Preparation of novel saw-toothed and riblike alpha-Si3N4 whiskers

alpha-Si(3)N(4) whiskers with novel saw-toothed and riblike structures have been synthesized in a high yield by a carbothermal reduction and nitridation route. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), and selected-area electron diffraction (SAED). The results show that the saw-toothed whiskers with one smooth surface and another toothlike surface have lengths about several tens of microns and widths in the range of 600-1200 nm. The riblike whiskers are composed of Si(3)N(4) rod-arrays, which grow closely packed perpendicular to the central axial whiskers with uniform diameter and length. The growth mechanism of the products can be considered as a combination of VS mechanism and secondary epitaxial nucleation process. The photoluminescence (PL) spectrum of the whiskers shows a strong blue light emission peak at 406 nm and a weak peak at 485 nm, suggesting their potential applications in light and electron emission devices.     

Surface treatment of magnesium oxysulfate whiskers through plasma polymerization

The surface of magnesium oxysulfate (MOS) whiskers was treated through plasma polymerization to increase the compatibility between the MOS whiskers and a polymer matrix. Different plasma parameters were chosen to determine the most hydrophobic coating. The surface structure of the plasma-treated MOS whiskers was examined. The MOS whiskers retained their crystal structure after plasma treatment, as shown by X-ray powder diffraction (XRD) analyses. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FT-IR) spectroscopy analyses revealed that a polymer sheath was formed on the surface of the MOS whiskers, and interfacial chemical bonds were generated between the polymer sheath and the MOS whiskers. The thin-layer polymer sheath was uniform around the entire surface of the MOS whiskers and exhibited a typical amorphous structure, as determined by transmission electron microscopy (TEM) combined with selected area electron diffraction (SAED) analyses. The possible reaction mechanism on the surface of the MOS whiskers under plasma treatment was then proposed. Finally, the effect of surface treatment was evaluated by scanning electron microscopy (SEM), measurement of the contact angle and contact angle hysteresis, and torque rheometer. Results showed that plasma treatment could markedly increase the hydrophobicity of the MOS whiskers' surface, effectively reducing the agglomeration and improving the dispersibility of the MOS whiskers in the matrix, which results in the improved compatibility between the MOS whiskers and the polyvinyl matrix, as well as the processability of the composites.     

Polymer-assisted growth of molybdenum oxide whiskers via a sonochemical process

Whiskers of molybdenum oxides with high aspect ratios were synthesized from peroxomolybdate precursor solutions in the presence of small amounts of poly(ethylene glycol) (PEG) via a sonochemical process at temperatures of 25-70 degrees C. Irradiation with ultrasound reduces the time needed for the growth of micrometer-sized whiskers from weeks to a few hours. The simplicity of the sonochemical approach also compares favorably to a hydrothermal/solvothermal process. The morphology, crystal structure, and other characteristics of the whiskers were characterized by scanning electron microscopy, transmission electron microscopy, selective area electron diffraction, energy-dispersive X-ray spectroscopy, wide-angle X-ray diffraction, Raman spectroscopy, thermogravimetric analysis, differential scanning calorimetry, and the Brunauer-Emmett-Teller method. The surface area of the calcified molybdenum oxide whiskers (55.4 m2/g) was found to be much higher than those of molybdenum oxide nanofibers (35 m2/g) or nanorods (13.4 m2/g) The growth rate of various crystal faces could be postulated to be controlled by the binding of peroxomolybdate ions to pseudo-crown ether cavities formed by PEG. The reduction of molybdenum oxide to produce mixed-valent oxides and their growth could also be controlled by the reducing ability of PEG. The aspect ratio of the molybdenum oxide whiskers increased with decreasing concentration in the initial peroxomolybdate precursor solution. Whether the precursor solution species was H2Mo2O3(O2)4(H2O)2, H2MoO2(O2)2, or MoO2(OH)(OOH), the peroxide group in all the species disproportionates to give the final product MoO3 by a catalytic process. On the basis of experimental evidence of the dual role of glycols, a mechanism for the growth of the molybdenum oxide whiskers is proposed.     

T-ZnO晶须化学镀铜复合粉体的制备及其电磁性能的研究

采用化学镀的方法制备了Cu包覆四脚状氧化锌晶须(T-ZnO晶须)的复合粉体.使用X射线衍射分析仪(XRD)进行了物象分析,扫描电镜(SEM)观察了粉体的形貌.运用能谱仪(EDS)进行了成份分析.结果表明,晶须为纯氧化锌,晶体结构为六方晶系纤锌矿结构,镀层为纯铜. SEM观察晶须外观形貌为四脚状结构.同时使用波导法对T-ZnO晶须和化学镀铜得到的Cu/T-ZnO晶须复合粉体进行了电磁参数的测量.微波电磁性能试验表明,化学镀后晶须的微波吸收性能明显增加,在频率为13 GHz处反射率可达－12 dB左右,而且最大吸收峰的频率随铜析出量的不同而发生改变,这样有利于实现吸收频带的展宽.     

三步升温法合成阵列碳纳米管

本文使用结构简单的单温炉设备, 以二茂铁/三聚氰胺混合物为原料, 采用独特的三步升温方法于光滑的SiO₂衬底上合成出了大面积的阵列碳纳米管, 并对碳纳米管的形貌和结构进行了研究.     

莫来石晶须/堇青石表面层的制备及准超疏水性能

采用溶胶-凝胶法制备了硅铝混合凝胶粉体, 再通过熔盐反应在堇青石陶瓷基体上生长莫来石晶须, 制得莫来石晶须/堇青石表面层微结构. 表征结果表明, 莫来石晶须紧密生长在堇青石基体上, 晶须直径为100~300 nm, 长度可达几个微米. 莫来石晶须表面含有大量Si—OH和Al—OH极性亲水基团, 采用十二烷基三甲氧基硅烷与活性基团间的偶联反应将非极性基团引入莫来石晶须表面, 获得了静态润湿角为146°的莫来石晶须/堇青石表面层. 动态润湿研究表明, 合成的莫来石晶须增大了堇青石陶瓷的表面粗糙度, 使亲水的莫来石晶须/堇青石表面更加亲水, 而硅烷偶联剂修饰的堇青石/莫来石晶须表面则成为准超疏水表面.     

电化学法沉积氧化锌晶须

应用阳极氧化法沉积氧化锌(ZnO)松针状晶须,SEM和XRD观察、表征样品形貌与结构.结果表明,电沉积氧化锌晶须直径为20～50 nm、长度200～300 nm、长径比10～15,纯度高,结晶度好,属六方晶系纤锌矿(JCPDS 36-1451).循环伏安法研究了该氧化锌结晶过程,并考察了电解液的锌酸盐[Zn(OH)4]2-浓度和基底表面氧化膜对晶须生成的影响.     

丙三醇-变频微波-水热法制备氢氧化镁晶须

以MgCl₂·6H₂O和NaOH为原料, 采用丙三醇-变频微波-水热法制备了优质氢氧化镁晶须. 采用XRD, SEM和TEM进行了物相、粒度、晶体形貌和结构分析. 考察了丙三醇-变频微波-水热法工艺对氢氧化镁晶须晶形、结构及分散性的影响. 实验发现, 在水热反应体系中加入体积分数为15%的丙三醇, 用变频微波加热, 在180 ℃反应6 h, 可获得粒度分布均匀、晶形和分散性好、表面光滑及缺陷少的优质氢氧化镁晶须. 在透射电镜下估算晶须直径约为0.1～0.3 μm, 长度约为80～110 um. 初步分析了变频微波和丙三醇对氢氧化镁晶须生长的作用.     

Bamboo-shaped carbon tubes from coal

Bamboo-shaped carbon tubes (BCTs) were first synthesized in high yields from iron-loaded carbon electrodes prepared from coal by arc discharge. The BCTs were characterized by scanning electron microscopy and transmission electron microscopy (TEM). The TEM characterization reveals that the tubes have bamboo-like structures consisting of hollow compartments separated with conical shaped graphite layers. The diameters of BCTs are in the range of 40–60 nm with their length being about several micrometers. For some BCTs, the hollow compartments are quite uniform with a size of 100 nm. A growth model is suggested to explain the formation of bamboo structure in tubes.     

Synthesis of calcium sulfate hemihydrate whiskers using oyster shells

Herein, the feasibility of preparing long and homogeneous hemihydrate (HH) whiskers using waste oyster shell was investigated. The whiskers formed from the sintered raw material had higher aspect ratios and more uniform morphology than non-sintered. The effect of reaction temperature, reaction time, and concentration were investigated. It was found that the optimum reaction temperature, reaction time, and concentration for stable and well-grown whiskers were 140 °C, 5 h, and 4 wt%, respectively. Direct transition from calcium sulfate dehydrate (DH) to HH was detected by X-ray diffraction (XRD) patterns, and the result showed DH completely transformed to HH after 5 h. The preferred direction of growth along the c-axis was confirmed by XRD pattern, selected area diffraction pattern, and high-resolution transmission electron microscopy (HRTEM).     

Synthesis and synchrotron light-induced luminescence of ZnO nanostructures: nanowires, nanoneedles, nanoflowers, and tubular whiskers

ZnO nanostructures, including single-crystal nanowires, nanoneedles, nanoflowers, and tubular whiskers, have been fabricated at a modestly low temperature of 550 degrees C via the oxidation of metallic Zn powder without a metal catalyst. Specific ZnO nanostructures can be obtained at a specific temperature zone in the furnace depending on the temperature and the pressure of oxygen. Scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and X-ray diffraction (XRD) studies show that ZnO nanostructures thus prepared are single crystals with a wurtzite structure. X-ray excited optical luminescence (XEOL) from the ZnO nanostructures show noticeable morphology-dependent luminescence. Specifically, ZnO nanowires of around 15 nm in diameter emit the strongest green light. The morphology of these nanostructures, their XEOL, and the implication of the results will be discussed.     

Hybrid Nanomaterial Architectures: Combining Layers of Carbon Nanowalls,Nanotubes, and Particles

The paper focuses on the integration in hybrid architectures of plasma produced nanomaterials. The routes for the fabrication of layered structures consisting of carbon nanowalls on carbon nanotubes (CNW/CNT), of carbon nanotubes on carbon nanowalls (CNT/CNW), and nanoparticles on carbon nanowalls (NP/CNW) are presented. The morphology and structure of the hybrid architectures were investigated by electron microscopy techniques. We show that higher substrate temperature promotes the formation of high mass hydrogenated carbon clusters which favors the dominance of CNW growth over that of CNT. On this basis, a procedure of obtaining CNT/CNW architectures by switching the growth regime via substrate temperature is described. The specific limitations or advantages concerning the control or the properties of the obtained architectures are discussed.     

Synthesis and Characterization of ZnO Ellipsoid-like Nanostructures

"ZnO ellipsoid-like structures assembled by ZnO nanrods were fabricated from common ZnO whiskers by autoclave tests and pyrolysis integrated method. X-ray diffraction, scanning electron microscopy, transmission electron microscopy, selected area electron diffraction, and high resolution transmission electron microscopy studies reveal ZnO ellipsoidal structures are single-crystals and formed from direct oriented attachment of nanorods. Raman and room temperature photoluminescence spectra are also discussed."     

Carbon film growth on iron substrates by a CVD method

Carbon film coatings have been produced by a hot‐wall chemical vapor deposition (CVD) method under moderate conditions from pyrolysis of a mixture of propane and argon on an Fe(110) substrate at temperatures of 800–900 °C for different deposition times. The effects of temperature and reaction time on the growth of the carbon films were studied. Field‐emission scanning electron microscopy (FESEM), Raman microscopy, Auger electron spectroscopy (AES) and x‐ray diffraction methods have been performed to study the surface morphologies, growth features and microstructures of the carbon film coatings. The FESEM analyses indicated that carbon films on an Fe substrate consisted of flat‐layer and filamentous morphologies. Raman and AES analyses showed that the carbon initially was crystalline but the degree of disorder in the top layer of the carbon film increased with increasing deposition temperature. High‐resolution transmission electron microscopy studies are also in agreement with Raman results. The same trend was observed when the deposition time was increased from 5 to 30 min. Copyright © 2005 John Wiley & Sons, Ltd.     

Synthesis and characterization of TiO2@C core-shell nanowires and nanowalls via chemical vapor deposition for potential large-scale production

TiO(2) nanowires and nanowalls core structures covered with carbon shell were selectively synthesized by a simple chemical vapor deposition (CVD) method using commercial titanium powder as the starting material. Morphology and structure of the products were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The core shell structure is composed of single crystalline rutile titanium dioxide wrapped by amorphous carbon shell. By adjusting the growth temperature, morphology of the products can be controlled from one-dimensional nanowires to two-dimensional nanowalls. While TiO(2)@C nanowires were a preferred structure at higher temperature, TiO(2)@C nanowalls dominated the final product at lower temperature. A growth mechanism was proposed based on the initial growth state of these nanostructures, in which solid-state diffusion of the elements involved in the reaction was assumed to play an essential role. The obtained TiO(2)@C core shell structures may find potential applications in various nanoscale realms such as optoelectronic, electronic and electrochemical nanodevices and the simple synthesis procedure promises large scale production and commercialization of the titanium oxide@carbon nanostructures.     

Investigation into hemp fiber- and whisker-reinforced soy protein composites

Whiskers, designated as W, were prepared from hemp fibers. Both fibers and whiskers were characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis. Scanning electron microscopy and transmission electron microscopy were used to evaluate the dimensions of the fibers and whiskers, respectively. By incorporating different weight fraction of the fibers and whiskers into soy protein isolate, we prepared two different composites designated as SC and SC-W, respectively. Thiodiglycol was used as a plasticizer for the preparation of composites. The SC and SC-W composites were characterized and compared in terms of mechanical properties, volume fraction of porosity, and water uptake. The results indicated that there was not much significant difference in the properties of the composites. In fact, mechanical properties of fiber-reinforced composites were higher than whisker-reinforced composites at optimum weight fractions. This study can give us the idea about the judicious use of fibers or whiskers as reinforcement materials.     

New boron nitride whiskers: showing strong ultraviolet and visible light luminescence

Boron nitride whiskers with a special structure have been synthesized by a thermal reaction process. The as-prepared BN whiskers have a length of tens of micrometers and a mean diameter of 500 nm. High-resolution TEM analysis shows that the as-prepared BN whiskers can be described as a nanofiber-interweaved network. Infrared and electron energy loss spectra reveal that the BN whiskers are composed of both sigma-sp2 and sigma-sp3 chemical bonds. The UV-vis absorption spectrum displays the energy band gap of the BN whiskers and multiple fine absorption peaks of the phonon-electron coupling. Both photoluminescence (PL) and cathodoluminescence (CL) measurements show the specially structured BN emits strong UV and visible luminescences, which is a promising material for deep-blue and UV applications.     

La~2NiO~4催化制备纳米碳管

制备了四方结构复合氧化物La~2NiO~4,并以其为催化剂前体,甲烷和一氧化碳为碳,合成出大量高纯度的纳米碳管。XRD结果表明La~2NiO~4经还原后,在La~2O~3的隔离作用下Ni晶粒实现纳米级均匀分散。利用TEM,HRTEM,SEM,XRD,Raman等手段对所制备的纳米碳管进行了观察和表征。所制备的纳米碳管管径均匀、石墨化程度较高,该法制备纳米碳管工艺简单、产量较高,产品易于纯化。     

碳纳米管向金刚石纳米晶粒的转变

在碳60（C60）[1]和碳纳米管(CNTs)[2]发现之前,人们知道碳通常显示石墨和金刚石两种晶体结构.自从C60和碳纳米管发现后,由于其独特的纳米结构而具有广泛的应用前景,国内外许多学者致力于研究它们的物理和化学特性,而C60、巴基葱（多层碳纳米球）、碳纳米管和金刚石之间的转变是所研究的焦点之一.目前,由碳的其他形式向金刚石转变的主要方法有：Meilunas等人[3]以C60和C70薄膜为基底气相生长多晶金刚石,C60和C70的稳定性和微平面结构在外界条件下,有利于金刚石成核和外延生长;Banhart[4]小组研究了在电子束辐射作用下巴基葱转变…     

Mineralization of simulated flue gas to prepare CaCO3 whisker using suspended CaSO4

CaCO₃ whiskers were synthesized controllably by introducing simulated flue gas containing CO₂ and N₂ into a CaSO₄ suspension. The effects of solution pH, reaction temperature, and simulated flue gas on the formation of CaCO₃ whiskers were studied. The growth mechanism and growth model of CaCO₃ whiskers had also been provisionally recommended. The reaction product was characterized by scanning electron microscopy analysis, thermogravimetric analysis, and X-ray diffraction analysis. CaCO₃ whiskers with 97% purity were synthesized at pH 7.5, 80°C, 0.1 L/min CO₂ flow rate, and 16.7% CO₂ purity, with a length between 15 and 20 μm and an aspect ratio of about 12.