一款小角X射线散射测量专用样品旋转装置

在小角X射线散射实验中经常需要对各向异性结构样品进行旋转。针对传统样品架为固定方式,旋转调整困难的特点,本文设计了一款小角X射线散射专用的样品旋转装置。该装置主要由步进电机、高精度回转轴承、传动系统、样品架、控制器及配套软件等组成,它具有结构简单、回转精度高、可远程控制的特点。在北京同步辐射小角X射线散射实验站应用该样品旋转装置对石墨纤维样品进行了测试,验证了该装置的可行性。     

用小角X射线散射法研究溶胶结构

采用溶胶凝胶方法在碱性条件下制备了SiO2和ZrO2溶胶,应用同步辐射小角X射线散射(SAXS)法研究了溶胶的结构.结果表明,溶胶粒子是多分散的,其生长、聚集受RLCA和Eden模型的共同控制,是一种非线性的动力学过程,所形成的聚集体呈随机、分岔、稠密不同的结构,具有质量分形的特征.同时还发现所研究溶胶的散射曲线均不遵守Porod定理,形成负偏离或正偏离,这说明在溶胶粒子与分散介质间有过渡相存在.对上述偏离进行了定性和定量的分析,提出了正偏离时的定量解析方法,从而得到了胶体系统中有关过渡层(界面层)结构的 关键词：     

小角X射线散射实验数据的初步处理

介绍北京同步辐射装置(BSRF)小角X射线散射实验站实验数据的初步处理方法,即由成像板探测器检测到的散射信号转换成角度及其对应的强度数据的方法,并对数据转换过程中可能遇到的问题进行了详细的讨论.     

北京同步辐射装置新建的X射线小角散射站投入运行

北京同步辐射装置（BSRF）是利用同步辐射光源进行科学研究的装置、对社会开放的大型公用科学设施，是我国凝聚态物理、材料科学、化学、生命科学、资源环境及微电子等交叉学科开展科学研究的重要基地。随着小角X射线散射（SAXS）用户的增长。BSRF原有的小角X射线散射站与X射线衍射站分时使用、共享489A光束线已远不能满足需求，广大用户强烈要求新建一条小角X射线散射站。     

同步辐射小角X射线散射研究

应用同步辐射小角X射线散射研究了二醋酸纤维素接枝聚甲基丙烯酸甲酯在二氯甲烷和甲醇4:1的混合溶剂中的尺寸和形态. 结果表明接枝共聚物在溶剂中形成单分子微球. 微球的尺寸随支链的长度增加而增大.     

小角X射线散射法测定溶胶平均界面厚度

溶胶界面层厚度通常是用Porod法对高角区负偏离的Porod曲线进行拟合求算,但本文研究表明还可通过分别测定Porod负偏离校正前后体系粒子的平均半径之差而获得平均界面厚度.应用上述方法测定了在不同制备条件下制备的二氧化硅溶胶的平均界面厚度 关键词： 小角X射线散射 溶胶 平均界面厚度     

小角X射线散射法测定溶胶平均界面厚度

溶胶界西层厚应通常是用Porod法对高角区负偏离的队Porod曲线进行拟合求算,但本文研究表明还可通过分别测定Porod负偏离校正前后体系粒子的平均阗径之差而获得平均界面厚度。应用上述方法测定了在不同制备条件下制备的二氧化硅溶胶的平均界面厚度。     

新建北京同步辐射小角X射线散射站的必要性

本文分析了同步辐射小角X射线散射的特点与应用、国内外现状及新建北京同步辐射小角X射线散射站的必要性与机遇。     

我国同步辐射小角X光散射装置

小角X光散射是当X光照射到物质上时发生的在原光束附近小角度范围内的电子相干散射,凡是存在纳米尺度的电子密度不均匀区的物质均会产生小角X光散射现象,因此它是表征纳米、多孔材料结构的理想手段。普通X光源产生的X光强度弱,限制了小角X光散射的应用,采用同步辐射为X光源,则可以大大提高X光强度。目前我国已建立同步辐射小角X光散射站,本文对其装置进行了介绍。     

小角X射线散射中宇宙线噪声去除方法

针对小角X射线散射（SAXS）测量图样中的宇宙线提出一种去除方法,以纳米结构的周期信息为物理先验计算得到周期性散射信号的坐标信息,对各光斑级次有效信号区域内的宇宙线进行检测并去除。数值模拟了含宇宙线的SAXS测量图样序列,测试该方法对SAXS测量图样序列宇宙线的检测和去除效果,并与现有的宇宙线去除方法进行对比。计算不同曝光时间下去噪前和各方法去噪后SAXS测量图样的评价指标,可以说明该方法对于SAXS测量图样中的宇宙线具有良好的去除效果,并能在长曝光条件下获得明显的信噪比增益。     

In situ SAXS studies of the formation of sodium jarosite

This paper reports the results of time‐resolved synchrotron small‐angle scattering and powder diffraction experiments where natrojarosites were synthesized in situ in order to observe the species produced at the earliest stages of nucleation. The sample temperatures were 333, 353 and 368 K. These compounds were synthesized by co‐precipitation from solution on the Small and Wide Angle Scattering and Powder Diffraction beamlines at the Australian Synchrotron. Scattering data were collected continuously throughout the syntheses. The results presented here show that the first particles to form in solution appear to be amorphous and nucleate on the walls of the reaction vessel. Crucially, there is a single nucleation event which forms particles with an elliptical disc morphology which then grow uniformly before natrojarosite crystallization is observed in complementary powder diffraction data. This nucleation event may represent the key to controlling the growth of jarosites in industrial and environmental settings.     

In Situ Liquid SAXS Studies on the Early Stage of Calcium Carbonate Formation

Calcium carbonate is a model system to investigate the mechanism of solid formation by precipitation from solutions, and it is often considered in the debated classical and nonclassical nucleation mechanism. Despite the great scientific relevance of calcium carbonate in different scientific areas, little is known about the early stage of its formation. Therefore, contactless devices are designed that are capable of providing informative investigations on the early stages of the precipitation pathway of calcium carbonate in supersaturated solutions using classical scattering methods such as wide‐angle X‐ray scattering (WAXS) and small‐angle X‐ray scattering (SAXS) techniques. In particular, SAXS is exploited for investigating the size of entities formed from supersaturated solutions before the critical conditions for amorphous calcium carbonate (ACC) nucleation are attained. The saturation level is controlled and kept constant by mixing four diluted solutions (i.e., NaOH, CaCl₂, NaHCO₃, H₂O) at constant T and pH. The scattering data are collected on a liquid jet generated about 75 s after the mixing point. The data are modeled using parametric statistical models providing insight about the size distribution of denser matter in the liquid jet. Theoretical implications on the early stage of solid formation pathway are inferred.     

Real-Time Reconstruction of Arbitrary Slices for Quantitative and In Situ 3D Characterization of Nanoparticles

A detailed 3D investigation of nanoparticles at a local scale is of great importance to connect their structure and composition to their properties. Electron tomography has therefore become an important tool for the 3D characterization of nanomaterials. 3D investigations typically comprise multiple steps, including acquisition, reconstruction, and analysis/quantification. Usually, the latter two steps are performed offline, at a dedicated workstation. This sequential workflow prevents on-the-fly control of experimental parameters to improve the quality of the 3D reconstruction, to select a relevant nanoparticle for further characterization, or to steer an in situ tomography experiment. Here, an efficient approach to overcome these limitations is presented, based on the real-time reconstruction of arbitrary 2D reconstructed slices through a 3D object. Implementation of this method may lead to generalized implementation of electron tomography for routine nanoparticle characterization in 3D.     

In Situ Transmission Electron Microscopy Observation of Melted Germanium Encapsulated in Multilayer Graphene

Germanene is a two-dimensional germanium (Ge) analogous of graphene, and its unique topological properties are expected to make it a material for next-generation electronics. However, no germanene electronic devices have yet been reported. One of the reasons for this is that germanene is easily oxidized in air due to its lack of chemical stability. Therefore, growing germanene at solid interfaces where it is not oxidized is one of the key steps for realizing electronic devices based on germanene. In this study, the behavior of Ge at the solid interface at high temperatures is observed by transmission electron microscopy (TEM). To achieve such in situ heating TEM observation, this work fabricates a graphene/Ge/graphene encapsulated structure. In situ heating TEM experiments reveal that Ge like droplets move and coalesce with other Ge droplets, indicating that Ge remains as a liquid phase between graphene layers at temperatures higher than the Ge melting point. It is also observed that Ge droplets incorporate the surrounding amorphous Ge as Ge nuclei, thereby increasing its size (domain growth). These results indicate that Ge crystals can be grown at the interface of van der Waals materials, which will be important for future germanene growth at solid interfaces.     

In Situ Dimensional Characterization of Magnetic Nanoparticle Clusters during Induction Heating

The study and fundamental understanding of magnetic nanoparticle induction heating remains critical for the advancement of magnetic hyperthermia technologies. Complete characterization of not only the nanoparticles themselves but their interparticle behavior in a sample matrix is necessary to accurately predict their heating response. Herein, an in situ method for measuring the extent of nanoparticle clustering during induction heating using small-angle and ultrasmall-angle neutron scattering facilities at the National Institute of Standards and Technology Center for Neutron Research is described and implemented by comparing two sets of iron oxide nanoparticles with differing structures and magnetic properties. By fitting the scattering profiles to a piecewise model covering a wide Q-range, the magnitude of nanoparticle clustering during induction heating is quantified. Observations of the low-Q intensity before and after heating also allow for relative measurement of the cluster volume fraction during heating. The use of this method can prove to be advantageous in both developing more encompassing models to describe magnetic nanoparticle dynamics during heating as well as optimizing nanoparticle synthesis techniques to reduce aggregation during heating.     

An In Situ Testing Method for Analyzing the Changes of Active Groups in Coal Oxidation at Low Temperatures

This study details an in situ Fourier transform infrared spectroscopy analytical system that was employed to follow chemical variations in the functional groups on coal surface during the oxidation process at low temperatures. In the reported in situ Fourier transform infrared spectroscopy system, a special chamber was used to contain the coal powders, and a gas inlet tube and a programmable heater were used to simulate different reaction atmospheres and temperatures. The comparisons between in situ and ex situ Fourier transform infrared spectroscopy spectra indicate that the in situ Fourier transform infrared spectroscopy data offer a more accurate reflection of changes in the functional groups. The real-time changes of aliphatic hydrocarbon groups and oxygen-containing groups in a lignite coal sample were analyzed from 30°C to 220°C using in situ Fourier transform infrared spectroscopy. The experimental results indicate that the chemical variations in the functional groups are affected by their relative chemical activities. The results show that the presence of aliphatic groups on the coal surface varies with temperature. Over the range of 30–70°C the presence of these groups decreases, but then their abundance increases over the range of 70–180°C and finally decreases again when the temperature is increased to between 180°C and 220°C. With respect to oxygen-containing functional groups, three various trends were observed as the test temperature was varied. Our conclusion was that these variations are a function of the reaction activities of the various oxygen-containing functional groups.     

催化研究中的原位Raman光谱技术

研制了分别适用于Ｍａｃｒｏ－Ｒａｍａｎ及Ｍｉｃｒｏ－Ｒａｍａｎ谱仪的高性能原位样品池。性能指标温度：从１７３Ｋ－１０７３Ｋ连续可调，精度±０．５－２Ｋ；压力：常压至１０ＭＰａ．真空度：１０－６ｔｏｒ：相态：气固相及液相。指标表明，多数类型的化学反应都可以在上述样品池内再现。此外，还提出了建立光谱——色谱——质谱——微型反应器联用装置的技术方案，用于考察反应过程催化剂表面结构，吸附物种与产物三者之间的内在联系，以期将催化反应机理的研究提高到原位动态分子水平。     

The stopped‐drop method: a novel setup for containment‐free and time‐resolved measurements

A novel setup for containment‐free time‐resolved experiments at a free‐hanging drop is reported. Within a dead‐time of 100 ms a drop of mixed reactant solutions is formed and the time evolution of a reaction can be followed from thereon by various techniques. As an example, a small‐angle X‐ray scattering study on the formation mechanism of EDTA‐stabilized CdS both at a synchrotron and a laboratory X‐ray source is presented here. While the evolution can be followed with one drop only at a synchrotron source, a stroboscopic mode with many drops is preferable for the laboratory source.     

Study of Morphology and Mechanical Properties of In Situ PP/PS Alloy

The in situ polypropylene (PP)/polystyrene (PS) alloy was prepared in the presence of dicumyl peroxide (DCP). Purified styrene (St) and pre‐polymerized styrene (PSt), forming a dispersed PS phase in the PP matrix would react with PP matrix to form PP‐g‐PS graft co‐polymers acting as a compatibilizer in these alloys, leading to the formation of in situ PP/PS alloys with in situ compatibilizer during reactive blending in a mixer. The morphology development of the alloy was examined by scanning electron microscopy (SEM) and was described using the characteristic length L and the average characteristic length L_m. The shape of the dispersed PS phase was regular and the distribution of PS particles was uniform. Tensile properties of the alloy were improved with mixing time and fluctuated in a certain composition range.