Synthesis of CdS, ZnS and Ag2S nanoparticles stabilized by sodium bis(2-ethylhexyl)sulfosuccinate and polyoxyethylenesorbitan monooleate in aqueous medium

The effect of synthesis conditions (molar ratio between precursors, concentration of surfactants, synthesis temperature) on the size of CdS, ZnS and Ag₂S nanoparticles (NPs) stabilized by sodium bis(2-ethylhexyl)succinate and polyoxyethylenesorbitan monooleate was studied. It was established that stabilization by polyoxyethylenesorbitan results in formation of smaller NPs (～8 nm) as compared to that in the presence of sodium bis(2-ethylhexyl)sulfosuccinate (14–60 nm), which is due to the difference between the adsorption rates of these surfactants onto the surface of synthesized NPs. The resulting aqueous dispersions of CdS, ZnS and Ag₂S NPs exhibit long-term stability to sedimentation. The nanoparticle size increases insignificantly with temperature increasing to 65–70°C and rises abruptly at higher temperatures. The increase in the ratio between concentrations of precursors (sulfide and metal ions) also results in an increase in NP size, allowing one to synthesize nanoparticles of prescribed sizes. The optical properties of the resulting nanoparticles were studied. The positions of the exciton peaks and the luminescence intensity peaks of the dispersions of synthesized CdS and ZnS NPs were determined.     

Converting Ag2SCdS and Ag2SZnS into AgCdS and AgZnS Nanoheterostructures by Selective Extraction of Sulfur

A mild three‐step solution strategy is developed to prepare Ag? MS (M=Zn, Cd) nanoheterostructures composed of MS nanorods with silver tips. First, Ag₂S? MS heterostructures are synthesized by following a solution–liquid–solid mechanism with Ag₂S nanoparticles as catalysts, then the Ag₂S sections of the heterostructures are converted into silver nanoparticles by selective extraction of sulfur. Notably, for the prepared Ag? CdS heterostructures, the localized surface plasmon resonance of silver remarkably intensifies the photoluminescence of CdS by enhancing the excitation light absorption, which is beneficial for potential applications of CdS nanoparticles in the fields of biolabeling, light‐emitting diodes, and so forth. The strategy reported herein would be useful for designing and fabricating other metal–semiconductor hybrid nanostructures with desirable performances.     

Synthesis of hybrid nanoparticles based on magnetic Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles and luminescent CdS nanoparticles

A new approach to the synthesis of hybrid nanoparticles based on magnetic Fe₃O₄ nanoparticles and CdS quantum dots, combining magnetic and luminescence properties, has been suggested. Conditions for preparation of their stable aqueous suspensions have been found, and their optical properties have been studied. Nanocomposites produced at the molar ratio Fe₃O₄: CdS = 5: 1, which exhibited the luminescence properties) and gave stable aqueous suspensions, have turned out to be most promising. The results are evidence that the synthesized nanoparticles can be used for the development of visualizing agents for in vitro biomedical research.     

Synthesis,characterization and stability of multicore-shell CdS-SiO<Subscript>2</Subscript> nanoparticles

Multicore-shell CdS-Si0₂ nanoparticles were synthesized in AOT/heptane/H₂O reverse micelles at room temperature. CdS-SiO₂ nanoparticles were characterized by UV-vis spectroscopy, TEM, and SEM methods. The results show that multicore-shell composites were formed. Fluorescence properties of composites were also investigated; the data imply that fluorescence properties of the silica-coated CdS nanoparticles were significantly improved when compared to those of the non-coated CdS nanoparticles. The stability of multicore-shell CdS-SiO₂ nanoparticles upon the UV irradiation was higher than that of non-coated CdS nanoparticles.     

Mechanism of the formation of photosensitive nanostructured TiO<Subscript>2</Subscript> with low content of CdS nanoparticles

A method for synthesizing a CdS/TiO₂ composite material, active in the visible region, was described. The CdS/TiO₂ composite was obtained by the sol–gel synthesis of nanostructured TiO₂ in a medium of a stable colloidal solution of CdS nanoparticles. The TiO₂ matrix produced by the sol–gel process is amorphous and contains a nanocrystalline anatase phase, the content of which depends on the Ti(OBu)₄ hydrolysis rate. The content of CdS nanoparticles forming in the colloidal solution and participating in the TiO₂ matrix sensitization is determined by the initial CdS: Ti(OBu)₄ ratio. Although the content of CdS nanoparticles in the composite is low (no more than 3 wt %), the composite demonstrates catalytic activity in the visible region, thus proving the possibility of reducing the content of toxic CdS nanoparticles in the TiO₂ matrix without decreasing the photosensitivity of the CdS/TiO₂ composite.     

Elektroanalyse der CdS-Leuchtfarbe

Zusammenfassung Die aktivierte CdS-Leuchtschicht einer Fernsehröhre besteht aus hexagonalem CdS (Greenockit), Ag₂S (Akanthit) und kubischem CdS. Die Aktivierung dieser Leuchtfarbe hÄngt von dem Kristallwachstum von CdS (Korngrö\e ca. 5 ) und der gleichmÄ\igen Verteilung des Ag₂S in ihm ab.

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Summary The activated CdS phosphor for the Braun tube has a composition consisting of hexagonal CdS, Ag₂S and cubic CdS. Activation of this phosphor depends on crystal growth of CdS (grain size about 5 ) and on uniform dispersion of Ag₂S.

     

Biomimetic synthesis of the arachidic acid/Ag<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Cd<Subscript><Emphasis Type="Italic">y</Emphasis></Subscript>S nanocomposite films

Ag _x Cd _y S nanoparticles were obtained in arachidic acid (AA) monolayer containing Ag⁺ and Cd²⁺ under H₂S flow. The AA/Ag _x Cd _y S monolayers were deposited onto solid substrate to prepare LB films. The UV-vis spectrum showed that the LB film exhibited notable quantum-size effect. The small-angle X-ray diffraction revealed periodic structure of the LB films. The molar ratio of Ag to Cd in AA/Ag _x Cd _y S film was ca. 1 : 5 as measured by the XPS. TEM and FTIR spectroscopy showed that the head-groups of arachidic acid molecules controlled formation of Ag _x Cd _y S nanoparticles in the monolayer.     

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.     

The design of hybrid materials based on magnetic Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles and luminescent CdS nanoparticles for cell visualization

Hybrid nanoparticles based on Fe₃O₄ and CdS combining magnetic and luminescence properties were synthesized. The possibility of visualization of various cells by 3-mercaptopropylsilane-modified CdS nanoparticles and hybrid nanoparticles based on them using a confocal microscope was demonstrated. The synthesized materials did not show a clear-cut cytotoxicity.     

Structure and spectral-optical characteristics of Se,Se/CdS,and Se/Cd<Subscript>0.5</Subscript>Zn<Subscript>0.5</Subscript>S nanoparticles,stabilized in polymer-containing media

A method was proposed for the production of colloidal nanoparticles of selenium stabilized by polymers and surfactants, and their structural and optical characteristics were studied. It was shown that during the deposition of CdS and Cd_0.5Zn_0.5S on the surface of the Se nanoparticles followed by dissolution of the selenium with sodium sulfite it is possible to obtain network “nanoframeworks” with size 30–50 nm, formed by CdS or Cd_0.5Zn_0.5S particles measuring 3–5 nm. __________ Translated from Teoreticheskaya i éksperimental’naya Khimiya, Vol. 43, No. 1, pp. 24–29, January–February, 2007.     

Synthesis of ZnS Nanospheres in Microemulsion Containing Cationic Gemini Surfactant

The reverse microemulsion containing cationic gemini surfactant trimethylene‐1,3‐bis(dodecyldimethyl ammonium bromide) (12‐3‐12, 2Br^?) is applied to synthesize ZnS nanospheres. Narrow size distributed ZnS nanospheres with controllable size and uniform morphology are successfully fabricated by direct reaction of ZnCl₂ and Na₂S in the reverse microemulsion systems. Except for the appearance of large aggregates owing to quantum size effects when the incubation time is 2 h, with increasing the incubation time from 12 to 48 h, the diameter of the ZnS nanosphere can be controlled as 20–25 nm and 140 nm, respectively. X‐ray diffraction (XRD), transmission electron microscopy (TEM), and UV‐visible absorption spectroscopy are applied to characterize the resulting ZnS nanoparticles. In the system used in the present study uniform nanosphere morphology can be synthesized, with the incubation time as an important factor in controlling the size of as‐prepared products.     

Controllable incorporation of CdS nanoparticles into TiO<Subscript>2</Subscript> nanotubes for highly enhancing the photocatalytic response to visible light

A constant current electrochemical deposition was employed to incorporate CdS nanoparticles into the TiO₂ nanotube arrays (TiO₂NTs). The size and amount of CdS nanoparticles in TiO₂NTs (CdS@TiO₂NTs) were controllable via modulating current, deposition time and electrolyte concentration. It was revealed, from the scanning electron microscopy (SEM) images and X-ray photoelectron spectroscopy (XPS) in depth profile, that CdS nanoparticles were filled into TiO₂ nanotubes. A shift of the absorption edge toward the visible region under the optimal electrodeposition condition was observed with the diffuse reflectance spectroscopy (DRS). A 5-fold enhancement in the photocurrent spectrum for TiO₂NTs was observed and the photocurrent response range was significantly extended into the visible region because of the CdS incorporation. Compared with pure TiO₂NTs, under a visible light irradiation, CdS@TiO₂NTs exhibited a 3.5-fold improvement of photocatalytic activity, which was demonstrated by the photocatalytic decomposition of Rhodamine B (RhB).     

Stabilization of Oil-in-Water Emulsions with SiO<Subscript>2</Subscript> and Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> Nanoparticles

Stabilization of oil-in-water Pickering emulsions with SiO₂ and Fe₃O₄ nanoparticles has been studied. Emulsions containing three-dimensional gel networks formed by aggregated nanoparticles in the dispersion media have been shown to be stable with respect to flocculation, coalescence, and creaming. Concentration ranges in which emulsions are kinetically stable have been determined. Stabilization with mixed Ludox HS-30 and Ludox CL SiO₂ nanoparticles leads to the formation of stable emulsions at a weight ratio between the nanoparticles equal to 2 and pH 6.7. In the case of stabilization with Ludox CL and Fe₃O₄ nanoparticles, systems resistant to aggregation and sedimentation are obtained at pH 8. The use of mixed Ludox HS-30 and Fe₃O₄ nanoparticles has not resulted in the formation of emulsions stable with respect to creaming, with such emulsions appearing to be resistant only to coalescence at pH 2–6.     

Synthesis and characterization of CdS nanoparticles prepared by precipitation in the presence of span 20 as surfactant

Cadmium sulfide nanoparticles with average size of ≈16 nm have been synthesized using chemical precipitation reaction of CdCl₂ and Na₂S in the presence of nonionic surfactant stabilized reverse emulsions. Sorbian monolaurate (Span 20) is used for the stabilization of emulsions. The influence of Span 20 on controlling the size and properties of CdS nanoparticles were studied. The obtained CdS nanoparticles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Energy-dispersive x-ray (EDX), and X-ray diffraction (XRD). The optical properties of CdS nanoparticles are investigated systematically by UV-visible absorption spectroscopy. The blue shift in the absorption region and increase in the bandgap to the larger value (2.77 eV) are attributed to the nanosize of the obtained particles.     

Preparation of inorganic nanoparticles in oil-in-water microemulsions: A soft and versatile approach

In this review, the synthesis of inorganic nanoparticles using oil-in-water (O/W) microemulsions as confined reaction media is discussed. Synthesis using (O/W) microemulsions has been demonstrated for a great variety of inorganic nanoparticles: metallic (Pt, Pd, Rh, Ag), single metal oxides (CeO₂, ZrO₂, TiO₂, Fe₂O₃), mixed and doped metal oxides (Ce_0.5Zr_0.5O₂, Ce_0.99Eu_0.01O₂, Zr_0.99Eu_0.01O₂, and Fe₂Mn_0.5Zn_0.5O₄), semiconductors (PbS, CdS, Ag₂S, ZnS, CdSe, PbSe, Ag₂Se), fluorides (CaF₂, YF₃, NdF₃, PrF₃), phosphates (CePO₄, HoPO₄), and chromates (BaCrO₄ and PbCrO₄). There are two synthetic strategies: 1) the use of oil-in water (O/W) microemulsions, in which the precursor is an ionic salt which is dissolved in the continuous aqueous phase; and 2) use of O/W microemulsions, in which the precursor is an organometallic salt dissolved in the oil droplets of the microemulsion. The latter approach keeps more resemblance to the typical W/O microemulsion reaction method, as it has the greatest level of precursor confinement.     

Enhancement on the structural,functional, optical and morphological properties of temperature treated silver sulfide nanostructures

The Silver Sulfide (Ag₂S) nanostructures were synthesized via the facile co-precipitation method. Thorough study and analysis were carried out to reveal and compare the structural, optical, functional, and morphological characteristics of as-synthesized samples annealed at various temperatures. The XRD analysis characterized the structural properties of Ag₂S nanoparticles, which unveiled the excellent crystallinity and monoclinic structure. The as-synthesized samples show an average crystallite size of 52 nm–41.7 nm. The modes of vibration and peak position of metal sulfides in Ag₂S nanoparticles were investigated through the FTIR technique. The optical attributes of prepared samples were scrutinized using UV–Vis analysis, which portrays the cut-off wavelength in the range of 1192–1223 nm for non-annealed and annealed Ag₂S nanoparticles, alongside the optical band gap is about 0.86 eV–0.96 eV. This work elucidates a novel approach to synthesis and scrutinises the characteristics of Ag₂S nanoparticles by subjecting them to distinct annealing temperatures precisely, as-prepared, 200 °C and 400 °C.     

1,4‐Bis((1H‐pyrrol‐2‐yl)methylene)thiosemicarbazide Complexes of Zn(II), Cd(II) and Hg(II): Single Source Precursor in Thermal Synthesis of Nanoparticle

Six complexes of Zn(II), Cd(II) and Hg(II) with sulphur containing Schiff base ligand, 1,4‐bis((1H‐pyrrol‐2‐yl)methylene)thiosemicarbazide in 1:1 and 1:2 ratio has been synthesized. Complexes were characterized by molar conductance measurement, elemental analyses, FT‐IR, ¹H‐NMR, and FAB/ESI‐Mass. The complexes were used as a single source precursor for the synthesis of ZnS/CdS/HgS nanoparticles by their thermal decomposition in the presence of different surfactants. The precursor: surfactant ratio and temperature plays important role in determining the size of the nanoparticles. The size and morphology of nanoparticles has been ascertained by UV‐Vis spectroscopy, XRD measurements and Transmission Electron Microscopy (TEM). Schiff base, complexes and nanoparticles were tested for antibacterial activity and MIC values against E. coli. The complexes were found more potent than the corresponding Schiff bases and nanoparticles.     

水溶性的CdSe/CdS/ZnS量子点的合成及表征

用L-半胱氨酸盐(Cys)作为稳定剂,合成了水溶性的双壳结构的CdSe/CdS/ZnS半导体量子点。吸收光谱和荧光光谱结果表明,双壳结构的CdSe/CdS/ZnS纳米微粒比单一的CdSe核纳米粒子和单核壳结构的CdSe/CdS纳米粒子具有更优异的发光特性。用透射电子显微镜(TEM)、ED、XRD、XPS和FTIR等方法对CdSe核和双壳层的CdSe/CdS/ZnS纳米微粒的结构、分散性及形貌分别进行了表征。     

Synthesis and Characterization of Silver Sulfide Nanoparticles Containing Sol-Gel Derived HPC-Silica Film for Ion-Selective Electrode Application

Silver sulfide nanoparticles dispersed in sol-gel derived hydroxypropyl cellulose (HPC)-silica films have been successfully synthesized using H₂S gas diffusion method. This is the first attempt to produce silver sulfide nanoparticles using this technique. Ag₂S nanoparticles are generated through reaction of H₂S gas with AgNO₃ precursor dissolved in the HPC-silica matrix. Transmission electron microscope (TEM) and atomic force microscope (AFM) analysis reveal nanoparticles size distribution from 2.5 nm to 56 nm for H₂S gas exposed sample. The surface chemistry of Ag₂S nanoparticles and sol-gel derived HPC-silica matrix is confirmed by X-ray photoelectron spectroscopy (XPS). The negative shifts in the core-level XPS Ag (3d) binding energy of Ag₂S nanoparticles are attributed to Ag : S surface atomic ratio exhibited by these nanoparticles with varying processing conditions. Following processing and characterization, suitability of the present method to produce silver sulfide ion-selective electrode is demonstrated by depositing Ag₂S nanoparticles on a graphite rod. The high reponse function of the electrode is due to the presence of nanoparticles.     

Integration of Semiconducting Sulfides for Full‐Spectrum Solar Energy Absorption and Efficient Charge Separation

The full harvest of solar energy by semiconductors requires a material that simultaneously absorbs across the whole solar spectrum and collects photogenerated electrons and holes separately. The stepwise integration of three semiconducting sulfides, namely ZnS, CdS, and Cu_2?xS, into a single nanocrystal, led to a unique ternary multi‐node sheath ZnS–CdS–Cu_2?xS heteronanorod for full‐spectrum solar energy absorption. Localized surface plasmon resonance (LSPR) in the nonstoichiometric copper sulfide nanostructures enables effective NIR absorption. More significantly, the construction of pn heterojunctions between Cu_2?xS and CdS leads to staggered gaps, as confirmed by first‐principles simulations. This band alignment causes effective electron–hole separation in the ternary system and hence enables efficient solar energy conversion.