银纳米粒子的一步合成与表征

在水和乙醇溶液中,以对巯基苯胺作为还原剂,利用一步法合成了银纳米微粒,并利用拉曼光谱仪考察了对巯基苯胺在银纳米微粒表面的自组装行为.结果表明,合成的银纳米微粒的形貌与介质的pH值密切相关;对巯基苯胺可在银纳米微粒表面自组装.     

球形SnO2 纳米微粒的合成及形成机理分析

以SnCl4*5H2O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 3.5 nm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.     

表面修饰ZrO_2纳米微粒的合成及结构表征(英文)

在溶液中化学合成了硬脂酸修饰ZrO2 纳米微粒 ,采用XRD、TEM和EA表征了ZrO2 纳米微粒的结构 ,结果表明成功合成了表面包覆硬脂酸分子的ZrO2 纳米微粒。     

聚合物为模板制备CdS, ZnS及其掺杂纳米材料

以聚苯乙烯-马来酸酐为模板,合成了CdS,CdS︰Mn,ZnS,ZnS︰Mn及ZnS︰Tb纳米微粒.紫外吸收光谱表明所得微粒尺寸均匀,TEM结果显示CdS纳米微粒的尺寸为2.5 nm.从荧光光谱观察到掺杂离子的特征发射峰,证实了基质到掺杂离子的能量传递.通过红外光谱研究了聚合物与金属离子的键合作用,金属离子首先与聚合物的羧基配位,生成硫化物纳米微粒后,聚合物又包覆在纳米微粒的表面形成保护层.     

热解单源前驱体方法可控制备纳米金属硫化物

本文简要综述了本研究组近年来在利用热解单源前驱体合成方法制备纳米金属硫化物方面的相关工作．通过采用不同的反应前驱体,改变反应时间、反应温度,选择不同的表面配体分子及反应溶剂等手段实现了对纳米金属硫化物形貌、尺寸、组成和晶相的精确调控．除了对合成方法和过程进行介绍外,本文还简要讨论了具有特定形貌的金属硫化物的形成机理,并对几类典型硫化物的应用研究进行了总结．     

无溶剂热分解单源前驱体法制备有机单分子层表面修饰NiS纳米微粒

纳米微粒由于具有很多特别的物理和化学性质,在光、电、磁、机械等各个领域显示出了广阔的应用前景,所以纳米微粒的制备与性能研究是近年来化学、物理和材料科学中最热门和最前沿的课题之一。尽管目前有多种纳米微粒的制备方法见诸文献报道,但是新的纳米微粒的制备方法依然是人们追求的目标之一。无溶剂合成纳米材料是近年来开始研究的制备纳米材料的新方法,在无溶剂环境中,微粒之间的碰撞基本不发生,微粒生长过程是通过单体加成来实现的,这样就较易得到形状和尺寸单分散的纳米材料。但是采用无溶剂合成纳米材料时通常需要加入捕获剂来控制…     

纳米硫化铜颗粒自组装为球、空心球和线形结构

用水和乙二醇混合物为溶剂,应用溶剂热合成方法制备了由纳米颗粒自组装的球、空心球和线形结构的铜的硫化物,如 Cu7S4, Cu1.8S, Cu1.81S 和 Cu2S。 考查了溶剂组成（水含量的变化）、反应时间、实验温度的变化对所制备样品的形貌和物相结构的影响。研究了其形成机理。结果表明,随着反应时间的变化,首先形成纳米颗粒的铜的硫化物。通过自组装形成线形结构。最后转化为球形或空心球形结构。     

Zn(Oxin)2·2H2O纳米晶的固相化学反应合成及表征

随着纳米微粒研究的深入,对纳米超细微粒提出了不同的物理、化学特性需求,制备高纯、超细、均匀的纳米微粒,发展新型的纳米材料,就显得非常重要,而解决问题的关键在于研究、发展新的合成技术.通常,纳米微粒制备的要求是:表面洁净;粒子形状及粒径、粒度分布可控,防止粒子团聚;易于收集;有较好的稳定性;产率高.     

水热法制备稳定的发光CdTe材料

采用水热合成技术将表面修饰有羧基的纳米CdTe微粒与表面活性剂和硅源进行自组装,得到了一种与氧化硅复合的稳定的CdTe发光材料.通过一系列表征手段(如TG-DTA,EDX,TEM,荧光光谱和N₂吸附)证实了CdTe微粒复合在氧化硅中.进一步通过烧结的方法除去表面活性剂,用稀酸除去金属氧化物,即得到多孔的氧化硅材料.     

含羧/酯基有机分子对氧化铝微粒形态调控作用研究

研究了液相法制备纳米微粒过程中，某些含羧／酯基有机分子（乙酸， 乙酰乙酸乙酯，聚酰胺羧酸盐等）分别在水相和有机相中对氧化铝纳米微粒形态的调控作用，通过选择该类有机物的种类和用量，制备了不同粒径范围的球形和不同长径比的纤维状Al2O3纳米粒子，并结合有关理论讨论了官能氧在不同合成介质中对颗粒形态调控的可能机理。     

Protein–Metal-Ion Networks: A Unique Approach toward Metal Sulfide Nanoparticles Embedded In Situ in Nanocomposites

Nanoscale metal sulfides are of tremendous potential in biomedicine. Generally, the properties and performances of metal sulfide nanoparticles (NPs) are highly related to their structures, sizes and morphologies. Recently, a strategy of using sulfur-containing protein–metal-ion networks for preparing metal sulfide embedded nanocomposites was proposed. Within the networks, proteins can play multiple roles to drive the transformation of these networks into protein-encapsulated metal sulfide NPs with ultrasmall size and defined structure (as both a template and a sulfur provider) or metal sulfide NP–protein hydrogels with injecting and self-healing properties (as a template, a sulfur provider, and a gelator) in a controlled manner. In this Concept, the synthesis strategy, the formation mechanism, and the biomedical applications of the gained nanocomposites are presented. Moreover, the challenges and opportunities of using protein–metal ion networks to construct functional materials for biomedical applications are analyzed.     

Nickel sulfide and copper sulfide nanocrystal synthesis and polymorphism

Nickel sulfide and copper sulfide nanocrystals were synthesized by adding elemental sulfur to either dichlorobenzene-solvated (copper sulfide) or oleylamine-solvated metal(II) precursors (nickel sulfide) at relatively high temperature to produce the metal sulfide. Nickel sulfide nanocrystals are cubic Ni(3)S(4) (polydymite) with irregular prismatic shapes, forming by a two-step reduction-sulfidation mechanism where Ni(II) reduces to Ni metal before sulfidation to Ni(3)S(4). Despite extensive efforts to optimize the Ni(3)S(4) nanocrystal size and shape distributions, polydisperse nanocrystals are produced. In contrast, copper sulfide nanocrystals can be obtained with narrow size and shape distributions. The copper sulfide stoichiometry depended on the Cu:S mole ratio used in the reaction: Cu:S mole ratios of 1:2 and 2:1 gave CuS (covellite) and Cu(1.8)S (digenite), respectively. CuS nanocrystals formed as hexagonal disks that assemble into stacked ribbons when cast from solution onto a substrate. CuS, Cu(1.8)S, and Ni(3)S(4) differ from the Cu(2)S and NiS nanocrystals obtained by solventless decomposition of metal thiolate single source precursors, in terms of stoichiometry for copper sulfide, and both stoichiometry and morphology for nickel sulfide [Ghezelbash, A.; Sigman, M. B., Jr.; Korgel, B. A. Nano Lett. 2004, 4, 537-542. Sigman, M. B. Ghezelbash, A.; Hanrath, T.; Saunders, A. E.; Lee, F.; Korgel, B. A. J. Am. Chem. Soc. 2003, 125, 16050-16057].     

Facile Method to Prepare Metal Sulfide(Ag2S,CuS, PbS) Nanoparticles Grown on Surface of Polyacrylonitrile Nanofibre and Their Optical Properties

Polyacrylonitrile-metal sulfide nanocomposites with metal sulfide(Ag₂S, CuS, PbS) nanoparticles homogeneously dispersed on the polyacrylonitrile(PAN) nanofibre were synthesized by means of electrospinning technology combined with gas-solid reaction. A series of experiments was performed to characterize the morphology variation and distribution of the nanocrystalline. The result shows that the concentration of metal salt aqueous solution affects the size and morphology of metal sulfide nanoparticles during the chelating process. Further more, these metal ions nanoparticles were attached to the surface of the nanofibre homogeneously through chelating effect which will be propitious to prevent nanoparticles from aggregation. These results suggest that the method reported here is extremely effective for synthesizing PAN-metal sulfide nanocomposites which have good visible light photocatalytic activity. Further more, this method could be extended to prepare other PAN-metal halides nanocomposites, too.     

Direct electrical measurement of the conversion of metal acetates to metal sulfides by hydrogen sulfide

Copper acetate and related metal salt films react directly with hydrogen sulfide at room temperature to form metal sulfides, resulting in conductivity changes as large as 108. The observed changes in conductivity are related to the solubility product constant (Ksp) and the difference in conductivity between the metal salt and the resulting metal sulfide. A smaller Ksp indicates a more stable metal sulfide and, therefore, greater metal salt reactivity. Polyaniline nanofiber/metal salt composites were also examined and show metal sulfide conversion with changes in resistance up to 106. The direct electrical measurement of the conversion of metal salt to metal sulfide has the potential to be the basis of a new type of sensitive, thin-film chemical sensor.     

纳米分子筛的合成及硫化氢吸附性能

利用无模板水热法合成纳米尺寸的小孔SOD型和大孔X型分子筛, 并考察了其硫化氢脱除性能. 通过对比两种分子筛的硫化氢吸附性能, 证实分子筛对硫化氢的吸附主要集中于孔道内和可及的活性位. 考察了晶粒尺寸、 体积空速和吸附温度等因素对硫化氢吸附的影响, 发现纳米尺寸X型分子筛具有更大的硫容, 并且在低温和低空速下分子筛中的硫化氢分子易于脱除. 随后对纳米X型分子筛进行了金属离子交换改性, 发现Cu改性的分子筛硫容优于其它离子改性的吸附剂, 能达到20.6 mg/g. NaX-N和Cu-NaX-N再生后的硫容分别为新鲜分子筛的62.4%和78.5%.     

Solvent‐free Synthesis of Hexagonal Iron Sulfide Nanoflowers

Employing green and economic solvent‐free synthesis route, hexagonal iron sulfide (Fe₇S₈) nanoflowers were successfully synthesized for the first time. In the experiment, ferric hexadecylxanthate was used as the precursor, and hexagonal iron sulfide (Fe₇S₈) nanoflowers were obtained by thermal decomposition of the precursor at 260°C without any additional solvent or inert gas protection. The as‐prepared iron sulfide nanoflowers were characterized by means of X‐ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive spectrometry (EDS). The characterization results indicated that the nanoflowers had uniform size distribution with an average size of about 160 nm. The proposed strategy provides a possible general route for the synthesis of other metal chalcogenide nanostructures.     

A facile "dispersion-decomposition" route to metal sulfide nanocrystals

In this paper, we demonstrate a simple and general "dispersion-decomposition" approach to the synthesis of metal sulfide nanocrystals with the assistance of alkylthiol. This is a direct heating process without precursor injection. By using inorganic metal salts and alkylthiol as the raw materials, high-quality Ag(2)S, Cu(2)S, PbS, Ni(3)S(4), CdS, and ZnS nanocrystals were successfully synthesized. The mechanism study shows that the reaction undergoes two steps. A key intermediate compound, metal thiolate, is generated first. It melts and disperses into the solvent at a relatively low temperature, and then it decomposes into metal sulfide as a single precursor upon heating. This method avoids using toxic phosphine agent and injection during the reaction process. The size and shape of the nanocrystal can be also controlled by the concentration of the reactant and ligands. Furthermore, the optical properties and assembly of the nanocrystals have also been studied. This report provides a facile, direct-heating "dispersion-decomposition" approach to synthesize metal sulfides nanocrystals that has potential for future large-scale synthesis.     

Synthesis and characterization of low dimensional ZnS- and PbS-semiconductor particles on a montmorillonite template

Low dimensional metal sulfide particles have been prepared in the interlayers of montmorillonites via reactions of the metal ion-exchanged clay minerals in aqueous dispersions with gaseous hydrogen sulfide. The montmorillonites separated from the Wyoming (USA) and Jel?ovy Potok (Slovakia) bentonites were saturated with Pb(2+) or Zn(2+). In the final nanohybrids, the smectite mineral can be incorporated with metal sulfide pillars and/or nanoparticles. Properties of the prepared materials were investigated by various analytical techniques. The formation of metal sulfide nanoparticles in the interlayer galleries was indicated by X-ray diffraction and energy dispersive X-ray analysis. About 50% of Pb(2+) or Zn(2+) present in montmorillonite has formed metal sulfide semiconducting units. Infrared spectroscopy and thermogravimetric analysis were used for characterization of starting materials and products. Ultraviolet-visible absorption and photoluminescence spectroscopies confirmed that final composite systems acquired the optical properties of the incorporated quantum low dimensional systems exhibiting blue shift of the energy gap and higher oscillator strength excitonic peaks. Larger amounts of metal sulfide nanoparticles were formed in montmorillonite Jel?ovy Potok probably as a consequence of its higher cation exchange capacity.     

Nanoparticles of amorphous ruthenium sulfide easily obtainable from a TiO2-supported hexanuclear cluster complex [Ru6C(CO)16]2-: a highly active catalyst for the reduction of SO2 with H2

TiO(2)-supported ruthenium-metal particles were derived from an anionic hexanuclear carbido carbonyl cluster [Ru(6)C(CO)(16)](2-) and compared with those prepared conventionally by impregnation of TiO(2) with a solution of RuCl(3) followed by reduction with H(2). The average sizes of the metal particles in both systems are similar, that is, 12 A for molecular cluster-derived particles and 15 A for those derived from the RuCl(3) precursor, although the size distribution is sharper in the former case. These supported particles efficiently promote the reduction of SO(2) with H(2) to give elemental sulfur. Their active form is ruthenium sulfide as confirmed by EXAFS and X-ray diffraction measurements. The nanoscale ruthenium sulfide particles, which originated from the cluster complex, have an amorphous character and show activity even at low temperature (463 K), whereas ruthenium sulfide formed from RuCl(3)-derived metal dispersion is a pyrite-type RuS(2) crystallite and needs a temperature above 513 K to effect the same catalysis. Amorphous ruthenium sulfide maintains its nano-sized scale (approximately 14 A) regardless of the reaction temperature, while RuS(2) crystallite aggregates to form larger nonuniform particles.