Small-angle X-ray scattering investigation of aging behavior of Al-Cu-Mg-Ag alloys using synchrotron radiation

The aging behavior of Al-Cu-Mg-Ag alloys with high Cu/Mg was studied by transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS) using synchrotron radiation. TEM study reveals that the major strengthening phases of the alloy after aging at 160?C for 10 h are Ω and less θ′. SAXS study shows that the scattering patterns are composed of several concentric circles at the beginning of aging process, which is replaced by the butterfly-wings scattering patterns with the increase of aging time. The butterfly-wings scattering patterns are composed of several branches. The angles between the branches are roughly equal to that between the habit planes of precipitates. The evolution of Guinier radius with aging time indicates the good coarsening resistance of the precipitates. The evolution of integrated intensity is consistent with the classical two-step precipitation process.

Investigation of the topological shape of bovine serum albumin in solution by small-angle x-ray scattering at Beijing synchrotron radiation facility

This paper reports that at a newly constructed small-angle x-ray scattering station of Beijing Synchrotron Radia- tion Facility, the topological shape of ligand-free bovine serum albumin in solution has been investigated. An appropriate scattering curve is obtained and the calculated value of the gyration radius is 31.2~=t=0.25 ~_ （11=0.1 nm） which is co- incident with other ones＇ results. It finds that the low-resolution structure models obtained by making use of ab initio reconstruction methods are fitting the crystal structure of human serum albumin very well. All of these results perform the potential of the beamline to apply to structural biology studies. The characteristics, the defects, and the improving measures of the station in future are also discussed.

The Significance of Solutions Obtained from Ill-Posed Systems of Linear Equations Constituted by Synchrotron Radiation Based Anomalous Small-Angle X-Ray Scattering

Synchrotron radiation based experimental techniques known as Anomalous Small-Angle X-ray Scattering (ASAXS) provide deep insight into the nanostructure of uncountable material systems in condensed matter research i.e. solid state physics, chemistry, engineering and life sciences thereby rendering the origin of the macroscopic functionalization of the various materials via correlation to its structural architecture on a nanometer length scale. The techniques constitute a system of linear equations, which can be treated by matrix theory. The study aims to analyze the significance of the solutions of the stated matrix equations by use of the so-called condition numbers first introduced by A. Turing, J. von Neumann and H. Goldstine. Special attention was given for the comparison with direct methods i.e. the Gaussian elimination method. The mathematical roots of ill-posed ASAXS equations preventing matrix inversion have been identified. In the framework of the theory of von Neumann and Goldstine the inversion of certain matrices constituted by ASAXS gradually becomes impossible caused by non-definiteness. In Turing’s theory which starts from more general prerequisites, the principal minors of the same matrices approach singularity thereby imposing large errors on inversion. In conclusion both theories recommend for extremely ill-posed ASAXS problems avoiding inversion and the use of direct methods for instance Gaussian elimination.

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.

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

Small angle X-ray scattering (SAXS) was used to study the effect of dissolved CO2 on the conformation of polystyrene (PS) in PS/tetrahydrofuran(THF) solution at 308.15 K and at pressures up to 3 MPa. The cloud pressure and the expansion curve of the solution were also determined. The dependence of the conformation on pressure was discussed.

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.

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.

同步辐射SAXS技术研究Al(OH)_(3)胶体的分形结构

本论文以Al(OH)_(3)胶体为研究对象,使用同步辐射SAXS技术并结合FTIR、SEM、DLS、Zeta potential表征手段,考察了Al(OH)_(3)胶体粒子在老化时间0-135 min下的分形结构演化规律,并提出了一种可能的生长机制。不同老化时间下的双对数坐标图呈现明显的线性,说明胶体样品存在分形结构。结果表明,随着老化时间的延长,质量分形维数D_(m)由25 min时的2.29增加至85 min的2.78;95 min-135 min时,D_(m)值在2.76-2.79范围内,基本不发生变化。这说明,老化时间在25 min-85 min时,体系初级颗粒由最初的相对分散状态快速团聚为大尺寸的团簇,最后形成致密的凝胶。95 min-135 min,凝胶过程已经完成,胶粒尺寸不发生变化,135 min时胶块可能发生破裂。

同步辐射小角X射线散射研究PAN原丝制备过程中孔结构的演变

采用同步辐射小角X射线散射研究了PAN原丝制备过程中纤维孔结构的演变。结果表明,在水洗工艺中,纤维孔隙较多、较大,孔径分布较宽,近似圆形;在热水牵伸工艺中,纤维孔隙仍较多、较大,孔径分布较宽,近似椭圆形,长轴约17 nm^21 nm,短轴约4 nm^11 nm;在干燥致密化工艺中,孔隙急剧减少、减小,孔径分布较窄,沿纤维轴向约7 nm^9nm,垂直纤维轴向约2 nm;经过蒸汽牵伸,孔隙又增多、增大,孔径分布变宽,孔隙沿纤维轴向被牵伸得很长,近似梭形;但是随后的松弛热定型又使孔隙减小,孔径分布变窄。

高密度聚乙烯的拉伸塑性形变与空洞化行为

通过改变高密度聚乙烯(HDPE)试样的结晶条件得到3种不同片晶厚度的HDPE试样。采用同步辐射小角X射线散射技术在线观察HDPE试样在单轴拉伸过程中的微观结构演变。实验结果表明,薄片晶试样(片晶厚度为13.8 nm)在拉伸过程中发生塑性形变,试样经历了应力诱导的晶块破碎和重结晶过程;厚片晶试样(片晶厚度分别为21.3 nm和28.1 nm)在拉伸初期出现空洞化现象,在线实验证明了空穴的发生及转向;具有相似结晶度但不同片晶厚度的体系,产生的空穴形状也不同,片晶越厚,塑性形变的能力越差。

剪切速率对等规聚丙烯的结晶和形貌的影响

利用同步辐射小角X射线散射、广角X射线衍射和差示扫描量热法研究了不同剪切速率下等规聚丙烯的结晶结构.结果表明,施加剪切会导致β晶生成,但基本不改变样品总结晶度.β晶含量随着剪切速率的提高先升高后降低,与α晶具有竞争关系.当剪切速率在10~32 s^(-1)之间时,α晶和β晶共存,并存在分属于两种晶型的两组长周期,其中较大的长周期属于β晶.