高频热等离子体气相合成一维纳米氧化锌研究

把锌粉原料加入到高频常压热等离子体弧中,使锌粉加热气化,然后与加入等离子体反应器中的氧气反应,合成出了直径为50nm、长度超过2靘的一维棒状纳米氧化锌.研究了氧分压和锌粉加料速度对合成产物形貌的影响,结果表明,通过控制这些参数,可以调控合成的氧化锌纳米棒长径比.采用XRD、SEM、TEM和HRTEM对产物的形貌和结构进行了表征,并衷征了合成的氧化锌纳米棒的光致发光性能.     

钛酸纳米管的制备及 TEM表征

采用水热合成法以金红石型纳米TiO2粉为原料制备钛酸纳米管，考察了搅拌、酸洗及焙烧温度对纳米管的形成和结构的影响，并通过TEM观察了产物的形貌、结构．结果显示：持续搅拌能促进原料粉末的定向生长，有利于形成钛酸纳米片；酸洗是纳米管的形成阶段；300℃是纳米管转变为长棒状晶柱的临界温度．实验表明以优化的水热合成法制得的纳米管形貌均一，长度超过1μm，钛酸纳米管长径比为125：1．     

水热合成Sb_2Se_3纳米线及其对Bi_2Te_3纳米粉末热电性能的影响

以SbCl3和Se粉为原料,水合肼(N2H4·H2O)为还原剂,采用水热法在150℃下,分别保温不同的时间合成Sb2Se3纳米粉末.通过X射线衍射(XRD)、场发射电子扫描电镜(FESEM)、透射电镜(TEM)以及高分辨透射电镜(HRTEM)等分析方法对产物的物相成分和微观形貌等进行了表征,实验结果表明保温时间达到24h时,获得产物为单相Sb2Se3纳米线晶体.根据实验结果还研究了水热合成Sb2Se3纳米线晶体可能的反应及生长机理,结果表明一维纳米线沿[001]方向生长,纳米线的形成与其独特的层状晶体结构有关.最后采用放电等离子体快速热压烧结法将水热合成的Bi2Te3纳米粉末与不同含量Sb2Se3纳米线进行复合,分析了Sb2Se3纳米线对Bi2Te3纳米材料热电性能的影响,发现复合约1at%Sb2Se3纳米线可以使Bi2Te3纳米材料热电性能有一定提高.     

合成条件对V2O5溶胶制备AgVO3准一维纳米材料的影响

以V2O5溶胶和Ag2O为反应物，用超声波辅助处理和水热反应成功制备了AgVO3准一维纳米材料。采用XRD、SEM等方法对产物的结构进行表征和测试，研究了水热反应温度、时间、搅拌与超声处理等条件对AgVO，一维纳米材料合成的影响。结果表明，得到的AgVO，准一维纳米材料长几到数十微米，直径100-400nm的纳米纤维聚集成束状结构。升高水热反应温度和延长反应时间均有利于AgVO，准一维纳米材料的形成，但当反应时间过长时，晶粒的择优取向生长变弱，产物逐渐生长为微米级的块状结构。搅拌和超声处理使固体反应物Ag2O充分、均匀进入到V2O5溶胶层间，使反应在较低温度下就可以进行。     

从零维到一维递变氧化锡纳米材料的可控制备

为了研究纳米半导体材料的量子限域效应与形貌和结构的关系,本文以SnCl4.5H2O和不同的有机酸以及不同的胺类有机物为反应物,通过溶剂热法制备了不同形貌的氧化锡纳米材料。在其它实验条件相同的前提下,通过配制不同的反应物体系,通过在同一反应体系中经过不同的溶剂热反应时间,均成功获得了从零维到一维递变的不同长径比的氧化锡纳米材料,包括纳米点、纳米棒、纳米线等。本文还尝试了在同一反应体系中使用不同的表面活性剂的方法,虽然没有获得从零维到一维递变的产物,但产物仍然具有不同形貌。     

一维硅纳米材料形貌的研究

一维硅纳米材料是重要的纳米电子器件材料,由于其形貌不同,导致的电学等特性也不相同,因此一维硅纳米材料的形貌是重要的研究内容之一.一维硅纳米结构包括纳米线、纳米带及纳米管等,同种一维硅纳米材料由于制备方法不同其形貌也不相同.评述了一维硅纳米材料的形貌及其制备方法.     

载气在CVD法制备纳米碳管工艺中的作用

纳米碳管是性能优异的具有准一维特征的纳米材料,CVD法是制备纳米碳管的典型工艺之一。本文以乙炔气体为原料气体、循环失效后的贮氢电极舍金材料作为反应催化剂,研究了在相同反应条件下,CVD法制备纳米碳管过程中载气对纳米碳管形貌和产率的影响。通过对产物TEM观察和TG分析发现,虽然载气不直接参与合成反应但对产物产率和形貌有很大的影响,氢气作为载气可以获得形貌和热稳定性更好的纳米碳管。     

温度对ZnO／Ag纳米复合抗菌剂前驱体及产物的影响规律研究

以硫酸锌、硝酸银为原料，碳酸氢氨为沉淀剂制备出高纯度ZnO／Ag纳米复合抗菌剂。重点研究了合成温度及煅烧温度对前驱体微观形貌及最终产物的结构、成份、形貌的影响规律。用TEM、XRD、TG-DTG对前驱体和ZnO／Ag纳米复合抗菌剂进行了表征，结果表明：随着合成温度的升高，前驱体产物的形态由线棒状逐渐变为球团状，并且由非晶态逐渐转化为晶态；450℃煅烧所得复合粉体由六方纤锌矿纳米ZnO和立方结构纳米Ag组成，粒径集中在15nm左右，粒子大小均匀，分散性良好；经权威机构检测本抗菌剂抗菌性能优异。     

一维β-SiAlON材料可控合成

以Si粉、Al粉和Al2O3粉为原料压制成条样,在1650~1850 K氮气和埋Si3N4颗粒气氛下分别合成了β-SiAlON晶须、带状和柱状晶,并系统研究了一维β-SiAlON材料可控合成条件,进而结合热力学分析了一维β-SiAlON材料的生长机制。结果表明:以Si粉、Al粉和Al2O3为原料,在氮气(纯度99.9%)和埋Si3N4颗粒气氛下在1650~1850 K保温6 h,可以合成不同形貌的一维β-SiAlON材料。生长温度是一维β-SiAlON材料形貌控制的关键因素。生长温度为1650 K时,合成了β-SiAlON晶须,晶须直径200~400 nm,长径比100~1000;生长温度在1700~1800 K时,可以合成β-SiAlON带状晶体,厚度为200 nm,宽度为1~4μm,长宽比在10~20之间;生长温度升高至1800 K时,出现大量柱状晶体。结合晶须显微结构形貌和热力学分析,β-SiAlON晶须的生长机制为气–固(VS)生长机制。     

乙醇火焰中的一维碳纳米材料及其生长机理研究

文章利用扫描电镜（SEM）、透射电镜（TEM）系统观察和研究了乙醇燃烧火焰中合成的具有各种不同形貌特征的一维碳纳米材料。观察发现燃烧产物中除了“空心”碳纳米管和平直“实心”碳纳米纤维以外,还包括锥状、单螺旋型、双螺旋型、带状、节状、疏松状、节状-螺旋混合型、平直-螺旋混合型等形貌特殊的一维碳纳米材料。研究认为影响它们生长的主要因素有：Fe和Ni元素与碳的亲和力的差异、基板预处理、火焰的宽区域和不稳定性等。对火焰中各种形貌一维碳纳米材料的生成机理和过程进行了分析和讨论。     

Fabrication of single-crystal ZnO nanorods and ZnS nanotubes through a simple ultrasonic chemical solution method

A simple and rapid method has been developed for the preparation of rod-like ZnO nanocrystals via ultrasonic irradiation. The as-synthesized ZnO nanocrystals were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). The ZnO nanorods had an average diameter of 15-70 nm that varied from the ultrasonic operation mode. The results showed that Zn powder played an important role in the synthesis of ZnO nanorods. Through adding a sulfur source in the reaction system, ZnO/ZnS nanocables and ZnS nanotubes could be obtained with continuous ultrasonic irradiation. The formation mechanism of ZnS nanotubes could be attributed to the Kirkendall effect.     

Fabrication of ZnS/ZnO hierarchical nanostructures by two-step vapor phase method

A simple two-step vapor phase method is presented to fabricate ZnS/ZnO hierarchical nanostructures in bulk quantities. That is ZnS nanobelts were first synthesized and then used as substrate for growth of ZnO nanorod arrays. Investigation results demonstrate that the polar surfaces of ZnS nanobelts could induce a preferred asymmetric growth of ZnO nanorods on the side surfaces. But it is believed that if the local concentration of ZnO was high enough, ZnO nanorods could also grow symmetrically on the top/bottom surface of the ZnS nanobelts. The optical property of the products was also recorded by means of photoluminescence (PL) spectroscopy.     

An efficient room-temperature route to uniform ZnO nanorods with an ionic liquid

Rod-like ZnO nanocrystals have been synthesized via an ultrasound-assisted way by the reaction between Zn(CH₃COO)₂·2H₂O and NaOH in the ionic liquid 1-butyl-3-methyl imidazole six hexafluorophosphoric acid salts ([BMIM][PF₆]) aqueous solution. The products were characterized by XRD, EDX, FESEM, TEM, HRTEM, UV-Vis and PL techniques. The as-prepared ZnO nanorods have a diameter of about 50 nm and a length of 1-2 μm. A plausible four-step mechanism was proposed to explain the formation of ZnO nanorods. It was found that the lowered ion diffusion velocity in the water-ionic liquid medium could largely contribute to the formation of the ZnO nanorods. The effects of experimental parameters on the formation of the products were also explored.     

Microemulsion-mediated solvothermal synthesis of ZnS nanowires

Uniform and high-aspect-ratio ZnS nanowires with length up to several micrometers and diameter of 30–50 nm are synthesized by a facile and low-cost microemulsion-mediated solvothermal method. Moreover, ZnS nanorods and bamboo-leaf-like ZnS nanostructures were also obtained by modulating the reaction parameters. Especially, hollow bamboo-leaf-like ZnS nanostructures formed by radiating those bamboo leaves with electron beam. A reasonable mechanism to the formation of the as-prepared one-dimension zinc blend ZnS nanocrystals is also discussed.     

Flame synthesis of zinc oxide nanocrystals

Distinctive zinc oxide (ZnO) nanocrystals were synthesized on the surface of Zn probes using a counter-flow flame medium formed by methane/acetylene and oxygen-enriched air streams. The source material, a zinc wire with a purity of ～99.99% and diameter of 1 mm, was introduced through a sleeve into the oxygen rich region of the flame. The position of the probe/sleeve was varied within the flame medium resulting in growth variation of ZnO nanocrystals on the surface of the probe. The shape and structural parameters of the grown crystals strongly depend on the flame position. Structural variations of the synthesized crystals include single-crystalline ZnO nanorods and microprisms (ZMPs) (the ZMPs have less than a few micrometers in length and several hundred nanometers in cross section) with a large number of facets and complex axial symmetry with a nanorod protruding from their tips. The protruding rods are less than 100 nm in diameter and lengths are less than 1 μm. The protruding nanorods can be elongated several times by increasing the residence time of the probe/sleeve inside the oxygen-rich flame or by varying the flame position. At different flame heights, nanorods having higher length-to-diameter aspect-ratio can be synthesized. A lattice spacing of ～0.26 nm was measured for the synthesized nanorods, which can be closely correlated with the (0 0 2) interplanar spacing of hexagonal ZnO (Wurtzite) cells. The synthesized nanostructures were analyzed by scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution TEM (HR-TEM), X-ray energy dispersive spectroscopy (EDS), and selected area electron diffraction pattern (SAED). The growth mechanism of the ZnO nanostructures is discussed.     

Preparation and characterization of ZnO/ZnS core/shell nanocomposites through a simple chemical method

In this paper, we reported the preparation of ZnO/ZnS core/shell nanocomposites by sulfidation of ZnO nanostructures via a simple hydrothermal method. The precursors of bare ZnO nanoparticles and ZnO nanorods were synthesized by a surfactant-assisted hydrothermal growth. The structural, morphological, and element compositional analysis of bare ZnO nanostructures and ZnO/ZnS core/shell nanocomposites were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and transmission electron microscopy techniques. The XRD results indicated that the phase of bare ZnO nanoparticles and ZnO nanorods was wurtzite structure, and the phase of coated ZnS nanoparticles on the surface of bare ZnO nanostructures was sphalerite structure with the size of about 8 nm. Photoluminescence measurement was carried out, and the PL spectra of ZnO/ZnS core/shell nanocomposites revealed an enhanced UV emission and a passivated orange emission compared to that of bare ZnO nanostructures. In addition, the growth mechanism of ZnO/ZnS core/shell nanostructures through hydrothermal method was preliminarily discussed.     

Zn_(1-x)Mn_xS稀磁半导体的合成与光学性能

通过水热法制备不同掺杂浓度的Zn_(1-x)Mn_xS(x=0.00,0.02,0.05,0.07)稀磁半导体材料,研究Mn~(2+)掺杂浓度对ZnS纳米棒微观结构和光学性能的影响。采用X射线衍射(XRD)、高分辨透射电子显微镜(HRTEM)、选区电子衍射(SAED)、X射线能量色散分析谱仪(XEDS)和紫外可见吸收光谱(UV-vis)对样品的晶体结构、形貌和光学性能进行表征。结果表明:制备的所有样品均具有结晶良好的纤锌矿结构,没有杂峰出现,生成纯相Zn_(1-x)Mn_xS纳米晶。样品形貌为纳米棒状结构,分散性良好。掺杂的Mn元素进入到ZnS纳米晶中,Mn~(2+)替代了Zn~(2+),而且随着Mn掺杂量的增加晶格常数减小。同时UV-vis光谱发现样品的光学带隙增大,发生了蓝移现象。     

Controllable synthesis of ZnO with various morphologies by hydrothermal method

ZnO microstructures with various morphologies have been controllably synthesized by hydrothermal route using different precipitant and zinc source in liquid solution. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to characterize the ZnO2, Zn(OH)2 and ZnO structures to understand the role of precipitant and precursors in the growth of various morphologies. The nucleation and growth process can regulate by changing the precipitant. When H2O2 was used as precipitant, ZnO particles with a rather uniform particle size of -500 nm and a rather rough surface was obtained. While, ZnO synthesized in this polyvinyl pyrrolidone (PVP) solution has the same granular morphology with particle size of 300-1000 nm. In contrast, ZnO sunflower and polyhedron aggregates composed of several smaller polyhedron were formed, when ammonium hydroxide and NH4HCO3 was applied, respectively. Meanwhile, precursors play an important role in the determination of the morphology of ZnO. Sunflower and dumbbell like ZnO composed of nanosheets were obtained, when different centrifugal component of Zn(OH)2 suspension was applied as zinc source. In contrast, sunflower and dumbbell like ZnO composed of nanorods and ZnO rods were obtained, when different centrifugal components of ZnO2 suspension were used as zinc sources. The growth mechanism of ZnO nanostructures fabricated by the hydrothermal process using different zinc sources was tentatively investigated.     

高质量四脚状ZnO纳米结构的制备及其影响因素

采用汽相传输法制备高质量四脚状ZnO纳米结构(T-ZnO).以ZnO纳米晶为同质催 化剂,在锌源-衬底间添加蒸汽过滤器,研究过滤器和纳米晶对产物组成和形态的影响,以及 T-ZnO的结构特征.实验结果表明,T-ZnO为纤锌矿结构,分布均匀、尺寸一致,由四个柱 状纳米棒和一个球形核心组成.纳米棒直径约为60nm,沿<0001>晶向生长.过滤器的使用可 有效地去除产物中颗粒,而ZnO纳米晶的使用明显降低其尺寸,提高其均匀性.     

Microstructure Characterization of Single-crystal ZnO Nanorods Synthesized by Solvothermal at Low Temperature

Single-crystalline ZnO nanorods have been synthesized by a simple solvothermal process at low temperature. Transmission electron microscopy （TEM） observations have confirmed that the as-synthesized products have rod-like morphologies with diameters ranging from several nanometers to 30 nm and lengths from 100 nm to 2 μm. Such hexagonal ZnO nanorods are structurally uniform and the growth direction is identified to be [0001]. Growth mechanism of the ZnO nanorods was proposed.