Template synthesis of well-aligned titanium dioxide nanotubes

TiO₂ nanotubes of the anatase form have been synthesized by sol-gel chemical method using anodic aluminum oxide (AAO) as a template. Transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray diffraction were used to investigate the structure and morphology of the TiO₂ nanotubes. The results showed that TiO₂ nanotubes obtained are highly ordered and uniform. The diameter and length of the obtained nanotubes were determined by the pore size and the thickness of AAO template. It was found that through control of immersion time of AAO membrane in sol, both tubules and fibrils can be prepared. PACS 61.46.+w     

Fabrication of low phase transition temperature vanadium oxide films by direct current reactive magnetron sputtering and oxidation post-anneal method

Vanadium oxide thin films were deposited on ordinary glass substrates by direct current (DC) magnetron sputtering from a vanadium metal target and subsequent oxidation annealing. The deposition and annealing parameters were given in detail. The samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM). The phase transitions of films were observed by measuring their electrical and optical property variations at different temperature. The results indicated that the films fabricated had a semiconductor–metal phase transition temperature of about 30 °C.     

钒氧化物薄膜的拉曼散射

用射频磁控溅射以纯金属钒做靶材在氩氧混合气体中制备了钒氧化物 (VO2 (B)、V6O1 3、V2 O5)薄膜。报导了钒氧化物薄膜的拉曼光谱 ,结合这些钒氧化物不同的结构特点 ,对它们的拉曼光谱进行了分类讨论     

Synthesis and characterization of H2V3O8 nanorods for electrochemical devices

Vanadium oxide hydrate (H₂V₃O₈) nanorods to be used as cathode material in secondary batteries were synthesized using a hydrothermal method without templates and reducing agents. The obtained pristine product was characterized using X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy. Cyclic voltammetry and charge/discharge studies were conducted to examine the electrochemical performance of cathodes made of these vanadium oxide hydrate nanorods. The specific capacity of the vanadium oxide hydrate nanorods is 292 mAh/g, the columbic efficiency is about 95%. The calculated capacities are 42.8 F/g at 5 mV/s and 39.2 F/g at 10 mV/s scan rate.     

From crystalline V2O5 to nanostructured vanadium oxides using aromatic amines as templates

Nanoneedles, nanorods of B-VO₂, and vanadium oxide nanotubes with high crystallinity were synthesized via a one-step hydrothermal treatment using crystalline V₂O₅ as a precursor and aromatic amines (C₆H₅-(CH₂)_n-NH₂ with n=0, 1, 3) as structure-directing templates. Samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRD), thermal analysis, nitrogen adsorption/desorption isotherms and infrared spectroscopy. Nanoneedles, 0.5-5 μm in length and about 50 nm in average diameter and VO₂(B) nanorods about 20-100 nm wide and up to 2.5 μm long, have been obtained. The inner and the outer diameters of the vanadium oxide nanotubes vary, respectively, between 15-25 and 70-100 nm with a length up to 4 μm.     

Synthesis of lanthanum nickelate perovskite nanotubes by using a template-inorganic precursor

A new route to obtain metal oxide nanotubes is presented: an inorganic coordination complex precursor containing the metal ions and impregnated into alumina membrane templates yield hollow tubular nanostructures of LaNiO₃ by calcination at 600 °C as characterized by powder X-ray diffraction (XRD). Scanning electron microscopy (SEM) shows that the resulting nanotubes have 200 nm in diameter in good agreement with the template pore. Transmission electron microscopy (TEM) and dark field transmission electron microscopy (DF-TEM) show that the nanotubes with 10-20 nm walls and internal separations are composed of 3-5 nm crystals.     

LiFePO4纳米管的制备与表征

采用溶胶凝胶法在氧化铝模板中成功的制备了LiFePO4一维纳米管阵列．扫描电子显微镜和透射电子显微镜表征结果表明所制备的LiFePO4纳米管具有单分散性,互相平行,高度有序。综合选区电子衍射、X射线衍射以及X光线能谱表征结果,所制备的LiFePO4纳米管为单一的橄榄石型结构．这种在室温和温和条件下合成的一维LiFePO4纳米管,可以做为新型的锂离子电池正极材料．     

Synthesis and characterization of highly-ordered barium-strontium titanate nanotube arrays fabricated by sol—gel method

Highly uniformed barium-strontium titanate nanotube arrays were fabricated using a porous anodic aluminum oxide template from a barium-strontium titanate sol--gel solution. Electron microscope results showed that nanotubes with uniform length and diameter were obtained. The diameters and lengths of these nanotubes were dependent on the pore diameter and the thickness of the applied anodic aluminum oxide template. High resolution transmission electron microscopy and the selected-area electron diffraction pattern investigations demonstrated the perovskite structure and the polycrystalline of the fabricated barium-strontium titanate nanotubes. The characterization of the electrical and dielectric properties had also been made. Compared to thin film material, the intrinsic leakage current density is almost the same. Besides, at 30~℃, the dielectric constant and dielectric loss of the fabricated nanotube is 80 and 0.027 at 1~MHz respectively.     

石墨炉内石墨探针表面上的原子化机理研究 Ⅳ钒的原子化机理

本文通过X-射线衍射分析(XRD),扫描电子显微镜分析(SEM),化学分析光电子能谱分析(ESCA),并结合原子吸收测量,研究了钒在普通石墨管中石磨探针表面上发生的固相化学反应。结果表明,钒化合物在灰化阶段即可转化为热稳定性较高的碳化物,原子化的最后步骤为碳化物的热分解。     

Structural transformation of MoO<Subscript>3</Subscript> nanobelts into MoS<Subscript>2</Subscript> nanotubes

The structural transformation of MoO₃ nanobelts into MoS₂ nanotubes using a simple sulfur source has been reported. This transformation has been extensively investigated using electron microscopic and spectroscopic techniques including scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), electron diffraction (ED), and energy-dispersive X-ray analysis (SEM-EDAX and TEM-EDX). The method described in this report will serve as a generic route for the transformation of other oxide nanostructures into the chalcogenide nanostructures.     

Integration and characterization of aligned carbon nanotubes on metal/silicon substrates and effects of water

We report here a facile way to grow aligned multi-walled carbon nanotubes (MWCNTs) on various metal (e.g. gold, tungsten, vanadium and copper)/silicon electrically conductive substrates by aerosol-assisted chemical vapor deposition (AACVD). Without using any buffer layers, integration of high quality MWCNTs to the conductive substrates has been achieved by introducing appropriate amount of water vapor into the growth system. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) determination indicate tidy morphology and narrow diameter distribution of the nanotubes as well as promising growth rate suitable for industrial applications. Raman spectra analysis illustrates that the structural order and purity of the nanotubes are significantly improved in the presence of water vapor. The growth mechanism of the nanotubes has been discussed. It is believed that water vapor plays a key role in the catalyst-substrate interaction and nucleation of the carbon nanotubes on the conductive substrates. This synthesis approach is expected to be extended to other catalyst-conductive substrate systems and provide some new insight in the direct integration of carbon nanotubes onto conductive substrates, which promises great potential for applications in electrical interconnects, contacts for field emitters, and other electronic nanodevices.     

ZnO nanotubes by template wetting process

ZnO nanotubes have been fabricated within the nanochannels of porous anodic alumina templates by template wetting process. In this method, pore walls of the alumina template were wetted by polymeric ZnO source. After heat treatment procedures, the template was selectively etched off to release the nanotubes. Field-emission scanning electron microscopy (FE-SEM) investigations showed that nanotubes have smooth wall morphologies and well-defined diameters corresponding to the diameter of the applied template. In addition, X-ray diffraction measurements showed that our ZnO nanotubes realized in the template-wetting process have polycrystalline-structural properties.     

Cost-saving synthesis of vanadium oxide nanotubes

The synthesis of vanadium oxide nanotubes has been achieved by using V₂O₅ as vanadium oxide precursor. Due to its low cost, high yield and ease of handling, the synthesis starting from V₂O₅ provides an advantageous access to large quantity of the tubular vanadium oxide nanotubes.     

Low reflectance sputtered vanadium oxide thin films on silicon

Vanadium oxide thin films on silicon (Si) substrate are grown by pulsed radio frequency (RF) magnetron sputtering technique at RF power in the range of 100–700 W at room temperature. Deposited thin films are characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) techniques to investigate microstructural, phase, electronic structure and oxide state characteristics. The reflectance and transmittance spectra of the films and the Si substrate are recorded at the solar region (200–2300 nm) of the spectral window. Substantial reduction in reflectance and increase in transmittance is observed for the films grown beyond 200 W. Further, optical constants viz. absorption coefficient, refractive index and extinction coefficient of the deposited vanadium oxide films are evaluated.     

Evolution from vanadium pentoxide xerogel to sodium-containing vanadates in thin films on ITO-coated glasses

In this work, the mechanism of the “gelation” process and the thermal-induced structural modifications of thin film of vanadium pentoxide xerogels deposited on indium tin oxide (ITO)-coated glasses have been studied. Vanadium pentoxide xerogel has been prepared by using the sol–gel proton exchange resin route without any resin pretreatment. To monitor the effect of the “resin efficiency” on the gelation process, the solution coming out from the resin has been collected in a sequence of different containers (vials), separately investigated by Raman spectroscopy. After the spin coating deposition, the thin films of vanadium pentoxide gel have been subjected to different annealing treatments. The highest thermal treatment (600 °C) induces a complete transformation of the gel phase into an anhydrous polycrystalline phase of a sodium-containing vanadate, different from the usual V₂O₅ crystal. It is due to the diffusion of foreign ions (mainly sodium) coming from the substrate into the vanadium oxide layer.     

Peculiarities of the decoration of carbon nanotubes with transition metal atoms

Carbon nanotubes decorated with transition metal, in particular, scandium, titanium, and vanadium, atoms offer promise for use in various applied science fields. We report the results of quantum-chemical calculations of the structure of the metallic layer of atoms of these metals coating the surface of (9, 0) and (10, 0) carbon nanotubes. It was shown that uniform one-layer coating by scandium and titanium could form on nanotubes with diameters no less than the diameter of (10, 0) nanotubes. Vanadium atoms could not uniformly cover nanotubes irrespective of their diameters.     

The effect of thermal annealing and laser irradiation on the microstructure of vanadium oxide nanotubes

The microstructure of vanadium oxide nanotubes (VONTs) have been characterized using FTIR spectroscopy and Raman spectroscopy. The temperature effects on the VONTs were studies by changing the laser irradiation power and thermal annealing temperature in air. Raman spectroscopy studies showed that the VONTs could be decomposed even at low laser power irradiation. Also, together with scanning electron microscopy, it was found that thermal annealing in air could lead to the collapse of the tubular structure and convert the nanotubes into V₂O₅ nanoparticle. It was found that the thermal stability of VONTs was relatively low and the tubular morphology was destroyed at temperatures higher than 300 °C. The spectroscopic analyses showed that the Raman signature of the VONTs could be established for probing tubular structure.     

Zinc oxide catalyzed growth of single-walled carbon nanotubes

We demonstrate that zinc oxide can catalyze the growth of single-walled carbon nanotubes (SWNTs) with high efficiency by a chemical vapor deposition process. The zinc oxide nanocatalysts, prepared using a diblock copolymer templating method and characterized by atomic force microscopy (AFM), were uniformly spaced over a large deposition area with an average diameter of 1.7 nm and narrow size distribution. Dense and uniform SWNTs films with high quality were obtained by using a zinc oxide catalyst, as characterized by scanning electron microscopy (SEM), Raman spectroscopy, AFM, and high-resolution transmission electron microscopy (HRTEM).     

脉冲溅射V2O5薄膜结构和性能研究

V2O5薄膜具有很好的离子注入/退出可逆性,是最有潜力的锂离子储存层的候选材料之一,它的电学特性与制备方法、化学计量比、结构和取向等有直接关系,仔细控制工艺参量是制备出在锂电池上应用的V2O5薄膜关键。研究中采用脉冲磁控反应溅射方法,通过精确地控制氧分压、基底温度等关键工艺参量,在石英玻璃和硅片上制备V2O5薄膜。利用X射线衍射和X射线光电子谱,分析了薄膜的成分、相结构、结晶和价态情况,用原子力显微镜表征了薄膜的微观结构,用分光光度计测量从200—2500nm波段V2O5薄膜纯度高、相结构单一、结晶度好。高低温电阻变化2个量级,薄膜的光学能隙为2.46eV。     

Highly ordered zinc oxide nanotubules synthesized within the anodic aluminum oxide template

Zinc oxide (ZnO) nanotubules were prepared by sol-gel synthesis within the pores of an anodic aluminum oxide (AAO) template. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected-area electron diffraction (SAED) and X-ray Diffraction (XRD) were used to investigate the morphology and crystalloid structures of the ZnO nanotubules. The results indicate that polycrystalline ZnO nanotubules are very uniformly assembled and parallel to each other in the membrane pores of the AAO template. Received: 15 January 2001 / Accepted: 1 February 2001 / Published online: 27 June 2001