原位液相透射电子显微镜及其在 纳米粒子表征方面的应用

近年来,基于透射电子显微技术、微纳加工技术和薄膜制造技术的发展,原位液相透射电子显微技术产生,为构建多种纳米级分辨率尺度下的微实验平台,发展新型纳米表征技术和众多领域的相关研究提供了途径.本文首先介绍了应用于原位液相透射电子显微技术的液体腔设计要求,然后介绍了液体腔的发展和典型的制备工艺,最后综述了近年来液体腔透射电子显微镜在纳米粒子成核和生长方面的应用研究,并探讨了该技术前沿发展面临的机遇和挑战.本文将为提高我国先进纳米表征技术和原子精准构筑技术提供相关讨论和支持.     

电子束敏感材料的原子尺度结构研究

分子筛和金属有机骨架(MOF)材料以其独特的孔道和骨架结构在催化、 储能、 干燥及净化和吸附分离等领域有着广泛应用, 对其结构的原子尺度表征对于深入理解其构效关系具有重要意义. 但其大孔道结构和有机骨架使得它们对电子束辐照极为敏感, 在常规透射电镜成像模式下结构会很快被破坏变为非晶, 从而无法获得孔道和骨架的原子排列信息. 最近发展起来的基于积分差分相位衬度扫描透射电子显微(iDPC-STEM)技术在电子敏感材料和轻元素组分成像方面展现出明显优势, 使得对多孔骨架材料及烃池物种的表征成为了可能. 本文综述了本课题组近期利用该技术对分子筛和MOF材料原子尺度结构方面的研究. 将iDPC-STEM技术应用到ZSM-5分子筛催化剂中, 实现了对该分子筛的原子级骨架结构的成像分析. 在MOF体系中, 利用该技术观察到MIL-101骨架内部有机连接体与金属节点的配位方式, 在此基础上解析了MIL-101结构中有机配体的连接和金属节点的苯环结构, 并观察了MOF的原子级表面、 界面和缺陷等局域结构特征. 最后对iDPC-STEM技术在原子尺度成像方面的应用潜力进行了总结与展望.     

透射电镜三维重构确定杂化嵌段共聚物两相空间分布

多金属氧酸盐(POM)簇-聚合物杂化物是一类兼有无机材料催化性能和聚合物可加工性的,具有优异应用前景的杂化材料。POM簇-聚合物杂化物中两相的空间分布对材料的性能有至关重要的影响。但该材料纳米尺度的3D两相空间形貌和结构无法用常规的透射电镜观察和表征。本文利用透射电镜的三维重构技术,选择合适的参数和方法进行二维图像的采集、图像匹配对中及重构,并完成立体模型的构建,从而通过构建的模型对三种杂化共聚物的两相空间分布进行了确认和分析。     

沉淀对A1-Cu—Mg合金中锯齿形屈服现象影响及其微观实验研究

经固溶处理的A1-Cu—Mg合金在常应变率拉伸实验中具有显著的锯齿形屈服现象，且屈服行为随固溶处理温度的改变而呈现不同的特征。塑性变形特性与合金材料的微细观结构，尤其是位错运动的演化密切相关。本文运用透射电子显微镜，研究在不同温度下固溶处理的Al—Cu—Mg合金的微观结构，尤其是析出颗粒的大小和含量。并结合宏观的拉伸实验结果，分析Al—Cu—Mg合金动态应变时效的机制。     

TDX-200TEM物镜磁路缺陷对物镜性能影响研究

基于TDX-200透射电子显微镜(Transmission Electron Microscope,TEM),利用ANSYS软件仿真物镜磁路存在空隙、凹陷、凸起缺陷时物镜轴上的磁场分布,在此基础上利用MEBS软件仿真物镜激励、球差系数等性能参数,分析了各磁路缺陷对物镜分辨率的影响。结果表明,在相同加速电压下,相对于空隙缺陷、凸起缺陷对物镜分辨率的影响,凹陷缺陷对物镜分辨率的影响最大。在200k V加速电压下,当物镜存在直径为0.5mm的半圆形凹陷环缺陷时,实际分辨率相对于理想分辨率的变化量可达到9.68%。     

JEM-2100PLUS透射电子显微镜操作方法与技巧及常见故障排除

以JEM-2100PLUS透射电子显微镜为例，介绍了电镜的基本结构、操作面板和成像原理。使用透射电子显微镜的最终目的就是要得到高质量的照片，结合透射电镜的操作步骤，总结了如何拍摄高质量的照片以及常见故障排除方法。     

不同变质程度煤的高分辨率透射电镜分析

利用高分辨率透射电子显微镜(HRTEM)分析了三种不同变质程度煤样的结构特征。基于傅里叶-反傅里叶变换方法,并结合Matlab、Arcgis和Auto CAD软件,通过图像分析技术,获得了HRTEM照片的晶格条纹参数。结果表明,三种煤样的晶格条纹呈现不同特征,按条纹长度分别归属于1×1-8×8共计八个类型。以3×3为临界点,在1×1和2×2中,ML-8中芳香层片的比例高于DP-4和XM-3;在3×3-8×8中,ML-8中芳香层片的比例低于DP-4和XM-3。对比HRTEM和XRD参数d002发现,随着镜质组反射率的增加d002都呈现递减趋势。     

Preparation and Photocatalytic Activity of Ce,H3PW12O40 co-doped TiO2 Hollow Fibers

A series of Ce, H3PW12O40 co-doped TiO2 hollow fibers photocatalysts have been prepared by sol-gel method using ammonium ceric nitrate, H3PW12O40 and tetrabutyltitanate as precursors and cotton fibers as template, followed by calcination at 500 ℃ in N2 atmosphere for 2 h. Scanning electron microscopy, X-ray diffraction, nitrogen adsorption-desorption mea- surements, and UV-Vis spectroscopy are employed to characterize the morphology, crystal structure, surface structure, and optical absorption properties of the samples. The photo- catalytic performance of the samples has been studied by photodegradation phenol in water under UV and visible light irradiation. The results show that the TiO2 fiber materials have hollow structures, and the co-doped TiO2 hollow fibers exhibit higher photocatalytic activities for the degradation of phenol than un-doped, single-doped TiO2 hollow fibers under UV and visible light. In addition, the recyclability of co-doped TiO2 fibers is also confirmed that the TiO2 fiber retains ca. 90% of its activity after being used four times. It is shown that the co-doped TiO2 fibers can be activated by visible light and may be potentially applied to the treatment of water contaminated by organic pollutants. The synergistic effect of Ce and H3PW12O40 co-doping plays an important role in improving the photocatalytic activity.     

Study of In Situ Formation of Magnesium Hydroxide Whisker via Basic Magnesium Chloride Whisker Regulated by Organic Parcels at Low Temperature

In this work, we demonstrate an in situ phase conversion from basic magnesium chloride（BMC） into magnesium hydroxide whisker by using polar organic solvent at low temperature. The morphology and phase composition of magnesium hydroxide whiskers prepared at different reaction temperature, alkali concentration and organic solvent were analyzed by X-ray diffraction（XRD） and scanning electronic microscope（SEM）. It was found that when one of the organic solvents such as absolute ethyl alcohol, butanol, polyethylene glycol（PEG-400）, acetone, et al. was selected as the template, the precursor BMC can transform into whisker-like magnesium hydroxide through precipitate transformation in low temperature and non-hydrothermal system. It can be reasonably explained that the regulation of Mg^2＋ solubility by those organic solvents and the sustained release of Mg^2＋ dissolution by organic adsorption played a significant role in the formation of magnesium hydroxide whisker via BMC whisker as the precursor.     

Electrospinning of nylon-6,6 solutions into nanofibers: Rheology and morphology relationships

The relationship between the rheological properties of nylon-6,6 solutions and the morphology of their electrospun nanofibers was established. The viscosity of nylon-6,6 in formic acid(90%) was measured in the concentration range of 5 wt%-25 wt% using a programmable viscometer. Electrospinning of nylon-6,6 solutions was carried out under controlled parameters. The chemical structure, morphology and thermal properties of the obtained nanofibers were investigated using Fourier transform infrared spectroscopy(FTIR), scanning electron microscopy(SEM) and differential scanning calorimetry(DSC), respectively. Entanglement concentration(ce) was found to be 15 wt% and a power law relationship between specific viscosity and solution concentration was observed with exponents of 2.0 and 3.3 for semi-dilute unentangled(c ce) and semi-dilute entangled(c ce) regimes, respectively. The diameter and uniformity of the nanofibers were found to be dependent on the viscosity. Moreover, the average diameter of electrospun nanofibers was found to be dependent on zero shear rate viscosity and normalized concentration(c/ce) in a power law relationship with exponents of 0.298 and 0.816, respectively. For nylon-6,6 solutions, the entanglement concentration(ce = 15 wt%) provides the threshold viscosity required for the formation of a stable polymeric jet during electrospinning and producing uniform beadless fibers. For concentrations less than ce, beaded fibers with some irregularities are formed. DSC analysis showed an increase in crystallinity of all electrospun samples compared to original polymer. Furthermore, Based on FTIR spectroscopy, α phase is dominant in electrospun nanofibers and minor amount of β and γ phases is also available.