Ag/ZnS核壳结构纳米棒的制备及其光催化性能分析

在制备的Ag纳米线的基础上,用水热法合成了Ag/ZnS核壳结构纳米棒.使用X射线衍射仪(XRD)、场发射扫描电子显微镜(FESEM)、X射线能谱仪(EDS)、高分辨透射电子显微镜(HRTEM)、紫外-可见双光束分光光度计(UV-vis)、光致发光扫描仪(PL)等检测设备对样品的成分、形貌、微结构及光学性能进行了表征.结果显示,制备的Ag/ZnS复合材料为ZnS纳米颗粒包覆Ag纳米线的核壳结构,其紫外吸收峰位于350 nm处,相对于ZnS纳米颗粒变宽并发生红移,PL发射峰位于462 nm处,相对于ZnS纳米颗粒发生了蓝移,强度明显降低.光催化结果显示,Ag/ZnS核壳结构纳米棒的光催化性能优于ZnS纳米颗粒,分析了光催化反应机理.     

ZnS空心微球的制备及其光催化性能研究

采用简单的一步溶剂热法合成了ZnS空心微球.利用X射线衍射(XRD)、扫描电子显微镜(SEM)、高分辨透射电子显微镜(HRTEM)、X射线光电子能谱(XPS)和紫外可见吸收光谱(UV-vis)等测试手段对其形貌、结构和光学性质进行了分析,并以罗丹明B(RhB)为模型污染物研究了样品的光催化性能.结果表明:样品为纯度较高的立方闪锌矿型ZnS微球,且球体由纳米级小微粒组装而成;在降解RhB的光催化研究中,以乙醇-水为溶剂合成的ZnS微球光催化性能较优.     

Al3+掺杂ZnS纳米晶的合成、表征及其光催化性能

在较温和的溶剂热条件下制备了一系列Al3+掺杂的ZnS纳米晶光催化剂.利用N2物理吸附、扫描电镜(SEM)、X射线衍射(XRD)、紫外可见漫反射光谱(UV-vis DRS)、红外光谱(FT-IR)和光致发光(PL)谱等技术对合成的样品进行了表征.考察了不同含量的Al3掺杂对ZnS的结晶度、比表面积、表面羟基、光吸收性能及其对不同染料的光催化降解性能的影响.结果表明,在140℃下合成的球状ZnS纳米晶具有较好的结晶度;Al3+掺杂在增加催化剂的比表面积的同时丰富了催化剂的表面羟基;此外,掺杂的Al3+可以明显抑制光生电子(e-)和空穴(h+)的复合,提高光催化反应效率.当掺杂最佳含量的6mol; Al时,可使催化剂光催化降解染料酸性橙Ⅱ、亚甲基蓝和罗丹明B的降解率分别提高3.5、1.0和0.9倍.     

声化学法制备ZnS: Mn纳米晶及其光学性能

以无水氯化锌,四水氯化锰以及硫代乙酰胺为原料,采用声化学法成功制备了锰掺杂的ZnS(ZnS: Mn)纳米晶.采用透射电子显微镜镜(TEM)、X射线能谱仪(EDS)、X射线粉末衍射(XRD)和光致发光谱(PL)对所制得的纳米进行了表征.结果表明:所制备ZnS: Mn为立方闪锌矿结构,纳米粒子的形貌接近于球形.平均晶粒尺寸为10 nm左右.PL光谱分析表明:所制备试样有两个主要的发射峰,分别位于在480 nm和570 nm左右,后者与体材料ZnS: Mn相比发生了明显蓝移,但仍表现为橙黄色发光.Mn2+掺杂浓度对ZnS: Mn的光致发光性能有显著影响,原料中Zn: Mn: S(物质的量比)为3: 1: 4,Mn2+掺杂浓度为2.64 at;时,光致发光光谱发射峰强度达到最大值.     

ZnS/g-C3N4复合型催化剂的制备及其可见光光催化性能

利用共沉淀的方法制备了ZnS/g-C3N4复合型催化剂,并考察其在可见光区对罗丹明B的光降解性能的影响机制.采用TEM、BET、XRD、ICP、FT-IR和XPS等分析手段表征了样品,并评价了样品的光催化活性.结果表明,与g-C3N4相比,ZnS负载量为5wt;的ZnS/g-C3N4催化剂活性会更高一些,且经过四次循环实验后样品的光催化性能未明显失活.这可能归因于ZnS和g-C3N4所形成的异质结构提高了光催化效率.     

氧化锌空心球的制备及其光催化性能研究

以葡萄糖、尿素和醋酸锌为原料在低温下合成了炭微球,高温煅烧后制备了氧化锌空心微球.通过X-射线衍射(XRD)、扫描电子显微镜(SEM)等手段对制得的样品进行了表征.以甲基橙溶液为研究对象考察了氧化锌空心微球的光催化性能.实验结果表明,当葡萄糖和醋酸锌质量比为3∶1时,制备的ZnO微球具有较好的光催化性能.     

用化学气相沉积(CVD)法制备硫化锌(ZnS)体块材料中晶体缺陷和生长工艺的研究

本文报道了用化学气相沉积(CVD)法制备高质量红外光学体块材料硫化锌(ZnS)的制备工艺,研究了晶体缺陷对其光学性能的影响.XRD,XEM及IR表明,采用优化的沉积工艺和热等静压后处理,减少晶体中杂质、微孔、六方结构ZnS及Zn-H键的形成,使生长的CVD ZnS具有高的红外透过率,提高了材料的光学品质.     

ZnS/镍锌铁氧体磁性光催化剂的制备与光催化活性

采用共沉淀法制备了镍锌铁氧体,并用氨水、乙二胺四乙酸进行表面改性;然后以醋酸锌、硫代乙酰胺和表面改性的镍锌铁氧体为原料,采用超声化学法制备了ZnS/镍锌铁氧体的复合粉体.采用X射线粉末衍射(XRD),高分辨透射电子显微镜(HRTEM)以及所带能谱仪(EDS)对所制得的样品进行了表征,并以太阳光为光源,甲基橙为目标降解物,对其光催化活性进行了研究.结果表明:镍锌铁氧体负载的ZnS为立方闪锌矿结构,单个ZnS颗粒尺寸分布在15 ～25 nm之间;ZnS/镍锌铁氧体复合粉体在可见光下具有一定的光催化活性,且具有磁性能可实现磁分离回收.     

TiO2/ZnO复合微球的制备及其光催化性能研究

以碳微球为模板,采用溶胶凝胶法、水热法等方法分别制备了TiO2微球、ZnO微球和TiO2/ZnO复合微球,采用扫描电子显微镜、X-射线衍射仪等对样品进行了表征,结果表明:制备的TiO2微球、ZnO微球和TiO2/ZnO复合微球,各微球直径在5 ～ 10 μm之间.在紫外光和可见光下研究了制备的光催化剂对亚甲基蓝溶液和湖水的光催化性能,光催化实验表明:三种微球中TiO2/ZnO复合微球具有良好的光催化性能.     

反相微乳液法制备CdS/ZnS纳米晶及其表征

用反相微乳液法制备了CdS纳米粒子,以ZnS对其表面进行包裹,得到了核壳结构的CdS/ZnS纳米晶.采用X射线衍射(XRD)、透射电镜(TEM)表征其结构、粒度和形貌,紫外-可见吸收光谱(UV-VIS)、光致发光光谱(PL)表征其光学特性.制得的CdS纳米微粒近似呈球形,直径约3.6nm;包裹以后颗粒仍为球形,粒径约10nm,以XRD、UV-VIS和PL证实了CdS/ZnS核壳结构的实现.文章还研究了不同Zn/Cd的摩尔比对CdS/ZnS纳米微粒光学性能的影响,UV-VIS谱表明随着壳层厚度的增加CdS/ZnS纳米晶的吸收带边有轻微的红移;PL谱表明壳层ZnS的包覆可减少CdS纳米微粒的表面缺陷,带边直接复合发光几率增大,且具有合适的壳层厚度时,CdS核层的发光效率有较大提高.     

Homoepitaxial growth and photoluminescence of self‐assembled In‐doped ZnS nanowire bundles

Self‐assembled In (Indium)‐doped ZnS nanowire bundles were synthesized via a thermal evaporation method without using any template. Vapor ‐ solid homoepitaxial growth was found to be the key reason for the formation of close‐packed nanowire bundles grown on the surface of microscale sphere‐shaped ZnS crystal. X‐ray diffraction (XRD), selected area electron diffraction (SAED), and transmission electron microscopy (TEM) analysis demonstrate that the In‐doped ZnS nanowires have the cubic structure, and there are numerous stacking faults along the <111> direction. Photoluminescence (PL) spectrum shows that the spectrum mainly includes two parts: a weak violet emission band centering at about 380 nm and a strong green emission band centering at about 510 nm. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

溶剂热法制备双螺旋ZnS纳米结构研究

采用溶剂热法以醋酸锌和硫化钠反应成功制备了具有双螺旋结构的一维ZnS纳米棒,利用X射线衍射(XRD)、高分辨透射电子显微镜(HRTEM)、选区电子衍射(SAED)、X射线能量色散分析谱仪(XEDS)、紫外吸收光谱(UV-vis)和光致发光谱(PL)等测试手段对样品的化学成分、形貌、晶体结构和光学性质等进行了表征分析.实验结果表明样品为一维六方纳米晶结构,沿着[001]方向生长,并具有双螺旋结构,长度分布在100～200 nm范围,直径约为5 ～15 nm,螺距约为20 nm.双螺旋ZnS纳米结构的吸收峰与块体材料相比发生了蓝移.     

表面活性剂对水热法合成ZnS:Cu,Al纳米晶光致发光特性的影响

采用水热法直接合成了ZnS∶Cu,Al纳米荧光粉,并且系统研究了加入表面活性剂在不同S/Zn下,清洗样品和不清洗样品的结晶性、傅立叶红外光谱(FT-IR)及光致发光(PL)光谱.XRD和TEM测试结果表明:合成纳米晶为纯立方相结构,球形纳米晶尺寸约15 nm, 尺寸分布窄,分散性好.未清洗样品的结晶性比清洗样品的好,且加入表面活性剂和未清洗都导致粒径增大,影响纳米材料的表面态.改变[S~(2-)]/[Zn~(2+)]物质的量比、清洗和加入表面活性剂都会影响材料的PL强度.这说明其发光机理为紫外光激发材料表面的发光中心,即PL强度决定于纳米材料的表面态.     

Self‐template hydrothermal synthesis ZnS microspheres

Zinc sulfide (ZnS) microspheres were synthesized by a self‐template hydrothermal route using thiourea as sulphur source. The formation of these hollow spheres was mainly attributed to the oriented aggregation of ZnS nanocystals around the gas‐liquid interface between gas (H₂S, NH₃, or CO₂) and water followed by an Ostwald ripening process. The gas bubbles of H₂S, NH₃, or CO₂ produced during the reaction might play a soft‐template to form ZnS hollow microspheres. The products were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), electron diffraction (ED), and photoluminescence (PL). The crystal structure of prepared ZnS microspheres is hexagonal phase polycrystalline. The average microspheres diameter is 1.5 ‐ 6 µm. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

微乳液法制备二氧化硅包覆ZnS:Mn/CdS纳米晶

采用微乳液法制备核壳结构ZnS:Mn/CdS(～4.5nm)纳米晶,为获得水溶性纳米晶,继续向此微乳液添加硅酸乙酯(TEOS),并使用氨水作为催化剂,通过TEOS水解缩聚反应,在ZnS:Mn/CdS粒子表面生长连续的二氧化硅壳层.采用透射电子显微镜(TEM)、X射线衍射(XRD)、红外光谱(IR)、光致发光谱(PL)对其表面形貌、结构和光学特性进行表征.ZnS:Mn /CdS纳米粒子表面被二氧化硅壳层完全包覆,粒径大小约为10nm左右,粒子均匀性好.由于二氧化硅相无定形且透光性良好,二氧化硅包覆ZnS:Mn/CdS纳米晶的光学特性与未包覆的ZnS:Mn/CdS极其相似.     

High intense UV-luminescence of nanocrystalline ZnO thin films prepared by thermal oxidation of ZnS thin films

High quality zinc oxide (ZnO) films were obtained by thermal oxidation of high quality ZnS films. The ZnS films were deposited on a Si substrate by a low-pressure metalorganic chemical vapor deposition technique. X-ray diffraction spectra indicate that high quality ZnO films possessing a polycrystalline hexagonal wurtzite structure with preferred orientation of (0 0 2) were obtained. A fourth order LO Raman scattering was observed in the films. In photoluminescence (PL) measurements, a strong PL with a full-width at half-maximum of 10 nm around 380 nm was obtained for the samples annealed at 900°C at room temperature. The maximum PL intensity ratio of the UV emission to the deep-level emission is 28 at room temperature, providing evidence of the high quality of the nanocrystalline ZnO films.     

ITO玻璃衬底上生长的Zn0.9Mg0.1S多晶薄膜特性研究

以ZnS和Mg粉末为原料,采用真空蒸镀技术在ITO玻璃上成功地制备了宽禁带三元化合物Zn0.9Mg0.1S多晶薄膜.原子力显微镜和X射线衍射研究表明:薄膜生长形貌和结晶性能良好,为择优取向的立方闪锌矿结构,晶粒直径约20nm,薄膜的X射线衍射峰较之ZnS的衍射峰向大角度方向移动了0.46°;室温下的拉曼谱峰相对于ZnS的拉曼谱峰出现蓝移,且347.67cm-1谱峰比较强;光致发光谱显示,Zn0.9Mg0.1S薄膜在410nm处有一个较强的发光峰.良好的结晶质量和发光特性为开发多功能材料和器件提供了可能性.     

Structural,optical and photoluminescence properties of ZnS: Cu nanoparticle thin films as a function of dopant concentration and quantum confinement effect

Thin films of ZnS: Cu nanoparticles were deposited in chemical bath by a pH controlled solution synthesis technique. The copper concentration was varied from 0 to 0.1M%. XRD and SEM indicated variations in diffracted intensity and morphology with Cu concentration. The PL spectrum of the undoped ZnS nanoparticles showed emission peaks at 393 and 432nm that could be attributed to the intrinsic defect states of ZnS nanoparticles. For ZnS: Cu samples three peaks in the range of 390nm, 480nm and 525nm were observed. With increase in Cu concentration from 0.001 to 0.1M%, the peak position of 480nm and 525nm did not change, whereas 390nm peak red shifted to longer wavelength region to 422nm. In addition, it was found that the overall photoluminescence intensity reached maximum at 0.01M% and quenched with further increase in Cu concentration. Enhancement of blue and green light emission by seven and twenty fivefold respectively compared to undoped ZnS was observed in ZnS: Cu with optimal dopant concentration. Time resolved decay of photoluminescence showed faster decay for 390 – 420nm purple/ blue emission compared to green (525nm) Cu related emission which is in the microsecond time scale. Optical absorption measurements indicate enhancement of band gap (3.89eV) for undoped ZnS suggesting the quantum confinement effect in the developed nanoparticles of size below the Bohr diameter. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation,structure and photoluminescence properties of SiO2–coated ZnS nanowires

It is essential to passivate one‐dimensional (1D) nanostructures with insulating materials to avoid crosstalking as well as to protect them from contamination and oxidation. The structure and influence of thermal annealing on the photoluminescence properties of ZnS‐core/SiO₂‐shell nanowires synthesized by the thermal evaporation of ZnS powders followed by the sputter deposition of SiO₂ were investigated. Transmission electron microscopy and X‐ray diffraction analyses revealed that the cores and shells of the core‐shell nanowires were single crystal zinc blende‐type ZnO and amorphous SiO₂, respectively. Photoluminescence (PL) measurement showed that the core‐shell nanowires had a green emission band centered at around 525 nm with a shoulder at around 385 nm. The PL emission of the core‐shell nanowires was enhanced in intensity by annealing in an oxidative atmosphere and further enhanced by subsequently annealing in a reducing atmosphere. Also the origin of the enhancement of the green emission by annealing is discussed based on the energy‐dispersive X‐ray spectroscopy analysis results. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)