多孔纳米氧化锌的模板法优化制备与电致发光特性

采用溶胶-凝胶法在中性条件下合成了孔径大小不同的介孔ZnO前驱体. 通过热氧化法, 在空气中煅烧前驱体制备了ZnO纳米晶颗粒. 讨论了反应条件对发光强度的影响, 并确定了最佳反应条件. 电致发光测试结果表明, 前驱体制备过程中, 表面活性剂的处理不会使发光特征峰发生移动; 相同测试条件下, 由介孔结构前驱体煅烧而成的ZnO样品其电致发光强度明显增强, 十八胺、F-127处理过的样品发光强度分别是普通样品的3.7倍和5.6倍. 发光强度的显著增强可能是由颗粒内介孔结构引起.     

分级介孔结构组成的ZnO微球及光催化性能

以硝酸锌、脲素及酒石酸为反应物, 采用水热法制备碱式碳酸锌前驱体微球, 通过煅烧前驱体制备了介孔氧化锌微球。通过扫描电子显微镜(SEM)可以观察到, 氧化锌微球的直径约为2~4 μm, 由大量厚度约为10 nm的介孔纳米片组装而成。X 射线衍射(XRD)和透射电镜(TEM)结果表明: ZnO微球为六方纤锌矿结构, 并结晶较好。比表面积测试(BET)表明ZnO微球为介孔材料, 孔径为20~50 nm, ZnO微球比表面积约为29.8 m²/g。以亚甲基蓝为目标降解物, 对介孔氧化锌微球进行了光催化降解实验。实验结果表明, 所合成的介孔ZnO微球对亚甲基蓝的光催化性能较好。     

多孔结构ZnO及其电致发光性能

利用Sol-gel法制备了含制孔剂P123的ZnO前驱体,通过无皂乳液聚合法和分步乳液聚合法制备了不同粒径的PS小球,采用共沉积法得到P123-PS-ZnO凝胶。高温煅烧去除有机模板剂P123和PS,从而制备出系列孔径可控的多孔ZnO电致发光材料。研究表明,多孔结构可以显著改善ZnO的电致发光性能;ZnO发光强度随PS粒度的改变而改变,当使用100nm PS小球为模板时,多孔ZnO材料的相对发光强度较未使用PS模板提高了4.03倍。     

微生物模板辅助制备ZnO空心微球

以白葡萄球菌作为模板,通过醋酸锌和三乙醇胺(TEA)反应成功得到ZnO空心微球。采用SEM、TEM、XRD和TG表征所得的ZnO空心微球,得到了空心微球的基本形貌,并发现了细菌模板在高温下易去除的特点。还研究了不同细菌和三乙醇胺(TEA)加入量以及静置时间对空心微球的影响,发现加入高浓度的细菌液和TEA溶液以及长时间的静置有利于空心微球的制备。最后确定了细菌在整个ZnO空心微球制备过程中的模板作用,但单纯的细菌不足以使ZnO覆盖在其表面形成空心微球结构,需要对其表面进行修饰,而实验中加入的TEA就是用于修饰细菌表面的。     

低温无模板法制备TiO2多孔球及其光催化性能研究

以钛酸四丁酯为钛源,乙二醇和丙酮为溶剂,以低温无模板法制备纳米TiO_2多孔微球。XRD分析可知,随着沸水处理时间的增长,纳米晶粒TiO_2多孔微球的晶化程度逐渐提高。沸水处理120 min时得到的锐钛型TiO_2已具有较高的晶化程度。TEM和SEM研究表明,经沸水处理后的有机前驱体表面由光滑转变粗糙,多孔结构形成。BET数据分析表明,在其它相同条件下,沸水处理120 min时得到的纳米晶粒TiO_2多孔微球具有较高的BET比表面积,且介孔体积较大,表面反应活性位点较多,更有利于对RhB的吸附。光催化结果表明,沸水处理120 min时得到的的TiO_2多孔微球具有较好的光催化活性,其一级反应速率常数为沸水处理30 min时得到的纳米晶粒TiO_2多孔微球的11.29倍,为P25的1.74倍。这是由于纳米晶粒TiO_2多孔微球的介孔结构和较高的比表面积能引入更多的表面反应活性位点所致。     

Ce掺杂ZnO分级结构微球的制备及其光催化性能研究

以硝酸锌、氢氧化钠、硝酸铈为原料,采用沉淀法制备了一系列Ce掺杂的Ce/ZnO分级结构微球。采用X射线衍射仪、场发射扫描电子显微镜、能量色散谱仪和紫外-可见漫反射光谱仪等对样品进行表征。以甲基橙的光催化降解为模拟反应,考察了Ce掺杂量对Ce/ZnO分级结构微球光催化性能的影响。结果表明:Ce/ZnO分级结构微球由ZnO微纳米片相互交错构建而成,Ce的掺杂提高了Ce/ZnO分级结构微球的光催化活性,其中Ce摩尔分数为1.5%的Ce/ZnO对甲基橙的光催化降解效果最好,紫外光照射60min甲基橙降解率为98.3%,循环使用4次,其催化活性未明显下降。     

中空ZnO微球的制备及其光催化性能

以葡萄糖和醋酸锌为原料,采用模板法制备中空ZnO微球。并对所制样品进行表征,讨论了碳微球与醋酸锌物料比、煅烧温度、煅烧时间对ZnO催化剂光催化活性的影响。结果表明:在碳微球与醋酸锌物料比为1∶2、煅烧温度500℃、煅烧时间2h条件下,所制备的中空ZnO微球直径约为3~5μm,六方晶系结构,具有较好的光催化活性。     

大孔-介孔分级孔结构炭材料制备及性能研究

以聚苯乙烯微球以及F127嵌段共聚物自组装结构为模板,酚醛树脂低聚物为碳前驱体,双模板法合成了大孔-介孔分级孔结构的炭材料.对样品进行了X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和氮吸附-脱附测试,并研究了样品的电化学性能.结果表明,利用这种简便的合成方法可以得到具有三维连通大孔以及二维有序介孔结构的分级孔结构炭材料,大孔尺寸在1μm左右,介孔孔径集中分布在5nm,比表面积为353.8m2/g,孔容0.36cm3/g.利用三电极体系测试了产品作为电化学双电层电容器电极材料的性能,在50mA/g的电流密度下,放电质量比电容为40F/g.     

CdS/ZnO复合颗粒的制备与电致发光性能

以sol-gel法制备了ZnO前驱体,并通过水热反应得到了CdS/ZnO复合颗粒.采用红外光谱(IR)、X射线衍射(XRD)、扫描电镜(SEM)表征其结构、组成及形貌,并对其电致发光(EL)特性进行表征.结果表明CdS纳米晶生长在ZnO基体上;EL谱表明没有煅烧的CdS/ZnO复合颗粒表现为CdS的激子发射,发光强度较纯CdS有了明显的提高;而煅烧后的CdS/ZnO复合颗粒则表现为ZnO的缺陷发射,发光谱的半高宽较纯ZnO有所减小.     

以模板法制备介孔碳及其性能研究

活性炭、卡宾、石墨、富勒烯和纳米碳管以及金刚石等是炭材料家族的代表,随着科学技术的进步和分析手段的提高,越来越被人们所重视。日常生活中人们接触到的各种炭材料差不多都可归结为无定形炭的范畴,如类金刚石炭、玻璃炭、活性炭以及各种炭黑、焦炭等。     

沸石矿模板制备多孔炭及其电性能研究

为降低模板法制备多孔炭的成本,使用一种天然沸石矿为模板来制备多孔炭。利用XRD、N2吸附和循环伏安法研究多孔炭的物相组成、孔结构和电化学性能。研究表明,所制备多孔炭的比表面积仅为411m2/g,但富含中大孔,并具有较宽的孔径分布;在1mol/L的H2SO4溶液中,1mV/s的扫描速度下,多孔炭的比容量为185F/g,扫描速度增加到500mV/s,其比容量保持率高达72%,比在相同条件下,比表面积2322m2/g的商业微孔活性炭的容量保持率23%高得多,且保持了良好的扫描曲线。     

溶胶-凝胶法制备多孔纳米金属铜膜

为了制备多孔纳米金属膜材料,以醋酸铜为前躯体、聚乙二醇为模板剂、二乙醇胺为络合剂,通过溶胶-凝胶法在玻璃基片上制备了多孔纳米金属铜膜.利用XRD、IR、TG-DTG和SEM对所制备的纳米金属铜膜材料进行了分析及表征,并研究了溶胶浓度、PEG添加量、退火温度对多孔铜膜结构的影响.结果表明,当溶胶浓度为0.6 mol/L时,铜离子与PEG1000的毫克分子比值是42.86∶1,退火温度为500℃时,可以得到较好的多孔结构纳米Cu薄膜.不同的PEG加入量、溶胶浓度以及热处理温度都会对薄膜的形貌有较大的影响.     

纺锤形氧化锌的水热制备及其对三乙胺的气敏性能

采用水热法,用氨水调节溶液pH,合成了纺锤及花状的ZnO。利用X射线衍射仪、扫描电子显微镜对不同pH下合成的ZnO的物相及形貌进行了表征,并采用静态配气法测试了其对三乙胺的气敏性能。结果表明,不同pH制备了不同形貌的ZnO材料。pH=9时制备的纺锤形ZnO对三乙胺的灵敏度最高,在340℃的最佳工作温度下对100mg/L三乙胺气体的灵敏度高达90.0,呈现出良好的选择性。并且元件具有较好的响应-恢复特性,响应时间为27s,恢复时间仅需3s。     

Facile synthesis and enhanced photocatalytic activity of hierarchical porous ZnO microspheres

In this paper, hierarchical porous ZnO microspheres were successfully synthesized by calcining the microspheric zinc hydroxide carbonate (ZHC) precursor, which were the precipitate products of a hydrothermal reaction by zinc nitrate hexahydrate and urea in the presence of trisodium citrate. The as-prepared ZnO microspheres with diameters of 4-5 μm were assembled by numerous porous nanosheets which had the uniform thickness of about 10 nm. The photocatalytic activity of the ZnO microspheres was evaluated by photodegradation reaction of methylene blue (MB). The as-prepared ZnO microspheres exhibited a significantly enhanced photocatalytic activity than commercial ZnO and TiO₂. This was mainly attributed to the larger specific surface area and stability against aggregation.     

Preparation and characterization of bowl-like porous ZnO film by electrodeposition using two-dimensional photonic crystal template

A rapid and low-cost method combining electrodeposition with two-dimensional (2D) photonic crystal template technique to prepare large scale bowl-like porous ZnO films is described. The 2D photonic crystal templates were fabricated by self-assembly of monodispersed polystyrene (PS) microspheres on indium-tin-oxide coated glass substrates using spinning coating method. The interstitial spaces among the spheres of the templates were filled with ZnO via electrodeposition from an aqueous solution containing 0.02 M zinc nitrate as electrolyte under a constant potential of ?1.0 V at 65 °C for 10 min. After removal of the PS photonic crystal template, bowl-like porous ZnO film was obtained. The entire process can be accomplished within 30 min. Scanning electron microscopic images showed good homogeneity in morphology, X-ray diffraction spectra demonstrated the wurtzite structure of the obtained ZnO film, and transmission electron microscopy indicated the single-crystallinity of the ZnO. Ultraviolet–visible (UV–vis) spectrophotometer was used to detect the absorption in UV–vis region of the PS template, opal ZnO-PS composite and inverse opal ZnO respectively. Two strong emission bands at 400 and 550 nm were displayed in photoluminescence spectrum.     

Electrodeposition of template free hierarchical ZnO nanorod arrays via a chloride medium

We have successfully grown template and buffer free ZnO nanorod films via chloride medium by controlling bath temperature in a simple and cost effective electrochemical deposition method. Thin films of ZnO nano-rods were obtained by applying a potential of ?0.75 V by employing Ag/AgCl reference electrode for 4 h of deposition time. The CV measurements were carried out to determine potential required to deposit ZnO nanorod films whereas chronoamperometry studies were carried out to investigate current and time required to deposit ZnO nanorod films. The formation of ZnO nanorod has been confirmed by scanning electron microscopy (SEM) and Raman spectroscopy. Low angle XRD analysis confirms that ZnO nanorod films have preferred orientation along (101) direction with hexagonal wurtzite crystal structure. The SEM micrographs show nice surface morphology with uniform, dense and highly crystalline hexagonal ZnO nanorods formation. Bath temperature has a little influence on the orientation of nanorods but has a great impact on their aspect ratio. Increase in bath temperature show improvement in crystallinity, increase in diameter and uniform distribution of nanorods. Compositional analysis shows that the amount of oxygen is ~49.35 % and that of Zn is ~50.65 %. The optical band gap values were found to be 3.19 and 3.26 eV for ZnO nanorods prepared at bath temperature 70 and 80 °C respectively. These results indicate that by controlling the bath temperature band gap of ZnO nanorods can be tailored. The obtained results suggest that it is possible to synthesize ZnO nanorod films by a simple, cost effective electrodeposition process which can be useful for opto-electronic devices fabrication.     

木材结构分级多孔ZnO的同步辐射XAFS研究

利用同步辐射XAFS (X-ray AbsorptionFine Structure)实验及FEFF计算进行数据拟合,研究遗态转化工艺制备的ZnO产物的微观晶体结构参数.研究结果表明,遗态转化工艺得到了ZnO产物,木材结构分级多孔ZnO产物的第一壳层Zn-O距离为0.1986nm,第二壳层Zn-Zn距离为0.3240n...     

Synthesis and optical properties of hierarchical pure ZnO nanostructures

We report the catalyst-free synthesis of hierarchical pure ZnO nanostructures with 6-fold structural symmetry by two-step thermal evaporation process. At the first step, the hexagonal-shaped nanowires consisting of a great deal of Zn and little oxide were prepared via the layer-by-layer growth mechanism; and at the second step, hierarchical pure ZnO nanostructures were synthesized by evaporating the Zn source on the basis of the step-one made substrate. Scanning electron microscopy, transmission electron microscope images, and the corresponding selected area electron diffraction pattern have been utilized to reveal the screw dislocation growth mechanism, through which the single crystal ZnO nanorods are epitaxially grown from the side-wall of central axial nanowires. Raman and photoluminescence spectra further indicate that, for the hierarchical ZnO nanostructures, the ultraviolet peak is related to the free exciton recombination, while the oxygen vacancies and high surface-to-volume ratio are responsible for the strong green peak emission.     

Modified nano-CaCO3 hard template method for hierarchical porous carbon powder with enhanced electrochemical performance in lithium-sulfur battery

Lithium-sulfur (Li-S) battery was the most promising energy storage devices with ultrahigh energy density (2600 Wh kg⁻¹). But it was impeded by poor electronic conductivity, serious shuttle effect, and enormous volume expansion. Herein, hierarchical porous carbons were simply prepared by a modified nano-CaCO₃ hard-template method from glucose. The template-removal step was modified from HCl washing to HCl soaking. This allowed the microstructure of carbon product significantly involved. Furthermore, the mass ratio of CaCO₃ nanoparticles and glucose played an important role in booming of hierarchical porous and specific surface area. When integrated with S, functioned as cathode in Li-S battery, improved electrochemical performances were exhibited, such as high initial discharge capacity and good capacity retention. This modified hard-template method suggested a promising way to fabricate hierarchical porous carbon matrix available to apply in advanced Li-S battery.     

PEG辅助的溶胶凝胶法制备多孔ZnO薄膜

以醋酸锌为前驱体,乙醇为溶剂,二乙醇胺为络合剂,通过聚乙二醇(PEG)辅助的溶胶--凝胶法在玻璃基片上制备了ZnO多孔薄膜.利用IR、TG-DTA、XRD及SEM等测试方法对薄膜的结构和特性进行了分析.探讨了样品在溶胶-凝胶及煅烧过程中的物理化学变化.研究了前驱体浓度、PEG2000加入量对薄膜结构和性能的影响.结果表明,当Zn2 的浓度为0.6mol/L的溶胶在70℃水浴时,加入PEG2000后,有利于ZnO多孔结构的形成,而且孔尺寸及密度也随PEG加入量的增大而增大.