SiO2/ZnO复合纳米粒子的制备及表征

采用双注控制沉积法(Controlled Double-Jet Precipitation,CDJP)将反应物添加到含有SiO₂的溶液中,通过直接的表面反应来制备单分散的SiO₂/ZnO复合纳米粒子,并对其进行了表征。透射电镜(TEM)观察表明,SiO₂表面有一层ZnO纳米颗粒或薄层。对复合纳米粒子SiO₂/ZnO进行X射线衍射(XRD)分析,复合颗粒的衍射峰与单独的氧化锌的衍射峰完全一致。能量弥散X射线法(EDX)分析表明,复合颗粒中含有Zn、Si、O元素。荧光光谱表明有ZnO的吸收峰。     

Preparation and characterization of porous TiO_2/ZnO composite nanofibers via electrospinning

<正>Porous TiO_2/ZnO composite nanofibers have been successfully prepared by electrospinning technique for the first time.It was generated by calcining TiO_2/ZnCl_2/PVP[PVP:polyvinyl pyrrolidone)]nanofibers,which were electrospun from a mixture solution of TiO_2,ZnCl_2 and PVP.Transmission electron microscopy(TEM) and X-ray diffraction(XRD) analyses were used to identify the morphology of the TiO_2/ZnO nanofibers and a formation of inorganic TiO_2/ZnO fibers.The porous structure of the TiO_2/ZnO fibers was characterized by N_2 adsoption/desorption isotherm.Surface photovoltage spectroscopy(SPS) and photocatalytic activity measurements revealed advance properties of the porous TiO_2/ZnO composite nanofibers and the results were compared with pure TiO_2 nanofibers,pure ZnO nanofibers and TiO_2/ZnO nanoparticles.     

Hydrothermal synthesis of 2D ordered macroporous ZnO films

The ZnO films with two-dimensional ordered macroporous structure were successfully fabricated through hydrothermal crystal growth of ZnO on the ZnO substrate covered with a monolayer of polystyrene (PS) spheres as template. The precursor solution of hydrothermal crystal growth of ZnO were prepared by equimolar solution of Zn(NO₃)₂·6H₂O and hexamethylenetramine (HMT). The confinement effect of the PS spheres template on the growth of ZnO nanorods and the influence of sodium citrate on the crystal growth of ZnO had been studied. The film surface morphology and the preferential growth of ZnO crystal were investigated by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. Also, the photoluminescence spectrum of ZnO films had been measured, and the corresponding mechanism was discussed. __________ Translated from Chemistry, 2007, 70 (8): 587–592 [译自: 化学通报]     

Sb2S3纳米粒子修饰ZnO纳米片微纳分级结构的光电化学性能

采用恒电位方法,选择氯化钾和乙二胺(EDA)为添加剂,在氧化铟锡(ITO)导电玻璃上制备了高度有序的ZnO纳米片阵列,通过二次电沉积得到了ZnO纳米片上生长纳米棒的微纳分级结构.利用化学浴沉积法在ZnO基底上沉积Sb₂S₃纳米粒子制备出了Sb₂S₃/ZnO纳米片壳核结构和Sb₂S₃/ZnO微纳分级壳核结构.利用扫描电子显微镜(SEM)、X射线衍射(XRD)、紫外-可见(UV-Vis)吸收光谱、瞬态光电流等对其形貌、结构组成和光电化学性能进行了表征和分析.结果表明, Sb₂S₃/ZnO纳米片上生长纳米棒分级壳核结构的光电流明显高于Sb₂S₃/ZnO纳米片壳核结构.在Sb₂S₃/ZnO纳米片壳核结构和Sb₂S₃/ZnO微纳分级壳核结构的基础上旋涂一层P3HT薄膜形成P3HT/Sb₂S₃/ZnO复合结构,以上述复合结构薄膜为光活性层组装成杂化太阳电池,其中, P3HT/Sb₂S₃/ZnO分级壳核结构杂化太阳电池的能量转换效率最高,达到了0.81%.     

Photocatalytic decomposition of dyes using ZnO doped SnO2 nanoparticles prepared by solvothermal method

ZnO doped SnO₂ has been successfully synthesized by the solvothermal method using methanol as organic solvent. The effect of ZnO/SnO₂ molar ratios on the crystal structure, microstructure, optical and photocatalytic properties has been investigated. The synthesized samples are characterized by X-ray diffraction, transmission electron microscopy, N₂ physical adsorption, FT-IR spectroscopy and UV–Vis spectroscopy. XRD results revealed that all diffraction peaks positions agree well with the reflection of a tetragonal rutile structure of SnO₂ phase without extra peaks at 0.1ZnO:0.9SnO₂ and 0.2ZnO:0.8SnO₂ molar ratios. However, the secondary phase of ZnO at 0.3ZnO:0.7SnO₂ molar ratio was investigated. TEM images revealed that the shape of SnO₂ particles was spherical and the particle sizes of SnO₂ and 0.3ZnO:0.7SnO₂ molar ratio were 6.2 and 16.4 nm, respectively. The newly prepared samples have been tested by the determination of photocatalytic degradation of methylene blue (MB). The results indicated that Zn²⁺ doping at 0.3ZnO:0.7 SnO₂ molar ratio showed the highest photocatalytic activity for the MB photodegradation. The heightened photocatalytic activity of ZnO/SnO₂ could be ascribed to the enhanced charge separation derived from the coupling of ZnO with SnO₂ due to the potential energy differences between SnO₂ and ZnO. The recycling tests demonstrated that 0.3ZnO:0.7 SnO₂ photocatalysts were quite stable during that liquid–solid heterogeneous photocatalysis since no decrease in activity in the first four cycles was observed.     

CeO_2/ZnO复合纳米管的制备及其光催化性能的研究

用纳米CeO2掺入ZnO纳米管制备了CeO2/ZnO复合纳米管,考察了复合纳米管的光学及其光催化性能,并运用X射线衍射、透射电镜、比表面积测定和紫外-可见漫反射光谱等技术对样品进行了表征.结果表明,与ZnO纳米管相比,CeO2/ZnO复合纳米管的比表面积虽有所降低,但光催化活性有所提高,随着复合纳米CeO2量的增加,催化剂的光催化活性相应降低,太阳光下CeO2/ZnO复合纳米管对甲基橙溶液也有较高的催化活性.     

Synthesis and Characterization of TiO2 Doped ZnO Microtubes

The TiO₂-doped ZnO microtubes have been successfully fabricated via a wet chemicalmethod, using zinc chloride and titanium sulphate as the starting materials. The as-synthesized products were characterized by X-ray diffraction, field emission scanning electronmicroscopy and room temperature photoluminescence measurement. The photocatalytic ac-tivity in degrading methyl orange was measured with a UV-Vis spectrophotometer. The pure ZnO microtubes exhibit an exact hexangular hollow structure with a diameter of about 700 nm, a length of 3 μm and a wall thickness of about 40 nm. The TiO₂-doped ZnO microtubes with TiO₂/ZnO ratio less than 5% have the same dimension with the pure ZnO microtubes, a smooth column shape, not a hexangular structure. The growth of ZnO may be inhibited by the more Ti⁴⁺ doped into ZnO structure to achieve a small dimension or a multiphase. The crystallinity of ZnO microtubes decreases with increasing TiO₂ content, and then a multiphase containing ZnO, Ti₃O₅ and TiO occur when the TiO₂/ZnO ratio is more than 5%. The UV emission intensity of the TiO₂-doped ZnO obviously increases and then tends to decrease with TiO₂/ZnO ratio increasing. The photocatalytic properties of the TiO₂-doped ZnO microtubes are very effcient in degrading organic dyes of methyl orange and are well identical with its PL properties and the crystallinity.     

ZnO/Cu2O异质结中深能级表面光伏特性

采用恒电压沉积法在导电玻璃(FTO)上制备了具有三棱柱金字塔状的ZnO/Cu2O异质结薄膜. 利用场发射扫描电镜(FESEM)与X射线衍射仪(XRD)对薄膜的微观形貌和晶体结构进行了表征. 利用表面光电压谱(SPS)、场诱导表面光电压谱(FISPS)和相位谱(PS)研究了单一Cu2O与ZnO/Cu2O异质结薄膜的表面光伏性质. 结果表明, 与单一Cu2O薄膜相比, ZnO/Cu2O异质结薄膜的光伏响应范围拓展到了600~800 nm. 根据SPS, FISPS和PS的作用原理, 拓展部分的光伏响应归因于ZnO/Cu2O异质结中Cu2O层的深能级跃迁, 该跃迁在ZnO-Cu2O界面电场(方向由ZnO指向Cu2O)的作用下得到加强, 同时深能级跃迁产生的电子-空穴对在ZnO-Cu2O界面电场的作用下得到了有效分离和传输.     

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.     

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."     

ZnO nanorods on ZnO seed layer derived by sol–gel process

Well-aligned ZnO nanorods are obtained by a liquid phase epitaxial growth on the indium-doped tin oxide glass deposited with a ZnO thin film as the seed layer, which is prepared by combining a sol–gel process and a spin coating technique. The effects of water content in the sol and heat treatment temperature on the properties of the ZnO thin film are investigated. Relationship among the seed layer, the growing time, the growing temperature, the concentration of Zn²⁺ in the solution, the anions in the solution and the resulting ZnO nanorods are discussed in detail. X-ray diffraction analysis and scanning electronic microscopy are employed to characterize the structural and morphological properties of the resulting ZnO nanorods. Results indicate that the ZnO nanorods with a preferred orientation show a single crystal with a wurtzite structure in the direction of [0001], the diameter of the ZnO nanorods seems to depend on the size of the seed grain, while the length of the ZnO nanorods is determined by the growing time and the growing temperature.     

不同形貌ZnO纳米粒子的超声化学法制备与表征

One-dimensional ZnO nanorods and shuttle-like ZnO nanoparticles have been successfully achieved by ultrasonic irradiation of Zn (CH3COO)2 aqueous solution and Zn-NH3 complexcs solution. The obtained ZnO nanoparticles have been characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM) and selected area electronic diffraction (SAED). And the formative mechanism of the prepared different morphological ZnO nanoparticles is also discussed under ultrasonic irradiation.     

ZnO纳米环的可控合成

以六次甲基四胺(Hexamethylenetetramine, C6H12N4)和水合硝酸锌[Zn(NO3)2·2H2O]为原料, 表面活性剂聚丙烯酰胺-氯化二烯丙基二甲基铵[poly(acrylamide-co-diallyldimethylammonium chloride, 缩写为PAM-CTAC]为形貌控制剂, 采用液相沉淀法合成了ZnO纳米环. 产物的结构与形貌经X射线粉末衍射(XRD)和扫描电子显微镜(SEM)表征. 研究了不同实验条件(如表面活性剂的浓度、反应物浓度、反应温度和反应时间等)对产物形貌与尺寸的影响. 讨论了PAM-CTAC作用下ZnO纳米环可能的形成机理. 结果表明, 合成产物为六方Wurtzite型结构的ZnO纳米环, 环内径约为220 nm, 壁厚约为70 nm. 反应物浓度、反应温度对ZnO纳米环的形成以及纳米环的尺寸都有一定的影响, 但起关键作用的是PAM-CTAC. 通过改变PAM-CTAC的浓度, 能有效地实现ZnO纳米环的可控合成. 室温荧光光谱显示, ZnO纳米环的紫外发射峰具有较窄的半高宽(FWHM)(约7 nm), 表明合成产物具有较窄的尺寸分布.     

Electrical investigation and ultraviolet detection of ZnO nanorods encapsulated with ZnO and Fe-doped ZnO layer

Encapsulated ZnO nanorod arrays were fabricated using a two-step method; hydrothermal followed by dip-coating. Intensity of X-ray diffraction peaks of ZnO nanorod films increased by encapsulation with ZnO and Fe doped ZnO layer. Encapsulation process increased diameter of the rods in a range of 20–40 nm. The optical studies indicated that the band-gap decreased with increment of the nanorod diameter, and increased with Fe doping in the ZnO layer. The electrical resistance of the samples demonstrated a remarkable reduction due to encapsulation, especially in the sample encapsulated with Fe doped-ZnO layer. The photoresponse behavior of ZnO nanorod films was investigated under different powers of ultraviolet illumination. The photoresponsivity was improved for encapsulated nanorods as compared to bare nanorods.     

Growth mechanism of ZnO nanocrystals with Zn-rich from dots to rods

ZnO nanocrystals from dot to rod were synthesized by simply changing Zn2+ concentration in ZnO seed solutions. The growth of ZnO nanocrystals was sensitive to the amount of Zn2+ in the solution. The growth process of ZnO from dot to rod was observed by optical spectra, transmission electron microscopy and X-ray diffraction spectra. From these results, the growth mechanism of ZnO from dots to rods was discussed.     

Improved performance of dye sensitized ZnO nanorod solar cells prepared using TiO2 seed layer

Zinc oxide (ZnO) nanorods of different structures have been grown on indium-doped tin oxide substrates by using TiO₂ as seed layer. The ZnO nanorods have been prepared using TiO₂ seed layers annealed at different temperatures via a simple sol–gel method. The X-ray diffraction result indicates that the prepared samples are of wurtzite structure. Dye sensitized solar cells have been fabricated using the prepared ZnO nanorods. The open circuit voltage, short circuit current density, fill factor, and power conversion efficiency of the ZnO nanorod based dye sensitized solar cells prepared using TiO₂ seed layers annealed at different temperatures have been determined. The improvement in power conversion efficiency may be due to the flower like structured ZnO nanorods with smaller diameter and large specific surface area which paves way for the efficient electron transfer in hybrid solar cells.     

Synthesis,characterization, and biosensing application of ZnO/SnO2 heterostructured nanomaterials

In this work, zinc oxide/tin oxide (ZnO/SnO₂) heterostructured nanomaterials were synthesized by hydrothermal method. Transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray diffraction measurements revealed that the product was composed of ZnO nanowires and SnO₂ nanobranches. The novel ZnO/SnO₂ heterostructured nanocrystals were for the first time used as a supporting matrix to explore a novel immobilization and biosensing platform of redox proteins. UV–visible absorption investigation indicated that hemoglobin (Hb) intercalated well in the ZnO/SnO₂ heterostructured nanocrystals retained its native structure. Comparative experiments have confirmed that the ZnO/SnO₂-based biosensor not only had enhanced direct electron transfer capacity but also displayed excellent electrocatalytic properties such as higher sensitivity and wider linear range to the detection of hydrogen peroxide in comparison with the ZnO- and SnO₂-based biosensors.     

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     

加热覆盖有ZnCl2溶液的锌片制备ZnO亚微米棒阵列

将表面覆盖有ZnCl2溶液的锌片加热到400 ℃反应1 h, 在锌片上生长出了ZnO亚微米棒阵列. 采用扫描电镜、透射电子显微镜和X射线衍射仪对所制备的产物进行了表征和分析. 结果表明产物为六方相纤锌矿单晶结构的ZnO亚微米棒, 其直径和长度分别为300～650 nm和6 μm, 提出了ZnO亚微米棒可能的生长机理. 在波长为300 nm光的激发下, 发现了ZnO亚微米棒阵列具有发光峰位于395 nm强的紫外光发光和位于490 nm弱的蓝绿光发光, 这两种发光分别起源于ZnO宽带隙带边发射和ZnO中相应的缺陷结构.     

纳米结构ZnO在TiO_2薄膜上的电化学沉积及其表征

在三电极体系中,以硝酸锌水溶液作为电解液,采用阴极还原电沉积法成功实现了一维纳米结构ZnO阵列在TiO2纳米粒子/ITO导电玻璃薄膜基底上的沉积,并通过XRD、SEM、EDS和PL光谱等方法对样品进行了表征.重点研究了薄膜基底、电解液浓度、沉积时间、六次亚甲基四胺(HMT)的引入对ZnO沉积及其发光性质的影响.结果显示:与ITO玻璃基底相比,ZnO更易于在TiO2纳米粒子薄膜上实现电化学沉积.ZnO属于六方晶系的铅锌矿结构,并且沿着c-轴方向表现出明显的择优化生长,以形成垂直于基底的ZnO纳米棒阵列.延长沉积时间、增加电解液浓度和引入一定量的HMT等均对ZnO的生长有促进作用,进而使其纳米棒的结晶度和取向程度提高,进而解释了所得的薄膜分别约在375和520nm处表现出ZnO的强而窄的带边紫外光发射峰和弱而宽的表面态绿光发射带.