Towards property nanom easurements by in- situTEM- presentand prospects

纳米材料的研究无论是在基础科学还是在应用技术上都面临着许多新的挑战。纳米材料的性能极大地取决于它们的尺寸和形状。测量大面积或大量的纳米材料所得的性能是整个样品的平均值,因此,单个纳米颗粒或单根纳米管的不寻常的特性就被掩盖了。测量由原子结构所决定的单一纳米结构的性能是纳米科学的一个基本方向。对现有的测试技术和试验方法来说,表征单一纳米颗粒纳米管纳米纤维的性能是一难题。首先,因为它的尺寸(直径和长度)相当小,现有的实验手段不适用,像纤维类材料的弹性和蠕变实验,要求样品的尺寸足够大,能够固定在试样台的夹具上,这种简单易行的方法对于纳米结构的纤维则不适用。其次,纳米结构的小尺寸使得手工操作相当困难,需要有一种针对单一纳米结构设计的专门测试技术来进行操作。因此,为了准确测量单一纳米结构的性能,开发新的方法和手段是十分必要的。我们的工作目的就在于此。本文综述了我们在开拓和发展原位透射电子显微学在表征纳米材料的力学,电学和热力学性能方面的现状和展望。该研究的焦点集中在如何定量测试一微结构已知的单一纳米结构的物理性能,从而实现了表征结构—性能关联中的一对一关系,开拓了原位透射电子显微镜在纳米材料科学研究中的新方向和新天地。     

JEM-2010 FEF-FEM对纳米材料显微结构的研究

纳米材料的性质和纳米微颗粒的形状、大小和分布有密切的关系。因此深入研究纳米材料的显微结构，了解其结构特征，以便为制备纳米材料时有效地控制纳米颗粒的大小、形状和尺寸分布提供必要信息。我们用JEM-2010FEF场发射能量过滤透射电子显微镜对Pd-Al2O3催化剂和金纳米颗粒、单壁C纳米管及SiO2纳米颗粒标样进行了分析研究。     

NiS纳米丝的制备和表征

纳米材料的性质与纳米粒子的大小和形状密切相关，因此，合成纳米粒子时，在控制其大小及尺寸分布的同时控制其形状是十分重要的。一维纳米结构如纳米棒、纳米线和纳米管等由于具有新奇的光、电等特性和潜在的应用前景，已引起人们极大的兴趣，是当前纳米材料研究中的热点之一。     

JEM-2010 FEF-TEM对纳米材料显微结构的研究

纳米材料的性质和纳米微颗粒的形状、大小和分布有密切的关系。因此深入研究纳米材料的显微结构,了解其结构特征,以便为制备纳米材料时有效地控制纳米颗粒的大小、形状和尺寸分布提供必要信息。我们用JEM-2010FEF场发射能量过滤透射电子显微镜对Pd-Al2O3催化剂和金纳米颗粒、单壁C纳米管及SiO2纳米颗粒标样进行了分析研究。在工作中,我们采用能量损失谱和能量过滤方法取得了高分辨的图像及元素面分布。图1为B、N、C能量损失谱曲线,根据这个谱线确定了B、N、C的元素面分布(图2)。图3是金纳米颗粒的高分辨像,大颗粒为五次孪晶结构,小…     

透射电镜多图像拼接法测量纳米氧化镍的颗粒粒径

本文介绍了利用透射电镜多图像拼接法测量纳米氧化镍的粒度分布.该方法通过SIS软件附带的MLA多图像拼接功能拍照得到拼接图像,经过独立测量每个照片中不少于100个纳米氧化镍颗粒的尺寸,并由此计算出颗粒平均粒径尺寸为20.6nm,该结果与X射线衍射的测量结果非常吻合.通过MIA拼接方法可大幅度提高数字CCD相机的视野范围,从而有效解决了透射电镜法测量小尺寸纳米材料粒径的采样代表性问题,为纳米材料粒径测量提供了新思路.     

纳米磁性材料技术

纳米磁性材料是指材料尺寸线度在纳米级,通常在1～100nm之间的准零维超细微粉,一维超薄膜或二维超细纤维(丝)或由它们组成的固态或液态磁性材料。 纳米磁性材料是纳米材料的—个重要门类,所以除在物理、化学方面具行纳米材料的介观(即介于宏观体与微观分子、原子之间)特性外,还具有其特殊的磁性能(?)介观磁性,主要有:量子尺寸效应、超顺磁性、宏观量子隧道效应、磁有序颗粒的小尺寸效应、特异的表观磁性等,因而导致它的奇特应用。     

透射电镜下纳米材料的操纵

纳米材料以其不同于体材料的优异性能和广阔的应用前景成为材料和物理学研究的热点。纳米材料的性能与其结构密切相关，例如纳米碳管，可以表现为半导体性或金属性。传统的测量手段只能分别得到结构和性能的信息，无法满足纳米材料研究的需要，而且，作为未来电子器件的基本构成单元，纳米材料的原位操控和测量对纳米材料的性能研究和进一步构造新型电子器件也是非常有益和必要的。     

纳米线、纳米管的制备、表征及其应用

在高度集成化浪潮的推动下,现代技术对纳米尺度功能器件的需求将越来越迫切。纳米线、纳米管等一维材料作为纳米器件中必不可少的功能组件,在纳米研究领域中的地位显得愈发重要。本文从一维纳米材料的研究范畴入手,介绍了纳米线、纳米管的制备方法,技术要点以及各种相关表征方法,并涉及了当前一维纳米材料的一些应用研究,为基于纳米线、纳米管功能器件的研制提供前期参考。     

ZnS纳米带的显微结构分析

ZnS是一种典型的Ⅱ-Ⅵ族半导体化合物，可用于平板显示器，电致发光器件，红外窗口等材料，最近引起了研究者的普遍关注，便如纳米颗粒、纳米带、纳米线、纳米管及纳米电缆等。利用简单的热矿散方法，我们合成了几种带状纳米材料。众所周知，ZnS有两种典型结构：     

宁波材料所在硬磁纳米颗粒的绿色和宏量制备方面取得进展CSCD

磁性纳米颗粒在催化、生物医用、磁记录以及高性能永磁体等领域都具有重要的应用前景。在这些应用以及相关研究中,纳米颗粒的尺寸、形貌对磁性及其相关性能影响至关重要,因此如何探索出一种简便的纳米颗粒的合成方法具有重要意义。在各种磁性纳米材料中,     

多孔氧化铝模板的制备及性质研究

多孔氧化铝由于具有规则的纳米多孔结构,是制备各种纳米材料的良好模板,因此,研究多孔氧化铝的制备和物理性质具有重要的意义.采用阳极氧化方法制备了多孔氧化铝有序孔洞阵列,通过场发射扫描电镜(SEM)和X射线衍射(XRD)观测了样品的表面、截面的形貌和晶态结构,分析了样品的透射光谱性质.结果表明,制备的多孔氧化铝模板的孔洞分布有序,孔径大小均匀,严格垂直底面;模板具有非晶态结构,在可见光和红外波长范围内具有较高的透射性能.     

铁电纳米材料和纳米结构研究的进展

铁电纳米材料和纳米结构(如纳米线、纳米管、纳米环)具有新型尺寸效应特性,在铁电基电子器件的微型化方面受到广泛关注.近年来在铁电纳米材料和纳米结构的制备和(电性能和微结构)表征及理论模拟方面取得了相当进展,本文对这方面的最新进展进行评述.首先对高质量的铁电纳米材料和纳米结构的制备方法进行了简短评述,然后介绍铁电纳米材料和纳米结构的纳尺度物性表征.随后介绍了最近发展的四种理论模型(尤其对铁电纳米管、纳米线、纳米点),以及从第一原理出发理论模拟铁电纳米结构的新现象,如铁电纳米结构的自发极化螺旋有序和自发极化涡旋结构.最后总结了铁电纳米材料和纳米结构的微结构研究进展,并讨论了有关铁电纳米结构中自发极化螺旋畴的一些基础物理问题以及实验上寻找自发极化螺旋畴的研究进展.     

Biologically Inspired and Magnetically Recoverable Copper Porphyrinic Catalysts: A Greener Approach for Oxidation of Hydrocarbons with Molecular Oxygen

An efficient synthetic method for magnetically recoverable hybrid copper porphyrinic nanomaterials is reported. These functionalized magnetic materials prove to be efficient bioinspired oxidation catalysts of olefins and thiols, using molecular oxygen as oxidant, in total absence of reductants and solvents, with the highest TON (turnover number) yet achieved for this reaction (≈200 000). A comparative study between homogeneous and heterogeneous oxidation of cyclohexene is discussed, revealing the heterogeneous system to be the most promising concerning stability and reusability of the catalysts. The full characterization of the magnetic hybrid porphyrinic nanomaterials, by transmission electron microscopy, flame atomic absorption spectrometry, thermogravimetry, N₂ sorption, and infrared spectroscopy, is also described.     

HoCoO_3纳米材料的结构改性与气敏性能

利用溶胶–凝胶法成功合成了Cu2+掺杂改性的HoCoO3纳米材料。经X射线粉末衍射(XRD)仪和扫描电镜(SEM)表征后发现,所得HoCoO3纳米材料具有纯相的钙钛矿结构,其晶粒粒径为50~130 nm。将改性及未改性HoCoO3纳米材料分别制成气敏元件,并对其电性能和气敏性能进行对比研究,结果发现Cu2+掺杂可以明显降低HoCoO3气敏元件的电阻,并显著提高其对汽油的灵敏度和选择性。这表明Cu2+掺杂改性的HoCoO3纳米材料将来极有可能成为一种良好的汽油敏感材料。     

Creation and physical properties of the molybdenum-containing polyethylene-based nanomaterials

The thermal decomposition of molybdenum carbonyl is employed for the creation of the composite nanomaterial that represents molybdenum-containing nanoparticles stabilized in the high-pressure polyethylene matrix. The resulting nanomaterials are studied using the transmission electron microscopy, X-ray phase analysis, and electron paramagnetic resonance. The experiments show that the Mo-containing nanoparticles have a mean size of 3–5 nm and consist of several components (Mo, MoC, MoO₃, and MoO₂). The concentration dependences of the electrophysical properties of the synthesized nanomaterials are analyzed.     

A Graphene Oxide˙Streptavidin Complex for Biorecognition – Towards Affinity Purification

In our postgenomic era, understanding of protein‐protein interactions by characterizing the structure of the corresponding protein complex is becoming increasingly important. An important problem is that many protein complexes are only stable for a few minutes. Dissociation will occur when using the typical, time‐consuming purification methods such as tandem affinity purification and multiple chromatographic separations. Therefore, there is an urgent need for a quick and efficient protein‐complex purification method for 3D structure characterization. The graphene oxide (GO)·streptavidin complex is prepared via a GO·biotin·streptavidin strategy and used for affinity purification. The complex shows a strong biotin recognition capability and an excellent loading capacity. Capturing biotinylated DNA, fluorophores and Au nanoparticles on the GO·streptavidin complexes demonstrates the usefulness of the GO·streptavidin complex as a docking matrix for affinity purification. GO shows a high transparency towards electron beams, making it specifically well suited for direct imaging by electron microscopy. The captured protein complex can be separated via a filtration process or even via on‐grid purification and used directly for single‐particle analysis via cryo‐electron microscopy. Therefore, the purification, sample preparation, and characterization are rolled into one single step.     

Synthesis and photoluminescence properties of wash-board belt-like ZnSe nanostructures

Washboard belt-like zinc selenide （ZnSe） nanostructures are successfully prepared by a simple chemical vapor deposi- tion （CVD） technology without catalyst. The phase compositions, morphologies and optical properties of the nanos- tructures are investigated by X-ray diffraction （XRD）, scanning electron microscopy （SEM）, high-resolution transmis- sion electron microscopy （HRTEM） and photoluminescence （PL） spectroscop, respectively. A vapor-liquid mecha- nism is proposed for the formation of ZnSe belt-like structures. Strong PL from the ZnSe nanostructure can be tuned from 462 nm to 440 nm with temperature varying from 1000 ℃ to 1200 ℃, and it is demonstrated that the washboard belt-like ZnSe nanostructures have potential applications in optical and sensory nanotechnology. This method is ex- pected to be applied to the synthesis of other II-VI groups or other group＇s semiconducting materials.     

The Role of Sulfur in the Synthesis of Novel Carbon Morphologies: From Covalent Y‐Junctions to Sea‐Urchin‐Like Structures

A detailed characterization, using high resolution electron microscopy/microanalysis (SEM, TEM, HRTEM, and EDX), reveals tubular carbon nanostructures exhibiting complex and fascinating morphologies. The materials were obtained by sulfur‐assisted chemical vapor deposition. It is demonstrated that S not only acts on the catalyst, but also can be detected in the carbon lattice of the nanostructures. The experimental data presented here confirms the critical role of S, which is responsible for inducing curvature and therefore influencing the final carbon nanostructure morphology. In particular, different types of covalent Y‐junctions of CNTs and even sea urchin‐like nanostructures were produced and their experimental conditions are listed and discussed.     

Quantum Dots Decorated with Magnetic Bionanoparticles

A new class of water‐soluble, fluorescent, magnetic quantum dots––magnetoferritin bioconjugate––is prepared. The nanostructures are patterned mainly as dimer particles as characterized by high‐angle annular dark‐field scanning transmission electron microscopy and electron energy loss spectroscopy. Magnetic (high spontaneous magnetization values, superparamagnetism) and fluorescent (narrow emission peaks, uniform brightness) properties of both nanoblocks are maintained in the final nanostructure.     

Fast and Ultraclean Approach for Measuring the Transport Properties of Carbon Nanotubes

In this work, a fast approach for the fabrication of hundreds of ultraclean field‐effect transistors (FETs) is introduced, using single‐walled carbon nanotubes (SWCNTs). The synthesis of the nanomaterial is performed by floating‐catalyst chemical vapor deposition, which is employed to fabricate high‐performance thin‐film transistors. Combined with palladium metal bottom contacts, the transport properties of individual SWCNTs are directly unveiled. The resulting SWCNT‐based FETs exhibit a mean field‐effect mobility, which is 3.3 times higher than that of high‐quality solution‐processed CNTs. This demonstrates that the hereby used SWCNTs are superior to comparable materials in terms of their transport properties. In particular, the on–off current ratios reach over 30 million. Thus, this method enables a fast, detailed, and reliable characterization of intrinsic properties of nanomaterials. The obtained ultraclean SWCNT‐based FETs shed light on further study of contamination‐free SWCNTs on various metal contacts and substrates.