银催化合成Tb(BO2)3纳米棒

采用固相反应银作催化剂成功合成出棒状结构的稀土硼酸盐Tb(BO₂)₃发光材料. 利用X射线衍射和区域电子衍射研究了产物的结构特性,在700 oC煅烧时,Tb(BO₂)₃纳米棒具有良好晶形. 透射电镜分析表明,Tb(BO₂)₃纳米棒直径为100～200 nm,厚度为30～50 nm,长约3 μm. 基于Ag纳米颗粒附在Tb(BO₂)₃纳米棒的顶端和中部的事实,探讨了Tb(BO₂)₃纳米棒的生长机理. 荧光光谱研究表明,在369 nm紫外光激发下,Tb(BO₂)₃能发出Tb³⁺的特征绿色荧光,发射主峰位于546 nm,归属于⁵D₄→⁷F₅跃迁. 同时,也探讨了煅烧温度对产物的结构、形貌以及发光性质的影响.     

从可溶性单源分子前驱体采用溶胶凝胶法制备ZnO/TiO2 纳米复合物

合成了单源分子前驱体Cl₂TiZn(dmae)₄ (dmae为2-二甲基乙醇胺),并以乙醇为溶剂,加入等摩尔量的水对其进行可控水解得ZnO/TiO₂纳米复合凝胶,经pH=9沉淀,在200、400和600 oC 烧结得到不同的产物T₂₀₀、T₄₀₀、T₆₀₀. XRD分析表明未烧结产物为无定形粉末并随着烧结温度升高晶型改善. ZnO呈纤锌矿结构(六方晶系),TiO₂呈板钛矿型结构(正交). BET分析和扫描电镜表明颗粒的大小随着烧结温度的提高而增加. 红外光谱证明Zn-O和Ti-O的特有的振动频率,OH基团烧结后的产物中被去掉. 所有的样品都显示良好的光催化活性, 且T₆₀₀活性最高.     

溶剂热合成法制备的Zn1-xMnxO和Zn1-2xMnxLixO纳米材料的磁学性质

用溶剂热合成法在160oC制备出Zn_1-xMn_xO纳米棒和Zn_1-2xMn_xLi_xO纳米颗粒. XRD和拉曼测试结果表明Mn离子已很好地掺入ZnO母体中. M-H图中未观察到磁回滞,ESR谱中的精细结构说明掺杂的Mn离子间没有铁磁相互作用. 共掺Li仅仅改变了产物的形貌,并不能改变其磁学性质.     

二氧化钛纳米晶/石墨烯复合物的制备及其光催化性能 (cited: 1)

以氧化石墨和TiO₂溶胶为前驱物,结合絮凝与水热技术制备了TiO₂纳米晶/石墨烯复合物,表征了产物的结构、形貌、孔隙率、光谱吸收性质. 结果表明：TiO₂纳米晶的存在一定程度上阻止了石墨烯片层的重组,TiO₂纳米晶/石墨烯复合物较单纯TiO₂材料具有更强的吸光性能、对亚甲基蓝分子更强的吸附性能以及更高的电荷分离效率. 在紫外光和太阳光下,TiO₂纳米晶/石墨烯复合物对亚甲基蓝的光催化降解效率均高于P25和纯TiO₂.     

钼酸根离子钝化层对氧化铁薄膜光电催化氧化水的性能影响研究

本文研究了氧化铁(α-Fe₂O₃)薄膜光阳极的合成及其光电催化分解水产氧的性能. 在合成氧化铁过程中,采用原位和非原位方式引入钼酸根离子,调控氧化铁薄膜的生长模式和表面特性. 实验发现原位引入钼酸根离子会显著影响氧化铁薄膜的形貌以及厚度. 而非原位表面修饰钼酸根离子则会保持氧化铁的纳米棒形貌,并有效提高其光电催化分解水的性能. 文章通过紫外-可见吸收光谱,透射电子显微镜(TEM),扫描电子显微镜(SEM),莫特-肖特基测试(M-S),电化学阻抗(EIS)以及光电催化性能测试等手段对材料的结构和性能进行了研究.     

二氧化钒纳米棒的相变行为

研究了VO₂(M)纳米棒的金属绝缘体相变(MIT)行为．在VO₂(M)纳米棒的DSC分析曲线上发现了两个MIT,分别位于低温和高温区．低温MIT总是伴随出现VO₂(B)纳米棒,而独立的高温MIT出现在纯VO₂(M)纳米棒．分析和讨论了这两个MIT的机制．     

Gd2O3:Eu3+纳米晶的燃烧合成及光致发光性质

采用柠檬酸作燃烧剂用燃烧合成法制备了Gd₂O₃:Eu³⁺纳米晶.用X射线衍射仪(XRD)、高分辨透射电子显微镜(HRTEM)和荧光分光光度计等对Gd₂O₃:Eu³⁺纳米晶的结构、形貌和发光性能进行了分析.结果表明：不同柠檬酸与稀土离子配比(C/M)制备的样品经800℃ 退火1 h后，均得到了纯立方相的Gd₂O₃:Eu³⁺纳米晶，晶粒尺寸约为30 nm，尺寸分布较窄，其中以C/M=1.0时制备的纳米晶结晶性最好，发光强度最大.Gd₂O₃:Eu³⁺纳米晶主发射峰位置均在612 nm处 (⁵D₀→⁷F₂跃迁)，激发光谱中电荷迁移态发生红移，观察到Gd³⁺向Eu³⁺的有效能量传递.对柠檬酸与稀土离子配比(C/M)对结晶度、发光性质等的影响也进行了分析和讨论.     

La2Zr2O7:Eu3+纳米棒的合成、表征及其荧光性能

采用传统固相法和水热法成功地制备出棒状La₂Zr₂O₇:Eu³⁺荧光粉. 利用X射线粉末衍射仪、透射电镜和荧光光谱仪等分析了产物的结构、形貌和发光特性. 结果表明红色荧光粉La₂Zr₂O₇:Eu³⁺有良好的晶相,属于立方结构,空间点群为Fd3m; 其形貌主要为纳米棒, 平均直径约47 nm, 长度为50～700 nm. 并对纳米棒的生长机理进行了探讨. 在466 nm蓝光激发下,La₂Zr₂O₇:Eu³⁺荧光粉能发射出Eu³⁺的特征红色荧光,发射主峰位于616 nm处,归属于Eu³⁺的⁵DO_→⁷F2_{超灵敏电偶极跃迁.此外,在产物的发射光谱中能够观察到⁵D}1_→⁷FJ _{(J=0, 1, 2)跃迁和⁵D}1_→⁷FJ _{(J=1, 2, 4)跃迁的劈裂峰,这说明Eu³⁺处在低对称性的晶体场格位中.}     

锂离子正极材料正交相γ-LiV2O5的制备及性能

分别采用LiOH·H₂O, NH₄VO₃, HNO₃, C₂H₅OH作为原料在没有PVP和有PVP存在下合成了棒状和棒束状两种相貌的γ-LiV₂O₅. 棒状γ-LiV₂O₅材料中棒的直径为500～800 nm,而棒束状的γ-LiV₂O₅材料则是直径为100～600 nm的棒组成的,形貌比较均匀. 同时研究了此体系中γ-LiV₂O₅的合成机制. 将合成的材料进行电化学测试,棒束状的γ-LiV₂O₅ 的电化学性能更好,在电流密度为30 mA/g时的初始放电比容量为269.3 mAh/g,循环20次之后容量仍保持在228 mAh/g.     

苝四甲酸二酐有机单晶纳米结构的制备及形成机理的研究

在分子束外延(MBE)系统中, 利用物理气相沉积(PVD)的方法在阳极氧化铝(AAO)模板上制备了有机 染料分子苝四甲酸二酐(PTCDA)的不同纳米结构; 并使用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、 高分辨透射电子显微镜(HRTEM)以及选区电子衍射(SAED)技术进行了系统的研究. 结果发现, 当衬底温度(T_s)为330 ℃时得到的是纳米丝、针、带以及棒; T_s为280 ℃, 230 ℃, 180 ℃时得到的主要是纳米棒, 并且纳米棒的长度随T_s的降低而变短; T_s为50 ℃时只能得到连续的PTCDA薄膜. HRTEM以及SAED结果证实了纳米针与棒为单晶. 依据SEM结果, 提出纳米结构的生成主要受T_s以及衬底表面曲率的影响.     

Synthesis of CdS hollow/solid nanospheres and their chain-structures by membrane technique

CdS hollow/solid nanospheres and their chain-structures were successfully synthesized through supporting liquid membrane (SLM) system with bio-membrane. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), UV–Vis spectroscopy, and photoluminescence (PL) spectroscopy have been used for the characterization of the products. The average diameters of CdS solid/hollow spheres are about 10, 40 nm, respectively. The wall of the hollow spheres is about 5 nm. CdS products are all cubic face-centered structure with the cell constant a = 5.830 Å. We also explore the morphology, structure and possible synthesis mechanism. A possible template mechanism has been proposed for the production of the hollow CdS nanocrystals, that is, CdS nanoparticles grow along the non-soakage interface between CHCl3 and reactant solution. During this process, the organic functional groups were crucial to the control of crystal morphologies.     

醇溶剂粘度对N,N′-(2,4-二氯苯基)硫脲/CdS纳米复合材料形貌及性能的影响

采用液相原位沉淀法,在不同的醇-水混合溶剂中反应合成了N,N′-(2,4-二氯苯基)硫脲/CdS纳米复合材料.通过扫描电子显微镜分析(SEM)、X射线衍射分析(XRD)、傅里叶变换红外光谱分析(FT-IR)、紫外可见吸收光谱分析(UV-Vis)、荧光光谱分析(PL)等对产物形貌及光学性能进行了表征.结果表明,所得的Cd...     

Controlling morphology and structure of nanocrystalline cadmium sulfide (CdS) by tailoring solvothermal processing parameters

Cadmium sulfide (CdS) with different morphologies was successfully prepared by solvothermal process by controlling the processing parameters, including nature of precursor and solvent, reaction temperature and process time. X-ray diffraction patterns revealed that, in all cases highly pure and crystallized CdS with hexagonal structure were obtained. In addition, it was found that the processing parameters influence on preferable growth direction of CdS nanostructures. Field emission scanning electron microscope analysis showed that CdS nanowires with different aspect ratios were obtained (depending upon the reaction temperature and process time) in presence of sulfur powder and ethylenediamine, whereas CdS nanoparticles were produced by sulfur powder and ethanolamine. Moreover, CdS nanorods were prepared using thiourea and ethylenediamine. Transmission electron microscope image confirmed that CdS nanowire with one of the highest aspect ratio reported in the literature (i.e., 255) was achieved using sulfur powder and ethylenediamine at 200 °C reaction temperature for 72 h process time. UV–Vis absorption spectra of CdS nanostructures prepared under different conditions displayed a blue shift relative to that of bulk CdS due to the quantum size effect.     

Microemulsion-directed synthesis of different CuS nanocrystals

Through a microemulsion-directed route, CuS nanoparticles, nanorods, nanowires and tube-like structures were prepared while different quantities of surfactant were used. The arrangement of the microemulsion vesicles directed the growth behavior of the nanocrystals. Transmission electron microscopy (TEM) was used to investigate the different morphology of the as-synthesized products. X-ray powder diffraction (XRD) and electron diffraction (ED) were applied to characterize the properties of the products obtained. The mechanism of the nanocrystals with different shapes is discussed.     

反应前驱物中n(S)∶n(Cd)对CdS薄膜结构及发光特性的影响

采用化学水浴以CdCl2·H2O、CS( NH2)2、NH4Cl、NH3·H2O和去离子水作为反应前驱物制备CdS纳米晶薄膜.采用扫描电镜( SEM)、X射线衍射(XRD)、透射光谱和稳态荧光光谱,研究了反应前驱物中不同的n(S)∶n(Cd)对所制备的CdS薄膜的形貌、结构和光学性能的影响.结果表明:反应前驱物中n(S...     

快速吸附与脱附的声表面波H2S传感器

本文主要研究了基于SnO₂/CuO薄膜的声表面波（SAW）传感器（室温下,工作频率约为147.8 MHz）检测H₂S气体的特性。以36°YXLiTaO₃为基片制作声表面波器件,通过采用射频磁控溅射法在其表面淀积SnO₂/CuO的复合薄膜制作出H₂S气体传感器。由场发射电子扫描电镜观察薄膜,薄膜连续均匀且表面分布大量微气孔,因而具有良好的吸附性。然后本文在85℃～205℃范围内对传感器的吸附和脱附速率、灵敏度及选择性等进行了实验研究。实验结果表明,所制备的传感器在较低温度下同时具备快速吸附和脱附特性,工作在190℃时气体吸附和脱附速率最快,检测20ppm H₂S的响应和恢复时间分别为30s、15s;工作在160℃时,传感器检测20ppmH₂S的灵敏度最高,工作频率变化约230 kHz,且对于低浓度2 ppm H₂S,频率变化可达45 kHz。同时,传感器也表现出良好的重复性和选择性。     

Chemical synthesis of zinc oxide nanorods for enhanced hydrogen gas sensing

Zinc oxide(ZnO) nanorods are prepared using equimolar solution of zinc nitrate((Zn(NO3)2) and hexamethylenetetramine(C6H12N4) by the hydrothermal technique at 80 C for 12 h. Epitaxial growth is explored by X-ray diffraction(XRD) patterns, revealing that the ZnO nanorods have a hexagonal(wurtzite) structure. Absorption spectra of ZnO are measured by UV–visible spectrometer. The surface morphology is investigated by field emission scanning electron microscopy(FESEM). The synthesized ZnO nanorods are used for detecting the 150 C hydrogen gas with a concentration over 1000 ppm. The obtained results show a reversible response. The influence of operating temperature on hydrogen gas detecting characteristic of ZnO nanorods is also investigated.     

A complexant-assisted hydrothermal procedure for growing well-dispersed InP nanocrystals

Well-dispersed InP nanocrystals have been synthesized via a hydrothermal reaction of In–ethylenediamine tetraacetic acid (EDTA) complex with red phosphorus and KBH₄ in aqueous solution at 160–200 °C for 26 h. The InP nanocrystals were characterized by powder X-ray diffraction (XRD), Raman spectroscopy and transmission electron microscopy (TEM). The XRD patterns showed (1 1 1), (2 0 0), (2 2 0), (3 1 1), (2 2 2), (4 0 0) and (3 3 1) diffraction lines of the cubic InP nanocrystals. The TEM study revealed that the morphology of InP nanocrystals are of well-dispersed spherical shape. The size of InP nanocrystals can be controlled by changing the reaction temperature. The average InP nanocrystallites diameter is increased from 8.7 to 15.8 nm as the temperature increases from 160 to 200 °C. The Raman spectrum showed the transverse-optic (TO) and longitudinal-optic (LO) mode from InP nanocrystallites, and the LO and TO modes shift to lower frequencies with a decrease in the size of InP nanocrystals. The EDTA plays a key role in the nucleation and growth of InP nanocrystals, and the reaction mechanism is discussed.     

LnPO4: RE3+ (La = La, Gd; RE = Eu, Tb) nanocrystals: solvo-thermal synthesis, microstructure and photoluminescence

Through altering the solvents, we have obtained the Eu³⁺/Tb³⁺ ions-doped LnPO₄ (Ln = La, Gd) phosphors with different particle sizes, microstructures and morphologies via a facile solvo-thermal technology. X-ray powder diffraction (XRD), transmission electron microscope (TEM), and scanning electron microscope (SEM) have shown that the products using different solvents have various structures and morphologies. With the increase of DMA/water volume ratio, the microstructure has changed from hexagonal phase to monoclinic one, and the morphology from nanorod to nanoparticle, revealing the decreased oriented growth. The presence of DMA is an important factor in guiding the anisotropic growth of hexagonal lanthanide phosphates. Besides, N-methyl-2-pyrrolidone has been used as solvent to induce the Eu³⁺/Tb³⁺ ions-doped LnPO₄ (Ln = La, Gd) phosphors with different morphologies and structures. Finally, the photoluminescence behaviors of these nanocrystals have been investigated, which are dependent on their microstructures and morphologies.     

温和的苯热溶剂条件下GaP纳米棒的形成机理研究

采用金属Na，白磷和GaCl₃为原料，在温和的苯热溶剂条件下制备了直径为20—40nm，长度为200—500nm的GaP纳米棒和直径为20—40nm的球形颗粒.利用X射线衍射(XRD)、透射电子显微镜(TEM)和X射线光电子能谱(XPS)研究了反应条件对产物结晶性和形貌的影响.实验结果表明，当反应温度低于250℃时，产物基本上为GaP纳米棒，并随着反应温度升高，产物逐渐转化为球形纳米颗粒；当反应温度超过280℃时，产物完全为规则的球形.同时，GaP纳米棒的生长遵循SLS生长机理. 关键词： 纳米GaP 苯热 SLS生长机理