Pt/C催化剂中纳米Pt颗粒团聚效应的小角X射线散射

应用小角X射线散射(SAXS)技术,对乙二醇合成法、浸渍还原法和微波加热法制备的Pt/C催化剂粉体内纳米Pt颗粒的团聚效应进行了研究,得到了不同方法制备的Pt颗粒及其团聚体的特征尺寸、体积分布、表面积变化、团聚程度等信息,并利用透射电镜（TEM）对3种样品进行了测试。实验结果表明:微波加热法制备的催化剂中,Pt颗粒较好地分散于C载体上,且Pt颗粒具有尺度小、分布范围窄、总表面积大和团聚体较少等特征;常规浸渍和乙二醇还原两种方法制备的催化剂中Pt颗粒大小分布相似,但乙二醇还原法制备的催化剂总表面积和团聚体尺度更大,数量也更多。     

用小角X射线散射研究纳米粒子的粒度分布

采用小角X射线散射中的对数高斯分布函数的方法，确定了纳米粒子的粒度分布。通过理论分析、计算，对氧化锌纳粒子进行实验测试。结果表明，氧化锌纳米粒子的平均半径尺寸为3．34nm，分布的标准偏差为1．35。     

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。     

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.     

小角X射线散射表征非晶合金纳米尺度结构非均匀

表征纳米尺度结构非均匀对于理解非晶合金的变形、弛豫等动力学行为至关重要.受时空尺度限制,非晶合金纳米尺度结构非均匀的实验表征具有很大的挑战性.本文针对一种典型的锆基非晶合金,开展了同步辐射小角X射线散射原位拉伸实验.通过对散射曲线的定量分析,揭示了非晶合金在纳米尺度的非均匀结构图像.首先,Porod散射曲线呈现正偏离行为,表明非晶合金属于非理想两相散射体系,两相界面弥散且任一相内都存在电子密度涨落.基于散射曲线的Guinier定律分析,进一步揭示非晶合金中散射体形状远偏离球形,其特征尺度主要分布在0.8—1.6 nm之间,且在弹性变形阶段几乎不变.最后,通过Debye相关函数分析,发现这些纳米尺度散射体仅在1 nm之内存在强关联,符合非晶合金短程有序、长程无序的结构特征.研究结果表明非晶合金中存在具有复杂空间分布的纳米尺度非均匀结构.     

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。     

纳米催化剂Pt/C的X射线衍射线形分析

X射线衍射线形与晶体材料的微观结构密切相关.在晶粒尺寸衍射线形和微应变衍射线形可由Voigt函数近似描述的前提下,本文较详细地论述了由X射线衍射线形分析获取晶粒尺寸和位错等微观结构信息的方法.采用这种方法,对乙二醇还原法制备的Pt/C催化剂进行了X射线衍射线形分析.样品晶粒尺寸分布的对数正态均值为0.95 nm,对数正态方差为0.37.X射线衍射线形分析所得晶粒尺寸分布与透射电镜的测试结果符合较好.对样品的衍射线形积分宽度进行细致的比较,发现存在各向异性展宽现象.如果衍射线的各向异性展宽主要是由伯格斯矢量为1/2〈110〉的位错引起,可进一步计算位错密度值.结果表明,位错组态无论是螺型位错还是刃型位错,位错密度值的量级均约为1015/m2.     

Effect of borohydride as reducing agent on the structures and electrochemical properties of Pt/C catalyst

In this paper, we found that boron deposited on the surface of support when sodium borohydride used as reducing agent during the preparation of Pt/C catalyst. The deposition of boron markedly reduces particle size of Pt, raises electrochemical active surface (EAS) area of catalyst and electrochemical activity for hydrogen evolution or oxygen reduction reaction (ORR) compared with which prepared using other reducing agents (hydrogen and formaldehyde).     

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.     

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 developing 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 1W2A 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.     

Small angle neutron scattering and small angle X-ray scattering studies of platinum-loaded carbon foams

The morphology of carbon nanofoam samples comprising platinum nanoparticles dispersed in the matrix was characterized by small angle neutron scattering (SANS) and small angle X-ray scattering (SAXS) techniques. Results show that the structure of pores of carbon matrix exhibits a mass (pore) fractal nature and the average radius of the platinum particles is about 2.5 nm. The fractal dimension as well as the size distribution parameters of platinum particles varies markedly with the platinum content and annealing temperature. Transmission electron micrographs of the samples corroborate the SANS and SAXS results.      

Tunable interface anisotropy in a Pt/Co_(1-x)Fe_x/Pt multilayer

Interfacial magnetic anisotropy in a Pt/Co1-xFex /Pt multilayer is tuned by doping iron atoms into the cobalt layer.The perpendicular magnetic anisotropy and out-of-plane coercivity are found to decrease with increasing x.For a specific x,the out-of-plane coercivity acquires a maximal value as a function of the thickness of the CoFe layer.At low temperature,the coercivity is enhanced.Small coercivity but reasonably large perpendicular magnetic anisotropy can be obtained by controlling the x and CoFe layer thickness.     

Structural and magnetic properties of Pt in Co/Pt multilayers

[Co(30 Å)/Pt(x Å)]₂₀ multilayers with the Pt layer thicknesses varying from 5 Å to 20 Å were characterized structurally by high angle X-ray diffraction, X-ray reflectivity, X-ray absorption spectroscopy and magnetically by X-ray magnetic circular dichroism. It is found that the structure and magnetic properties of Pt have a strong correlation with the Pt layer thickness. The 20 Å thickness Pt layer is not almost influenced by the adjacent Co layer and the nearest neighbors are dominated by Pt-Pt shells. With decreasing Pt layer thickness, the nearest neighbors are gradually dominated by Pt-Co shells and the Pt-Co intermixing regions also remarkable increase at the interfaces, especially for the 5 Å thickness Pt layer. The orbital and spin magnetic moments as well as the ratio m_orb/m_spin all decrease systematically with increasing Pt layer thickness, indicating that the interface atoms are polarized by direct Pt-Co hybridization, but that the adjacent layers are polarized by Pt-Pt interactions.     

Field-driven creep motion of a composite domain wall in a Pt/Co/Pt/Co/Pt multilayer wire

We have studied the field-driven motion of a pair of coupled Bloch domain walls in a perpendicular magnetic anisotropy Pt/Co/Pt/Co/Pt multilayer Hall bar. The nucleation of an isolated but coincident pair of walls in the two Co layers, observed by Kerr microscopy, took place at an artificial nucleation site created by Ga⁺ ion irradiation. The average velocity v of the wall motion was calculated from time-resolved magnetotransport measurements at fixed driving field H, where the influence of the extraordinary Hall effect leads to the observation of voltages at the longitudinal resistance probes. We observed a good fit to the scaling relation lnv∝H^−1/4, consistent the motion of a single 1-dimensional wall moving in a 2-dimensional disordered medium in the creep regime: the two walls are coupled together into a 1-dimensional composite object.     

Small angle X-ray scattering evidence for the absence of voids in chalcogenide glasses

Small angle X-ray scattering measurements show no evidence for the presence of voids in chalcogenide glasses, in contrast to the situation found in deposited films of Ge and Si. This result and the observation of a diffraction peak near $\text{k = 1.2}\text{A}\text{?}{}^{\mathrm{?1}}$ are found to be consistent with the existence of a layer structure in glassy As₂S₃ and As₂Se₃.