全谱拟合法研究聚丙烯腈基碳纤维形成过程中晶态结构演变

通过全谱拟合法对碳纤维制备过程中不同阶段纤维的XRD谱图进行处理,得到不同阶段纤维的微观结构参数,研究了聚丙烯腈(PAN)基碳纤维制备过程中晶态结构的演变.全谱拟合法基于晶体衍射的严格物理理论,拟合目标为整个衍射谱,并不是个别衍射峰,所得结果具有更高的可信度.研究结果表明:PAN原丝中的高分子链沿纤维轴高度取向,表观晶粒尺寸为6.5 nm左右;经过预氧化处理,纤维中的有序结构遭到破坏,表观晶粒尺寸锐减.纤维中逐渐形成梯形结构并沿纤维轴取向,从而形成新的有序结构;经过碳化处理后,环状梯形结构转变为碳的层状结 关键词： 碳纤维 晶体结构 XRD 全谱拟合法     

GISAXS and SAXS studies on the spatial structures of Co nanowire arrays

The spatial structures of magnetic Co nanowire array embedded in anodic aluminium membranes were investigated by grazing incidence small angle X-ray scattering (GISAXS) and conventional small angle X-ray scattering (SAXS) techniques. Compared with SEM observation, the GISAXS and SAXS measurements can get more overall structural information in a large-area scale. In this study, the two-dimensional GISAXS pattern was well reconstructed by using the IsGISAXS program. The results demonstrate that the hexagonal lattice formed by the Co nanowires is distorted (a ≈ 105 nm, b ≈ 95 nm). These Co nanowires are isolated into many structure domains with different orientations with a size of about 2 μm. The SAXS results have also confirmed that the nanopore structures in the AAM can be retained after depositing Co nanowires although the Co nanowires can not completely but only just fill up the nanopores. These results are helpful for understanding the global structure of the Co nanowire array.     

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.     

用于同步辐射光源的成像板粉末衍射系统

报道了我们研制的一套成像板粉末衍射装置,对其误差来源进行了详细的分析讨论,并与衍射仪进行了比较.该装置的半径为143.3mm,最大测量角度范围不160°，最大角度(2q )偏差小于0.03°,这些性能指标已被实验所证实,完全可应用于粉末衍射全谱的测量.     

PVP掺杂-ZrO2溶胶-凝胶工艺制备多层激光高反射膜的研究

以丙醇锆(ZrPr)为锆源,二乙醇胺(DEA)为络合剂,原位引入聚乙烯吡咯烷酮(PVP),在乙醇体系中成功地合成了PVP掺杂-ZrO2溶胶.采用旋涂法在K9玻璃基片上制备了PVP-ZrO2单层杂化薄膜.用不同掺杂量的PVP-ZrO2高折射率膜层与相同的SiO2低折射率膜层交替沉积四分之一波堆高反射膜.借助小角X射线散射研究胶体微结构,用红外光谱、原子力显微镜、紫外/可见/近红外透射光谱、椭圆偏振仪以及1064nm的强激光辐照实验对薄膜的结构、光学和抗激光损伤性能进行表征.研究发现,体系组成的适当配置可以在溶胶稳定的前提下实现ZrPr的充分水解,赋予薄膜良好的结构、光学和抗激光损伤性能.杂化体系中,DEA与ZrPr之间强的配合作用大大降低了ZrO2颗粒表面羟基的活性,使得PVP大分子只是以微弱的氢键与颗粒的表面羟基作用而均匀分散于ZrO2颗粒的周围,对颗粒的形成和生长无显著影响.因而在实验研究范围内,随PVP含量的增大,PVP-ZrO2杂化膜层的折射率和激光损伤阈值均无显著变化.但是,薄膜中均匀分布的PVP柔性链可以有效促进膜层应力松弛,显著削弱不同膜层之间的应力不匹配程度、大大方便多层光学薄膜的制备.当高折射率膜层中PVP的质量分数达到15%-20%时,膜层之间良好的应力匹配使得多层高反射膜的沉积周期数可达到10以上.沉积1O个周期的多层反射膜,在中心波长1064nm处透射率约为1.6%-2.1%,接近全反射特征,其激光损伤阈值为16.4-18.2J/cm2(脉冲宽度为1ns).     

三相系统部分结晶聚合物结构参数小角X射线散射分析

使用小角X射线散射技术分析了部分结晶聚合物结构参数,结晶度和片层厚度与两相系统中的结果不一致,对一些部分结晶聚合物样品的分析表明它们的Bragg长周期接近相关函数长周期与过渡层厚度的和,这个结论也与部分结晶聚合物存在中间过渡层一致.     

葡萄糖氧化酶电极的研制和血清中葡萄糖的测定

葡萄糖氧化酶电极是研究得最多的酶电极之一。本文以牛血清白蛋白-戊二醛为交联剂,将葡萄糖氧化酶固定于醋酸纤维膜上,自制氧电极作电化学敏感元件,研制成葡萄糖氧化酶电极,并用流动注射法分析血清中葡萄糖量,线性响应范围10~(-6)—10~(-3)M,每张酶膜可连续测定400次血样,用该电极测定血清中葡萄糖,所得结果与酶光度法一致。     

镨叶绿素a分子结构的确定

通过合成镨叶绿素a(Pr-Chla)研究了稀土在叶绿素中的结合方式.Pr-Chla的紫外可见光谱(UV-Vis)、红外光谱(FTIR)证实镨离子已配位到叶绿素a的卟啉环上.其磁圆二色谱(MCD)在Soret带具有双层夹心卟啉的特征结构;通过扩展X射线吸收精细结构谱(EXAFS),采用双层夹心结构模型拟合,确定了Pr周围的近邻结构.表明合成镨叶绿素a具有双层夹心结构.Pr(Ⅲ)夹于两个卟啉环之间,与上下卟啉环上共8个N原子配位,Pr-N键平均键长0.242nm.     

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

The nanopore structures in precursors are crucial to the performance of PAN-based carbon fibers. Four carbon-fiber precursors are prepared. They 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.     

Hierarchical structure and biomineralization in cricket teeth

The cricket is a truculent insect with stiff and sharp teeth as a fighting weapon. The structure and possible biomineralization of cricket teeth are always interesting. Synchrotron radiation X-ray fluorescence, X-ray diffraction, and small angle X-ray scattering techniques were used to probe the element distribution, possible crystalline structures and size distribution of scatterers in cricket teeth. A scanning electron microscope was used to observe the nanoscaled structure. The results demonstrate that Zn is the main heavy element in cricket teeth. The surface of a cricket tooth has a crystalline compound like ZnFe2(AsO4)2(OH)2(H2O)4 . The interior of the tooth has a crystalline compound like ZnCl2 , which is from the biomineralization. The ZnCl2-like biomineral forms nanoscaled microfibrils and their axial direction points towards the top of the tooth cusp. The microfibrils aggregate randomly into intermediate filaments, forming a hierarchical structure. A sketch map of the cricket tooth cusp is proposed and a detailed discussion is given in this paper.