Non-Basic Solution Routes to Prepare ZnO Nanoparticles

Nanocrystalline ZnO particles were prepared from alcoholic solutions of zinc acetate dihydrate without using base such as NaOH or LiOH through a colloid process carried out at a low temperature of 60°C. A comparative study of chemical reactions from zinc acetate dihydrate to ZnO was made using different types of monool solvents, i.e. methanol, ethanol, and 2-methoxyethanol. It was revealed that layered hydroxide zinc acetate was formed as an intermediate and its transformation into ZnO was a key reaction step in any of the solutions. Reaction time necessary for the precipitation of ZnO was greatly influenced by the solvents used. Methanol was useful for the preparation of the ZnO nanoparticles, which were chemically pure in terms of cation impurities and exhibited green photoluminescence by the ultraviolet excitation.     

Properties of Luminescent Si Nanoparticles in Sol-Gel Matrices

In this wor e preparation and properties of silica sol-gels incorporating luminescent Si nanocrystallites extracted from porous Si are described for the first time. These sol-gel/Si nanocrystallite composite materials are characterized by BET isotherm measurements, photoluminescence spectroscopy, and infrared spectroscopy. To stabilize the photoluminescence (PL) of Si crystallites within the silica matrix, a fatty acid (capric (C₁₀), myristic (C₁₄) or arachidic acid (C₂₀)) is added as a passivation agent during the hydrolysis of tetraethoxysilane. The presence of the fatty acid is crucial to the long-term stability of the Si nanocrystallite luminescence, as the Si visible light emission remains essentially unchanged for more than a month when the fatty acid is present in the mixture but degrades quickly (within days) when absent. The thermal stability of the Si luminescence within the sol-gel is also reported. Fluorescence microscopy reveals that the light-emitting Si crystallites aggregate into micron-sized domains somewhat unevenly throughout the silica matrix. This distribution of Si crystallites can be improved by employing a surfactant, dioctyl sodium sulfosuccinate (DSS).     

纳米ZnO的制备及发光特性研究

The samples of nano-size ZnO were prepared by precipitation, hydrolysis, sol-gel method and characterized by X-ray diffraction, Uv-Vis diffuse reflection spectrum, and time resolved luminescent spectrum. The results showed that the crystallite dimensions of all ZnO samples were coarsening with increasing annealing temperature and the grain sizes prepared by sol-gel method were obviously smaller than the others prepared by precipitation and hy-drolysis method. Under excitation of monochromatic light of wavelength 300nm, a strong and broad photolumines-cence (PL) emissions were observed in the wavelength range of 420～780nm. As the grain size decreased, the PL peak positions moved to shorter wavelengths. And as the annealing temperature increased, the peak intensity de-creased. The photoluminescence decay profile of ZnO was well described by three decay components of 46ns, 330ns and 1630ns.     

The Optical Properties of ZnO Nanoparticles Capped with Polyvinyl Butyral

ZnO nanoparticles capped with polyvinyl butyral (PVB) have been synthesized by the sol-gel process. Photoluminescence (PL) spectra show a remarkable decrease in visible emission intensity after ZnO nanoparticles are capped with PVB, which indicates that dangling bonds and defect states at the surface of ZnO nanoparticles are markedly passivated. As a result, the process of surface-trapped hole tunneling back into the particles to form V**_O recombination center is blocked. The PL spectra of thin films show a strong ultraviolet (UV) emission with very weak visible emission. The typical intensity ratio of the UV emission at 3.45 eV to the visible emission at about 2.41 eV is 43.3, which shows an obvious improvement in luminescence properties by the surface passivation with PVB. Low-temperature PL spectra of ZnO powder at 93.8 K are dominated by free exciton, bound exciton and the LO-phonon replica of the bound exciton.     

ZnO纳米粒子自建场的形成及对其光电特性的影响

The effect of built-in field on the surface photovoltage(SPV) response of ZnO nanoparticles was investigated by means of surface photovoltage spectroscopy(SPS). From the results of in situ SPS in atmosphere and in vacuum, we suggest that the built-in field should be a main condition for producing SPV response. By comparison of SPS with PL in vacuum as well as in atmosphere, we deduce that by changing the ambience of ZnO, its functional properties can be modulated.     

纳米氧化锌的机械力化学表面改性

采用机械力化学表面改性工艺,以硬脂酸为改性剂,在气流粉碎机中对纳米氧化锌进行解团聚和表面改性,并借助SEM、XRD、FF—IR和XPS对改性前后的氧化锌粉体进行结构表征．结果表明：硬脂酸分子化学键合在氧化锌表面．改性前后氧化锌的晶体结构相同,其颗粒的团聚性降低,二次粒径明显减小．通过测定改性样品的活化指数和亲油化度,选择最佳的改性剂用量为氧化锌质量的10％,氧化锌表面亲油疏水,在有机溶剂中有较好的分散性．     

三维花状ZnO纳米材料的制备及发光性质

常压下用溶胶凝胶和化学溶液生长两步法在3种不同的衬底上制备出三维花状ZnO纳米材料.采用X射线衍射仪(XRD)、扫描电镜(SEM)、透射电镜(TEM)、选区电子衍射(SAED)、紫外吸收(UV)光谱和光致发光光谱(PL)对样品进行分析,结果表明,花状ZnO的组成单元为沿c轴方向生长的ZnO纳米棒,直径约为100 nm,...     

纳米金属铜与纳米氧化锌之间相互作用的EPR和XPS研究

由于纳米材料独特的表面效应、电子效应及量子尺寸效应 ,已被广泛应用于各个领域 .有关纳米材料研究的报道很多 [1～ 7] ,大部分是关于纳米材料的制备[1～ 4 ] 及其特性研究 .对于纳米金属及纳米氧化物之间相互作用的研究迄今尚未见报道 .本文采用超声分散和机械研磨法物理混合纳米金属铜粉和纳米氧化锌 ,借助 EPR和 XPS技术对样品进行了表征 ,发现混合体系出现了 Cu2 + 的顺磁信号 ,Zn L3M4 5M4 5俄歇动能和 O1s的电子结合能亦发生了变化 ,表明纳米 Cu0 和纳米 Zn O之间存在相互作用 ,作用形式为 Cu— O—Zn.1　实验部分1 .1　样品…     

Antibacterial and Photocatalytic Properties of ZnO Nanoparticles Obtained from Chemical versus Saponaria officinalis Extract-Mediated Synthesis

In the present work, the properties of ZnO nanoparticles obtained using an eco-friendly synthesis (biomediated methods in microwave irradiation) were studied. Saponaria officinalis extracts were used as both reducing and capping agents in the green nanochemistry synthesis of ZnO. Inorganic zinc oxide nanopowders were successfully prepared by a modified hydrothermal method and plant extract-mediated method. The influence of microwave irradiation was studied in both cases. The size, composition, crystallinity and morphology of inorganic nanoparticles (NPs) were investigated using dynamic light scattering (DLS), powder X-ray diffraction (XRD), SEM-EDX microscopy. Tunings of the nanochemistry reaction conditions (Zn precursor, structuring agent), ZnO NPs with various shapes were obtained, from quasi-spherical to flower-like. The optical properties and photocatalytic activity (degradation of methylene blue as model compound) were also investigated. ZnO nanopowders’ antibacterial activity was tested against Gram-positive and Gram-negative bacterial strains to evidence the influence of the vegetal extract-mediated synthesis on the biological activity.     

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纳米颗粒锚定的亚微米碳纤维的制备及其吸波性能

使用静电纺丝技术结合水热法制备了表面锚定ZnO纳米颗粒的亚微米碳纤维（ZnO/SDCFs）复合物,并详细研究了反应溶液的pH值对复合物的结构、组成、电磁特性和吸波性能的影响。结果显示,随着pH值的升高,ZnO的含量增加,介电常数、介电损耗以及电磁衰减能力均下降,但阻抗匹配程度提高。相比于纯碳纤维,所有ZnO/SDCFs复合物的吸波性能均得到不同程度的加强。其中,pH值等于8时所制备的ZnO/SDCFs-8复合物拥有最好的吸波性能,主要归因于电磁衰减能力和阻抗匹配间的更好平衡。当ZnO/SDCFs-8的填充量仅为2.5%（质量分数）、厚度为1.7 mm时,相应吸波涂层的最小反射损耗达到-44.1 dB,低于-10 dB的有效吸收带宽为6.1 GHz,频率范围为11.9~18 GHz;当厚度为3.0 mm时,有效吸收带宽可提高到11.8 GHz（6.2~18 GHz）。     

Preparation of ZnO Nanoparticles: Structural Study of the Molecular Precursor

The structure of zinc acetate derived precursor currently used in the sol-gel synthesis of ZnO nanoparticles is described. The reaction products obtained before and after reflux of ethanolic zinc acetate solution have been studied by UV-Vis, photoluminescence, FTIR and EXAFS at the Zn K edge. EXAFS results evidence for both precursor solutions a change from the octahedral coordination sphere of oxygen atoms characteristic of the solid zinc acetate dihydrate compound into a four-fold environment. The EXAFS spectra of precursor solutions can be satisfactorily reproduced using the molecular structure reported for Zn₄O(Ac)₆ (Ac = COOCH₃). UV-Vis and FTIR measurements are also in agreement with the formation of this oligomeric precursor. The structural modification is more pronounced after reflux at 80°C, because the increase of the Zn₄O(Ac)₆ amount and the formation of nearly 3.0 nm sized ZnO nanoparticle.     

静电纺丝方法制备CaTiO3∶Er3+微米带及其上转换发光性质

CaTiO3:Er3+微米带由静电纺丝方法制备.用X射线衍射、傅里叶变换红外光谱、拉曼光谱、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)和上转换发光表征所制备的样品.SEM和TEM测试证实所得前躯体微米带尺寸均一,烧后得到的微米带是由纳米粒子组成的.在980 nm激光激发下,CaTiO3:Er3样品发出绿光,绿光发射峰位于546 nm,可归属于Er3+离子的4S3/2 →4I15/2跃迁.当Er3+离子的掺杂浓度提高,因为Er3+离子之间的能量传递,红光发射相对于绿光发射增强.     

Investigation of the Optical Properties of a Novel Class of Quinoline Derivatives and Their Random Laser Properties Using ZnO Nanoparticles

Quinoline Schiff bases display potential applications in optoelectronics and laser fields because of their unique optical properties that arise from extensive delocalization of the electron cloud, and a high order of non-linearity. In this context, a new class of conjugated quinoline-derivative viz. N-(quinolin-3-ylmethylene)anilines were synthesized from 2-hydroxyquinoline-3-carbaldehyde in two good yielding steps. The ability of these imines to accept an electron from a donor is denoted by their electron acceptor number and sites, which is calculated using density functional theory (DFT). The optical properties such as FT-IR, Raman, UV-VIS, and EDS spectra were calculated using TD-DFT, which also provided the energy gap, HOMO-LUMO structure. The optical properties of the synthesized imino quinolines were experimentally studied using photoluminescence and absorption spectroscopy. The properties such as Stokes shift and quantum yield were calculated using experimental data. Furthermore, the compound bearing a methyl group on the aryl ring and ZnO nanoparticles (hydrothermally synthesized) were dissolved in toluene, and optically excited with a 355 nm nanosecond laser, which produced a random laser.     

Cu-Doped ZnO Nanoparticles for Non-Enzymatic Glucose Sensing

Copper-doped zinc oxide nanoparticles (NPs) Cu_xZn_1−xO (x = 0, 0.01, 0.02, 0.03, and 0.04) were synthesized via a sol-gel process and used as an active electrode material to fabricate a non-enzymatic electrochemical sensor for the detection of glucose. Their structure, composition, and chemical properties were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier-transform infrared (FTIR) and Raman spectroscopies, and zeta potential measurements. The electrochemical characterization of the sensors was studied using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and differential pulse voltammetry (DPV). Cu doping was shown to improve the electrocatalytic activity for the oxidation of glucose, which resulted from the accelerated electron transfer and greatly improved electrochemical conductivity. The experimental conditions for the detection of glucose were optimized: a linear dependence between the glucose concentration and current intensity was established in the range from 1 nM to 100 μM with a limit of detection of 0.7 nM. The proposed sensor exhibited high selectivity for glucose in the presence of various interfering species. The developed sensor was also successfully tested for the detection of glucose in human serum samples.     

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%.     

纳米氧化锌的制备及其在太阳光下的光催化性能

本文以醋酸锌、浓氨水为原料,采用均匀沉淀法,制备了在太阳光下具有优良光催化性能的纳米氧化锌粉体,并利用透射电镜(TEM)、UV-Vis、X射线衍射(XRD)和ξ电位对所得样品进行了表征;以亚甲基蓝(MB)溶液的光催化脱色降解为模型反应,考察了煅烧温度对其结构与催化性能的影响。研究结果表明:在150℃下煅烧4h得到了具有良好分散性和结晶性能的纳米氧化锌粒子,粒径分布均匀、平均粒径约10nm;该纳米材料在太阳光下具有高的光催化活性和稳定性,照射2h可以使MB溶液的脱色率达100%,且重复使用5次时染料的脱色率仍在95%以上;所得样品的ξ电位均为负值,样品表面过剩的负电荷源自于样品的结构缺陷,即Zn2+空位或O2-过剩,且表面电荷量随煅烧温度的不同而不同;结构缺陷是其光谱响应范围的拓展和在太阳光条件下具有良好催化性能等的重要原因。     

Novel Green Route of Synthesis of ZnO Nanoparticles by Using Natural Biodegradable Polymer and Its Application as a Catalyst for Oxidation of Aldehydes

ZnO nanoparticles have been synthesized by using biodegradable natural biopolymer viz. Gum Tragacanth. This single step approach is very cost effective and reproducible. The reaction time and concentration of precursor zinc acetate play a major role in the nature and growth of ZnO nanoparticles. ZnO nanoparticles were characterized by X-ray diffraction, SEM, FTIR, EDAX, UV-visible spectroscopy and TEM. ZnO nanoparticles with 20-30 nm in diameter and hexagonal morphology were found; dispersed uniformly. Raman spectrum shows the mode E₂ high at 437 cm^?1 that is related to the vibration of wurtzite Zn-O bond in crystal structure of ZnO. The space between adjacent lattice fringes is ～ sharp 2.42 Å. UV-visible absorption spectrum shows the sharp absorption band at 308 nm assigned to the intrinsic transition from valance band to conduction band. The ZnO nanoparticles display superior catalytic activity of conversion of aldehyde to acid as compared to bulk-ZnO material, because of high surface area of ZnO nanoparticles. A trace amount of ZnO nanoparticles catalyst required for organic conversion. The ZnO nanoparticles as catalyst are highly stable, recyclable and efficient in its activity.     

凝胶网格控制合成纳米ZnO及其光催化活性

以明胶为反应介质,采用凝胶网格控制合成法制备了单分散球形纳米ZnO光催化剂.利用TG-DTA、XRD、TEM、BET、UV-Vis、HPLC等测试手段对制备过程、样品的结构和性能进行了研究,探讨了明胶浓度、煅烧温度对产物粒径和光催化活性的影响.结果表明:利用凝胶网格控制合成法不仅能够控制纳米微粒的形状和大小,而且可防止沉淀物相互聚集和团聚.以染料罗丹明B溶液为目标降解物,1 h的降解率为99.9%,最佳光催化剂的合成条件:13%明胶浓度、350℃煅烧2 h.