硅基AAO模板内电化学沉积ZnO纳米线及其光电性能研究

本文利用二次阳极氧化法在p型低阻〈100〉晶向的硅衬底上制备了AAO/Si,以硅基AAO为辅助模板,采用电化学沉积的方法以Zn(NO3).6H2O和HMT(C6H12N4)为原料,在80℃的水浴槽中制备了ZnO纳米线结构。采用SEM,XRD和拉曼光谱等手段对ZnO/AAO/Si复合结构进行表征。SEM图表明ZnO纳米线已成功组装到AAO/Si模板里,直径约45 nm,长度约为600 nm。XRD和拉曼光谱表明ZnO具有六角纤锌矿多晶结构。光致发光(PL)谱图表明ZnO/AAO/Si复合结构在565 nm附近有较宽黄绿发射峰,在395 nm附近有微弱的紫外发射峰。场发射测试结果表明,ZnO纳米线的场增强因子的β值为2490,场增强因子很高,具有广泛的应用前景。     

硅纳米线的制备及其光学性能的研究

通过金属催化化学刻蚀的方法中的两步法制备出了具有阵列结构的硅纳米线,研究了不同刻蚀条件对硅纳米线形貌的影响,分析了形成不同形貌的原因.测定了不同条件下制备的硅纳米线的光吸收性能,总结了影响光吸收性能的因素和原因,根据硅纳米线的光吸收图求出了硅纳米线的禁带宽度,说明了硅纳米线已经具备不同于硅片的性能.     

电场辅助电化学法沉积ZnO纳米线

采用电场辅助电化学沉积的方法成功的在阳极氧化铝模板中沉积出ZnO纳米线阵列.透射电子显微镜(TEM)、X射线衍射(XRD)测试结果表明,制备的纳米线是单晶ZnO纳米线,形貌均匀,直径大约为60nm,并且择优于(101)晶面.我们对生长过程中所加辅助电场的作用给出了初步的解释.     

预氧化法制备均匀硅纳米线阵列

利用双氧水溶液对硅片表面进行预氧化处理,并用改良的RCA法清洗硅片,结合金属辅助化学刻蚀(MACE)制备硅纳米线阵列(SiNWs).通过表征发现:预氧化清洗相较于传统RCA清洗,能够降低硅片表面微粗糙度,同时提高后续制备的硅纳米线阵列的均匀性.此外,在300～800 nm波段,当硅纳米线的长度相近时,经预氧化清洗制备的硅纳米线阵列反射率降低,当硅纳米线长度为500 nm左右时,反射率降低值大于2.4;.最后分析了均匀硅纳米线阵列的形成机理.     

不同生长方向的GaN纳米线的可控制备与性能表征

采用化学气相沉积法,通过改变催化剂和衬底,以Ga2 O3和GaN的混合粉末为镓源制备出了不同生长方向的GaN纳米线,制备的平躺于衬底的GaN纳米线的直径约为60 nm,长度为10 μm到30 μm之间.垂直于衬底的GaN纳米线阵列的直径约为300 nm,长度约为5μm.使用扫描电子显微镜(SEM)、X射线衍射(XRD)、光致发光谱(PL)和透射电子显微镜(TEM)对样品进行了分析表征,结果表明所得样品为六方纤锌矿结构的GaN单晶纳米线.通过改变催化剂和衬底等生长条件,研究了衬底和催化剂对纳米线生长方向的影响,为以后的大量制备以及纳米器件的制作提供了依据.     

纤蛇纹石制备硅纳米线的研究

以天然矿物纤蛇纹石制备的氧化硅纳米线为氧化剂和模板,镁粉为还原剂,采用镁热还原法制备了系列硅纳米线.利用热分析仪、X射线衍射仪、扫描电子显微镜(SEM)和透射电子显微镜(TEM)对其进行表征.结果表明:温度对反应产物硅的结构和形貌有显著影响,随着温度的上升,样品的结晶度先减小后增大;在温度650℃条件下硅“继承”了氧化硅纳米线的微观结构,而随着温度升高至700℃纳米线的结构出现坍塌,形成硅纳米颗粒.     

柠檬酸含量对LiFePO4/C复合正极材料形貌及电化学性能的影响

采用水热-高温煅烧法制备了具有不同形貌的LiFePO4/C复合材料,探讨了柠檬酸含量对其形貌和电化学性能的影响.结果表明,柠檬酸的添加对LiFePO4/C复合材料的形貌具有显著的影响.通过添加柠檬酸调控LiFePO4/C复合材料的形貌,可以极大地改善LiFePO4/C复合材料的电化学性能.当柠檬酸与LiFePO4的摩尔比为1∶2时,LiFePO4/C复合材料呈纳米片状,颗粒粒径最小,比表面积最大,在0.1C和5C时放电比容量为160.3mA·h·g1和130.9 mA·h·g-1.     

络合-水热法制备碱式硫酸镁纳米线

以MgSO4·7H2 O和NaOH为原料,邻苯二甲酸氢钾(KHpht)作为络合剂,采用络合-水热法制备碱式硫酸镁(MOS)纳米线.考察了反应条件对MOS纳米线形貌的影响,并对产物进行了表征和分析.确定了制备MOS纳米线的较优条件:MgSO4浓度为0.3 mol/L,n(NaOH)/n(MgSO4)为2.5,n(KHpht)/n(MgSO4)为1.1,无水乙醇作为分散剂,水热合成温度160℃,反应时间10 h.所得到MOS纳米线形貌均匀,长度在10～20μm,直径在20～100 nm,纳米线沿[010]方向生长.     

金属铝粉直接氮化工艺中镁粉催化作用研究

首先分析了Mg在直接氮化制备AlN中的催化作用,然后采用实验的方法进行验证.实验中对Mg的含量比例进行优化,并通过XRD、SEM、EDS、TG和DTG进行测试、分析和表征.结果表明,当铝粉与镁粉的质量比例不同时,镁粉起到不同程度的催化作用,产物表现为不同的外观形貌及不尽相同的物相组成.当铝粉与镁粉的质量比例为9/1,可得到直径均匀、长度可观的AlN纳米线结构.此外,结合V-S机制对纳米线的生长机理进行了解释.     

磷化铟纳米线的溶剂热制备及其表征

以氯化铟和无毒红磷为主要原料,十六烷基三甲基溴化铵为表面活性剂,采用溶剂热法低温合成磷化铟纳米线,并用X射线衍射仪(XRD)和场发射扫描电镜(FESEM)对所制备产物的结构和形貌进行了分析表征;能谱仪(EDS)和荧光分光光度计对所制备产物的成分,含量和发光性质进行了表征.结果表明:采用该方法制备出的磷化铟纳米线长短不同,最小直径为20 nm.在合适的条件下,改变反应温度、增加反应时间或改变碱溶液都可生长出高品质的磷化铟纳米线.     

ZnO超细纳米线阵列的制备及其电化学性能

以Zn(NO₃)₂· 6H₂O和C₆H₁₂N₄为原材料,采用二步水热法在碳纤维布上合成了形貌尺寸均匀的ZnO超细纳米线阵列。用 X 射线衍射(XRD)和扫描电镜(SEM)对其晶体结构和形貌进行了表征,利用恒流充放电测试等手段对其进行电化学性能测试。测试结果表明,材料表现出优异的电化学性能。在200 mA/g的电流密度下循环150次后,ZnO超细纳米线阵列仍然约有730 mAh/g的充放电比容量,库伦效率保持在95%以上。在1 200 mA/g的大倍率条件下,材料的充放电比容量依旧可达481 mAh/g左右,表现出十分良好的循环稳定性和可逆性能,是一种较为理想的锂离子电池负极复合材料。     

Synthesis,characterization and electrical properties of hybrid Zn2GeO4–ZnO beaded nanowire arrays

We report the syntheses of vertically aligned, beaded zinc germinate (Zn₂GeO₄)/zinc oxide (ZnO) hybrid nanowire arrays via a catalyst-free approach. Vertically aligned ZnO nanowire is used as a lattice matching reactive template for the growth of Zn₂GeO₄/ZnO nanowire. The morphology and structure of the as-prepared samples were characterized using X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS). TEM studies revealed the beaded microstructures of the Zn₂GeO₄/ZnO nanowire. The thickness and microstructures of crystalline beads could be easily controlled by tuning the growth duration and temperature. The photoluminescence spectrum of the Zn₂GeO₄/ZnO nanowires is composed of two peaks, i.e., the ultraviolet (UV) peak and the defect peak. For longer treatment duration of the samples, both the UV and defect peak intensities decrease dramatically. One application of the as-prepared Zn₂GeO₄/ZnO nanowire is to use the nanowire as template for the growth of three-dimensionally (3D) aligned, high-density ZnO nanobranches en route to hierarchical structure. The study of field emission properties of the as-prepared samples revealed the low turn-on voltage and high current density electron emission from the 3D ZnO nanobranches as compared to the ZnO nanowires and Zn₂GeO₄/ZnO nanowires. Furthermore, the electrical transport behavior of single hybrid nanowire device indicates the formation of back-to-back Schottky barriers (SBs) formation at the contacts and its application in white-light response has been demonstrated.     

用AAO模板法制备高度定向碳纳米管阵列的研究进展

用二步氧化法可以在草酸或硫酸中制备多孔氧化铝（AAO）模板，这种模板成本低，高度有序，六角排列。利用化学气相沉积技术可以制备高度定向生长的碳纳米管，这将有利于研究碳纳米管的性质和它在纳米电子器件及其他领域的应用。本文介绍了AAO模板的阳极氧化工艺，成膜机理以及不同电解液，氧化电流、电压等因素对纳米孔道的影响。讨论了催化剂和气相沉积温度对碳纳米管特性的影响，并指出这种制备碳纳米管的技术需要深入研究的问题。     

Synthesis and characterization of Bi3.15Nd0.85Ti3O12 nanotube arrays

Nd-substituted bismuth titanate (Bi_3.15Nd_0.85Ti₃O₁₂, BNT) nanotube arrays are fabricated by means of a sol–gel method utilizing porous anodic aluminum oxide (AAO) template. The morphologies and structures have been determined by scanning electron microscopy (SEM), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The diameter and length of these nanotubes are about 200 nm and 60 μm, respectively, and their wall thickness is about 30 nm. The average grain size is around 40 nm. XRD data show that the BNT nanotubes possess bismuth-layered perovskite structure. High-resolution electron microscopy (HRTEM) image demonstrates that the BNT nanotubes are polycrystalline. Polarization–electric field (P–E) response curves of BNT nanotube arrays were measured, and a size induced polarization reduction phenomenon is observed.     

Engineering ZnO nanowire surfaces via a chemical method

Quasi‐aligned porous ZnO nanowire arrays are promising architectures for potential applications in catalysts, gas sensors and solar cells. However, processes for conversion of ZnO nanowire arrays into porous ones have rarely been reported. Here, we report a facile chemical method for the synthesis of ZnO nanowire array with porous surface. The morphology and structure of the obtained products have been investigated with field‐emission scanning electron microscopy and high‐resolution transmission electron microscopy. Time‐dependent experiments have also been carried out to better understand the formation process of porous structures on the nanowire surfaces. The obtained porous ZnO nanowire arrays may find potential applications in catalysts, solar cells and gas sensors due to the large surface area of the yielded products.     

用热CVD法制备片状碳纳米材料的研究

采用阳极氧化法在草酸溶液中制备了孔径约为100nm的多孔氧化铝(AAO)模板。利用此模板在不负载任何催化剂的条件下,利用热CVD装置制备出片状碳纳米薄膜,并对此片状薄膜做了SEM,TEM显微观察和EDS能谱分析,对其形成条件和生长机理等方面做了探讨分析,为在氧化铝模板上生长包括管状、片状、棒状等形状的碳纳米材料提供了一定的借鉴意义。     

Growth of aragonite calcium carbonate nanorods in the biomimetic anodic aluminum oxide template

In this study, a biomimetic template was prepared and applied for growing calcium carbonate (CaCO₃) nanorods whose shape and polymorphism were controlled. A biomimetic template was prepared by adsorbing catalytic dipeptides into the pores of an anodic aluminum oxide (AAO) membrane. Using this peptide-adsorbed template, mineralization and aggregation of CaCO₃ was carried out to form large nanorods in the pores. The nanorods were aragonite and had a structure similar to nanoneedle assembly. This aragonite nanorod formation was driven by both the AAO template and catalytic function of dipeptides. The AAO membrane pores promoted generation of aragonite polymorph and guided nanorod formation by guiding the nanorod growth. The catalytic dipeptides promoted the aggregation and further dehydration of calcium species to form large nanorods. Functions of the AAO template and catalytic dipeptides were verified through several control experiments. This biomimetic approach makes possible the production of functional inorganic materials with controlled shapes and crystalline structures.     

TiO_2纳米管阵列的制备及其光催化性能研究

采用阳极氧化法在钛箔上制备了TiO_2纳米管阵列,利用场发射扫描电子显微镜(FSEM)、X射线衍射仪(XRD)和紫外-可见分光光度计对TiO_2纳米管的形貌、结构和光学性能进行表征,详细考察了阳极氧化工艺参数对纳米管阵列形貌的影响,探讨了氧化钛纳米管阵列的形成机理,并对其光催化活性进行了测试,研究结果表明:在0.5 wt; HF和1 mol/L H3PO_4电解液中,控制氧化电压为20 V,反应60 min后,在钛箔表面可获得垂直导向的TiO_2纳米管阵列,管内径为60~80 nm,管壁厚约10 nm;600 ℃热处理后的TiO_2纳米管阵列薄膜对349.7 nm近紫外光和443.9 nm可见光有较强的吸收能力;煅烧温度对纳米管的晶型结构和光催化活性有显著影响.     

EDTA‐assisted synthesis of rose‐like ZnO architectures

Rose‐like ZnO nanostructures were prepared by a low‐temperature solution route with assistance of ethylenediaminetetraacetic acid disodium (EDTA‐2Na). The morphology of ZnO nanostructures was found to change from nanowire arrays to rose‐ and tower‐like architectures with increasing the molar ratio of EDTA‐2Na/Zn²⁺. Also, the shape evolution of ZnO nanostructures with time was observed from flat nanosheets to wrinkled nanosheets and to rose‐like nanostructures. EDTA‐2Na as a strong complexing agent was found to play a key role in the shape evolution. Photoluminescence spectra show that the rose‐like ZnO architectures have more defects than the nanowire arrays. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)