高分子材料电镜试样的几种制备方法

目前电子显微镜已在材料学科的一些领域得到了广泛的应用。但是电镜试样制备是比较复杂的。使用电镜进行高分子材料的结构与性     

透射电子显微镜侧插式CCD相机数字图片放大倍数的解析

针对数字化透射电子显微镜与传统透射电子显微镜在观察记录系统上存在的差异,通过比较分析数字化透射电子显微镜侧插式电荷耦合器件(CCD)相机采集的图像、操作界面View视窗观察到的图像与电镜示数放大倍数之间的差异,详细地分析了数字化透射电子显微镜侧插式CCD相机采集的数字图片的放大倍数发生变化的原因.可以帮助应用电镜的广大教师及科研工作者更加快速、直观地掌握数字图片确切的放大倍数,更有利于结果的分析.     

CM200透射电子显微镜保护关机的故障分析及维修

介绍了CM200透射电子显微镜电镜保护(LPR)的工作原理,分析了电镜保护关机的故障原因并介绍了几个维修实例.     

电镜油箱绝缘油变质的处理

高压油箱是电子显微镜(以下简称电镜)的关键性部件。它的工作正常与否会直接影响电镜的性能和使用。由于它是处于高电压的工作状态,技术条件很严格。如果油箱绝缘油老化变质或被污染而使其性能破坏时,应当如何处理呢?现介绍如下方法供参考。     

非水纳米分散系的冷冻蚀刻电镜表征及与激光散射法的对比研究

报道了利用改进的冷冻蚀刻制样技术对非水介质中原位合成的纳米分散系进行的电子显微镜表征结果。研究了冷冻蚀刻电镜技术观测原位合成纳米分散系的制样步骤、制样方法，并利用冷冻蚀刻电镜技术原位观测了3种纳米分散相的粒径、粒径分布和聚集状态。激光散射法与冷冻蚀刻电镜表征的对比表征结果表明：纳米分散系中纳米相的粒径和粒径分布用两种表征方法所得结果基本一致，但冷冻蚀刻电镜表征与激光散射法相比具有准确、直观、清晰、立体的特点，并且可同时采集多种信息。与激光散射法相比，是一种表征非水纳米分散系的理想方法。     

SEM法测量T颗粒厚度

本文利用扫描电子显微镜(SEM)的二次电子影像富有很强的立体感这一特点,对卤化银T颗粒的厚度及宽厚比进行了测量和观察,介绍了这种电镜样品的制备技术,以及利用SEM的倾斜角效应拍摄能反映微粒空间立体形状和T颗粒厚度的方法。     

冷冻电镜技术——2017年诺贝尔化学奖介绍

介绍了2017年诺贝尔化学奖的3位获得者在冷冻电镜领域的主要贡献，同时介绍了冷冻电镜技术的用途、一般工作流程和其局限性，以及中国学者在冷冻电镜技术应用研究中的贡献。     

17O固体核磁共振谱学区分不同晶面取向的氧化物纳米晶

正氧化物纳米晶在催化等领域的应用与其暴露晶面密切相关,因此确定晶面结构是建立构效关系、设计性能更优越的新材料的关键~(1–3)。目前,纳米材料的表面结构主要借助各种电子显微镜技术表征。然而,电镜技术因为观测视野小,所给出的结果可能未必很好地代表整个样品。近期,南京大学化学化工学院彭路明研究员、华东理工大学龚学庆教授等人,以具有代表性的两种锐     

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。     

JSM-5610LV扫描电镜的日常维护及常见故障排除

在扫描电子显微镜的日常维护管理中,应当控制好室内环境因素,保持电镜内部长期处高真空状态,定期检查其附属设备是否达到要求,介绍电镜经常出现的死机、黑屏显示图像不正常等故障的排除方法。     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

A carbanion induced synthesis of highly congested pyrazole and imidazole containing heterocycles

An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Selective synthesis of 4,5-dihydroimidazo- and imidazo[1,5-a]quinoxalines via modified Pictet–Spengler reaction

An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction.     

Understanding the Diels-Alder reactivity of 1,2-azaborine analogues

The Diels-Alder reactivity of 1,2-heteroborines (H₄C₄B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed.