亚稳态MInS2(M=Ag，Cu)花状微米球的热分解法合成及其生长机理

采用热分解法制备了三维的亚稳态正交相AgInS₂和六方相CuInS₂花状微米球。通过X射线衍射（XRD）,场发射扫描电子显微镜（FESEM）等对样品进行表征,对AgInS₂的光催化性能进行了评估,并借助于热重分析（TG-DTA）等手段研究了亚稳态正交相AgInS₂和六方相CuInS₂花状微米球的生长机理。实验结果表明,反应温度和反应物中金属离子的投料比对生成纯相的MInS₂均有影响,而AgInS₂花状微米球能在可见光下较好地催化降解亚甲基蓝。     

MnS纳米线阵列上MnS花状球的水热合成

通过水热处理的方法,在氧化铝模板表面生成的MnS纳米线阵列上合成了六方相MnS花状球。利用场发射扫描电镜,透射电子显微镜,高分辨透射电子显微镜,选区电子衍射和X射线衍射对制备的样品进行了分析与表征。结果表明MnS花状球是在MnS纳米线阵列上生长的,纳米线的直径为70～80nm,与氧化铝模板的孔径一致且结晶性较好。随着阳极氧化氧化铝模板(AAO)的孔洞长度的减少,MnS花状球的数量快速增加。提出了MnS复合纳米结构可能的生长机制:氧化铝模板和反应中硫脲分解产生的H2S气体对产物的最终形貌有很重要的影响。室温光致发光光谱显示在420nm处存在一个很强的MnS带边发射峰。     

三维花状Fe2（MoO4）3微米球的水热制备及电化学性能

以FeCl₃·7H₂O和Na₂MoO₄为原料,采用水热合成法制备三维花状Fe₂（MoO₄）₃微米球。探讨不同合成温度对样品形貌的影响,利用XRD、SEM和EDS等分析技术对样品的结构、形貌进行了表征,对该材料的电化学性能进行了测试。结果表明：Fe₂（MoO₄）₃微米球是由二维纳米片自组装而成的花状结构,合成温度为160℃时,制备的样品具有良好的电化学性能,当电流密度为100mA·g^-1,首次放电比容量为1431mAh·g^-1;并具有较好的循环性能和倍率性能。并对160℃合成样品表现较好电化学性能的原因进行了探讨。     

自组装α-Fe2O3亚微米球的制备及其光催化性质

在乙二醇体系中, 通过简单的二步方法成功合成了α-Fe₂O₃亚微米球。第一步,以Fe(NO)₃和C₆H₁₂N₄为主要反应物160 ℃溶剂热反应8h制备出前驱体;第二步,煅烧前驱体成功合成了斜方相的α-Fe₂O₃产物。利用X射线粉末衍射(XRD),扫描电子显微镜(SEM),透射电子显微镜(TEM),红外吸收光谱(FTIR),能谱分析(EDS)和热重分析(TGA)等手段对产物进行了表征。在300 W紫外灯(主波长为365 nm)照射下降解一定浓度的甲基橙溶液,研究不同光催化剂对甲基橙溶液降解效果。由于制备产物的形貌和粒径影响其比表面积和对反应物的吸附能力以及带隙能,使得制备产物具有良好的光催化性能。结果表明,α-Fe₂O₃亚微米球在紫外光照射条件下对甲基橙溶液有光降解作用。     

三维花状Fe_2(MoO_4)_3微米球的水热制备及电化学性能

以Fe Cl3·7H2O和Na2Mo O4为原料,采用水热合成法制备三维花状Fe2(Mo O4)3微米球。探讨不同合成温度对样品形貌的影响,利用XRD、SEM和EDS等分析技术对样品的结构、形貌进行了表征,对该材料的电化学性能进行了测试。结果表明:Fe2(Mo O4)3微米球是由二维纳米片自组装而成的花状结构,合成温度为160℃时,制备的样品具有良好的电化学性能,当电流密度为100 m A·g-1,首次放电比容量为1 431 m Ah·g-1;并具有较好的循环性能和倍率性能。并对160℃合成样品表现较好电化学性能的原因进行了探讨。     

共沉淀法制备六方相ITO纳米粉体及其光电性能

以金属In、SnCl_4·5H_2O为原料、尿素为沉淀剂,采用共沉淀法加入(NH_4)_2SO_4,制备出六方相ITO纳米粉体。通过XRD、TEM、四探针电阻仪、荧光光谱仪以及XPS,研究了ITO粉体的晶型、颗粒形貌、电性能以及光性能。结果表明:加入(NH_4)_2SO_4后,ITO粉体形貌由类菱面体和类球形混合体转变为类球形;不加(NH_4)_2SO_4时晶型为立方相结构,当(NH_4)_2SO_4与铟的物质的量之比为1∶3.45和1∶1.73时粉体晶型转变为六方相结构,继续添加(NH_4)_2SO_4晶型又转变为立方相结构。立方相ITO粉体的电阻率较低为0.64Ω·cm,六方相ITO粉体在相同激发波长下,发射光强度相对较高。     

WO3/TiO2 复合纤维的制备及储能光催化性能

以钛酸正丁酯为前驱体, 采用静电纺丝技术制得了纯锐钛矿TiO2纤维, 并以其为基质, 通过水热法制备了具有异质结构的WO3/TiO2复合纤维. 利用X射线衍射仪(XRD)、 扫描电子显微镜(SEM)、 能量色散光谱仪(EDS)、 透射电子显微镜(TEM)和高分辨透射电子显微镜(HRTEM)等对样品的结构和形貌进行了表征. 以罗丹明B的脱色降解为模型反应, 考察了样品的光催化性能和储能光催化性能. 结果表明, 花状WO3微球包裹在TiO2纤维上, 得到了具有异质结构的WO3/TiO2复合纤维光催化剂. WO3与TiO2复合有利于光生载流子的输运和分离, 增强了体系的量子效率, 提高了光催化活性. WO3/TiO2 复合纤维经光照处理后, 在黑暗条件下显示出储能光催化特性.     

NiO纳米片和多孔纳米片自组装的空心微球的无模板水热法制备与磁学性质

报道一种非常简单的制备NiO和Ni(OH)₂空心微球的无模板水热法, 即通过NiCl₂与氨水在140 ℃水热反应12 h, 制备了Ni(OH)₂纳米片自组装的空心微球, 经400 ℃热处理2 h得到了NiO空心微球. 采用X射线衍射仪、扫描电镜和透射电子显微镜对产物进行表征, 并在室温下测试了它的磁学性能, 结果表明, Ni(OH)₂空心微球的直径约为3～4 μm, 它是由尺寸1.1～1.3 μm左右的六方相结构的Ni(OH)₂纳米片组装而成; NiO空心微球是由立方相纳米片和多孔纳米片组装而成, 它具有弱的铁磁性, 其矫顽力为583 Oe, 剩余磁化强度为0.213 emu/g. 研究了氨在Ni(OH)₂纳米片的形成与组装过程中的作用, 提出了可能的生长机理.     

乙二胺四乙酸辅助水热法合成NaYF_4纳米晶

用络合剂乙二胺四乙酸(EDTA)辅助水热法合成了NaYF4纳米球和微米棱柱,通过控制反应条件得到了立方相和六方相纳米晶体;采用X射线粉末衍射仪(XRD)、扫描电子显微镜(SEM)及荧光光谱仪(PL)分析了产物的结构、形貌及发光性能.结果表明,络合剂EDTA和氟化物的物质的量对NaYF4的形貌和粒度有很大影响,且产物的荧光性能呈现出尺寸依赖性.     

TiO2纳米微球的制备及在染料敏化太阳能电池中的应用

以四氯化钛、盐酸为原料,制备出花状TiO_2纳米微球,利用扫描电子显微镜(SEM)、X射线衍射(XRD)等测试方法,对样品的结构和形貌进行了表征。为了提高TiO_2微球电池的光电性能,利用TiO_2微球作为反射层构造了双层结构的薄膜电极,结果表明,双层结构染料敏化太阳能电池在100 m W·cm-2(1.5 G)光照条件下,短路光电流Jsc=17.64 m A·cm-2,开路光电压Voc=0.74 V,填充因子FF=0.63和光电转化效率η=8.33%。相比TiO_2微球制备的太阳能电池,双层结构染料敏化太阳能电池光电转化效率提高至5.3倍。最后对电极中染料的吸附量、电极的光散射性能和电池的电化学阻抗做了进一步研究和分析,研究表明,双层结构电池增强光的捕获能力,从而提高光伏性能。     

AgInS2纳米粒子的制备及其可见光催化活性

以水为溶剂,硫代乙酰胺为硫源,巯基乙酸为包覆剂,于低温下制备了正交相的AgInS2纳米粒子。用TEM、EDS和XRD对所制备的AgInS2纳米粒子的形貌、组成和晶相进行了表征。并考察了反应时间对AgInS2纳米粒子的晶相及其可见光催化降解活性的影响。结果表明:延长反应时间可以提高AgInS2纳米粒子的结晶性和可见光催化活性。     

Growth of CuInS2 Nanotubes from Cu2S-CuInS2 Heterostructures as a Potential Photovoltaic Material

Chemically synthesized nanostructures possess well-defined domains with an interconnected network, which helps the carriers to bypass the other material in the solar cell while moving to their respective electrodes. In this work, CuInS₂ films constituting CuInS₂ nanotubes and nanoparticles were fabricated using a hot-injection chemical technique, followed by sulfurization. Structural and microstructural investigations reveal Cu₂S nanoparticle formation at an early stage of growth of nanotubes, serving as possible catalyst sites for the subsequent anisotropic growth of the heterostructured hexagons. The crossover takes place over a number of intermediate stages. This sharing of the heterostructure by the hexagonal Cu₂S and chalcopyrite CuInS₂ minimizes the lattice distortion. The Cu₂S- CuInS₂ interface in the heterostructure acts as the nucleation center for CuInS₂ nanotubes. Optical absorption and Raman spectroscopy studies reveal better optical properties for CuInS₂ nanoparticles as compared to CuInS₂ nanotubes. Compared to all other nanostructures, nanowires or nanotubes tend to provide single-crystalline nanograins for direct characterization. These nanoparticles, especially the nanotubes, can be used to form an interconnected network structure of p- and n-type materials in bulk heterojunctions providing the key to improve solar cell efficiencies.     

Synthesis of CuInS2@CdS Core‐Shell Nanocrystals

CuInS₂@CdS core‐shell nanocrystals were prepared in a wet chemical process. Transmission electron microscope (TEM), x‐ray energy dispersive spectroscopy (EDAX), x‐ray diffraction (XRD), absorption, and photoluminescence (PL) spectra were used to confirm the formation of the CuInS₂@CdS core‐shell structure. The growth of CdS shell not only increased the PL intensity, but also restrained the transformation of CuInS₂ from nanoparticles to nanorods after annealing, which was attributed to an effective chemical passivation of the CuInS₂ core by the CdS shell.     

Synthesis of CuInS2 Nanocubes by a Wet Chemical Process

Cube‐shaped CuInS₂ nanoparticles were successfully prepared through a simple low‐temperature solution route. Mercaptoacetic acid was used as capping agent. The product was characterized by means of X‐ray diffraction (XRD), energy dispersive analysis of X‐rays (EDAX), transmission electron microscopy (TEM), and photoluminescence spectroscopy (PL). The CuInS₂ nanocubes obtained were of a chalcopyrite structure. The EDAX analysis shows that as‐synthesized CuInS₂ nanocubes were slightly Cu‐rich and nearly stoichiometric.     

TiO2 nanoparticles incorporated with CuInS2 clusters: preparation and photocatalytic activity for degradation of 4-nitrophenol

TiO₂ nanoparticles incorporated with CuInS₂ clusters were prepared in a solvothermal process and characterized with X-ray diffraction (XRD), transmission electron microscopy (TEM), and energy-dispersion X-ray analysis (EDX). Compared with pure TiO₂ nanoparticles, the TiO₂ nanoparticles incorporated with CuInS₂ clusters display higher photocatalytic activity with 99.9% of degradation ratio of 4-nitrophenol after 2 h irradiation. In order to investigate the effect of the CuInS₂ clusters on the photocatalytic activity of TiO₂ nanoparticles, diffuse reflectance UV–Vis spectra (DRS), photoluminescence (PL) spectra, and photocurrent action spectra were measured. The results indicate that the enhanced photocatalytic activity is probably due to the interface between TiO₂ and CuInS₂ as a trap of the photogenerated electrons to decrease the recombination of electrons and holes.     

SILAR法制备化学计量CuInS2薄膜

在室温下，以不同c_Cu/c_In的CuCl₂和InCl₃混合溶液作为阳离子前驱体，Na₂S水溶液为硫源，利用连续离子层吸附反应法(SILAR)在玻璃基底上制备了CuInS₂薄膜。XRD结果表明，当c_Cu²⁺/c_In³⁺在1～1.5范围内均可形成具有黄铜矿结构的CuInS₂薄膜。SEM观察到随c_Cu²⁺/c_In³⁺的升高，薄膜表面颗粒长大并出现团簇聚集。通过XPS测定薄膜表面的化学组成证明当c_Cu²⁺/c_In³⁺=1.25时，CuInS₂薄膜接近其标准的化学计量组成。此时薄膜的吸收系数大于>10⁴ cm^-1，禁带宽度E_g为1.45 eV。     

Formation of Rod-Like CuInS2 Nanocrystals on the Glass Substrate

Rod-like CuInS₂ nanocrystals on the glass substrate were prepared by annealing the coat of CuInS₂ nanoparticles. The products were characterized by means of energy dispersive analysis of x-ray (EDAX), x-ray diffraction (XRD) and scanning electron microscopy (SEM). The results of XRD and EDAX show that the rod-like CuInS₂ nanocrystals obtained are of a chalcopyrite structure and are nearly stoichiometric. The aggregation mechanism of “oriented attachment” of nanocrystals is believed to be operative and compatible in this study.     

Alloyed (ZnS)x(CuInS2)1−x Semiconductor Nanorods: Synthesis,Bandgap Tuning and Photocatalytic Properties

Rod-like nanocrystals of the semiconductor alloy (ZnS)_x(CuInS₂)_1−x (ZCIS) have been colloidally prepared by using a one-pot non-injection-based synthetic strategy. The ZCIS nanorods crystallize in the hexagonal wurtzite structure and display preferential growth in the direction of the c axis. The bandgap of these quarternary alloyed nanorods can be conveniently tuned by varying the ratio of ZnS to CuInS₂. A non-linear relationship between the bandgap and the alloy composition is observed. The ZCIS nanorods are found to exhibit promising photocatalytic behaviour in visible-light-driven degradation of Rhodamine B.     

油溶性CuInS2/ZnS量子点的制备及其温敏性聚丙烯酰胺胶束介导的水相转移

采用非热注法成功制备了高质量的油溶性CuInS₂/ZnS核壳量子点, 量子点的荧光发射峰在可见光到近红外范围内可调(550~800 nm), 且荧光量子产率最高达80%。本文进一步利用具有温敏特性的聚丙烯酰胺胶束作相转移剂, 成功地将油溶性的CuInS₂/ZnS核壳量子点转移入水相。水相中自组装形成的CuInS₂/ZnS量子点-胶束复合物不仅具有良好的荧光性质, 而且胶束原有的灵敏的热响应性被保留。这些研究初步表明, 无镉的低毒的CuInS₂/ZnS量子点可作为纳米胶束的荧光示踪探针。