沉淀溶解法制备纳米硫化锌

以烷基黄原酸锌和硫化钠分别为锌源和硫源，采用烷基黄原酸锌沉淀溶解法制备了粒度可调、粒径分布比较窄的面心硫化锌纳米粒子，利用比表面积(BET)测定、透射电镜(TEM)、粉末X射线衍射(XRD)、傅里叶转换红外光谱(FTIR)等方法对合成的硫化锌纳米粒子进行了表征。结果表明随着烷基黄原酸锌链长的增长，通过添加硫化钠而生成的硫化锌纳米粒子的粒径逐渐减小。本文还对沉淀溶解法制备纳米硫化锌的溶液化学反应机理进行了探讨。     

Zinc oxide prepared by homogeneous hydrolysis with thioacetamide, its destruction of warfare agents, and photocatalytic activity

Zinc sulfide (ZnS) nanoparticles were prepared by homogeneous hydrolysis of zinc sulfate and thioacetamide (TAA) at 80 degrees C. After annealing at a temperature above 400 degrees C in oxygen atmosphere, zinc oxide (ZnO) nanoparticles were obtained. The ZnS and ZnO nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and Brunauer-Emmett-Teller (BET)/Barrett-Joyner-Halenda (BJH) methods were used for surface area and porosity determination. The photocatalytic activity of as-prepared zinc oxide samples was determined by decomposition of Orange II dye in aqueous solution under UV irradiation of 365 nm wavelength. Synthesized ZnO were evaluated for their non-photochemical degradation ability of chemical warfare agents to nontoxic products.     

硫化锌胶体标准溶液稳定性研究

采用去离子除氧水,由淀粉、乙酸锌、氯化钠、硫化钠等配制了硫化锌胶体标准溶液。实验结果表明,硫化锌胶体标准溶液的吸光度与硫化钠标准溶液基本一致,可以替代硫化钠标准溶液。采用t检验对硫化物胶体标准溶液稳定性进行了检验,表明该法配制的硫化锌胶体标准溶液在室温下可稳定保存2个月,解决了硫化物标准溶液只能现配现标现用的问题。     

荧光光谱法研究纳米硫化锌与牛血清白蛋白的相互作用

采用水相法合成了ZnS纳米颗粒,通过XRD及TEM技术对纳米ZnS进行了表征,结果表明纳米ZnS的粒径约为7～8 nm.利用荧光光谱考察了纳米ZnS与牛血清白蛋白(BSA)的相互作用,结果显示,两者的相互作用可导致BSA内源荧光猝灭,推测其猝灭机理为静态猝灭,结合常数Ka=1.73×105 L·mol-1,结合位点数n...     

DNA Hybridization at Magnetic Nanoparticles with Electrochemical Stripping Detection

A simple and practical method for electrochemical DNA hybridization assay has been developed to take advantage of magnetic nanoparticles for ssDNA immobilization and zinc sulfide nanoparticle as oligonucleotide label. Magnetic nanoparticles were prepared by coprecipitation of Fe²⁺ and Fe³⁺ with NH₄OH, and then amino silane was coated onto the surface of magnetite nanoparticles. The magnetic nanoparticles have the advantages of easy preparation, easy surface modification and low cost. The target ssDNA with the phosphate group at the 5′ end was then covalently immobilized to the amino group of magnetite nanoparticles by forming a phosphoramidate bond in the presence of 1‐ethyl‐3‐(3‐dimeth‐ylaminopropyl)carbodiimide (EDAC). The zinc sulfide (ZnS) nanoparticle‐labeled oligonucleotides probe was used to identify the target ssDNA immobilized on the magnetic nanoparticles based on a specific hybridization reaction. The hybridization events were assessed by the dissolution of the zinc sulfide nanoparticles anchored on the hybrids and the indirect determination of the dissolved zinc ions by anodic stripping voltammetry (ASV) at a mercury film glassy carbon electrode (GCE). The proposed method couples the high sensitivity of anodic stripping analysis for zinc ions with effective magnetic separation for eliminating nonspecific adsorption effects and offers great promise for DNA hybridization analysis.     

Synthesis and characterizations of ultra-small ZnS and Zn(1-x)Fe(x)S quantum dots in aqueous media and spectroscopic study of their interactions with bovine serum albumin

This work reports a new experimental methodology for the synthesis of ultra small zinc sulfide and iron doped zinc sulfide quantum dots in aqueous media. The nanoparticles were obtained using a simple procedure based on the precipitation of ZnS in aqueous solution in the presence of 2-mercaptoethanol as a capping agent, at room temperature. The effect of Fe(3+) ion concentration as dopant on the optical properties of ZnS was studied. The size of quantum dots was determined to be about 1nm, using scanning tunneling microscopy. The synthesized nanoparticles were characterized by X-ray diffraction, UV-Vis absorption and photoluminescence emission spectroscopies. The presence and amount of iron impurity in the structure of Zn((1-x))Fe(x)S nanocrystals were confirmed by atomic absorption spectrometry. A blue shift in band-gap of ZnS was observed upon increasing incorporation of Fe(3+) ion in the iron doped zinc sulfide quantum dots. The photoluminescence investigations showed that, in the case of iron doped ZnS nanoparticles, the emission band of pure ZnS nanoparticles at 427nm shifts to 442nm with appearance of a new sharp emission band around 532nm. The X-ray diffraction analysis indicated that the iron doped nanoparticles are crystalline, with cubic zinc blend structure, having particle diameters of 1.7±022nm. Finally, the interaction of the synthesized nanoparticles with bovine serum albumin was investigated at pH 7.2. The UV-Vis absorption and fluorescence spectroscopic methods were applied to compare the optical properties of pure and iron doped ZnS quantum dots upon interaction with BSA. It was proved that, in both cases, the fluorescence quenching of BSA by the quantum dots is mainly a result of the formation of QDs-BSA complex in solution. In the steady-state fluorescence studies, the interaction parameters including binding constants (K(a)), number of binding sites (n), quenching constants ( [Formula: see text] ), and bimolecular quenching rate constants (k(q)) were determined at three different temperatures and the results were then used to evaluate the corresponding thermodynamic parameters ΔH, ΔS and ΔG.     

溶液沉淀法制备ZnS-氟碳聚合物电纺纤维光催化复合材料

利用含有羧基的氟碳聚合物电纺纤维为载体和模板材料,常温溶液条件下利用均匀沉淀法,在纤维表面负载硫化锌纳米粒子。通过控制反应条件,得到氟碳聚合物电纺纤维表面均匀分布、无团聚的直径在十几纳米左右的硫化锌-氟碳聚合物电纺纤维光催化复合材料。光催化复合材料的高比表面积和水中有机物富集能力使其在紫外光辐照条件下对次甲基蓝降解效率明显高于ZnS粉体。重复降解实验显示复合材料具有较好的稳定性和重复光催化能力。     

Preparation of copper and zinc sulfide nanoparticles and their modification with cysteine

A new method for the preparation of copper and zinc sulfides nanoparticles in homogeneous aqueous solutions using cysteine as a surface modifier was proposed. The size of the particles obtained is 5–7 and 1.5–3 nm for copper and zinc sulfides, respectively, depending on the concentration of the reactants. Associates of the nanoparticles 10–30 nm in size are formed in the system with an increase in the total concentrations of the sulfides. Sols of the nanoparticles obtained in cysteine solutions are resistant to oxidation and coagulation within several weeks. The variation of the synthesis conditions makes it possible to obtain zinc sulfide particles with optical properties related to size effects.     

Preparation and study of colloid-chemical and optical properties of the nanocrystals of zinc sulfide modified with amino acids

The effect of some amino acids: cysteine, methionine, glycine, lysine, and aspartic acid, on the formation of nanoparticles of zinc sulfide in aqueous solutions at pH 5.5–10.0 was investigated. A method of obtaining stable sols of ZnS particles of 2–4 nm size with narrow distribution of the particle size was developed. The investigated nanoparticles are shown to be sphalerite, the cubic modification of zinc sulfide. The ZnS sols modified with methionine and glycine show intense luminescence at 415–425 nm.     

Size- and shape-dependent phase transformations in wurtzite ZnS nanostructures

This paper describes the equilibrium morphologies of zinc sulfide nanoparticles in the wurtzite phase as a function of size, determined using ab initio Density Functional Theory (DFT) simulations and a shape-dependent thermodynamic model predicting the Gibbs free energy of a nanoparticle. We investigate the relative stabilities of a variety of nanoparticle shapes based on the wurtzite structure and show how the aspect ratio of wurtzite nanorods moderates the size-dependent phase transformation to the zinc blende phase. We find that while wurtzite nanoparticles are thermodynamically unstable with respect to the low energy rhombic dodecahedron morphology in the zinc blende phase at all sizes, shape- and size-dependent phase transformations occur when other zinc blende morphologies are present. Despite popular synthesis of zinc sulphide nanoparticles in the wurtzite phase, an in-depth thermodynamic study relating to the relative stability of wurtzite shapes and comparison with the zinc blende phase does not exist. Therefore this is the first thermodynamic study describing how shape can determine the solid phase of zinc sulfide nanostructures, which will be of critical importance to experimental applications of nanostructured zinc sulfide, where phase and shape determines properties.     

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.     

Photochemical reduction of sulfur in the presence of ZnO nanoparticles in ethanol

The photochemical reduction of sulfur by the action of ZnO nanoparticles of various shapes and sizes under the conditions of stationary and pulsed photoexcitation was studied. The mechanism of this process was proved; the main route to the formation of the reaction product zinc sulfide is reduction of the sulfur by photochemically produced metallic zinc. It was demonstrated that ordered agglomerates of ZnS nanoparticles in the form of nanotubes and nanorods are formed in the systems based on ZnO nanorods.     

Continuous tuning of cadmium sulfide and zinc sulfide nanoparticle size in a water-in-supercritical carbon dioxide microemulsion

The size and size dispersion of cadmium sulfide and zinc sulfide semiconductor nanoparticles can be continuously tuned over a wide range of values by adjusting the density of the fluid phase in water-in-supercritical CO2 microemulsions. The average size of the ZnS nanoparticles decreases linearly from approximately 9.1 to 1.9 nm with increasing fluid density from 0.86 to 0.99 g cm(-3) at a water-to-surfactant ratio (W value) of 10. At a W value of 6, the particle size can be tuned from 7.0 to 1.5 nm in the same density range. In the case of CdS nanocrystals, the size varied from 7.1 to 2.0 nm when the W value was 10 and from 4.0 to 1.3 nm when the W value employed was 6, in the same density range. Monodispersive CdS and ZnS nanoparticles were synthesized by chemical reaction of cadmium or zinc nitrate with sodium sulfide, using two water-in-supercritical CO2 microemulsions as nanoreactors followed by protection with a fluorinated-thiol stabilizer. The stabilizer is introduced at 6 and 16 minutes after the mixing of the two microemulsions where the intensity of the characteristic absorption peak due to the quantum confinement properties of the CdS and ZnS nanoparticles (280 and 360 nm) reaches a maximum, respectively. The supercritical CO2 microemulsion method represents a simple approach to use a density-tunable solvent for synthesizing size-controlled semiconductor nanoparticles over a broad range of values.     

NH3 gas sensing properties of nanocrystalline ZnO based thick films

Zinc acetate derived precursor used in the present sol-gel synthesis of zinc oxide nanoparticles is described. The reaction product obtained before and after reflux of propanolic zinc acetate solution have been studied by UV-vis, photoluminescence and FT-IR studies which confirm the formation of oligomeric precursor Zn4O(Ac)6 (Ac=CH3COO). The formation of approximately 7 nm zinc oxide nanoparticles were confirmed by X-ray diffraction (XRD) and Transmission electron microscopic studies (TEM). The gaseous ammonia gas sensing characteristics of the nano-zinc oxide sensor showed high sensitivity compared to sensor fabricated with commercial zinc oxide powder.     

Preparation of lead sulfide nanoparticles in the photolysis of aqueous solutions of lead thiosulfate complex

It was found from spectroscopic and microscopic data that lead sulfide nanoparticles are formed during the UV irradiation of aqueous solutions of lead thiosulfate complex. The yield and the size of the lead sulfide nanoparticles depend on the concentration of solution and the lead to thiosulfate ion ratio in the solution.     

Zinc sulfide nanoparticles: a mechanism of formation in aqueous solutions and optical properties

The formation of sols and precipitates of zinc sulfide as a result of the exchange reaction in an aqueous solution was studied. The precipitates consist of aggregates of primary particles about 3 nm in size. The primary ZnS particle size in aqueous sols increases with an increase in the concentration of zinc sulfate and sodium sulfide, with the accumulation of the final reaction product, and with temperature. This effect does not exceed an 1.5-fold increase. At the first step, the particles with a considerable fraction of the amorphous phase are formed and undergo intragrain crystallization. The photoluminescence properties of aqueous sols of zinc sulfide were studied. They are caused by defects in the ZnS lattice and by the presence of the lattice oxygen.     

Photochemical synthesis of cadmium sulfide nanoparticles

The formation of cadmium sulfide nanoparticles upon UV irradiation of aqueous solutions of cadmium thiosulfates was established on the basis of spectroscopic and macroscopic data. The yield and size of the cadmium sulfide nanoparticles depend on the ratio of cadmium to thiosulfate ions in solution, the concentration of the solution, and the irradiation duration. The cadmium sulfide nanoparticles with a diameter of 4 nm were obtained by the photolysis of solutions with a concentration of 10⁻³ mol L⁻¹ at the ratio S₂O₃ ²⁻: Cd²⁺ = 2: 1.     

ZnS nanoparticles incorporated in polyaniline composite: Preparation and optical characterization

Hybrid polyaniline based composites incorporating zinc sulfide nanoparticles have been synthesized by using chemical oxidation technique. Morphological and optical properties of the nanocomposite were characterized by scanning electron microscopy, Fourier transform infrared and UV–Vis spectroscopy measurement. The results were compared with pure polyaniline. The characteristic FTIR peaks of polyaniline were found to shift to lower wave-number in nanocomposite. The band gap of nanocomposites increases and the refractive index of the nanocomposites decreases with increasing content of ZnS nanoparticles. These results showed the interaction between ZnS nanoparticles and polyaniline.     

Structure and properties of nanocomposites based on zinc sulfide and poly(vinylidene fluoride)

The structure and properties of nanocomposites based on zinc sulfide and poly(vinylidene fluoride) were studied. The nanocomposite material was prepared by the matrix isolation technique: ZnS nanoparticles are formed by chemical reactions in a poly(vinylidene fluoride) powder of particle size 0.5–1.0 μm.     

Regularities of formation and luminescence of zinc sulfide nanoparticles modified with amino acids

The regularities of formation and luminescence of zinc sulfide nanoparticles modified with various amino acids were studied. The luminescence intensity of ZnS sols depends strongly on the nature of the modifier and from 30 to 40 times increases in the case of methionine and glycine or nearly completely disappears in the case of cysteine. Two main stages of formation of unmodified and surface-modified ZnS were revealed: a very rapid formation of ZnS nanoparticles and a relatively slow process of ordering of the internal particle structure with the formation of luminescence centers. In the case of modified objects, the role of such centers could be played by surface zinc ions bound to amino acids.