Zn基片上ZnO及ZnS/ZnO复合纳米阵列的液相合成及发光性质

采用温和的溶液路线在Zn基片上合成了单晶态的ZnO纳米棒阵列、 纳米片阵列和ZnS/ZnO复合双层纳米棒阵列. 使用X射线粉末衍射仪、 扫描电子显微镜、 高分辨透射电子显微镜、 X射线光电子能谱仪等对产物的组成、 结构及形貌进行了表征. 讨论了表面活性剂在液相合成中对产物形貌的调控作用. 通过室温发射光谱的测定, 研究了所得纳米阵列材料的发光性质.     

水热法生长方式对ZnO纳米棒阵列结构和性能的影响

本文系统地比较了三种方式制备的ZnO纳米棒阵列的结构和性能的异同.根据水热法生长液中碱来源的不同,ZnO纳米棒阵列的生长方式分为三种:N方式(氨水)、H方式(六次甲基四胺)和NH方式(两次N方式和一次H方式).通过扫描电子显微镜,对这三种方式生长的ZnO纳米棒阵列形貌进行了表征.此外,利用X射线衍射仪、透射电子显微镜和激光拉曼光谱对ZnO的结晶性能进行比较.结果表明,ZnO纳米棒阵列的取向性N≈NH>H,ZnO的晶体质量H>NH>N.NH方式综合N方式和H方式的优势,得到了取向性和晶体质量优良的ZnO纳米棒阵列.这将为在进一步应用中有效地选择ZnO纳米棒阵列的制备方式提供重要信息.     

氧化锌纳米棒的水热合成及其光催化性能

以分析纯ZnO作为锌源、NaOH为矿化剂、盐酸为反应溶液pH调节剂,利用水热反应制备了花状ZnO纳米棒;采用扫描电子显微镜和X射线衍射仪分析了产物的形貌和结构,考察了水热温度以及Zn2+和OH-浓度比对产物形貌的影响;以甲基橙为目标降解物,采用紫外-可见分光光度计研究了ZnO纳米棒的光催化性能.结果表明,在水热反应温度80℃、Zn2+/OH-浓度比1∶7.5条件下所得ZnO纳米棒呈花状聚合,直径约为200nm,长度约为2μm,具有六方纤锌矿结构.当甲基橙初始浓度为30 mg.L-1、ZnO纳米棒的投放量为1.5g.L-1时,以300W紫外灯照射150min,甲基橙的降解率可达90%.     

基底对电沉积制备ZnO纳米棒阵列的影响

采用恒电位电沉积方法, 在未经修饰的ITO导电玻璃基底上通过控制实验条件制备出不同形貌的纳米ZnO结构, 而在经过ZnO纳米粒子膜修饰后的ITO导电玻璃基底上, 制备出透明、高取向、粒径小于30 nm的ZnO纳米棒阵列. 用扫描电子显微镜(SEM)、X射线衍射(XRD)以及透射光谱对制备出的ZnO纳米棒阵列的结构、形貌和透明性进行了表征. 测试结果表明, ZnO纳米棒阵列的平均直径为21 nm, 粒径分布窄, 约18～25 nm, 择优生长取向为[001]方向, 垂直于基底生长. 当入射光波长大于400 nm时, ZnO纳米棒阵列的透光率大于95%.     

金纳米棒负载的静电纺丝纤维的制备及其表面增强拉曼光谱性能

为简单有效地制备高活性表面增强拉曼光谱(Surface-enhanced Raman Spectroscopy,SERS)基底。本文采用静电纺丝聚乙烯醇(PVA)/聚丙烯酸(PAA)纳米纤维为支撑材料,通过直接浸泡的方法,利用金纳米棒与电纺纤维之间的静电力,使纳米棒在纤维表面自组装,得到了性能优异的SERS基底。通过透射电子显微镜、扫描电子显微镜对金纳米棒以及不同状态下的电纺纤维的形貌进行表征,结果表明,金纳米棒均匀且密集地负载在纤维表面。通过设置不同的浸泡时间确定了金纳米棒组装平衡的时间为12 h,并通过调控纺丝时间和金纳米棒的浓度发现随着纺丝时间和金纳米棒浓度的增加,复合纤维膜SERS增强效果随之提升。该复合纤维膜具有优异的SERS均匀性,并且能够检测到浓度低至10~(-10)mol/L的4-氨基苯硫酚的存在。     

不同形貌ZnO纳米结构的电子显微分析

控制实验合成条件,利用溶胶-凝胶法和化学溶液生长法制备出不同形貌的ZnO纳米结构。采用X射线衍射仪(XRD)、扫描电子显微镜( SEM) 以及透射电子显微镜(TEM)等多种测试手段对ZnO纳米结构的微观形态及晶相进行了分析。结果表明:3种ZnO纳米结构形貌虽不同,但均具有Z nO六方纤锌矿晶相结构。ZnO纳米棒和花状ZnO纳米结构为单晶,生长方向均沿(0001)方向。ZnO纳米球则为多晶。     

金修饰ZnO纳米棒阵列制备及对甲醛气敏性能

通过两步溶液法在氧化铝陶瓷管上先制备出ZnO纳米棒阵列,再用真空蒸镀法在ZnO纳米棒表面形成一层均匀Au膜,于500℃下热处理得到Au纳米颗粒修饰的ZnO(Au-ZnO)纳米棒阵列体系。通过场发射扫描电子显微镜(FE-SEM)和X射线衍射仪(XRD)对ZnO纳米棒阵列和Au-ZnO纳米复合体系进行表面形貌表征和结构分析。气敏性能测试结果表明,Au-ZnO纳米复合体系在300℃下对1000μL·L-1甲醛的灵敏度为41.5,而在200℃下灵敏度仍能达到10.3,表明可以制备低工作温度下气敏性能良好的甲醛气敏传感器。     

以CuC2O4微球为模板可控合成一维CuC2O4/ZnO异质结构

以CuC2O4纳米微球为模板,通过水热法在120 ℃、1 h时成功合成了一维CuC2O4/ZnO异质结构。 采用热重分析（TGA）、场发射扫描电子显微镜（FE-SEM）、能量散射Ｘ射线谱（EDX）、透射电子显微镜(TEM)和Ｘ射线粉末衍射(XRD)等测试技术对产物的结构和形貌进行了表征。 结果表明,所得产物为一维CuC2O4/ZnO纳米棒束,长约1 μｍ,直径约500 nm。 每个棒束由许多纳米棒沿同一方向组装而成。 TEM照片和EDX光谱表明,CuC2O4和ZnO形成了均匀的异质结构。     

溶剂热法制备六角锥形ZnO及其光致发光性能

通过乙酸锌和醇溶液反应得到了六角锥形纳米ZnO颗粒, 反应过程中不使用碱溶液和表面活性剂. 利用透射电子显微镜(TEM)、选区电子衍射(SAED)及扫描电子显微镜(SEM)对其形貌和结构进行了表征分析. 结果表明, 此方法制备的ZnO颗粒为单晶, 而且六角锥形ZnO的室温光致发光谱(PL)在378 nm处显示出了单纯的紫外发射峰, 而不是通常报道的可见光区发射, 这也预示着这种特殊结构的纳米ZnO将会成为一种具有良好应用前景的光学材料.     

一种在固体基底上制备高度取向氧化锌纳米棒的新方法

采用廉价、低温的方法，在修饰过ZnO纳米粒子膜的ITO基底上成功制备出具有 高长径比、高度取向的ZnO纳米棒阵列，用扫描电子显微镜(SEM)，X射线衍射(XRD) ，高分辨透射电子显微镜(HRTEM)以及拉曼光谱对制备出的ZnO纳米棒的结构和形貌 进行了表征，测试结果表明，ZnO纳米棒是单晶，属于六方晶系，与基底直，上仍 沿(001)晶面择优生长的特征，并且ZnO纳米棒基本上无氧空位的存在，统计结果显 示，水热反应2h后90%以上的ZnO纳米棒直径为120～190nm，长度为4μm     

Solvent-Free Synthesis of ZnO Nanoparticles by a Simple Thermal Decomposition Method

This paper reports on a novel processing route for producing ZnO nanoparticles by solid-state thermal decomposition of zinc(II) acetate nanostructures obtained by the sublimation of zinc(II) acetate powder. The sublimation process of the Zn(OAc)₂ powder was carried out in the temperature 150 °C for 2 h. In addition, nanoparticles of ZnO were obtained by solid-state thermal decomposition of the synthesized Zn(OAc)₂ nanostructures. The synthesized products were characterized by X-ray diffraction (XRD), scanning electron microscopy, transmission electron microscopy, photoluminescence spectroscopy, and energy dispersive X-ray spectroscopy. The sublimation process of the Zn(OAc)₂ powder was carried out within the range of 150–180 °C. The XRD studies indicated the production of pure hexagonal ZnO nanoparticles after thermal decomposition.     

Straight and thin ZnO nanorods: hectogram-scale synthesis at low temperature and cathodoluminescence

A novel seed-assisted chemical reaction at 95 degrees C has been employed to synthesize uniform, straight, thin, and single-crystalline ZnO nanorods on a hectogram scale. The molar ratio of ZnO seed and zinc source plays a critical role in the preparation of thin ZnO nanorods. At a low molar ratio of ZnO seed and zinc source, javelin-like ZnO nanorods consisting of thin ZnO nanorods with a diameter of 100 nm and thick ZnO nanorods with a diameter of 200 nm have been obtained. In contrast, straight ZnO nanorods with a diameter of about 20 nm have been prepared. Dispersants such as poly(vinyl alcohol) act spatial obstructors to control the length of ZnO nanorods. The morphology, structure, and optical property of the ZnO nanostructures prepared under different conditions have been characterized by transmission electron microscopy, field emission scanning electron microscopy, X-ray powder diffraction, high-resolution transmission electron microscopy, and cathodoluminescence. The formation mechanisms for the synthesized nanostructures with different morphologies have been phenomenologically presented.     

Morphology-controlled synthesis of ZnO nanostructures by a simple round-to-round metal vapor deposition route

One-dimensional ZnO nanostructures with different morphologies have been successfully synthesized through a simple round-to-round metal vapor deposition route at 550 degrees C with a zinc powder covered indium film as the source material. The structures and morphologies of the products were characterized in detail by using X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Studies found that the morphology of the products can be easily tuned from one experimental round to another. Possible growth mechanisms for the formation of one-dimensional ZnO nanostructures with different morphologies are discussed. Photoluminescence studies show that there are sharp UV emission and broad defect-related green emissions for the products obtained in all experimental rounds. Relative intensity of the UV emission to defect-related emissions gradually increased from one experimental round to another.     

Cellulose nanofibers from white and naturally colored cotton fibers

Suspensions of white and colored nanofibers were obtained by the acid hydrolysis of white and naturally colored cotton fibers. Possible differences among them in morphology and other characteristics were investigated. The original fibers were subjected to chemical analysis (cellulose, lignin and hemicellulose content), X-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM). The nanofibers were analyzed with respect to yield, elemental composition (to assess the presence of sulfur), zeta potential, morphology (by scanning transmission electron microscopy (STEM)) and atomic force microscopy (AFM), crystallinity (XRD) and thermal stability by thermogravimetric analysis in air under dynamic and isothermal temperature conditions. Morphological study of several cotton nanofibers showed a length of 85–225 nm and diameter of 6–18 nm. The micrographs also indicated that there were no significant morphological differences among the nanostructures from different cotton fibers. The main differences found were the slightly higher yield, sulfonation effectiveness and thermal stability under dynamic temperature conditions of the white nanofiber. On the other hand, in isothermal conditions at 180 °C, the colored nanofibers showed a better thermal stability than the white.     

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.     

Zinc oxide prepared by homogeneous hydrolysis with thioacetamide, its destruction of warfare agents, and photocatalytic activity

Zinc sulfide (ZnS) nanoparticles were prepared by homogeneous hydrolysis of zinc sulfate and thioacetamide (TAA) at 80 degrees C. After annealing at a temperature above 400 degrees C in oxygen atmosphere, zinc oxide (ZnO) nanoparticles were obtained. The ZnS and ZnO nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and Brunauer-Emmett-Teller (BET)/Barrett-Joyner-Halenda (BJH) methods were used for surface area and porosity determination. The photocatalytic activity of as-prepared zinc oxide samples was determined by decomposition of Orange II dye in aqueous solution under UV irradiation of 365 nm wavelength. Synthesized ZnO were evaluated for their non-photochemical degradation ability of chemical warfare agents to nontoxic products.     

微波诱导燃烧法合成类花状ZnO纳米材料及其晶体结构、荧光性质研究

以硝酸锌[Zn(NO3)2.6H2O]和尿素[CO(NH2)2]作前驱体,通过微波诱导燃烧技术可控合成具有不同形貌的ZnO纳米晶体,并用热重分析和差热分析进行了研究。对各种生长条件:微波功率,辐射时间和尿素/Zn2+物质的量的比对ZnO纳米晶体形貌的影响作了分析。结果表明:尿素/Zn2+物质的量的比对ZnO纳米材料的形貌具有显著影响。X衍射图表明合成的ZnO纳米结构呈六角形。傅里叶变换红外光谱图中400~500 cm-1处明显的峰为Zn-O的振动峰。ZnO纳米结构的发光光谱在366 nm的带边发射,因缺陷又由许多可见光发射峰组成。用扫描电子显微镜、透射电子显微镜、选区电子衍射研究了花状ZnO纳米结构的增长机理。本方法仅需几分钟就获得的了ZnO纳米结构。     

In situ synthesis of ZnO nanocrystal/PET hybrid nanofibers via electrospinning

Hybrid nanofibers of ZnO precursors/PET were fabricated by electrospinning a nonaqueous poly(ethylene terephthalate) (PET) solution containing zinc acetate dihydrate. Scanning electron microscopy images showed that the as prepared nanofibers had smooth and uniform surfaces, and the diameter was decreased with increasing zinc acetate dihydrate content and reducing PET concentration. After the treatment by a mild process of immersing the fibers in ammonia‐ethanol mixtures (pH ≈ 9–11), the surface of the nanofibers became rough during the formation of ZnO nanocrystals in the fibers. High resolution transmission electron microscopy images showed that the mean particle size became smaller with increasing diameter of the polymer fibers and decreasing content of ZnO. Fourier transform infrared spectra confirmed the ZnO formation in the hybrid nanofibers. X‐ray diffractometry patterns indicated that ZnO had the Wurtzite structure. The formation and growth of ZnO nanocrystals in the nanofiber matrices was also influenced by the various other parameters, that is, the pH value of the reaction solution, the content of zinc acetate dihydrate within the fibers, the reaction time and temperature. Photoluminescence spectra under excitation at 300 nm revealed a broad and intense ultraviolet emission. The UV‐visible diffuse reflectance spectra demonstrated the blue shift in the absorbance curve, which was ascribed to the quantum confinement effects of ZnO nanoparticles in the hybrid materials. These hybrid nanofibers can potentially be used in light emitters, chemical sensors, photo‐catalysts and solar cells. © 2011 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 49: 1360–1368, 2011     

One-dimensional ZnO nanostructure arrays: synthesis and characterization

One-dimensional ZnO nanostructure arrays such as nanowires, nanonails, and nanotrees, have been synthesized by oxygen assisted thermal evaporation of metallic zinc on a quartz substrate over a large area. Morphological evolution of ZnO nanostructures at different time scales and different positions of the substrates have been studied by electron microscopy. A self-catalyzed vapor-liquid-solid (VLS) process is believed to be responsible for the nucleation and subsequently a vapor-solid process is operative for further longitudinal growth. The photoluminescence spectrum showed a weak UV and a broad green emission peak at 3.25 and 2.49 eV, respectively. The latter was attributed to the presence of zinc interstitial defects. Electrical resistivity as a function of temperature showed activated mechanisms to be present. The electrical response of the ZnO nanonail arrays to different gases (CO, NO2, and H2S) indicated that there could be possible application as gas sensors for this material.     

A Facile Room Temperature Synthesis of Zinc Oxide Nanostructure and Its Influence on the Flame Retardancy of Poly Vinyl Alcohol

In this work, poly vinyl alcohol–ZnO nanocomposites were synthesized via two different in situ and ex-situ methods. In ex-situ, at first zinc oxide nanostructures were synthesized by one-step precipitation reaction between zinc acetate and sodium hydroxide. The effect of different surfactants such as poly vinyl pyrrolidone, poly vinyl alcohol and poly ethylene glycol on the morphology of ZnO nanostructures was investigated. Nanostructures were characterized by X-ray diffraction, scanning electron microscopy. The influence of ZnO nanostructures on the flame retardancy of the poly vinyl alcohol matrix was studied using underwriter laboratories UL-94 analysis.