水热合成Zn1-xCrxO稀磁半导体晶体

采用水热法, 以3mol/L NaOH作为矿化剂, 在260℃下, 保温28h进行Cr合金化(x=0.10, 0.15, 0.20, 0.25), 合成Zn_1-xCr_xO稀磁半导体晶体. 研究了Cr合金化对水热合成Zn_1-xCr_xO稀磁半导体粉体结构和性能的影响. XRD测试表明, Cr元素进入到ZnO的晶格内, 实现了Cr的合金化, 晶粒尺寸分别为46.5、46.1、50.6和48.9nm. 从FE-SEM可以观察到, x>0.2时, 晶体的形貌从短柱状转变为长柱状. 通过UV/Vis测试可以观察到Cr离子的吸收, ZnO的禁带宽度依次降低为3.17、3.18、3.19和3.23eV. VSM测试表明, 所制备的Zn_1-xCr_xO纳米晶体在室温下均表现出弱顺磁性.     

热蒸发法制备Zn1-xCdxO纳米管及其生长机制研究

采用热蒸发纯Zn粉和Cd粉, 在湿反应气氛中氧化制备得到掺Cd的ZnO纳米管, 其Cd含量为3.3at%. 场发射扫描电镜(FESEM)及高分辨透射电镜(HRTEM)分析表明, 大部分纳米管外径约80~150nm, 长度达数微米, 壁厚约20nm. 通过与相同条件下制备的ZnO纳米结构的室温光致发光谱(PL) 进行对比发现, 由于Cd的掺入, Zn_1-xCd_xO纳米管的紫外近带边峰(UV NBE)从3.26eV红移到3.20eV附近.分析认为,Zn_1-xCd_xO纳米管遵循气液固(VLS)生长机制, 并在此基础上提出Zn_1-xCd_xO纳米管生长过程, 同时指出Kirkendall效应可能对纳米管的形成起到了重要作用.     

TiO_2/ZnO纳米管的制备及其光催化性能

采用电化学阳极氧化法制备了高度有序的TiO2纳米管阵列,并利用纳米管的光致超亲水特性,采用斜面毛细组装技术在无定形TiO2表面自组装ZnO溶胶后退火制备了TiO2/ZnO复合纳米管.探讨了阳极氧化各参数对纳米管形貌的影响.利用X射线衍射仪(XRD)、场发射扫描电子显微镜(FE-SEM)等方法对样品的结构和形貌进行了表征.以有机磷农药氯胺磷为光催化降解对象,研究了焙烧温度、管径、管长和TiO2/ZnO复合比例等因素对降解效果的影响.结果表明,焙烧温度、管径以及ZnO复合比例对光催化降解率影响较大.对于管径97 nm、管长315.8nm的TiO2/ZnO纳米管,ZnO最佳复合比例为4.2%(质量分数),5 h后降解率达到78%.     

ZnO/TiO2纳米管晶膜电极的制备及光电性能

采用水热法制备了ZnO纳米棒,以ZnO纳米棒为原料制备出ZnO/TiO2纳米管晶膜电极并应用于染料敏化太阳能电池.用扫描电镜(SEM)、X射线衍射仪(XRD)、X射线能谱仪(EDX)和N2吸脱附分析等研究了样品的结构、表面形貌和化学组成,并通过紫外可见光度计和电化学工作站探讨了煅烧温度在80~600℃范围内ZnO/TiO2纳米管电极的光电化学性能.此外,研究经TiCl4化学处理的ZnO/TiO2纳米管电极光电性能的改善情况.结果表明,600℃煅烧的ZnO/TiO2纳米管电极制备的染料敏化太阳能电池表现出较优的光电性能,其短路电流密度(Jsc)为2.28 mA/cm2,开路电压(Voc)为0.631 V,光电转换效率η为0.66%.600℃煅烧的ZnO/TiO2纳米管经TiCl4处理后的染料敏化太阳能电池的光电性能得到显著改善,其光电转换效率η提高到1.06%.     

电解液性质对TiO2纳米管阵列形貌及生长机理的影响

采用电化学阳极氧化法在纯钛片表面制备出了结构整齐有序的TiO₂纳米管阵列, 主要研究了电解液的性质、浓度以及氧化时间对TiO₂纳米管阵列形貌的影响, 并对不同电解液中TiO₂纳米管阵列的形成机理进行了初步探讨. 结果表明：在不同浓度的HF酸电解液中均可制备出规则、均匀的TiO₂纳米管阵列, 管径均匀, 表面平整, 但是纳米管的长度均较短, 约为300～350nm. 在高浓度HF电解液中, 同时获得了规则的纳米管阵列和纳米棒阵列. 在0.5wt% NaF和1mol/L Na₂SO₄中性电解液中也可以制备出表面光洁、排列整齐有序的TiO₂纳米管阵列, 纳米管长度明显长于HF酸电解液中获得的纳米管阵列, 达到了700nm, 但是阵列的表面平整度较差. 在乙二醇+0.6wt% NH₄F+2vol% H₂O有机电解液体系中可以制得超长的TiO₂纳米管阵列, 管径在150nm左右, 管长可达6μm.     

湿化学法ANNT纳米前驱体的反应机理与微观分析

利用柠檬酸盐法制备了(Ag_1-xNa_x)(Nb_1-xTa_x)O₃(简称ANNT)纳米粉体材料,通过TEM分析可观察到其颗粒度<50nm,且团聚较小.论文对柠檬酸盐法的反应机理进行了深入地探讨,分析了不同烧结温度下的显微结构变化,证实ANNT系统可在1040-1060℃范围内致密化.XRD分析结果表明系统中所生成的主晶相为ANNT.     

催化剂含量对共沉淀-烧结法制备氮化硼纳米管的影响

建立了一种不同催化剂含量下以无定形硼粉、活性碳粉、九水硝酸铁(催化剂)和尿素为原料的共沉淀-退火两步反应制备BN纳米管的方法。研究发现:催化剂含量的变化会影响BN纳米管的形貌和产量。当催化剂含量较低(摩尔比Fe(NO3)3/B=0.05)时,只有少量的竹节状纳米管生成,无颗粒存在,纳米管的平均直径约100nm。随着催化剂含量的升高(摩尔比Fe(NO3)3/B=0.1),纳米管的产量也升高,但有少量的颗粒形成,纳米管的平均直径仍然为约100nm。而当催化剂含量变得更高(摩尔比Fe(NO3)3/B=0.2)时,纳米管表面沉积着一层纳米片,管径升至250nm以上,同时颗粒也增多。分析表明纳米管的生长机理为气-液-固(VLS)生长机制。     

ZnO/TiO_2纳米管的制备及光降解性能研究

采用水热法合成TiO2纳米管,在碱性条件下与乙酸锌的无水乙醇溶液反应,得到表面负载ZnO的TiO2复合纳米管(ZnO/TNTs),并研究了复合纳米管在紫外光照射下对罗丹明B的光催化降解性能。通过透射电镜(TEM)、电子衍射能谱(EDS)、X射线衍射(XRD)、比表面积(BET)和紫外-可见光谱(UV-Vis)对所合成的材料进行了表征。结果表明,TiO2纳米管管径约5~10nm,管长约0.1~1μm;经ZnO表面修饰后,纳米管的结构没有发生明显变化,且ZnO粒子呈六方晶系纤锌矿结构均匀分散在纳米管的外表面,粒径约为6nm;光谱分析表明,ZnO/TNTs的吸收光谱有明显红移;且ZnO/TNTs的光催化活性较锐钛矿型TiO2纳米粉末、ZnO纳米粉末和TiO2纳米管有显著提高,且其光催化性能重复性好。     

脉冲激光沉积法室温下ZnO薄膜的制备与表征

在室温条件下,采用脉冲激光沉积技术在玻璃衬底上生长了ZnO薄膜.对薄膜的XRD分析表明,ZnO薄膜为六方纤锌矿结构并沿c轴取向生长,且(002)衍射峰的半高峰宽仅为0.24°.薄膜沿c轴方向受到一定的张应力为1.7×108 N/m2.原子力显微镜分析表明薄膜表面较为平整,平均粗糙度约为6.5 nm,晶粒尺寸约为50 nm.此外,透射光谱分析表明薄膜的禁带宽度为3.25 eV,与ZnO体材料的禁带宽度3.30 eV基本相同.     

ZnO纳米阵列的制备和稀土掺杂工艺及其发光性能的研究

以制备氧化铝模板为前提,采用电场辅助沉积法制备了纳米针尖阵列、纳米管阵列和纳米线阵列。利用X射线衍射仪、扫描电镜、透射电镜、能谱仪、热重分析等检测手段对制备的样品进行了相应的分析和表征。采用近场光学扫描显微镜和荧光分光光度计研究了样品的发光性能,并分析了发光机理。本实验的研究步骤、内容及得到的结论如下:(1)通过二次阳极氧化法制备了高度有序的氧化铝模板。在草酸溶液中合成了半壁氧化铝纳米管阵列,其阵列在302nm处的发射峰是由1B→1A的电子跃迁引起的,属于F+型发光。最后制备了氧化铝微米树,其树干的形成沿不同方向生长,呈明显的X交叉型生长模式。(2)制备出ZnO纳米针尖阵列。通过X射线衍射分析和高分辨图,可以判断该ZnO为多晶结构,且在[101]方向上有择优生长的趋势。随着退火温度的升高和退火时间的延长,510nm处的绿光发射带减弱,而379nm附近的带边发射增强。(3)合成了ZnO∶Tb3+纳米管阵列。通过对发射光谱图的分析,可以判断344nm处新的紫外发射带是由氧化铝模板本身发光而产生的。(4)合成了ZnO∶Eu3+纳米线阵列。高分辨透射电镜图和傅里叶变换可以断定该ZnO∶Eu3+纳米线是单晶结构,并且沿...     

Enhancement of photoluminescence from ZnO film by single wall carbon nanotubes

Optical emissions from ZnO films were enhanced by a formation of hybrid structures with single wall carbon-nanotubes (SWCNTs). The SWCNTs were characterized by the presence of the associated fibers and islands together with many carbon nanotube structures and their average height was about < or = 40 nm from atomic force microscope and scanning electron microscope measurements. The intensities of photoluminescence on ZnO films with SWCNTs were increased up to about 30 and 60% in the region of 3.3 eV (near band edge) and 2.3 eV (deep-level) bands, respectively. It was considered that the enhancement of optical emissions from ZnO might be resulted from the effects of an excitation light scattering by SWCNTs and a surface plasmon resonance between bandgap of ZnO and SWCNTs. The surface plasmon resonance mode in the ultra-violet regions is smaller than the deep-level region relatively. This result showed that the commercial ZnO/carbon nanotubes have a feasibility of application to optoelectronic device.     

氧化亚铜/碳纳米管超细复合球的合成及性能研究

采用溶液法原位制备了氧化亚铜/多壁碳纳米管(Cu₂O/MWNTs)超细复合球. 通过扫描隧道显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射仪(XRD)、紫外-可见分光光度计(UV-vis)和差热分析(DSC)等手段对产品进行了形貌分析和性能检测. 结果表明: 碳纳米管均匀嵌镶在Cu₂O球中; 相比于同粒径纯Cu₂O球, 复合球的特征吸收峰发生蓝移, 复合球使高氯酸铵(AP)的高温分解温度进一步降低了11.5℃. 另外, 对复合球的形貌影响因素及生长机理进行了探讨, 发现明胶是复合物成球的关键, 而聚乙二醇影响复合球粒径的均匀性.     

Preparation of cadmium-doped ZnO thin films by SILAR and their characterization

Cadmium-doped zinc oxide (Cd : ZnO) thin films were deposited from sodium zincate bath following a chemical dipping technique called successive ion layer adsorption and reaction (SILAR). Structural characterization by X-ray diffraction reveals that polycrystalline nature of the films increases with increasing cadmium incorporation. Particle size evaluated using X-ray line broadening analysis shows decreasing trend with increasing cadmium impurification. The average particle size for pure ZnO is 36·73 nm and it reduces to 29·9 nm for 10% Cd:ZnO, neglecting strain broadening. The strong preferred c-axis orientation is lost due to cadmium doping and degree of polycrystallinity of the films also increases with increasing Cd incorporation. Incorporation of cadmium was confirmed from elemental analysis using EDX. The optical bandgap of the films decreases with increasing Cd dopant. The value of fundamental absorption edge is 3·18?eV for pure ZnO and it decreases to 3·11?eV for 10% Cd:ZnO.     

Rapid growth of nanotubes and nanorods of würtzite ZnO through microwave-irradiation of a metalorganic complex of zinc and a surfactant in solution

Large quantities of single-crystalline ZnO nanorods and nanotubes have been prepared by the microwave irradiation of a metalorganic complex of zinc, in the presence of a surfactant. The method is simple, fast, and inexpensive (as it uses a domestic microwave oven), and yields pure nanostructures of the hexagonal würtzite phase of ZnO in min, and requires no conventional templating. The ZnO nanotubes formed have a hollow core with inner diameter varying from 140–160 nm and a wall of thickness, 40–50 nm. The length of nanorods and nanotubes varies in the narrow range of 500–600 nm. These nanostructures have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). The ZnO nanorods and nanotubes are found by SAED to be single-crystalline. The growth process of ZnO nanorods and nanotubes has been investigated by varying the surfactant concentration and microwave irradiation time. Based on the various results obtained, a tentative and plausible mechanism for the formation of ZnO nanostructures is proposed.     

ZnO/In2O3纳米异质结的合成及其光催化性能的研究

通过热水解法成功制备出了形貌均一的ZnO/In₂O₃异质结光催化材料, 采用场发射扫描电子显微镜(FESEM)、X射线衍射仪(XRD)以及透射电子显微镜(TEM)对样品的形貌及结构进行表征。结果表明: ZnO/In₂O₃异质结是由直径约200~300 nm、厚度约40~60 nm的六边形纳米片镶嵌着In₂O₃纳米小颗粒组成。对比纯ZnO、纯In₂O₃和该光催化材料对罗丹明B(RhB)的可见光降解效率, 发现ZnO/In₂O₃异质结光催化材料对RhB具有较高的光催化效率, 其原因是窄带系半导体In₂O₃能够有效地吸收可见光, 当ZnO与In₂O₃ 形成异质结时, In₂O₃能带上被可见光激发的电子会迁移到ZnO的导带上, 而光激发的空穴仍保留在In₂O₃价带, 这样有助于光生电子和空穴的分离, 降低其复合几率, 从而有效地提高了ZnO的光催化效率。     

Synthesis and characterization of SnS/ZnO nanocomposite by chemical method

SnS nanorods and SnS/ZnO nanocomposite have been synthesized by chemical method. Structure and phase purity of the samples were confirmed by powder X-ray diffraction. Transmission electron microscope image of SnS nanorods showed the average diameter of nanorods was about 85 nm and length was several micrometers. Transmission electron microscope image of SnS/ZnO nanocomposite showed the average particle size of ZnO nanoparticle was about 12 nm. The formation of SnS/ZnO nanocomposite was confirmed by elemental analysis using energy dispersive X-ray spectroscopy. From the microRaman spectrum of SnS/ZnO nanocomposite, it was observed that the intensity of B_2g mode of SnS nanorods decreased dramatically compared to that of pure SnS nanorods, since the surface of the SnS nanorods were coated with ZnO nanoparticles. Both direct and indirect band gap transitions were observed for SnS nanorods from the optical absorption spectrum and the optical absorption spectrum of SnS/ZnO nanocomposite showed absorption in the visible region.     

Synthesis of nano-dimensional ZnO and Ga doped ZnO thin films by vapor phase transport and study as transparent conducting oxide

We report synthesis of polycrystalline ZnO and Ga doped ZnO (ZnO:Ga) thin films (approximately 80 nm) on Si and quartz substrates in a non-vacuum muffle furnace, a simple and cost-effective route, without any catalyst/reactive carrier gases, at relatively low processing temperature of 550 degrees C. The crystalline phases of the films are identified by grazing angle X-ray diffraction (GAXRD). The growth of ZnO films is examined with scanning electron microscope (SEM) as a function of deposition time. An optical transmission of approximately 90% is observed for pure ZnO film having a resistivity of approximately 2.1 Omega-cm as measured by van der Pauw technique. Doping with Ga results in single phase ZnO:Ga films, retaining an optical transmission of about 80% and three orders of magnitude decrease in resistivity as compared to pure ZnO film.     

Ni掺杂ZnO制备及其热电性能研究

采用溶胶-凝胶法合成了Zn_1-xNi_xO纳米颗粒, 以放电等离子烧结成块体。扫描电镜照片发现, Zn_1-xNi_xO颗粒呈300~500 nm厚的片状结构, 表面存在大量蜂窝状小孔。由XRD数据可以看出, x≥0.05的样品中存在Zn_yNi_zO杂质相。热电性能分析表明, 随着Ni添加量的增加, 塞贝克系数的绝对值|S|逐渐减小, 而电导率得到大幅度提高。与ZnO块体材料相比, 溶胶-凝胶法合成的Zn_1-xNi_xO材料的热导率大幅度降低, 在750 K时, Zn_1-xNi_xO的热导率降低至3 W/(m·K), 是ZnO (11 W/(m·K))材料的1/3。电导率的增加和热导率的降低导致热电优值大幅度提高。在750 K下, Zn_0.925Ni_0.025O材料的热电优值达到0.045。     

The effect of substrate morphology on the diameter distribution of carbon nanotubes grown on silica and ceramic substrates

Large-scale well-aligned carbon nanotube film and carbon nanotube bundles have been fabricated on smooth silica and rough polycrystalline ceramic substrates by pyrolysis of ferrocene/melamine mixtures. The images of transmission electron microscopy (TEM) and scanning electron microscope (SEM) show that carbon nanotubes grown on the silica substrate have uniform outer diameters of about ∼ 25 nm and lengths of about 40 μm, while those on the ceramic substrate have outer diameters from 10 to 90 nm and lengths up to 100 μm. Electron energy-loss spectroscopy (EELS) spectra show that nanotubes grown on the two different substrates are pure carbon tubes. The effects of substrate micro-morphologies on the diameters of carbon nanotubes have been discussed.