空气中含 17O、18O的氧分子在CdO表面的富集

利用热脱附－离子捕获检测器(TPD-ITD）、四极质谱（QMS）、X光电子能谱（XPS）、X光衍射（XRD）等方法,研究了在CdO表面层中^17O、^18O的富集现象。所获得结果显示,CdO表面Cd(OH)2-CdCO3层在形成过程中对含^17O、^18O的氧分子有选择包结能力。     

溶剂热再结晶合成由纳米颗粒自组装成的一维CdS纳米棒

采用两种不同的溶剂热路径合成出了不同形貌和尺寸的CdS纳米晶, 一种是以无水乙二胺(en) 为溶剂, CdCl₂·2.5H₂O和硫脲(H₂NCSH₂N) 为镉源和硫源, 在不同反应温度(160 ℃-220 ℃ 下制备出了CdS纳米晶, 讨论温度对CdS纳米晶生长的影响; 另一种是以en为溶剂, 将在160 ℃下合成的产物在200 ℃下原位再结晶生长2-8 h, 分析原位生长时间对CdS纳米晶生长的影响. 通过X射线衍射(XRD)、 扫描电子电镜(SEM) 和透射电子电镜(TEM) 等表征产物的物相、 形貌和微结构, 分析可知: 两种路线合成的产物均为六方相CdS; 当温度为160 ℃时, 产物形貌为纳米颗粒状, 当温度高于160 ℃时, 产物为CdS纳米棒状; 同时, 在200 ℃下原位再结晶生长不同时间后发现产物形貌由纳米颗粒转变为纳米棒, 通过场发射扫描电镜(HRTEM) 分析可知: 纳米棒是由零维纳米颗粒自组装而成. 最后, 讨论了影响产物CdS纳米晶形貌转变的因素和纳米棒的生长机理.     

基于VO2@SiO2核壳纳米粒子的热致变色薄膜

为解决VO_2热致变色薄膜可见光透射率低、耐候性差以及热分解法制备VO_2纳米颗粒易团聚等问题,提出了一种基于VO_2@SiO_2核壳纳米粒子的热致变色薄膜。首先利用VO(OH)_2表面负电荷和γ-氨丙基三乙氧基硅烷中氨基正电荷间的静电相互作用,在前驱体VO(OH)_2表面进行SiO_2包覆得到VO(OH)_2@SiO_2核壳纳米粒子,然后在Ar气氛下对其进行高温热处理得到VO_2@SiO_2核壳纳米粒子,将其分散至树脂中并涂覆在玻璃基材上得到热致变色薄膜,并对热致变色薄膜的热致变色性能及核壳粒子的耐候性进行了研究。从透射电镜照片可以看出SiO_2壳层可以阻止前驱体VO(OH)_2在热分解过程中的团聚长大,对光学性能的研究表明低折射率的SiO_2和空气能够提高热致变色薄膜的光学性能,并且当VO(OH)_2@SiO_2纳米粒子的质量分数为10wt%时复合薄膜的光学性能最佳。SiO_2壳层对VO_2的保护作用可以有效提高其抗氧化性,并且可以提升纳米颗粒在酸性环境下的耐腐蚀性,延长热致变色薄膜的使用寿命。     

球形SnO2 纳米微粒的合成及形成机理分析

以SnCl4·5H2 O为主要原料 ,用溶剂热技术在油酸体系中成功地合成了球形SnO2 纳米微粒 ,在无水乙醇体系中合成了菱形的SnO2 纳米微粒 .通过X射线粉末衍射 (XRD) ,选区电子衍射 (SAED)和透射电镜 (TEM )对两种产物进行了表征 ,并对两种产物的形成机理进行了分析 .透射电镜 (TEM)结果表明 :在油酸体系中得到了平均尺寸约为 3.5nm的球形SnO2 纳米微粒 ,此微粒趋向于特殊高的比表面积 ,适合于作气敏探测器材料方面的应用     

Co3O4 纳米棒的溶剂热合成及形成机理分析

以Co(NO3) 2 ·6H2 O为主要原料 ,H2 O2 为氧化剂 ,在油酸和正十二烷烃的混合溶液中 ,利用溶剂热技术于 160℃反应 10h ,成功地合成了Co3O4 纳米棒 .用X射线粉末衍射 (XRD)、透射电子显微镜 (TEM)和振动样品磁强计 (VSM)等手段对产物进行了表征 ,并对产物的形成机理进行了初步分析 .结果表明 ,产物为立方型Co3O4 纯相 ,优化实验条件可得到棒状Co3O4 ,其平均尺寸约为 2 5× 10 0nm .Co3O4 纳米棒的形成与微乳液的棒状结构有关 ,棒状结构的胶束是形成这种纳米棒的模板 .在室温下 ,产物的矫顽力 (Hc)为 3 5 3Oe ,剩余磁化率 (Mr)为 0 .4emu/g .     

纳米二氧化钛分离富集ICP-AES测定镉、钴、锌的研究

建立了纳米二氧化钛分离富集 ,电感耦合等离子体原子发射光谱 (ICP AES)测定镉、钴和锌的新方法。考察了溶液 pH值、洗脱条件和干扰离子等因素对分析物分离富集的影响。结果表明 ,在pH 9～ 10范围内 ,Cd ,Co和Zn可被纳米TiO2 定量富集 ,吸附于纳米TiO2 上的金属离子可用 0 . 1mol·L-1的硝酸溶液完全解脱。在优化的实验条件下 ,纳米TiO2 对Cd ,Co和Zn的吸附容量分别为 8 1,6 9和 15 1mg·g-1。本法对Cd ,Co和Zn的检出限 (3σ)分别为 :5 . 1,3. 4和 2 . 9ng·mL-1,相对标准偏差 (RSD)分别为 4 .3% ,4 .6 %和 4 . 9% (n =9,c=0 1μg·mL-1)。该方法已成功地应用于环境样品中镉、钴和锌的测定 ,分析结果满意。     

CdTe/CdO nH2O核壳纳米复合粒子的水相合成及光学特性.

"研究了CdTe/CdO?nH2O核壳纳米复合物的水相合成及其光学特性． 以巯基乙酸为稳定剂通过氯化镉和碲氢化钠反应制备了碲化镉纳米晶． 在反应过程中, 反应前驱溶液中镉离子与碲离子的摩尔浓度比对最终制备的碲化镉纳米晶的荧光强度起到了极其重要的作用． 在pH值为8.2, 镉离子与碲离子摩尔浓度比为4.0的情况下,制备出了具有最强荧光强度的碲化镉量子点．之后,CdTe/CdO?nH2O核壳纳米复合物在水相中制备出来．在适当的氢氧化镉沉积在碲化镉纳米粒子表面后,碲化镉量子点的荧光大大增强．所制备的CdTe/C     

花状硫化铜级次纳米结构的制备及可见光催化活性研究

本实验以氯化铜 (CuCl₂·2H₂O) 和二硫化碳(CS₂)为原料, 以乙二醇(C₂H₆O₂) 为溶剂, 通过溶剂热法成功制备了具有可见光活性的花状硫化铜(CuS) 级次纳米结构. 并利用X射线粉末衍射技术(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM) 等技术对其进行了表征, 利用紫外可见吸收光谱(Uv-vis)分析了其光学性能, 并以甲基橙为目标降解物对其可见光催化活性进行了研究. 结果表明: 花状CuS级次纳米结构具有很高的可见光催化活性, 与体相CuS粉末相比有很大的提高, 在自然光照射下对甲基橙的降解率可以达到100%. 同时本文对花状级次纳米结构的形成机理进行了分析. 关键词： 硫化铜 溶剂热 级次纳米结构 光催化     

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     

热退火、激光束和电子束等作用对纳米硅制备及其局域态发光特性的影响

在纳米晶体硅制备的过程中, 晶化处理是影响和提高纳米硅发光效率的重要制备环节. 热退火、激光退火和电子束辐照是使纳米硅样品晶化的不同方式. 实验表明: 选取适当的晶化方式和参量对制备纳米硅晶体结构至关重要, 特别是在制备硅量子点和量子面的过程中控制好参量, 可以得到较高的发光效率. 有趣的是, 在实验中发现: 当晶化时间较短(如低于20 min)时, 可以获得较好的纳晶硅结构(如量子点结构), 对应于较好的纳晶硅光致发光(PL)和掺杂局域态发光; 当晶化时间较长(如超过30 min)时, 纳米晶体硅结构被破坏, 致使PL谱逐渐减弱与消失. 结合热退火、激光退火和电子束辐照对纳米硅晶化过程, 本文建立起晶化时间对纳米硅局域态发光影响机理的物理模型, 解释了晶化时间对纳米硅局域态发光的影响.     

Synthesis of nano and micro crystals of Cd(OH)2 and CdO in the shape of hexagonal sheets and rods

Cd(OH)₂ and CdO nano/micro crystals were synthesized in ethanol-water medium using cadmium foil as a source under solvothermal condition. The experimental parameters such as ratio of ethanol to water, concentration of NaOH and synthesis temperature all play important role in determining the size, shape and crystalline phase of the products. The products were characterized by X-ray diffraction and scanning electron microscopy. Nano/micro crystals of CdO were also achieved by thermal treatment of Cd(OH)₂ crystals in air at different temperatures.     

Morphology controlled solvothermal synthesis of Cd(OH)2 and CdO micro/nanocrystals on Cd foil

Cadmium hydroxide (Cd(OH)₂) and cadmium oxide (CdO) nano and micro crystals were synthesized in ethanol-water medium using cadmium foil both as a source and substrate under solvothermal condition. Different concentrations of ammonium hydroxide, hydrazine hydrate, sodium hydroxide and potassium hydroxide were added to study the structural and morphological variations in the products. Synthesis was carried out at different temperatures to study the growth stages of the nano/microstructures. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The as-prepared Cd(OH)₂ products were transformed to CdO by thermal treatment in air. The possible growth mechanism for the formation of different morphologies at different basic medium has been proposed. The optical absorption measurement was carried out to determine the values of the band gap of CdO.     

Solvothermal synthesis of Cd(OH)2 and CdO nanocrystals and application as a new electrochemical sensor for simultaneous determination of norfloxacin and lomefloxacin

Cadmium hydroxide (Cd(OH)₂) microcrystals were synthesized in ethanol–water medium by using cadmium chloride as cadmium source and 1,10-phenanthroline as complexation agent under solvothermal condition. The sample was characterized by FT-IR, X-ray diffraction (XRD), scanning electron microscopy (SEM) and TEM. The as-prepared Cd(OH)₂ product were transformed to hexagonal CdO nanocubes by thermal treatment in air at 500 °C. The possible growth mechanism for the formation of different morphologies at basic medium has been proposed. DPV experiments were carried out for the simultaneous determination of norfloxacin and lomefloxacin in the acetate buffer solution with pH 4.5.     

Preparation, conversion, and comparison of the photocatalytic property of Cd(OH)2, CdO, CdS and CdSe

In this paper, we report the hydrothermal preparation of Cd(OH)₂ nanowires and further conversion to CdO nanobelts, CdS nanowires and CdSe nanoparticles through thermal treatment, solvothermal and mixed-solvothermal routes, respectively. The as-obtained products were characterized by means of powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FEMSEM). Research showed that four cadmium compounds were good photocatalysts for the degradation of organic dyes such as Safranine T and Pyronine B, under irradiation of 365 nm UV light. The order of catalytic activity of different materials was found to be Cd(OH)₂<CdO<CdS<CdSe.     

Formation of CdO films from chemically deposited Cd(OH)2 films as a precursor

Formation of cadmium hydroxide at room temperature onto glass substrates from an aqueous alkaline cadmium nitrate solution using a simple soft chemical method and its conversion to cadmium oxide (CdO) by thermal annealing treatment has been studied in this paper. The as-deposited film was given thermal annealing treatment in oxygen atmosphere at 450 °C for 2 h for conversion into cadmium oxide. The structural, surface morphological and optical studies were performed for as-deposited and the annealed films. The structural analyses revealed that as-deposited films consists of mixture of Cd(OH)₂ and CdO, while annealed films exhibited crystalline CdO. From surface morphological studies, conversion of clusters to grains after annealing was observed. The band gap energy was changed from 3.21 to 2.58 eV after annealing treatment. The determination of elementals on surface composition of the core-shell nanoparticles of annealed films was carried out using X-ray photoelectron spectroscopy (XPS).     

Investigation of chemical bath deposition of CdO thin films using three different complexing agents

Chemical bath deposition of CdO thin films using three different complexing agents, namely ammonia, ethanolamine, and methylamine is investigated. CdSO₄ is used as Cd precursor, while H₂O₂ is used as an oxidation agent. As-grown films are mainly cubic CdO₂, with some Cd(OH)₂ as well as CdO phases being detected. Annealing at 400 °C in air for 1 h transforms films into cubic CdO. The calculated optical band gap of as-grown films is in the range of 3.37-4.64 eV. Annealed films have a band gap of about 2.53 eV. Rutherford backscattering spectroscopy of as-grown films reveals cadmium to oxygen ratio of 1.00:1.74 ± 0.01 while much better stoichiometry is obtained after annealing, in accordance with the X-ray diffraction results. A carrier density as high as 1.89 × 10²⁰ cm⁻³ and a resistivity as low as 1.04 × 10⁻² Ω-cm are obtained.     

Linear and nonlinear optical properties of hydrogenated CdO thin films

The linear and nonlinear optical properties of a CdO film post-annealed in a hydrogen atmosphere for 30 min (CdO:H) were studied. The prepared CdO and CdO:H films were characterized by X-ray diffraction and UV-VIS-NIR absorption spectroscopy. Experimental data indicated that annealing in an H₂ atmosphere slightly compresses the CdO unit cell and widens the energy gap of CdO by about 3% relative to a nonhydrogenated film. This effect can be explained by the Burstein-Moss energy effect. The nonlinear absorption and nonlinear refractive index coefficients were determined and found to be higher than the values previously determined for nonhydrogenated CdO.     

乙醇与水协同修饰Bi_2WO_6纳米片形貌及改善其光致发光性

通过控制前驱体中乙醇与水的体积比,采用溶剂热法得到不同形貌的Bi2WO6纳米片,探讨了Bi2WO6形貌与光致发光性能之间的关系。Bi2WO6的结晶度、纳米片的棱长以及片层间距随醇水比增大而逐渐提高,当醇水比为1∶1时,Bi2WO6纳米片的棱长、片层间距和比表面积(BET)最大,表现出优异的光致发光性能;而在醇水比大于1∶1时,纳米片的棱长、片层间距和BET随之降低,光致发光性能继而减弱。以上表明醇水比为1∶1时,复配乙醇与水协同修饰Bi2WO6纳米片形貌的效果最佳,BET最大,从而促进其光致发光性能的改善。     

Sonochemical syntheses of a new nano-plate cadmium(II) coordination polymer as a precursor for the synthesis of cadmium(II) oxide nanoparticles

Nanoplates of the three-dimensional coordination polymer, {[Cd(3)(3-pyc)(4)(N(3))(2)(H(2)O)](n) (1), 3-pyc(-)=pyridine-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Cadmium(II) oxide nanoparticles were prepared from thermal decomposition in oleic acid and direct calcination of compound 1 at different temperatures. The thermal stability of nano-sized compound 1 was studied by thermal gravimetric (TG) and differential thermal analyses (DTA). Results show that the size and morphology of the CdO nanoparticles are dependent upon the particles size of compound 1 and the thermolysis temperature. A decrease in the particle size of compound 1 leads to a decrease in the particle size of the CdO, while an increase in the processing temperature leads to an increase in the particle size of the produced cadmium(II) oxide nano-particles.     

Spray deposition of highly transparent fluorine doped cadmium oxide thin films

The cadmium oxide (CdO) and F:CdO films have been deposited by spray pyrolysis method using cadmium acetate and ammonium fluoride as precursors for Cd and F ions, respectively. The effect of temperature and F doping on the structural, morphological, optical and Hall effect properties of sprayed CdO thin films was investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), optical absorption and electrical measurement techniques. TGA and DTA studies, indicates the formation of CdO by decomposition of cadmium acetate after 250 °C. XRD patterns reveal that samples are polycrystalline with cubic structure and exhibits (2 0 0) preferential orientation. Considerable broading of (2 0 0) peak, simultaneous shifting of corresponding Bragg's angle have been observed with respect to F doping level. SEM and AFM show the heterogeneous distribution of cubical grains all over the substrate, which are randomly distributed. F doping shifts the optical gap along with the increase in the transparency of CdO films. The Hall effect measurement indicates that the resistivity and mobility decrease up to 4% F doping.