水热合成NiX（WYMo1-Y）1-XS2纳米管

无机类富勒烯纳米粒子具有良好的润滑性能．宏量制备高纯度的样品以满足性能测试的要求，是目前面临的主要技术难题．本文采用剥离-掺杂-水热处理这一工艺流程制备了多元金属二硫化物纳米粒子，应用XRD、TEM、HRTEM和EDS等分析手段对其形貌、晶相组成、结构和化学组成进行了表征．实验结果表明，多元金属二硫化物纳米颗粒具有管状形貌，管壁为多层状结构，化学组成为NiX（WYMo1-Y）1-XS2，同时，样品中具有类富勒烯结构的纳米粒子大幅度提高；并依据实验结果对多元金属二硫化物纳米管的形成机理进行了探讨．     

多元金属二硫化物纳米管的制备与结构特征

为解决无机类富勒烯纳米化合物的制备过程中存在的技术问题，．本文以二硫化钼和二硫化钨为主要原料，采用了剥离一重新堆垛一结构控制这一技术方法，用正丁基锂将上述二硫化物剥离成单层，通过掺杂将金属锰离子引入反应体系中，以将单层二硫化物重新堆垛起来，并进行结构控制．XRD、TEM、HRTEM结果表明，应用上述方法制备出了真空管状多元金属二硫化物纳米化合物；纳米管为多壁管，其微细结构具双层结构特征；并探讨了其形成机理．     

电弧放电条件下内包金属洋葱状富勒烯生成机理的研究

采用电弧法制备内包纳米金属微粒的洋葱状富勒烯.通过XRD、SEM和HRTEM对样品进行结构表征和分析,讨论影响纳米洋葱状富勒烯生成的因素.结果表明:可以宏量地制备内包金属微粒的NSOFs,且晶化程度很高;优化工艺参数可获得合适的气相温度及温度梯度,有利于NSOFs的生成;建立了汽-液-固(VLS)生长模型以解释其形成机理.     

水下放电制备内包金属洋葱状富勒烯的研究

以二茂铁和纳米Ni粒子为催化剂,在水下放电条件下,制备了内包金属洋葱状富勒烯(Onion-like Fullerenes:OLFs),利用高分辨透射电镜(HRTEM)和X射线衍射(XRD)对所得产物进行了表征.结果表明:二茂铁和纳米Ni粒子均可催化得到内包金属洋葱状富勒烯,内包Fe洋葱状富勒烯直径分布在5～50nm之间,内包Ni洋葱状富勒烯直径分布在10～35nm之间.     

疏水性二氧化硅气凝胶性能表征

目前SiO2气凝胶是世界上最轻、隔热性最好、孔隙率较高且声传播速率较低的固体材料,由于其特殊的网络结构使其具有很多独特的性能,而制备疏水性气凝胶是解决常压干燥过程中体积收缩和开裂的关键.采用溶胶-凝胶法以三甲基氯硅烷(TMCS)为化学表面修饰剂通过衍生法制备了疏水性二氧化硅气凝胶,并利用X射线衍射光谱、扫描电镜、能量色散谱、透射电镜、红外光谱、差热-热重分析等测试方法对其结构、形貌及化学组成进行了分析.研究表明:该样品是表面连有疏水基团-CH3的疏水性SiO2气凝胶,且组成其连续网络结构的球状纳米粒子纯度较高、粒径均匀,是热稳定性较高的非晶、多孔、轻质纳米材料.     

Pd/SiO2有机-无机薄膜的制备及其在N2气氛中的热稳定性

采用溶胶-凝胶法,在甲基化改性SiO2溶胶中掺杂PdCl2,制备Pd/SiO2有机-无机薄膜.通过XRD、红外光谱、TG-DTG分析、接触角以及SEM测试,考察该样品在N2气氛中的热稳定性.结果表明,Pd/SiO2膜材料经200℃以上温度焙烧后,样品中即出现了少量纳米金属Pd粒子,这些金属Pd为PdCl2还原所得.随着焙烧温度的升高,金属Pd粒子的衍射峰强度增加,膜材料中的Si-CH3吸收峰和Si-OH吸收峰减弱.样品中的Si-CH3吸收峰在750℃时完全消失.金属Pd的掺杂对SiO2膜材料的化学结构基本没影响.保持Pd/SiO2有机-无机薄膜及分离膜疏水性的最适宜焙烧温度为350℃.     

高活性TiO2纳米晶的酸催化Sol-Gel法制备与表征

采用酸催化的溶胶-凝胶法制备出了纳米TiO2光催化剂，以甲基橙的光催化降解为探针反应，评价了其光催化活性．运用XRD、TEM、FT—IR以及PL光谱技术对纳米TiO2的微晶尺寸、晶体结构、表面组成和性能进行表征．结果表明，400℃焙烧的TiO2纳米粒子的颗粒形貌为近球形，晶粒尺寸为11．69 nm，样品分散性良好的锐钛矿型结构．在光催化降解甲基橙的实验中，400℃焙烧的TiO2纳米粒子表现出最高的光催化活性，这与表征结果一致．此外，550℃和650℃焙烧的具有锐钛矿型和金红石型混晶结构的TiO2纳米粒子，无混晶协同促进效应．     

低摩擦长寿命类富勒烯碳基薄膜的制备及其摩擦学特性

以甲烷(CH4)为前躯体,利用等离子体增强化学气相沉积(PECVD)技术,在单晶硅〈n-100〉基底表面制备含氢类富勒烯碳基薄膜(FL-C∶H)。采用高分辨透射电镜(HRTEM)、拉曼光谱仪(LABRAM)和多功能X射线光电子能谱仪(XPS)对薄膜及磨屑结构进行表征;利用摩擦磨损试验机、扫描电子显微镜(SEM)分别测试薄膜的摩擦学性能和观察磨屑的微观形貌。结果表明,所制备的碳基薄膜具有类富勒烯纳米结构,且磨屑的显微结构亦呈现类富勒烯结构的特征。同时,类富勒烯纳米结构的碳基薄膜具有优异的摩擦学性能,与传统非晶类金刚石薄膜相比,其磨损寿命显著提高,在载荷为30N、摩擦速率为0.1m/s下薄膜的磨损寿命为3 538.2m,摩擦系数低至0.012左右,显示出长寿命低摩擦特性。     

离子液体法制备铜的纳米粒子

利用化学还原方法，加入不同量的离子液体1-甲基-3-乙基咪唑硫酸乙酯盐，制备了不同大小的金属铜的纳米摘要粒子。采用X射线衍射和透射电子显微镜对所制备的样品进行了结构表征。结果表明，两个样品中的粒子都具有五边形和六边形结构，粒径约为200～300nm，离子液体不但作为分散剂影响粒子的大小，而且有一定的防氧化作用。     

中科院化学所在富勒烯衍生化研究方面取得系列新进展

对富勒烯和金属富勒烯进行笼外修饰能够调控这类功能分子的电子结构性能,是富勒烯化学重要的研究领域之一。最近,在中国科学院、国家自然科学基金委和科技部973项目的大力支持下,中科院化学所分子纳米结构与纳米技术院重点实验室科研人员与厦门大学科学家合作,在富勒烯和内嵌金属富勒烯衍生化方面取得了系列新研究成果,     

富勒烯和纳米管结构二硫化钨的研究进展

简要介绍了无机富勒烯结构二硫化钨(IF-WS2)纳米粒子和纳米管的发现和结构特点,详细介绍了IF-WS2纳米粒子和纳米管的化学气相反应、直接加热、模板法、化学气相输运等制备方法,阐述了它们的包裹形成机理、摩擦性质和在AFM针尖方面的潜在应用,旨在指出它们具有重要的科学研究价值和潜在的应用价值.     

Synthesis of inorganic fullerene-like MoS2 nanoparticles by a facile method

A facile and low-cost synthesis route was used to synthesize inorganic fullerene-like (IF) MoS₂ nanoparticles by reaction of sulfur powder and ammonium molybdate in a hydrogen atmosphere at 600 °C. As-synthesized IF-MoS₂ nanoparticles are of a closed hollow cage structure with size of 10-20 nm. Nanowires and nanotubes were also obtained at the same annealing temperature. The composition, structure, and morphology of the products were characterized by XRD, Raman, and TEM and the possible growth mechanism is proposed.     

Inorganic nanotubes

Following the discovery of carbon fullerenes and carbon nanotubes, it was hypothesized that nanoparticles of inorganic compounds with layered (two-dimensional) structure, such as MoS(2), will not be stable against folding and form nanotubes and fullerene-like structures: IF. The synthesis of numerous other inorganic nanotubes has been reported in recent years. Various techniques for the synthesis of inorganic nanotubes, including high-temperature reactions and strategies based on 'chemie douce' (soft chemistry, i.e. low-temperature) processes, are described. First-principle, density functional theory based calculations are able to provide substantial information on the structure and properties of such nanotubes. Various properties of inorganic nanotubes, including mechanical, electronic and optical properties, are described in brief. Some potential applications of the nanotubes in tribology, protection against impact, (photo)catalysis, batteries, etc., are discussed.     

Novel fabrication method of diverse one-dimensional Pt/ZnO hybrid nanostructures and its sensor application

A novel low-temperature, solution-phase method for the facile fabrication of a variety of one-dimensional (1D) metal/metal oxide hybrid nanostructures has been developed. This method is based on the wet chemical synthesis of metal oxide nanowires, followed by the surface coating of metal nanoparticles on metal oxide nanowire templates via reduction of metal ions along with controlled etching of metal oxide nanowires at the core, all in a low-temperature liquid environment. As a proof-of-concept, we applied this method to the fabrication of various 1D Pt/ZnO hybrid nanostructures including Pt nanoparticle-coated ZnO nanowires/nanotubes and Pt nanotubes on silicon and polymer substrates. The diverse morphology tuning is attributed to the control of pH in the solution with different metal precursor concentrations and amounts of reducing agent. The change of morphology, crystalline structure, and composition of various 1D Pt/ZnO hybrid nanostructures was observed by SEM, TEM (HRTEM), XRD and ICP-AES, respectively. Further, we have demonstrated a highly sensitive strain sensor (gauge factor = 15) with a Pt nanotube film fabricated by the developed method on a flexible polymer substrate.     

Inorganic nanotubes and fullerene-like nanoparticles

Although graphite, with its anisotropic two-dimensional lattice, is the stable form of carbon under ambient conditions, on nanometre length scales it forms zero- and one-dimensional structures, namely fullerenes and nanotubes, respectively. This virtue is not limited to carbon and, in recent years, fullerene-like structures and nanotubes have been made from numerous compounds with layered two-dimensional structures. Furthermore, crystalline and polycrystalline nanotubes of pure elements and compounds with quasi-isotropic (three-dimensional) unit cells have also been synthesized, usually by making use of solid templates. These findings open up vast opportunities for the synthesis and study of new kinds of nanostructures with properties that may differ significantly from the corresponding bulk materials. Various potential applications have been proposed for the inorganic nanotubes and the fullerene-like phases. Fullerene-like nanoparticles have been shown to exhibit excellent solid lubrication behaviour, suggesting many applications in, for example, the automotive and aerospace industries, home appliances, and recently for medical technology. Various other potential applications, in catalysis, rechargeable batteries, drug delivery, solar cells and electronics have also been proposed.     

Structure and Electronic Spectrum of Fullerene-like Nanoclusters Based on Mo, Nb, Zr, and Sn Disulfides

Modeling results are presented on the atomic structure, electronic spectra, and interatomic interaction parameters of quasi-zero-dimensional fullerene-like nanoparticles of Mo, Nb, Zr, and Sn disulfides. These characteristics are analyzed in relation to the chemical composition, size, and atomic configuration of the nanoparticles and are compared to those of nanotubes and crystals of the corresponding disulfides.     

Toward atomic-scale bright-field electron tomography for the study of fullerene-like nanostructures

We present the advancement of electron tomography for three-dimensional structure reconstruction of fullerene-like particles toward atomic-scale resolution. The three-dimensional reconstruction of nested molybdenum disulfide nanooctahedra is achieved by the combination of low voltage operation of the electron microscope with aberration-corrected phase contrast imaging. The method enables the study of defects and irregularities in the three-dimensional structure of individual fullerene-like particles on the scale of 2-3 A. Control over shape, size, and atomic architecture is a key issue in synthesis and design of functional nanoparticles. Transmission electron microscopy (TEM) is the primary technique to characterize materials down to the atomic level, albeit the images are two-dimensional projections of the studied objects. Recent advancements in aberration-corrected TEM have demonstrated single atom sensitivity for light elements at sub?ngstr?m resolution. Yet, the resolution of tomographic schemes for three-dimensional structure reconstruction has not surpassed 1 nm3, preventing it from becoming a powerful tool for characterization in the physical sciences on the atomic scale. Here we demonstrate that negative spherical aberration imaging at low acceleration voltage enables tomography down to the atomic scale at reduced radiation damage. First experimental data on the three-dimensional reconstruction of nested molybdenum disulfide nanooctahedra is presented. The method is applicable to the analysis of the atomic architecture of a wide range of nanostructures where strong electron channeling is absent, in particular to carbon fullerenes and inorganic fullerenes.     

Synthesis of carbon nanotubes within Pt nanoparticles-decorated AAO template

Template-based synthesis of Pt-doped carbon nanotubes has been conducted with a corona discharge enhanced chemical vapor deposition. In this paper, nanoporous anodic alumina template was firstly decorated with Pt nanoparticles upon its interior walls. As the fabrication of carbon nanotubes within the nanopores, Pt nanoparticles were simultaneously embedded into the carbon nanotubes. HRTEM indicated that the grain size of these Pt nanoparticles is 5 nm and they are homogeneously exposed on the outer surface of carbon nanotubes.     

Fabrication of polystyrene/gold nanotubes and nanostructure-controlled growth of aluminate

Direct adsorption of gold nanoparticles in the inner of alumina template and following immersion of polystyrene (PS) dichloromethane solution in the template resulted in the fabrication of composite nanotubes of PS and gold nanoparticles. Several methods have been used to characterize the tubular structure. Nanostructured sodium aluminates were formed when the anodic alumina oxide membrane was dissolved by the sodium hydroxide. A "flower" shape was found after etching the template while the synthesis process was recorded as function of a time. The results demonstrate that the shape and size of the aluminates nanostructure can be controlled by etching time and the pore diameter of the alumina membrane.     

The growth of carbon nanotubes on large areas of silicon substrate using commercial iron oxide nanoparticles as a catalyst

A new approach to chemical vapour deposition (CVD) growth of carbon nanotubes (CNTs) using commercial magnetite nanoparticles, avoiding its in situ synthesis, is reported. Commercial magnetite nanoparticles were used as catalyst material to growth multiwalled carbon nanotubes by chemical vapour deposition onto a silicon substrate of several square centimeters in area. It is shown that the application of an alternating electric field during the deposition of catalytical nanoparticles is an effective technique to avoid their agglomeration allowing nanotube growth. Scanning electron microscopy showed that the nanotubes grow perpendicularly to the substrate and formed an aligned nanotubes array. The array density can be controlled by modifying the deposited nanoparticle concentration.