Structure of cadmium sulfide nanoparticle micelle in aqueous solutions

The structure of cadmium sulfide (CdS) micelle in stable aqueous solution of ethylenediaminetetraacetic acid was determined by dynamic light scattering, small-angle X-ray scattering and neutron scattering. The micelle aggregate is a single CdS nanoparticle with an average size of about 3 nm, the nanoparticle organic shell and the solvation shell are about 1 nm and 5 nm thick, respectively. These parameters were confirmed by the scanning semi-contact atomic force microscopy and powder X-ray diffraction studies of dry micelle cores isolated by high-speed centrifugation. The CdS micelle was correctly described by a simple double-shell model and was found to possess the structure corresponding to CdS quantum dots.     

聚合物-二氧化硅复合基材中CdS纳米晶的合成

本文报道在Sol-gel基材中制备由聚合物稳定的CdS纳米晶的新方法， 即通过甲基丙烯酸镉与甲基丙烯酸羟乙酯共聚合合成了含有Cd 2+的聚合物微凝胶, 在聚合物微凝胶网络中原位聚合正硅酸乙酯形成聚合物互穿的Sol-gel复合基材. 再向该聚合物/二氧化硅复合基材中通入H2S气体得到CdS纳米晶. 在聚合物网络中原位聚合正硅酸乙酯可以降低纯二氧化硅材料的脆性; 另一方面, 二氧化硅可以作为增强剂增加聚合物材料的强度. 因此, 在我们合成的聚合物/二氧化硅复合基材中制备的CdS纳米晶将具有很好的应用前景.     

Size, volume fraction, and nucleation of Stober silica nanoparticles

29Si NMR, small-angle X-ray scattering (SAXS), and dynamic light scattering (DLS) are used to monitor the synthesis of silica nanoparticles from the base-catalyzed hydrolysis of TEOS in methanol and ethanol. The reactions are conducted at a [TEOS] =0.5 M, low concentrations of ammonia ([NH(3)] =0.01-0.1 M), and [H(2)O] =1.1-4.4 M to resolve the initial size of the first nuclei and to follow their structural evolution. It is found that after an induction period where there is a buildup of singly hydrolyzed monomer, the first nuclei are fractal and open in structure. Interestingly, the nuclei are twice as large in ethanol (R(g) approximately 8 nm) as those in methanol (R(g) approximately 4 nm). The data suggest that the difference in primary particle size is possibly caused by a higher supersaturation ratio of the singly hydrolyzed monomer in methanol than in ethanol if it is assumed that the surface energy of the first nuclei is the same in methanol and ethanol. The particle number concentration and the volume fraction of the silica particles are calculated independently from the SAXS, DLS, and 29Si NMR results. Finally, the rate of nucleation is obtained from the particle number concentrations.     

复合半导体光催化剂p-CoO/n-CdS的制备、表征及光催化性能

以醋酸镉、十二硫醇、硬脂酸和醋酸钴等为原料,采用新方法制备了CdS和一系列p-CoO/n-CdS复合半导体光催化剂.用X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、N2吸附-脱附和紫外-可见漫反射光谱(UV-Vis DRS)等对产物进行了表征.结果表明,p-CoO/n-CdS复合半导体中,CoO粒子紧密结合在CdS颗粒上,CdS的颗粒粒径在100 nm左右,为六方纤锌矿晶型,CoO的颗粒粒径在10 nm左右,颗粒粒径分布均匀.p-CoO/n-CdS的UV-Vis DRS分析结果表明,在400-550 nm范围内都有一强吸收带,属于CdS在可见光区的特征吸收.用光催化降解甲基橙测试了光催化性能,结果表明,p-CoO/n-CdS光催化活性是CdS光催化活性的2.2倍左右.光腐蚀测试结果表明,CdS的光腐蚀速率是p-CoO/n-CdS中CdS光腐蚀速率的2倍以上,说明CoO与CdS复合对CdS的光腐蚀具有明显的抑制作用.     

离子交换膜中CdS单分散纳米晶的合成及其光学性质

以硫代乙酰胺(TAA)为前驱体, 采用液相反应在全氟磺酸离子交换膜(Nafion)中自组装得到了均匀分布、单分散的纳米CdS晶体；与文献报道的前驱体如Na₂S和H₂S不同, TAA可以在全氟磺酸离子膜中均匀扩散, 最终在Nafion薄膜中得到均匀分布的纳米CdS晶体. 利用高分辨电子显微镜(HRTEM)、X射线衍射仪(XRD)和能量散射X射线分析(EDXA)研究了Nafion薄膜模板中CdS纳米晶体的形成机理、晶粒大小和分布；采用紫外- 可见吸收光谱和荧光光谱分析了Nafion薄膜中单分散纳米CdS晶体的光学性质. 结果表明, 随CdS纳米晶体尺寸的减小, 量子尺寸效应明显增强；在紫外吸收谱中表现为吸收边明显蓝移, 而在光致发光谱中, 表现为带边发射的蓝移.     

含有氨基酸基Schiff碱配体的锌、镍配合物的合成、结构及热分解动力学研究

合成了2种含有水杨醛氨基乙酸类(Schiff碱)配体的配合物: (C9H7NO3)Zn(C3H4N2)2(1)和(C9H7NO3)Ni(C3H4N2)2(C4H5N2O)•CH3OH•0.5H2O(2), 其中配合物(1)能够在激发波长为260 nm的条件下发出很强的蓝光.     

TiO2微球的合成及其作为散射层在量子点敏化太阳能电池中的应用

以十六烷基三甲基溴化铵（CTAB）为模板剂,通过TiCl₄在乙醇水溶液中的直接水解,制备了介孔TiO₂微球. X射线衍射（XRD）结果表明所制备的微球晶型为金红石,扫描电镜（SEM）结果显示微球的直径大约为700 nm,由粒径约为16 nm的小颗粒堆积而成. 通过刮涂法制备了在TiO₂小颗粒层上涂覆有作为散射层的TiO₂微球和未涂覆微球的薄膜. 并通过化学浴沉积（CBD）的方法在膜上生长CdS/CdSe量子点,得到了量子点敏化太阳能电池（QDSCs）. 紫外吸收和漫反射结果表明,这种微球结构有利于量子点的沉积,具有较强的光散射作用,有效地增加了光线的收集,从而提高了电池的光电流,最终得到了4.5%的光电转换效率,比不加散射层的电池的效率高27.7%,也比利用传统散射层（由20 nm TiO₂ 小颗粒和400 nm TiO₂ 固体颗粒组成）的电池效率高10.2%. 我们把电池效率的提升归因于较强的光散射作用和较长的电子寿命.     

Studies on optical absorption and structural properties of Fe doped CdS quantum dots

Fe doped CdS quantum dots have been prepared using simple precursors by chemical precipitation technique. Fe doped CdS quantum dots have been synthesized by mixing cadmium nitrate, sodium sulfide and adding Fe under suitable conditions. X-ray diffraction analysis reveals that undoped and Fe doped CdS crystallizes in hexagonal structure. The lattice constants of Fe doped CdS nanoparticles decreased slightly with incorporation of Fe and no secondary phase was observed. The average grain size of the nanoparticles is found to lie in the range of 2.8–4.2 nm. HRTEM results show that undoped and 3.75% Fe doped CdS nanoparticles exhibit a uniform size distribution and average size of the nanoparticles is about 2–3 nm. Raman spectra show that 1LO and 2LO peaks of the Fe doped CdS samples are slightly red shifted compared with those of undoped CdS. Optical absorption spectra of Fe doped CdS nanoparticles exhibited red shift.     

Q-CdS/聚合物纳米复合膜的制备与荧光性能

采用配位化学合成原理 ,分离制备出颗粒尺寸小于 10nm的单分散性的Q态CdS(Q CdS)纳米粒子 ,将Q CdS纳米粒子与聚合物复合成膜 ,制备出一系列Q CdS 聚合物纳米复合膜 .用紫外可见吸收光谱与透射电镜研究了纳米复合膜的量子尺寸效应和分散性 .通过荧光光谱探讨了不同聚合物基体材料和不同Q CdS含量的纳米复合膜的荧光发光性能 .结果表明 ,一方面这种以聚合物为基体的纳米复合膜 ,由于聚合物与Q CdS之间的相互作用 ,使纳米复合膜表现出与单一相组分完全不同的特征荧光发射峰 ;另一方面 ,随着纳米复合膜中Q CdS含量的不断增大 ,纳米复合膜的荧光强度不断增强 ,在一定浓度时达到最大值 .     

温度对聚酰胺-胺树形分子模板法制备CdS量子点的影响

为了研究温度对聚酰胺-胺(PAMAM)树形分子的模板法制备硫化镉(CdS)量子点的影响, 以4.5代(G4.5, 64个甲酯端基)PAMAM树形分子为模板, 在－10～30 ℃的温度范围内制备了分散良好的CdS量子点. 用透射电子显微镜(TEM)表征了CdS量子点的形貌、尺寸; 用紫外-可见光谱(UV-Vis)和光致发光光谱(PL)表征了CdS量子点的光学性能. 发现在相同条件下, 制备温度从－10 ℃升高到30 ℃, CdS量子点粒径从1.8 nm增大到3.4 nm, 其中在10 ℃时制备的量子点的尺寸分布最窄; CdS量子点的吸收和发射光谱均随温度增大而红移, 其中10 ℃时制备的量子点的室温光致发光效率最高. 这表明制备温度决定了树形分子的配位基团与Cd^2＋的分离速度, 并影响了CdS量子点的成核和生长过程, 从而最终决定了CdS量子点的尺寸及尺寸分布、光致发光颜色和发光效率.     

Preparation of CdS nanoparticles by hydrothermal method in microemulsion

CdS nanoparticles with good crystallinity were prepared by hydrothermal method in microemulsion composed of polyoxyethylene laurylether/water/cyclohexane/butanol. The structure and the size of the CdS nanoparticles were analyzed by TEM and XRD. The UV-Vis optical absorption of the samples was also investigated. The results show that hydrothermal treatment is an effective method to prepare CdS nanoparticles of hexagonal structure at lower temperature. The particles were in dimensional uniformity. The diameter of the CdS nanoparticles decreased with the increase of the molar ratio of water to surfactant. The minimum diameter of the CdS nanoparticles prepared in this work was about 10 nm. Obvious blue shift appeared in the UV-Vis absorption spectra. Translated from Chinese Journal of Inorganic Chemistry, 2006, 22(5): (in Chinese)     

明胶溶液中笤帚状纳米CdS的合成及其光谱特性研究

以明胶为稳定剂, 制备出CdS纳米棒, 并实现其向笤帚状纳米CdS的形貌转化. 扫描电镜(SEM)图像表明, 生长时间为2 d, 样品为棒状结构, 直径为50～140 nm, 长度为150～710 nm; 生长15 d的CdS微晶为笤帚状, 结节点直径340～620 nm, 长度2.7～8.4 μm. 探讨了其形貌转化的原因. 结合红外吸收(IR)和荧光光谱的测试结果, 提出了可能的离子络合转化和定位生长机理. 合成的CdS微晶具有一定的荧光性质, 并在紫外和荧光光谱上均表现出明显的量子尺寸效应.     

Sol-gel preparation and spectroscopic study of the pyrophanite MnTiO_3 nanoparticles

Titanium dioxide (TiO2) is one of the green cata-lysts, which has attracted much attention due to its promising applications in the purification of air, the bactericidal action of water, and environmental photocatalytic degradation of organic pollutant co…     

不同晶型纳米CdS的合成及其光催化活性

以醋酸镉为镉源,硫脲为硫源,采用配合物热分解法,通过改变硫脲/醋酸镉的摩尔配比,合成了具有不同晶型的纳米CdS．当n（S）／n（Cd）=0．5—3时,合成的CdS相分别为立方相（n（S）／n（Cd）=0．5）,立方相和六方相的混相（n（S）／n（Cd）=1．0～1．5）,六方相（n（S）／n（Cd）≥2）．通过XRD,TEM,UV—Vis光谱,IR光谱等对CdS的相组成,形貌,粒径,吸光性能,表面结构等进行了表征．光催化降解罗丹明B的活性结果表明,不同CdS相组成的活性顺序为立方相〉六方相〉混相（立方＋六方）,其中立方CdS相由于有较强的吸附作用、光吸收性能和较小的粒径（10～13nm）,对罗丹明B具有最好的光催化降解活性．     

LB型Q态CdS复合膜构象有序性研究

报道了在较高膜压及高沉积速度下硬脂镉ＬＢ膜与Ｈ２Ｓ反应制备纳米有序的机分子／ＣｄＳ纳米粒子复合膜,该膜反应后仍能保持良好的－ＣＨ２－全反式排列,即形成纵向有机－无机复合超晶格材料。     

Controlled synthesis of highly dispersed TiO2 nanoparticles using SBA-15 as hard template

Highly dispersed TiO2 nanoparticles were successfully synthesized by a wet impregnation method using SBA-15 as hard template for confining the growth of TiO2 nanocrystals, and then calcined at 550 degrees C in muffle furnace for 2 h. The as-synthesized samples were characterized with Fourier transform infrared spectra (FTIR), Raman spectroscopy, diffuse reflectance UV-visible spectroscopy (UV-vis), powder X-ray diffraction (XRD), small-angle X-ray diffraction (SAXRD), nitrogen adsorption, transmission electron microscopy (TEM) and photoluminescence spectra (PL). It was found that SBA-15 contained abundant silanol groups after removal of triblock copolymers by ethanol extraction and could easily adsorb a great number of titanium alkoxide via chemisorption. After subsequent hydrolysis of the anchored Ti complexes and calcination of the amorphous TiO2, anatase TiO2 nanocrystals with spherical shape and uniform particle diameter of about 6 nm were formed. A blue shift was observed in UV-vis absorption spectra due to the quantum size effect of TiO2 nanoparticles. Moreover, the as-prepared TiO2 nanoparticles showed a high PL intensity due to an increase in the recombination rate of photogenerated electrons and holes under UV light irradiation.     

IR+vacuum ultraviolet (118 nm) nonresonant ionization spectroscopy of methanol monomers and clusters: neutral cluster distribution and size-specific detection of the OH stretch vibrations

Small methanol clusters are formed by expanding a mixture of methanol vapor seeded in helium and are detected using vacuum UV (vuv) (118 nm) single-photon ionization/linear time-of-flight mass spectrometer (TOFMS). Protonated cluster ions, (CH3OH)(n-1)H+ (n=2-8), formed through intracluster ion-molecule reactions following ionization, essentially correlate to the neutral clusters, (CH3OH)n, in the present study using 118 nm light as the ionization source. Both experimental and Born-Haber calculational results clarify that not enough excess energy is released into protonated cluster ions to initiate further fragmentation in the time scale appropriate for linear TOFMS. Size-specific spectra for (CH3OH)n (n=4 to 8) clusters in the OH stretch fundamental region are recorded by IR+vuv (118 nm) nonresonant ion-dip spectroscopy through the detection chain of IR multiphoton predissociation and subsequent vuv single-photon ionization. The general structures and gross features of these cluster spectra are consistent with previous theoretical calculations. The lowest-energy peak contributed to each cluster spectrum is redshifted with increasing cluster size from n=4 to 8, and limits near approximately 3220 cm(-1) in the heptamer and octamer. Moreover, IR+vuv nonresonant ionization detected spectroscopy is employed to study the OH stretch first overtone of the methanol monomer. The rotational temperature of the clusters is estimated to be at least 50 K based on the simulation of the monomer rotational envelope under clustering conditions.     

Preparation and characterization of copper(II) tetrasulfonated phthalocyanine nanoparticles formed by laser ablation in poor solvents

Laser irradiation of copper(II) tetrasulfonated phthalocyanine (CuTsPc) microcrystals in poor organic solvents such as methanol, 2-methyl-2-propanol, ethanol, tetrahydrofuran, and acetone has produced CuTsPc nanoparticles with 15–112 nm in diameter. Field emission scanning electron microscopy (FESEM) images have shown the formation of CuTsPc nanoparticles in poor organic solvents used in this work. The mean diameters of CuTsPc nanoparticles obtained from transmission electron microscopy (TEM) images in methanol, 2-methyl-2-propanol, ethanol, tetrahydrofuran, and acetone were determined to be 26, 36, 35, 86, and 78 nm, respectively. A correlation between the size of CuTsPc nanoparticles and a solvent polarity could be found in this work.     

溶剂热合成单分散硫化镉纳米晶

在双表面活性剂十八胺和油酸存在条件下, 以氯化镉和硫粉作为反应前驱物, 通过简单的溶剂热方法合成单分散性闪锌矿硫化镉纳米晶, 粒径大小在13 nm. 用X射线衍射(XRD)、透射电子显微镜(TEM)对产物的结构和形貌进行了表征, 同时对硫化镉纳米晶的紫外吸收谱和光致发光谱(PL)性能进行了表征. 实验结果表明合成的样品具有很好的发光性能, 此外溶剂热反应的温度对纳米晶的单分散性有重要影响. 并对硫化镉纳米晶的形成机理做了初步的研究.     

聚丙烯酸辅助水热合成CdS纳米片

利用聚丙烯酸(PAA)和硫代乙酰胺(TAA)合成大分子硫源,采用水热的方法在180℃下制备立方相CdS纳米片,纳米片平均大小在100nm.用X射线衍射仪器(XRD),透射电子显微镜(TEM),红外吸收光谱(FTIR)和紫外吸收光谱(UV-Vis)对CdS纳米片进行了形貌和性能表征,并分析了CdS纳米片形成的可能机理.此外,反应的溶剂对CdS纳米材料的形貌有重要的影响.