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。     

电沉积制备ZnO纳米棒修饰电极上氧化还原蛋白的电化学行为

采用恒电位阴极还原法在金电极表面一步修饰ZnO纳米棒, 制备成ZnO纳米棒修饰电极. 扫描电子显微镜(SEM)和X射线衍射(XRD)结果显示制得的ZnO为直径约100 nm的六棱柱状纤锌矿晶体纳米棒. 使用ZnO纳米棒修饰的金电极研究细胞色素c的直接电化学行为, 结果表明: ZnO纳米棒修饰的金电极能有效探测到细胞色素c的铁卟啉辅基在不同价态下的电化学行为; 细胞色素c吸附后, ZnO纳米棒修饰的金电极对过氧化氢的电流响应呈现良好的线性关系.     

CdS and CdSe quantum dots subsectionally sensitized solar cells using a novel double-layer ZnO nanorod arrays

We report a novel approach for synthesizing CdS and CdSe quantum dots subsectionally sensitized double-layer ZnO nanorods for solar cells, which are comprised of CdS QDs-sensitized bottom-layer ZnO NRs and CdSe QDs-sensitized top-layer ZnO NRs. X-ray diffraction study and scanning electron microscopy analysis indicate that the solar cells of subsectionally sensitized double-layer ZnO NRs, which are the hexagonal wurtzite crystal structure, have been successfully achieved. The novel structure enlarged the range of absorbed light and enhanced the absorption intensity of light. The I-V characteristics show that the double-layer structure improved both the current density (J_sc) and fill factor (FF) by 50%, respectively, and power conversion efficiency (η) was increased to twice in comparison with the CdS QDs-sensitized structure.     

高度取向ZnO单晶亚微米棒阵列的制备与表征

通过低温压热的方法,在经过预先处理长满晶核的SnO2导电玻璃基底上制备出具有高度取向的ZnO亚微米棒阵列.用扫描电子显微镜(SEM)、选区电子衍射(SAED)及X射线粉末衍射(XRD),对制备出的ZnO亚微米棒的结构和形貌进行了表征.SEM测试结果表明,ZnO亚微米棒是六方型的,近乎垂直地长在基底上,棒的直径为400～500 nm,长度约为2 μm. SAED和XRD结果表明,ZnO亚微米棒为单晶,属于六方晶系,并且沿[001]方向择优取向生长.     

Temperature effect on the structure and characteristics of ZnS-based quantum dots

The synthesis of zinc sulfide (ZnS) quantum dots (QDs) by microwave heating in a water-ethanol medium is proposed. The effect of the synthesis temperature (80 °C, 100 °C, 120 °C, and 150 °C) on the QD characteristics is examined. Based on the analysis of X-ray diffraction profiles the conclusion is drawn that the hexagonal ZnS phase of wurtzite type with an average nanocrystal size of 2.6-3.7 nm forms in the synthesized QDs. The nanocrystallite size is found to increase with the QD synthesis heating temperature. The analysis of X-ray absorption spectra (XANES) at the zinc K-edge indicates a higher crystallinity of the QD samples prepared at higher synthesis temperatures. The combined analysis of X-ray diffraction profiles, optical diffuse reflectance spectra, and X-ray absorption spectra implies the following possible QD structure: the pure hexagonal ZnS phase of wurtzite type in the bulk of nanoparticles and the amorphous ZnO phase in the surface layer of nanoparticles.     

Room Temperature Magnetic Behavior of Sol-Gel Synthesized Mn Doped ZnO

Mn doped ZnO nano-crystallites were synthesized by state of the art sol-gel derived auto-combustion technique. As-burnt powder was investigated with different characterization techniques to explore the properties of Mn doped ZnO dilute magnetic semiconductor. X-ray diffraction measurements indicate that Mn doped ZnO retain wurtzite type hexagonal crystal structure like ZnO. Compositional and morphological studies were carried out by energy dispersive X-ray analysis and scanning electron microscopy, respectively. Tempera-ture dependent resistivity of the sample exhibited the semiconducting behavior of the DMS material. Room temperature magnetic properties determined by vibrating sample magne-tometer, revealed the presence of ferromagnetic and diamagnetic contributions in Mn doped ZnO.     

Sn掺杂ZnO纳米针的结构及其生长机制(英文)

利用包括磁控溅射和热氧化的两步法在Si(111)衬底上制备了Sn掺杂ZnO纳米针.首先用磁控溅射法在Si(111)衬底上制备Sn:Zn薄膜,然后在650℃的Ar气氛中对薄膜进行热氧化,制备出Sn掺杂ZnO纳米针.样品的结构、成分和光学性质采用X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HRTEM)、能量散射X射线(EDX)谱和光致发光(PL)光谱等技术手段进行分析.结果表明,制备的样品为具有六方纤锌矿结构的单晶Sn掺杂ZnO纳米针,Sn掺杂量为2.5%(x,原子比),底部和头部直径分别为200-500 nm和40 nm,长度为1-3μm,结晶质量较高.室温光致发光光谱显示紫外发光峰比纯ZnO的发光峰稍有蓝移,这可归因于能谱分析中探测到的Sn的影响.基于本实验的实际条件,简单探讨了Sn掺杂ZnO纳米针的生长机制.     

Synthesis and evolution of novel double tower-like ZnO by a simple method

Delicate double tower-like ZnO have been fabricated through the decomposition of the zinc nitrate hexahydrate (Zn(NO₃)₂6H₂O). The phase transformation and morphology evolution of the products were carefully studied and investigated with X-ray diffraction, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, and Raman spectra. The resultant results indicated that the obtained double tower-like ZnO materials possess pure wurtzite hexagonal phase, growing along the [100] direction. A reasonable formation mechanism was also presented in this paper.     

微观尺度高分子协同组装ZnO纳米片

以醇水混合体系作为反应介质,六水合硝酸锌和尿素为原料,聚乙烯吡咯烷酮(PVP)作为模板剂,经水热过程合成了由纳米片组装的花状微球碱式碳酸锌前驱体,经热处理得到相应的氧化锌(ZnO)产物。采用X射线衍射(XRD)和环境扫描电镜(SEM)对样品进行了表征,结果表明产物为六方纤维矿结构的ZnO,单分散花状微球直径约为2 μm,尺寸均一,组装成微球的纳米片构筑单元厚度为20 nm。红外分析表明PVP与Zn²⁺之间的化学配位作用发生在侧环的内酰基C=O键上的O位与Zn²⁺之间,研究表明PVP用量影响组装过程,在相同实验条件下,用聚乙二醇(PEG)代替PVP的模板作用,得到了粒径较大的纳米片组装的微球(φ～15 μm),在此基础上探讨了高分子结构对晶体生长和组装机制的影响。     

Photoconductivity and photoluminescence of ZnO nanoparticles synthesized via co-precipitation method

Photoconductivity and photoluminescence studies of ZnO nanoparticles (NPs) synthesized by co-precipitation method capped with thioglycerol are carried out. The effect of annealing at 300°C is also studied. The transmission electron micrograph (TEM) and X-ray diffraction (XRD) pattern confirm the hexagonal wurtzite structure of ZnO nanoparticles. The UV-vis absorption spectrum of ZnO NPs shows blue shift of absorption peak as compared to bulk ZnO. The photoluminescence (PL) spectra of as-synthesized ZnO NPs show band edge emission as well as blue-green emission. After annealing band edge emission is quenched. Photocurrent is found to vary super linearly at high voltage for both as-synthesized as well as annealed ZnO NPs. Time resolved rise and decay photocurrent spectra are found to exhibit anomalous photoconductivity for as-synthesized as well as annealed ZnO NPs wherein the photocurrent decreases even during steady illumination.     

微波辐射对纳米ZnO材料物理性质与光催化活性的影响

在采用沉淀法制备ZnO的过程中, 用不同功率(100, 150, 200, 250和300 W)的微波辐射ZnO前驱体, 获得了一系列纳米ZnO材料, 并对合成材料的晶型结构、 形貌及表面物理化学性质进行了表征. 结果表明, 与普通沉淀法制备的ZnO相比, 使用微波辐射后ZnO半导体材料的晶型仍为六方纤锌矿结构, 但吸收光谱发生了蓝移或红移, 且比表面积均有不同程度的增加. 同时, 微波辐射功率不同, ZnO形貌差异明显, 并随着微波功率变化分别呈现纳米颗粒、 椭圆形纳米团簇、 纳米片和球状纳米簇等多样化形态. 以罗丹明B为模型分子, 分别在紫外及微波辅助光催化条件下考察了所合成纳米ZnO材料的光催化性能. 结果显示, 经不同功率微波辐射作用后, ZnO的光催化活性均得到了不同程度的提高, 并且明显高于市售P25和未经微波辐射作用的ZnO.     

利用浮区法在高氧压下生长ZnO晶须

采用浮区法在高温高氧压下生长出大尺寸的ZnO晶须. X射线衍射和拉曼光谱分析结果表明, 生长的ZnO晶须结晶良好, 具有六方结构, 沿(001)方向有明显的择优生长取向. 光致发光光谱测量结果表明, 晶须在室温下有较高的紫外光致发光效率和较低的缺陷, 生长时选择大于0.3 MPa的氧压对提高IUV/Igreen有益.     

杨桃状ZnO纳米片微球的制备及气敏性能的研究

以六水合硝酸锌和尿素为原料,水为反应介质,油酸作为表面活性剂,经水热过程合成了由纳米片组装的碱式碳酸锌微球前驱体,经煅烧后得到形貌一致的氧化锌(ZnO)纳米片组装的杨桃状微球。采用X射线衍射仪(XRD)和环境扫描电镜(SEM)对样品进行表征,结果表明产物为六方纤维矿结构的ZnO,微球尺寸比较均一,直径约为20μm,组装单元扇形ZnO纳米片均匀排列,单元之间存在均匀空隙,BET测试显示纳米片呈现多级介孔结孔结构,比表面积为18.9m2·g-1,室温下的光致发光性能表明其结构表面存在大量氧空位,对产物ZnO气敏元件进行了乙醇和丙酮气体敏感性测试。     

Low temperature synthesis and characterization of rosette-like nanostructures of ZnO using solution process

Rosette-like structures of ZnO were synthesized at low temperature (60 °C) using solution process over 20 min of time. Hydroxylamine hydrochloride was used as capping agent with zinc nitrate hexahydrate and sodium hydroxide. Transition from triangular shaped plate like particles to rosette-like structure and to individual nanorods is observed with increasing refluxing temperature. Single-crystalline nature with wurtzite hexagonal phase is confirmed from transmission electron microscopic observations. Photoelectron spectroscopic measurement presented spectra close to the standard bulk ZnO, with an O 1s peak composed of surface adsorbed O–H group, O^2? in the oxygen vacancies on ZnO structure and ZnO.     

Preparation and characterization of ZnO nanocrystallines in the presence of an ionic liquid using microwave irradiation and photocatalytic activity

Fast, simple and template-free method is proposed for preparation of ZnO nanocrystallines in the presence of 1-ethyl-3- methylimidazolium ethyl sulfate, [EMIM][EtSO₄], a room-temperature ionic liquid (RTIL) under microwave irradiation. The powder X-ray diffraction (XRD) studies display that products are excellently crystallized in the form of wurtzite hexagonal structure. Energy dispersive X-ray spectroscopy (EDX) investigations reveal that the products are extremely pure. The results obtained by scanning electron microscopy (SEM) demonstrate that mean size of ZnO nanocrystallines decreases with microwave irradiation time and the RTIL content of media. Diffuse reflectance spectra (DRS) of the ZnO nanocrystallines shows blue shift relative to the bulk ZnO, which can be attributed to quantum confinement effect of ZnO nanocrystallines. A possible formation mechanism of the ZnO nanocrystallines in aqueous solution of the RTIL is presented. Photocatalytic activity of the ZnO nanocrystallines towards photodegradation of methylene blue (MB) was carried out. The results demonstrate that photocatalytic activity of the ZnO nanocrystallines increases with microwave irradiation time and the RTIL content of media.     

Sb掺杂大尺寸ZnO纳米棒的制备及其特性研究

采用化学气相沉积法,在没有采用任何催化剂的条件下,在Si(100)衬底上成功制备出Sb掺杂大尺寸ZnO纳米棒,并对样品进行了结构和光学性质的表征。结果表明:纳米棒为结晶质量较好的六角纤锌矿结构,在能量色散谱(EDS)中观测到了Sb元素的存在。此外,在低温光致发光(PL)光谱中还观测到了与Sb掺杂相关的中性受主束缚激子发光峰(A0X)、自由电子到受主能级跃迁的发光峰(FA)、施主受主对(DAP)以及DAP的一级纵向光声子伴线(DAP-1LO),因此证实Sb元素作为受主杂质掺杂已进入ZnO晶格。     

Polyvinylpyrrolidone-assisted growth and optical properties of ZnO hexagonal bilayer disk-like microstructures

ZnO hexagonal bilayer disk-like microstructures are successfully prepared assisted with polyvinylpyrrolidone (PVP), and the photoluminescence (PL) spectrum of as-prepared ZnO samples showed a very strong ultraviolet (UV) emission at the UV region.     

Fabrication of 3D rotor-like ZnO nanostructure from 1D ZnO nanorods and their morphology dependent photoluminescence property

A facile and eco-friendly sonochemical route to fabricate well-defined dentritic (rotor-like) ZnO nanostructures from 1D ZnO nanorods without alloying elements, templates and surfactants has been reported. Phase and structural analysis has been carried out by X-ray diffraction (XRD) and Fourier Transform Infra-Red (FTIR) spectroscopy, showed the formation of hexagonal wurtzite structure of ZnO. Scanning electron microscopic (SEM) study showed the formation of rotor-like ZnO nanostructure having a central core which is surrounded by side branches nanocones. Transmission electron microscopic (TEM) study showed that these nanocones grow along [0001] direction on the six {01–10} planes of central core ZnO nanorods. A plausible formation mechanism of rotor-like ZnO nanostructures was studied by SEM which indicates that the size and morphology of side branches can be controlled by adjusting the concentration of OH^? ions and time duration of growth. The photoluminescence (PL) spectrum of the synthesized rotor-like ZnO nanostructures exhibited a weak ultraviolet emission at 400 nm and a strong green emission at 532 nm recorded at room temperature. The influence of morphology on the origin of green emission was discussed in detail. The results suggested a positive relationship among polar plane, oxygen vacancy and green emission.     

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.     

Synthesis of aligned ZnO nanocolumn arrays by a vapor phase transport method

Vertically large-scale aligned ZnO nanocolumn arrays have been synthesized on Si(100) substrate at 550°C via a simple vapor phase transport process in a horizontal chemical vapor depositon (CVD) reactor. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations show that the ZnO nanocolumns have a uniform length of about 3 ??m with an average diameter of 80 nm. The clear lattice fringes in HRTEM image indicate the synthesis of good quality hexagonal single crystal ZnO. The X-ray diffraction (XRD) result shows the nanocolumns are c-axis preferentially oriented.