现代测试技术在纳米材料研究中的应用

对电子显微技术、衍射技术、谱学技术及热分析技术的原理、特点及其在纳米材料中的应用作了评述。在此基础上指出：综合使用各种不同的分析和结构表征方法,可对纳米材料的结构和性能进行有效研究,从而指导其应用。     

纳米材料生物效应及其毒理学研究进展

纳米科学与信息科学和生命科学并列, 已经成为21世纪的三大支柱科学领域. 由于纳米材料独特的物理化学性质, 纳米尺度及纳米结构的材料乃至器件, 已逐渐走出实验室, 进入人们的生活. 这些具有独特物理化学性质的纳米材料, 对人体健康以及环境将带来的潜在影响, 目前已经引起科学界, 乃至政府部门的广泛关注. 文中分析综述了几种纳米材料(纳米TiO₂、单壁碳纳米管、多壁碳纳米管及超细铁粉)目前已取得的部分生物效应及毒理学的研究结果, 包括纳米材料在生物体内的分布、作用的靶器官、纳米材料引起的细胞毒性、细胞凋亡等. 文中还评价了纳米颗粒的生物毒性. 纳米颗粒的尺寸越小, 显示出生物毒性的倾向越大; 尽管碳纳米管是由石墨层卷成的圆筒, 但是根据石墨的安全剂量来外推碳纳米管的安全剂量是不可行的, 碳纳米管的生物毒性远大于石墨粉; 表观分子量高达60万的水溶性纳米碳管, 在小鼠体内却显示出小分子的生理行为; 一种正在研究的磁性纳米颗粒在动物体内显示出迅速团聚、堵塞血管等现象. 纳米材料在生物体内呈现出的这些生理现象, 仅利用现有的知识尚无法解释. 最后还介绍了纳米物质生物效应(包括毒理学, 安全性)研究的部分实验方法; 展望了该新领域今后的发展方向和亟待研究的重要问题.     

硫化亚锡有序纳米孔道阵列薄膜的制备与表征

以阳极氧化铝为模板,采用两步复型技术首次制备了一种SnS有序纳米孔道阵列薄膜。SEM和TEM测试结果显示此SnS有序多孔薄膜具有几乎均一的、紧密堆积的、直形的纳米孔道阵列结构,孔道直径约200mm,长度约1μm。EDS,XPS和XRD分析结果表明此SnS有序多孔薄膜的SnS骨架具有正交SnS的晶体结构,薄膜中锡与硫的原子比接近化学计量比1:1。     

腐蚀后的镀锌钢板表面电子显微表征

通过扫描电子显微镜及其附带的X射线能谱仪对镀锌钢板表面出现腐蚀锈斑、耐腐蚀性能不合格的原因进行了分析.结果表明:镀锌钢板通过热镀工艺生产出来后,未给予足够的镀后防护,同时长时间露在腐蚀性环境中,受到腐蚀产生了白锈甚至红锈,最终导致其耐腐蚀性能不合格,通过一些改进措施可有效的解决质量问题.     

透光导电金属及氧化铂半导体薄膜的制备与表征

通过PPh~3对“非保护型”铂金属纳米簇进行表面修饰,并将其萃取至甲苯中,制备的PPh~3修饰的Pt金属钠米簇于空气中可自发地在玻璃表面生长出均匀透光的金属钠米簇薄膜。该金属钠米簇薄膜经空气中加热处理后可转化为透光导电的氧化铂半导体薄膜。考察了金属钠米簇薄膜生长过程中UV-vis吸收光谱的变化。采用SEM和TEM等方法,表征了纳米簇的粒径及膜的多孔结构,由此解释了其透光原因。研究了薄膜的导电性与处理条件的关系,并采用XPS表征了处理过程中的物质变化。初步探索了PPh~3-Pt纳米簇自发成膜过程的机理,确定了氧气在此过程中的重要作用。     

HMI体系下系列沸石子筛的动态合成与表征

在HMI体系中，采用水热动态晶化法，通过对Si/Al比，碱度，晶化温度，晶化 时间等反应条件进行调变，合成出纯相的MOR，ANA，MCM－56，MCM－49和MCM－22 等多种结构的沸石分子筛，发现反应物Si/Al比决定合成产物的物相，通过XRD， TG－DTA，SEM和TEM等方法研究了分子筛的物理化学性质并对HMI体系中合成的MOR 和ANA的晶体特征进行了表征分析。     

HMI体系下系列沸石子筛的动态合成与表征

在HMI体系中，采用水热动态晶化法，通过对Si/Al比，碱度，晶化温度，晶化 时间等反应条件进行调变，合成出纯相的MOR，ANA，MCM－56，MCM－49和MCM－22 等多种结构的沸石分子筛，发现反应物Si/Al比决定合成产物的物相，通过XRD， TG－DTA，SEM和TEM等方法研究了分子筛的物理化学性质并对HMI体系中合成的MOR 和ANA的晶体特征进行了表征分析。     

纳米材料研究进展Ⅱ：纳米材料的制备,表征与应用

本文综合介绍近十年来纳米材料的制备，表征与应用，探讨了各种方法的特点与适用性。     

纳米材料应用于无酶电化学生物传感器的研究进展

无酶电化学生物传感器具有环境适用性强、稳定性高、材料简单易得、灵敏度高、检测限低等特点,近年来受到研究者广泛关注。纳米材料有类酶活性,表现出类似天然酶的酶促反应动力学和催化机理,且能够增强界面吸附性能,增加电催化活性,并促进电子转移动力学,从而广泛应用于无酶电化学生物传感器。本文探索了具有电催化活性的纳米材料及其修饰电极的制备方法,介绍了无酶电化学传感器在医疗诊断、食品检测、环境检测以及其他领域中的应用,讨论了开发基于纳米材料的电化学传感器的未来机遇和挑战。     

扫描透射电子显微镜技术及其在中药研究中的应用

扫描透射电子显微镜(STEM)兼具透射电子显微镜(TEM)和扫描电子显微镜(SEM)的优势,具有高分辨成像、强原子衬度敏感以及图像易懂、直观等优点,已成为材料微结构和微区分析的必要性工具. 中药研究有着悠久历史,显微技术一直是研究药材微特征和作用机制的重要手段之一,具有其他手段不可替代的作用. 综述了STEM的原理、方法、技术特点,以及其在中药显微结构和纳米颗粒等方面的应用,以期为进一步扩展中药微特征领域的研究作参考.     

基于透射电子显微镜的沸石分子筛结构研究进展

透射电子显微镜是解析沸石分子筛新结构、 分析结构缺陷和研究活性位点等的有力工具. 应用于分子筛研究的透射电子显微术总体上可以分为图像法和衍射法, 包括透射电子显微镜和扫描透射电子显微图像、 选区电子衍射和三维电子衍射, 通常结合其中的几种方法进行分析. 近年来, 随着电子显微镜硬件性能的不断提升, 特别是球差矫正器的广泛应用及各种适用于分子筛等电子束敏感材料的探测器和图像处理技术的不断革新, 在原子尺度观察分子筛的结构已成为可能. 此外, 利用原位电子显微镜技术研究分子筛的生长和催化反应机理也在逐步展开. 本文按电子显微镜方法分类, 综述了近些年基于电子显微镜的分子筛研究, 包括新结构解析、 手性确认和金属负载等的最新进展.     

电子显微镜下的纳米世界

以高中阶段知识为基础,简述了扫描电子显微镜、透射电子显微镜等电镜技术的发展和基本原理,并以实际应用案例介绍了电镜技术在纳米科学领域的应用,最后给出了电镜技术的未来发展前景。     

扫描电镜中背散射电子成像功能的应用

简单介绍了扫描电镜背散射电子成像的工作原理及其应用.利用扫描电镜背散射电子成像结合X-射线能谱来研究样品的微区成分变化,从而快速的了解样品的组成和结构特征,为物相的鉴别提供了有效的分析手段.     

应用分析电子显微镜考察铂锡催化剂上的积炭

在高分散铂锡催化剂上分别以正丁烷,正己烷及长链烷烃为反应物经催化剂脱氢表面积炭。从电子显微镜图像观察到积炭有多种结构,最小的炭粒呈条纹排列,炭粒集聚形成球状炭黑及不同形状的石墨结晶。选区电子衍射分析炭(002)晶面间距有3.35～4.13A变化表明石墨化程度不同。三种积炭样品的电子能量损失谱相应地亦展示明显的差别。     

Atomic Level Characterization Based on Focus Modulation Electron Microscopy

Defocus image modulation processing and three-dimensional Fourier filtering methods are compared from the viewpoint of application to high-resolution phase transmission electron microscopy. Both methods can successfully correct the spherical aberration in TEM by image processing using through-focus images resulting in resolution improvement from the Scherzer resolution limit to the information limit. Comparing the processed images demonstrates that the potential to determine localized atomic structures between the two methods is at the same level when the sample thickness is thin. However, the achieved signal-to-noise ratio is better in images processed by the three-dimensional Fourier filtering method because the filtering process in Fourier space effectively reduces quantum noises involved in the original images. Spherical aberration-free phase observation by the latter method clearly shows the existence of individual gadolinium atoms in C₈₂ molecules encapsulated in single wall carbon nanotubes. It is demonstrated that the three-dimensional Fourier filtering method works effectively for atomic level characterization even when a sample consisting of light atoms is observed under the condition of a low electron dose.     

Studying Ice with Environmental Scanning Electron Microscopy

Scanning electron microscopy (SEM) is a powerful imaging technique able to obtain astonishing images of the micro- and the nano-world. Unfortunately, the technique has been limited to vacuum conditions for many years. In the last decades, the ability to introduce water vapor into the SEM chamber and still collect the electrons by the detector, combined with the temperature control of the sample, has enabled the study of ice at nanoscale. Astounding images of hexagonal ice crystals suddenly became real. Since these first images were produced, several studies have been focusing their interest on using SEM to study ice nucleation, morphology, thaw, etc. In this paper, we want to review the different investigations devoted to this goal that have been conducted in recent years in the literature and the kind of information, beyond images, that was obtained. We focus our attention on studies trying to clarify the mechanisms of ice nucleation and those devoted to the study of ice dynamics. We also discuss these findings to elucidate the present and future of SEM applied to this field.     

Characterization of 3D DNA Assemblies Using Cryogenic Electron Microscopy

DNA nanotechnology utilizes DNA double strands as building units for self-assembly of DNA nanostructures.The specific base-pairing interaction between DNA molecules is the basis of these assemblies.After decades of development,this technology has been able to construct complex and programmable structures.With the increase in delicate nature and complexity of the synthesized nanostructures,a characterization technology that can observe these structures in three dimensions has become necessary,and developing such a technology is considerably challenging.DNA assemblies have been studied using different characterization methods including atomic force microscopy(AFM),scanning electron microscopy(SEM),and transmission electron microscopy(TEM).However,the three-dimensional(3D)DNA assemblies always collapse locally due to the dehydration during the drying process.Cryogenic electron microscopy(cryo-EM)can overcome the challenge by maintaining three-dimensional morphologies of the cryogenic samples and reconstruct the 3D models from cryogenic samples accordingly by collecting thousands of two-dimensional(2D)projection images,which can restore their original morphologies in solution.Here,we have reviewed several typical cases of 3D DNA-assemblies and highlighted the applications of cryo-EM in characterization of these assemblies.By comparing with some other characterization methods,we have shown how cryo-EM promoted the development of structural characterization in the field of DNA nanotechnology.     

Characterization of Collagen/Lipid Nanoparticle–Curcumin Cryostructurates for Wound Healing Applications

Curcumin‐loaded collagen cryostructurates have been devised for wound healing applications. Curcumin displays strong antioxidant, antiseptic, and anti‐inflammatory properties, while collagen is acknowledged for promoting cell adhesion, migration and differentiation. However, when curcumin is loaded directly into collagen hydrogels, it forms large molecular aggregates and clogs the matrix pores. A double‐encapsulation strategy is therefore developed by loading curcumin into lipid nanoparticles (LNP), and embedding these particles inside collagen scaffolds. The resulting collagen/LNP cryostructurates have an optimal fibrous structure with ≈100 µm average pore size for sustaining cell migration. Results show that collagen is structurally unaltered and that nanoparticles are homogeneously distributed amidst collagen fibers. Hydrogels soaked in saline buffer release about 20 to 30% of their nanoparticles content within 24 h, while achieved 100% release after 25 days. When exposed to NIH 3T3 fibroblasts, these hydrogels provide a satisfactory scaffold for cell interaction as early as 4 h after seeding, with no cytotoxic counter effect. These positive features make the collagen/lipid cryostructurates a promising material for further use in wound healing.