Growth and morphologies of large-scale SnO2 nanowires, nanobelts and nanodendrites

Single-crystalline SnO₂ nanowires, nanobelts and nanodendrites were synthesized by a simple gas-reaction route on a large scale at 900 °C. They were characterized by means of X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) and selected-area electron diffraction (SAED). FE-SEM images showed that the products consisted of nanowires, nanobelts and nanodendrites that represent a novel morphology reported for the first time. XRD, SAED and EDS indicated that they were single-crystalline tetragonal SnO₂. The influence of experimental conditions on the morphologies of the products is discussed. Received: 3 June 2002 / Accepted: 10 June 2002 / Published online: 10 September 2002 RID="*" ID="*"Corresponding author. Fax: 86-10/82649531, E-mail: xlchen@aphy.iphy.ac.cn     

Synthesis of In-doped Ga2O3 zigzag-shaped nanowires and optical properties

In-doped Ga₂O₃ zigzag-shaped nanowires and undoped Ga₂O₃ nanowires have been synthesized on Si substrate by thermal evaporation of mixed powders of Ga, In₂O₃ and graphite at 1000 °C without using any catalyst via a vapor-solid growth mechanism. The morphologies and microstructures of the products were characterized by field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS) and photoluminescence spectroscopy (PL). The nanowires range from 100 nm to several hundreds of nanometers in diameter and several tens of micrometers in length. A broad emission band from 400 to 700 nm is obtained in the PL spectrum of these nanowires at room temperature. There are two blue-emission peaks centering at 450 and 500 nm, which originate from the oxygen vacancies, gallium vacancies and gallium-oxygen vacancy pairs.     

Growth mechanism and photoluminescence of the SnO2 nanotwists on thin film and the SnO2 short nanowires on nanorods

SnO2 nanotwists on thin film and SnO2 short nanowires on nanorods have been grown on single silicon substrates by using Au-Ag alloying catalyst assisted carbothermal evaporation of SnO2 and active carbon powders.The morphology and the structure of the prepared nanostructures are determined on the basis of field-emission scanning electron microscopy(FESEM),transmission electron microscopy(TEM),selected area electronic diffraction(SAED),high-resolution transmission electron microscopy(HRTEM),x-ray diffraction(XRD),Raman and photoluminescence(PL) spectra analysis.The new peaks at 356,450,and 489 nm in the measured PL spectra of two kinds of SnO2 nanostructures are observed,implying that more luminescence centres exist in these SnO2 nanostructures due to nanocrystals and defects.The growth mechanism of these nanostructures belongs to the vapour-liquid-solid(VLS) mechanism.     

球形SnO2 纳米微粒的合成及形成机理分析

以SnCl4·5H2 O为主要原料 ,用溶剂热技术在油酸体系中成功地合成了球形SnO2 纳米微粒 ,在无水乙醇体系中合成了菱形的SnO2 纳米微粒 .通过X射线粉末衍射 (XRD) ,选区电子衍射 (SAED)和透射电镜 (TEM )对两种产物进行了表征 ,并对两种产物的形成机理进行了分析 .透射电镜 (TEM)结果表明 :在油酸体系中得到了平均尺寸约为 3.5nm的球形SnO2 纳米微粒 ,此微粒趋向于特殊高的比表面积 ,适合于作气敏探测器材料方面的应用     

Synthesis of β-Ga2O3 nanowires through microwave plasma chemical vapor deposition

In this study, we demonstrate the large-scale synthesis of beta gallium oxide (β-Ga₂O₃) nanowires through microwave plasma chemical vapor deposition (MPCVD) of a Ga droplet in the H₂O and Ar atmosphere at 600 W. Unlike the commonly used MPCVD method, the H₂O, not mixture of gas, was employed to synthesize the nanowires. The ultra-long β-Ga₂O₃ nanowires with diameters of about 20-30 nm were several tens of micrometers long. The morphology and structure of products were analyzed by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscope (HRTEM). The growth of β-Ga₂O₃ nanowires was controlled by vapor-solid (VS) crystal growth mechanism.     

Determination of the crystal structure of U6Fe5Al8Si9 by electron crystallography

The crystal structure of U₆Fe₅Al₈Si₉ was re-determined by electron crystallography, using selected area electron diffraction (SAED) and high resolution (HRTEM) images, taken along the [0 0 1] direction. The obtained results are very similar to those found previously by X-ray powder diffraction. The differences between the atomic positions found by SAED and HRTEM images and those found by X-ray powder diffraction were 0.11 and 0.08 Å, respectively.     

Synthesis and characterization of axially periodic Zn2SnO4 dendritic nanostructures

Zn2SnO4 （ZTO） nanowires with a unique dendritic nanostructure were synthesized via a simple one-step thermal evaporation and condensation process. The morphology and microstructure of the ZTO nanodendrite have been investigated by means of field emission scanning electron microscopy （SEM）, x-ray diffraction （XRD） and high-resolution transmission electron microscopy （HRTEM）. SEM observation revealed the formation of branched nanostructures and showed that each branch exhibited a unique periodic structure formed by a row of overlaid rhombohedra of ZTO nanocrystals along the axis of the nanobranch. HRTEM studies displayed that the branches grew homoepitaxially as single-crystalline nanowires from the ZTO nanowire backbone. A possible growth model of the branched ZTO nanowires is discussed. To successfully prepare branched structures would provide an opportunity for both fundamental research and practical applications, such as three-dimensional nanoelectronics, and opto-electronic nanodevices.     

化学气相沉积法中SnO2一维纳米结构的控制生长

以Sn和SnO为源材料，化学气相沉积法中通过控制反应物配比及载气中的氧含量等宏观实验条件，实现了SnO₂一维纳米结构的控制生长，成功获得各种不同横向尺度的SnO₂纳米线、纳米带以及直径连续变化的针状纳米结构. 通过扫描电子显微镜、X射线衍射仪对不同实验条件下所制备的样品进行形貌和晶格结构表征，认为高温生长点附近锡与氧的相对含量是控制SnO₂一维纳米结构生长的关键因素；并在此基础上对SnO₂一维纳米结构的生长机理进行了深入的讨论.     

Synthesis and structural characterization of perovskite 0.65Pb(Mg1/3Nb2/3)O3-0.35PbTiO3 nanotubes

We report the synthesis and structural characterization of 0.65Pb(Mg_1/3Nb_2/3)O₃-0.35PbTiO₃ (PMN-PT) nanotubes prepared by a novel sol-gel template method. X-ray diffraction (XRD) and selected-area electron diffraction (SAED) investigations demonstrated that the postannealed (650 °C for 1 h) PMN-PT nanotubes were polycrystalline with perovskite crystal structure. The field emission scanning electron microscope (FE-SEM) shows that as prepared PMN-PT nanotubes were hollow with diameter to be about 200 nm. High resolution transmission electron microscope (HRTEM) analysis confirmed that the obtained PMN-PT nanotubes made up of nanoparticles (10-20 nm) which were randomly aligned in the nanotubes. Energy-dispersive X-ray spectroscopy (EDX) analysis confirmed the stoichiometric 0.65Pb(Mg_1/3Nb_2/3)O₃-0.35PbTiO₃. The possible formation mechanism of PMN-PT nanotubes was proposed at the end.     

氧氩比对SnO2/Ag/SnO2透明导电膜光电性能的影响

在室温及不同的氧氩比条件下,采用射频磁控溅射Ag层和直流磁控溅射SnO2层,在载玻片衬底上制备出了SnO2/Ag/SnO2多层薄膜.用霍尔效应测试仪、四探针电阻测试仪和紫外-可见-近红外光谱仪等表征了薄膜的电学性质和光学性质.实验结果表明:当氧氩比为1:14时,所制得的薄膜的光电性质优良指数最大,为1.69×10-2 Ω-1;此时,薄膜的电阻率为9.8×10-5Ω·cm,方电阻为9.68Ω/sq,在400～800 nm可见光区的平均光学透射率达85％;并且,在氧氩比为1:14时,利用射频磁控溅射Ag层和直流磁控溅射SnO2层在PET柔性衬底上制备出了光电性质优良的柔性透明导电膜,其在可见光区的平均光学透过率达85％以上,电阻率为1.22×10-4Ωcm,方电阻为12.05Ω/sq.     

Al2O3衬底无催化剂生长GaN纳米线及其光学性能

采用一种绿色的等离子增强化学气相沉积法,以Al2O3为衬底, Ga金属为镓源, N2为氮源,在不采用催化剂的情况下,成功制备获得了结晶质量良好的GaN纳米线.研究表明,生长温度可显著调控GaN纳米线的形貌,当反应温度为950℃时,生长出的GaN微米片为六边形;当反应温度为1000℃时,生长出了长度为10-20μm的超长GaN纳米线.随着反应时间增加, GaN纳米线的长度增加. GaN纳米线内部存在着压应力,应力大小为0.84 GPa.同时,也进一步讨论了GaN纳米线无催化剂生长机制. GaN纳米线光致发光结果显示, GaN纳米线缺陷较少,结晶质量良好,在360 nm处有一个较为尖锐的本征发光峰,可应用于紫外激光器等光电子器件.本研究结果将为新型光电器件低成本绿色制备提供一个可行的技术方案.     

Photoluminescence of polycrystalline CuIn0.5Ga0.5Te2 thin films grown by flash evaporation

Polycrystalline CuIn_0.5Ga_0.5Te₂ films were deposited by flash evaporation from ingot prepared by reacting, in stoichiometric proportions, high purity Cu, In, Ga and Te elements in vacuum sealed quartz. The as-obtained films were characterized by X – ray diffraction (XRD), transmission electron microscopy (TEM) combined with energy dispersive spectroscopy (EDS). XRD and TEM results showed that the layer has a chalcopyrite-type structure, predominantly oriented along (112) planes, with lattice parameters a?=?0.61?nm and c?=?1.22?nm. The optical properties in the near - infrared and visible range 600–2400?nm have been studied. The analysis of absorption coefficient yielded an energy gap value of 1.27?eV. Photoluminescence analysis of as-grown sample shows two main emission peaks located at 0.87 and 1.19?eV at 4?K.     

Fabrication and magnetic properties of ordered Fe60Pb40 nanowire arrays electrodeposited in AAO templates

Ordered ferromagnetic-nonmagnetic heterogeneous Fe₆₀Pb₄₀ nanowire arrays were successfully fabricated by alternating current (AC) electrodeposition into nanoporous alumina templates. Transmission electron microscopy (TEM) image and selected-area diffraction (SAED) pattern analysis showed that the Fe₆₀Pb₄₀ nanowires are polycrystalline with an average diameter of 22 nm and lengths up to several micrometers. X-ray diffraction (XRD) observations indicated that α-Fe and fcc Pb phase coexist and do not form metastable alloy phase. The as-deposited samples were annealed at 200, 300, 400 and 500 ^°C, respectively. Magnetic measurements showed that nanowires have high magnetic anisotropy with their easy axis parallel to the nanowire arrays, and the coercivity of the samples increased with the annealing temperature up to 400 ^°C and reached a maximum (2650 Oe). The change of magnetic properties associated with the microstructure was discussed.     

合成温度和N2/O2流量比对碳纤维衬底上生长的SnO2纳米线形貌及场发射性能影响

采用化学气相沉积法系统研究了合成温度和N₂/O₂流量对生长在碳纤维衬底上的SnO₂纳米线形貌及场发射性能的影响规律. 利用扫描电镜(SEM)、透射电镜(TEM), X射线衍射(XRD)及能谱仪(EDS)对产物细致表征, 结果表明, SnO₂纳米线长径比随反应温度的升高而增大; 随N₂/O₂流量比值的增大先增大后变小, 场发射测试表明, 合成温度780 ℃, N₂/O₂流量比为300 : 3 时SnO₂纳米线阵列具有最佳的场发射性能, 开启电场为1.03 V/μm, 场强增加到1.68 V/μm时, 发射电流密度达0.66 mA/cm², 亮度约2300 cd/m².     

Study of the synthesis and Cl2 gas-sensing properties of nanometer HNO3-doped SnO2

We focused on the effects of the inorganic acid HNO₃ on the gas-sensing properties of nanometer SnO₂ and prepared the powders via a dissolution-pyrolysis method. Furthermore, the powders were characterized by means of X-ray diffraction (XRD), scanning electron microscope (SEM), field emission scanning electron microscopy (FESEM) and energy-dispersive X-ray spectra (EDS). Several aspects were surveyed, including the calcining temperature, concentration of nitric acid and the working temperature. The results showed that the gas response of 3 wt% HNO₃-doped SnO₂ powders (calcined at 500 °C) to 10 ppm Cl₂ reached 316.5, at the working temperature 175 °C. Compared with pure SnO₂, appropriate HNO₃ could increase the gas sensitivity to Cl₂ gas more significantly.     

Observation of defects and growth orientations of YBa2Cu3Ox thin films with YSZ buffer layers on Si

We have investigated defects and in-plate orientations of YBa₂Cu₃O_x thin films prepared by pulsed laser deposition (PLD) with YSZ as a buffer layer. The films showed c-axis oriented growth with the transition temperature T_co up to 87 K. Several types of defects including thermally induced cracks, grain boundaries and outgrowths were observed by scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). The grain boundary provided a favorable path for crack propagation. The outgrowths nucleated on the YSZ surface grew with stoichiometric composition. According to X-ray diffraction (XRD) and HRTEM studies the YSZ buffer layer grew with the orientation relationship, YSZ110//Si110 and YSZ(001)//Si(001) up to the YBCO/YSZ interface. The superconducting YBCO films on top grew mainly with YBCO100//Si110 and YBCO(001)//Si(001), with some minor portions of YBCO110//Si110 and YBCO(001)//Si(001).     

锡催化剂助生长法制备孪晶ZnO纳米线及其结构表征

用SnO和Zn的均匀混合物在高温下共烧通过VLS机制制备出孪晶ZnO纳米线的均匀结构。SEM图像显示孪晶ZnO纳米线的直径在100~200nm之间,长度在几十微米到几百微米之间的范围内,有的甚至达到了毫米级,产率也非常的高。TEM图像中ZnO孪晶纳米线顶端的金属Sn颗粒表明了孪晶结构的Sn催化生长。高分辨电子图谱显示了氧化锌纳米线孪晶结构的特征。电子衍射分析发现孪晶氧化锌的晶带轴的方向是[0110],孪晶面为(1013),并且通过明场像和暗场像分析了孪晶纳米线的晶格关系,确定了孪晶纳米线的汽-液-固(VLS)生长机制。     

Synthesis, morphologies and Raman-scattering spectra of crystalline stannic oxide nanowires

SnO₂ nanowires were synthesized using a direct gas reaction route and were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), selected-area electron diffraction (SAED), high-resolution transmission electron microscopy (HRTEM) and Raman-scattering spectroscopy. XRD, SEM, SAED and HRTEM indicated that the products were tetragonal SnO₂ nanowires with diameters of 10–50 nm. The nanowires were single crystal and solid inside. Dendritic nanowires were observed for the first time. Three vibrational modes were observed in the Raman spectra of the samples. Received: 7 January 2002 / Accepted: 11 April 2002 / Published online: 19 July 2002     

Photoluminescence from Er3+ ion and SnO2 nanocrystal co-doped silica thin films

Er3+ ions embedded in silica thin films co-doped by SnO2 nanocrystals are fabricated by sol-gel and spin coating methods. Uniformly distributed 4-nm SnO2 nanocrystals are fabricated, and the nanocrystals showed tetragonal rutile crystalline structures confirmed by transmission electron microscope and X-ray diffraction measurements. A strong characteristic emission located at 1.54 μm from the Er3+ ions is identified, and the influences of Sn doping concentrations on photoluminescence properties are systematically evaluated. The emission at 1.54 μm from Er3+ ions is enhanced by more than three orders of magnitude, which can be attributed to the effective energy transfer from the defect states of SnO 2 nanocrystals to nearby Er3+ ions, as revealed by the selective excitation experiments.