 2013. This paper gives detailed descriptions about the status, performance and applications of the SAXS beamline.

Small Angle X-ray Scattering Study of Precipitation Kinetics in Al-Zn-Mg-Cu Alloys

The evolution of microstructure parameters （precipitate size and volume fraction） for two types of Al-Zn-Mg-Cu alloys （7075 and 7055） during aging has been studied by synchrotron-radiation small angle X-ray scattering （SAXS）.The results show that the precipitates are only a few nanorneters for both alloys ageing even at higher temperature of 160℃ for 72 h （4.44 and 5.82 nm, respectively）. The maximum of the precipitate volume fraction increases with in creasing Zn content and is about 0.023-0.028 and 0.052-0.054, respectively. The coarsening of precipitate is consistent with LSW （Lifshitz-Slyozov-Wagner） model even at the initial stage where volume fraction is still varying.The activation energy of coarsening regime has been determined to be about 1.22±0.02 eV and 1.25±0.02 eV for alloys 7075 and 7055, respectively.

Growth Kinetics of Nanocrystals and Nanorods by Employing Small-angle X-ray Scattering (SAXS) and Other Techniques

In this article, we report the results of our detailed investigations of the growth kinetics of zero-dimensional nanocrystals as well as one-dimensional nanorods by the combined use of small angel X-ray scattering （SAXS）, transmission electron microscopy （TEM） along with other physical techniques. The study includes growth kinetics of gold nanocrystals formed by the reduction of HAuCl4 by tetrakis（hydroxymethyl） phosphonium chloride in aqueous solution, of CdSe nanocrystals formed by the reaction of cadmium stearate and selenium under solvothermal conditions, and of ZnO nanorods formed by the reaction of zinc acetate with sodium hydroxide under solvothermal conditions in the absence and presence of capping agents. The growth of gold nanocrystals does not follow the diffusion-limited Ostwald ripening, and instead follows a Sigmoidal rate curve. The heat change associated with the growth determined by isothermal titration calorimetry is about 10 kcal·mol^-1 per I nm increase in the diameter of the nanocrystals. In the case of CdSe nanocrystals also, the growth mechanism deviates from diffusion-limited growth and follows a combined model containing both diffusion and surface reaction terms. Our study of the growth kinetics of uncapped and poly（vinyl pyrollidone） （PVP）-capped ZnO nanorods has yielded interesting insights. We observe small nanocrystals next to the ZnO nanorods after a lapse of time in addition to periodic focusing and defocusing of the width of the length distribution. These observations lend support to the diffusion-limited growth model for the growth of uncapped ZnO nanorods. Accordingly, the time dependence on the length of uncapped nanorods follows the L3 law as required for diffusion-limited Ostwald ripening. The PVP-capped nanorods, however, show a time dependence, which is best described by a combination of diffusion （L^3） and surface reaction （L^2） terms.

Scanning Microfocus Small Angle X-ray Scattering Study of the Avian Eggshell

Synchrotron microfocus small angle X-ray scattering was used to investigate the nanostructure and microscopic variation of eggshells. It uses a microbeam allowing the ability to probe interactions between the organic and inorganic components at nanometer level and is ideal for mapping over small areas to obtain a detailed analysis of structural variations. Thin sections of eggshells were scanned from the shell membrane （inner） to the cuticle （outer） surface. The data collected was used to produce two-dimensional maps showing microscopic changes within the different layers of the eggshell. The structural alterations ap- parently could have implications at the macroscopic level of the resulting eggshell. As the organic matrix is embedded within the eggshell this may contribute to the variations observed in calcite crystal form and texture, Structural information obtained about a biomaterial at different length scales is important in relating the structure to its functional properties. This knowledge and the principles behind the formation of biomaterials could be used in the attempt of bioengineering new systems.

Characteristics of AOT Microemulsion Structure: a Small Angle X-ray Scattering Study

The method of synchrotron radiation small-angle X-ray scattering (SR-SAXS) has been used to obtain structural information on the system of bis (2-ethylhexyl) sulfosuccinate (AOT)/H2O/isooctane. By using the Guinier plot (Ln I (q) versus q(2)) on the data sets in a defined small q range (0.03-0.06 Angstrom (-1)), the gyration radius at different water/surfactant molar ratio, W-0, was obtained. With the increase of W-0, the gyration radius (R-g) increased at the range of 23.2 similar to 52.7 Angstrom.

Probing Nanoscale Morphology of PS/PMMA/CdS &PS/PVC/CdS Polymeric Nanocomposites through Small Angle X-Ray Scattering Analysis

Polymeric nanocomposites of PS/PMMA/CdS and PS/PVC/CdS samples have been synthesized through dispersion solution casting technique. The nanoparrticles of CdS were prepared by simple chemical method using CdCl2 and H2S gas produced from thiourea. The nanoscale morphology of the prepared polymeric nanocomposite samples is probed through small angle X-ray scattering (SAXS). The SAXS study reveals that CdS nanoparticles take place at voids position in the respective plymer blend matrix and exhibit their nano nature with very little tendency to agglomerates.

Stability of the Dividing Distribution Function Method for ParticleSize Distribution Analysis in Small Angle X－Ray Scattering

The Dividing Distribution Function (DDF) method is one of the methods by which the particle size distribution of ultrafine powder can be evaluated from its small angle X-ray scattering data. In this paper, the stability of the solution obtained from DDF method has been investigated through optimizing the coefficient matrix, introducing a damping factor and a least square treatment. All calculations were accomplished with a microcomputer. It was shown that the average deviations of the size distribution obtained are not larger than the assigned random errors to the scattering intensities as long as the corresponding requirements are satisfied.

In situ grazing-incidence small-angle X-ray scattering observation of block-copolymer templated formation of magnetic nanodot arrays and their magnetic properties

The fabrication of bit-patterned media （BPM） is crucial for new types of hard disk drives. The development of methods for the production of BPM is progressing rapidly. Conventional lithography reaches the limit regarding lateral resolution, and new routes are needed. In this study, we mainly focus on the dependence of the size and shape of magnetic nanodots on the Ar＋-ion etching duration, using silica dots as masks. Two-dimensional （2D） arrays of magnetic nanostructures are created using silica-filled diblock-copolymer micelles as templates. After the self-assembly of the micelles into 2D hexagonal arrays, the polymer shell is removed, and the SiO2 cores are utilized to transform the morphology into a （Co/Pt）2-multilayer via ion etching under normal incidence. The number of preparation steps is kept as low as possible to simplify the formation of the nanostructure arrays. High-resolution in situ grazing-incidence small-angle X-ray scattering （GISAXS） investigations are performed during the Ar＋-ion etching to monitor and control the fabrication process. The in situ investigation provides information on how the etching conditions can be improved for further ex situ experiments. The GISAXS patterns are compared with simulations. We observe that the dots change in shape from cylindrical to conical during the etching process. The magnetic behavior is studied by utilizing the magneto-optic Kerr effect. The Co/Pt dots exhibit different magnetic behaviors depending on their size, interparticle distance, and etching time. They show ferromagnetism with an easy axis of magnetization perpendicular to the film. A systematic dependence of the coercivitv on the dot size is observed.

Nano-scale pore distribution characterisation of coal using small angle X-ray scattering

In the process of coal seam fracturing with liquid nitrogen(LN_(2)),the change of coal pore structure has an important influence on the efficiency of coalbed methane(CBM)extraction.The nano-scale pore size distribution(PSD)in coal particles before and after freezing with LN_(2) are experimentally studied in this work.Coal samples are collected from four coal mines,where coal and gas outburst accidents have occurred.Small angle X-ray scattering technology(SAXS)and scanning electron microscopy(SEM)are used to study the pore structure changes of coal samples quantitatively and qualitatively.It is found that the scattering intensity of coal samples increases after freezing.The PSD of all samples significantly changes in the range of 0.8–7 nm,showing new pore spaces in 0.8–4 nm and fewer pores in the 4–7 nm range.Both the pore fractal dimension and the radius of gyration of coal samples increase after freezing and are mainly affected by the changes in pores and the anisotropy of the coal matrix.Crack expansion and pore connections are observed in the surface structure of the coal sample using SEM.This study provides a better understanding of the nano-scale mechanism of coal seam fracturing with LN_(2) for the prevention of coal and gas outbursts.

Small angle X-ray scattering of the colloidal crystal

The monodisperse polystyrene spheres are assembled into the colloidal crystal on the glass substrate by vertical deposition method, which is aimed at the so-called photonic crystal applications. The structural information of the bulk colloidal crystal is crucial for understanding the crystal growth mechanism and devel- oping the various applications of colloidal crystal. Small-angle X-ray scattering （SAXS） technique was used to obtain the bulk structure of the colloidal crystal at Beamline lW2A of BSRF. It is found that the SAXS pattern is sensitive to the relative orientation between the colloidal sample and the incident X-ray direction. The crystal lattice was well distinguished and determined by the SAXS data.

DETERMINATION OF SIZE DISTRIBUTION OF THE CRYSTALLINE PARTICLE IN AGED METALLIC GLASS BY SMALL ANGLE X-RAY SCATTERING

Ⅰ. INTRODUCTIONAlthough many authors have investigated the structure of annealed metallic glass by means of small angle X-ray scattering (SAXS), there has been no report in which size distribution of the crystalline particle in aged metallic glass is determined. Determining size distribution of the crystalline particle will be beneficial to understanding the nucleation and growth process of the crystalline particle. In this note, size distribution of the crystalline parti-

DETERMINATION OF THE SHAPE AND DIMENSION OF PRECIPITATE FROM AGED Lc4 ALUMINIUM ALLOY BY SMALL ANGLE X-RAY SCATTERING

Small angle X-ray scattering (SAXS) is extensively used for determining the dimension of a particle, but rarely used for determining its shape. The difficulty is that it needs to do extensive calculations. In addition, it can only be carried out for the mono-dispersion system. In re cent years, Reuther et al. succeeded in determining the shape and dimension of the particle of a polymer gel.

Characterization of the nanopore structures of PAN-based carbon fiber precursors by small angle X-ray scattering

The nanopore structures in precursors Four carbon-fiber precursors are prepared. They are crucial to the performance of PAN-based carbon fibers are bath-fed filaments （A）, water-washing filaments （B） hot-stretching filaments （C） and drying-densification filaments （D）. Synchrotron radiation small angle X-ray scattering is used to probe and compare the nanopore structures of the four fibers. The nanopore size, discrete volume distribution, nanopore orientation degree along the fiber axis and the porosity are obtained. The results demonstrate that the nanopores are mainly formed in the water-washing stage. During the processes of the subsequent production technologies, the slenderness ratio of nanopores and their orientation degree along the fiber axis increase further and simultaneously, the porosity decreases. These results are helpful for improving the performance of the final carbon fibers.

Influence of energy bandwidth of pink beam on small angle X-ray scattering

Background Compared with the traditional monochromatic synchrotron radiation beam,a pink beam is a quasimonochromatic beam which can be obtained by screening a harmonic of the undulator.The energy bandwidth(E/E)of a pink beam is about 10−2.Despite the intensity gain from the quasi-monochromatic beam,the decrease in the energy resolution will lead the collected data to be smeared.Purpose To study the influence of the energy bandwidth on the small angle X-ray scattering(SAXS)by experiments and verify the feasibility of SAXS with a pink beam.Method Firstly,the influence of different energy bandwidths on SAXS has been studied by simulation and experiment.Then,TEM tests have been performed and compared with the experimental results.Result It has been shown that the scattering curves deviate slightly from the traditional monochromatic ones.This deviation does not influence the data processing for the maximum deviation of the results is just less than 2%.In return,the gain in the intensity(one to two orders of magnitude)makes the pink beam very important for the time-resolved SAXS.Further,the results of TEM and SAXS have shown an excellent agreement.Conclusion Thiswork proves that the pink beam could be used for SAXS directly without a desmearing procedure.Benefiting from the increase in the beam intensity,the exposure time can be greatly shortened,thus enhancing the utilization efficiency of the synchrotron radiation.

溶液法原位大面积制备钙钛矿光电薄膜成膜的同步辐射可视化结晶过程研究

溶液法是新型光电器件制备的重要手段,然而以钙钛矿半导体材料为代表的薄膜样品制备通常需要在手套箱环境下完成,传统的实验表征大多在空气环境下进行,这显然很难反映薄膜结构与器件性能间的真实关联,因此急需对溶液成膜过程的微结构演变开展原位实时研究.为了实现溶液法成膜中的结构与形貌的同步辐射掠入射广角散射实时观测,本文结合上海同步辐射光源线站布局,报道了一种基于手套箱的原位成膜观测装置,可实现标准手套箱环境(c(H_(2)O,O_(2))<1×10^(-6))下远程控制薄膜旋涂、涂布及样品后处理,并实时可视化监测微结构和形貌演变.基于该装置进行的钙钛矿薄膜狭缝涂布大面积成膜结晶过程的原位GIWAXS/GISAXS(gtrazing incidence wide and small angle X-ray scattering)可视化测试揭示了薄膜微结构转变的内在驱动力:钙钛矿薄膜沉积界面层的优化对提升钙钛矿成核速率、诱导结晶择优取向、形成晶粒有序堆叠等具有“共性作用”,同时在成膜过程中的新生中间相显著提升软晶格薄膜质量和稳定性.基于各层均采用卷对卷全溶液狭缝涂布方法制备的大面积全柔性三维钙钛矿薄膜太阳能电池转换效率提升至5.23%(单个器件面积约15 cm^(2)),为迄今报道的这一体系该尺寸的全溶液狭缝涂布柔性钙钛矿器件的最高器件效率之一.因而,基于该同步辐射原位GIWAXS/S/GISAXS装置可以获得控制薄膜生长界面特性和薄膜品质的关键工艺,指导优化制备薄膜的最佳工艺条件.

锗硅量子点掠入射小角X射线散射研究

采用同步辐射X射线对MBE制备的锗硅量子点试样进行了掠入射小角X射线散射(GISAXS,grazing incidence small angle X-ray scattering)研究。根据AFM测量得到的量子点尺寸、形状和间距等参数,采用DWBA理论以及合适的分布函数,利用IsGISAXS程序对一维和二维GISAXS测量结果进行了模拟,模拟结果与实验数据符合很好,表明GISAXS是一种探测锗硅量子点尺寸、形状和分布等结构信息有效的方法。

分形粗糙表面掠入射时的全极化指数计算

为分析经典解析法不能有效求解掠入射时粗糙表面的散射特性,用高阶微扰法计算了二维分形导体表面的后向散射系数。计算值与测量值的比较证明了高阶微扰法的有效性。对不同粗糙度下掠入射时全极化指数的研究,获得了不同入射条件下极化指数与掠入射角余切函数曲线的拟合和有效表达式,修正了前人的结论,并发现用高阶解析法可区分粗糙表面的类型。