A facile synthesis of CuInS2 nanoparticles from molecular single source precursors

CuInS2 nanoparticles have been synthesized via solvent thermolysis of novel bimetallic complexes of the general formula [(Ph3P)2CuIn(S2COR)4] (where R = CH3; C2H5; C(CH3)2); and [(Ph3P)2CuIn(SCH2CH2S)2]. These complexes have been prepared by the reactions of Na/KS2COR and NaSCH2CH2SNa with InCl3 and [(Ph3P)2CuNO3] in methanol, respectively. Solvent thermolyses of these complexes were carried out in ethylene glycol at 196 degrees C for different time periods. The nanoparticles obtained were characterized extensively by techniques like powder X-ray diffraction, transmission electron microscopy, selected area electron diffraction, and X-ray photoelectron spectroscopy. The optical band gap of the nanoparticles was determined by diffuse reflectance spectroscopy (DRS).     

One-pot synthesis of CuFeSe2 cuboid nanoparticles

Ternary semiconducting CuFeSe₂ nanocrystals of a particular shape and size were successfully synthesized using a cost-effective and simple one-pot chemical route. X-ray powder diffraction and field emission scanning electron microscopy results indicated that the as-synthesized CuFeSe₂ comprised cuboid nanoparticles with dimensions of 50–150 nm as well as a tetragonal phase. Elemental analysis yielded an atomic ratio of Cu:Fe:Se of 1:1.06:2.17. The synthesis temperature and the solvent octadecylamine were significant in determining the structural phases and morphologies of the final products. The optimal condition for synthesizing the tetragonal CuFeSe₂ phase with cuboid nanoparticles was a reaction temperature of 200 °C for 1 h in octadecylamine solvent. A possible mechanism of the formation of ternary CuFeSe₂ nanoparticles with controllable shapes is discussed.     

One-pot mechanical synthesis of the nanocomposite granule of LiCoO2 nanoparticles

The layered rock-salt LiCoO₂ granules consisted of the primary nanoparticles were successfully synthesized by one-pot mechanical method without external heating. The sizes of the primary nanoparticle and the granule observed using electron microscopy were 50–200 nm and 20 μm, respectively. The surface property of the primary nanoparticle was evaluated by STEM-EELS, which revealed that the primary particle possesses the lithium defective part at the surface. The penetration behavior of an electrolyte into the granule was also evaluated by STEM-EDX, which indicated that the electrolyte could not fully penetrate into the granule. The first charge and discharge capacities of Li-ion cell assembled with the synthesized LiCoO₂ granules were 140 and 120 mA h/g, respectively. The relationship between the particle structures of the synthesized LiCoO₂ granules and the electrochemical properties were discussed.     

One-pot solvothermal synthesis of size-controlled NiO nanoparticles

In this work, NiO nanoparticles with diameter of ～4.5?nm for application as electrode material in supercapacitor were directly synthesized by an one-pot solvothermal strategy using N,N-dimethylformamide (DMF) as solvent and hexadecyl trimethyl ammonium bromide (CTAB) as additive. The experiment results indicated that CTAB is the key for the phase formation of NiO. Ni(OH)₂ phase was formed in the absence of CTAB, while NiO phase was produced in the presence of CTAB as an additive. As compared with the NiO prepared by calcination on the layer-structured Ni(OH)₂ intermediate produced in the absence of CTAB, the NiO nanoparticles prepared by this strategy had smaller particle size. Due to large specific surface area, small size and residual Ni(OH)₂, these NiO nanoparticles presented high electrochemical performance. They had high specific capacitance of 1128?F?g^?1 at low current density of 3.1?A?g^?1 and 625.0?F?g^?1 at high current density of 62.5?A?g^?1.     

One-pot room temperature synthesis of biopolymer-capped ZnSe nanoparticles

The synthesis of monodispersed, starch-capped ZnSe nanoparticles via a facile, “green” and environmentally benign route at room temperature is being reported. The nanoparticles exhibited strong quantum confinement effect with respect to the bulk ZnSe. The transmission electron microscopy (TEM) image indicated that the particles were well dispersed and spherical in shape. The X-ray diffraction (XRD) analysis showed that the ZnSe nanoparticles were of the wurtzite structure, with average particle diameter of about 3.50 nm. The Fourier transform infrared (FT-IR) spectrum confirmed the presence of starch as passivating agent.     

One-pot morphology-controlled synthesis of various shaped mesoporous silica nanoparticles

A simple synthetic method has been developed for synthesis of mesoporous silica nanoparticles with versatile morphologies by adopting CTAB and C₁₂–OH as dual soft templates. In such a simple method, only by regulating the dose of C₁₂–OH and temperature, we can well-realize the silica nanoparticle morphological transformation from sphere to shell-like, rugby-like, peanut-like, hollow, and complex yolk–shell structures. These as-fabricated silica nanoparticles were characterized by scanning electron microscopy, transmission electron microscopy, Brunauer–Emmett–Teller (BET), and small-angle powder X-ray diffraction. The as-prepared mesoporous silica nanoparticles with versatile morphologies possessing varying BET surface areas, pore diameter, and pore distributions have some potential applications in separation, sensing, and heterogeneous catalysis.     

Solvothermal synthesis of CuInS2 powders and CuInS2 thin films for solar cell application

In this study, a facile solvothermal method was developed to prepare CuInS₂ powders and CuInS₂ thin films. The CuInS₂ powders and CuInS₂ thin films were prepared by solvothermal route using the precursor of Copper (II) chloride, indium (III) nitrate, thiourea, oxalic acid, hexadecyl trimethyl ammonium bromide and ethanol. The morphology, crystallographic structure, chemical composition and optical band gap of CuInS₂ powders and CuInS₂ thin films were investigated using scanning electronic microscope (SEM), X-ray diffraction (XRD), energy dispersive spectrometry (EDS) and UV–vis spectroscopy. The results reveal that both CuInS₂ powders and CuInS₂ thin films are in chalcopyrite phase. The CuInS₂ powders are mainly composed of flower-like microspheres. Both microstructure of the sphere surface and diameter of sphere are affected by indium nitrate concentration in precursors. The CuInS₂ thin films are composed of a large number of uniform flower-like nanosheets, and the nanosheets become smaller in size and denser in distribution density with increasing concentration of thiourea. The optical band gap is found to be 1.44 and 1.52 eV for CuInS₂ powders and CuInS₂ thin films, respectively. The deposition mechanism of the CuInS₂ is discussed.     

One-pot synthesis of magnetic γ-Fe2O3 nanoparticles in ethanol-water mixed solvent

Maghemite (γ-Fe₂O₃) nanoparticles were synthesized via a low-temperature solution-based method using ferric chloride hexahydrate and ferrous chloride tetrahydrate as precursors in the mixed solvent of ethanol and water. X-ray diffraction, energydispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy revealed that the obtained product was pure γ-Fe₂O₃. Transmission electron microscopy showed the morphology of the nanoparticles to be approximately spherical in shape with an average diameter of 11 nm. Magnetization measurements indicated the dry powders exhibit ferromagnetic behavior with a maximum saturation magnetization of 41.1 emu/g at room temperature.     

One-pot synthesis of AuPt alloyed nanoparticles by intense x-ray irradiation

We synthesized AuPt alloyed nanoparticles in colloidal solution by a one-pot procedure based on synchrotron x-ray irradiation in the presence of PEG (polyethylene glycol). The exclusive presence of alloyed nanoparticles with fcc structure was confirmed by several different experiments including UV-vis spectroscopy, x-ray diffraction (XRD) and transmission electron microscopy (TEM). The composition of the AuPt alloyed nanoparticles can be varied in a continuous fashion by simply varying the feed ratios of Au and Pt precursors. The nanoparticles exhibited colloidal stability and biocompatibility, important for potential applications.     

One-pot synthesis of hollow nickel phosphide nanoparticles with tunable void sizes using triphenylphosphine

Multifunctional nickel phosphide nanoparticles with hollow nanostructures are very attractive for their great potential in various applications. A facile one-pot synthetic technique was presented for preparing hollow Ni₂P nanoparticles with tunable void sizes using triphenylphosphine as a lower-price phosphorus source in mild temperature organic solution. Structural morphology and magnetic property of time-dependent products demonstrated the fabrication of interior voids induced by nanoscale Kirkendall effect. Void sizes tunable from about 5 to 60 nm in diameter were obtained using varied triphenylphosphine concentrations, showing that the triphenylphosphine can serve as a reactive surfactant to tune and heighten the void capacity based on the nanoscale Kirkendall effect.     

One-pot size and shape controlled synthesis of DMSO capped iron oxide nanoparticles

We report here the capping of iron oxide nanoparticles with dimethyl sulfoxide (DMSO) to make chloroform soluble iron oxide nanoparticles. Size and shape of the capped iron oxide nanoparticles are well controlled by simply varying the reaction parameters. The synthesized nanocrystallites were characterized by thermal analysis (TG-DTA), powder X-ray diffraction (XRD), transmission electron microscopy (TEM) for evaluating phase, structure and morphology. ¹H NMR spectra of the synthesized samples confirm DMSO, and the capping of DMSO on the ferrite samples. Shift of the S=O stretching frequency in Fourier transformed infra-red (FTIR) spectra indicates that the bonding between DMSO and ferrite is through an oxygen moiety. The magnetic measurements of all the synthesized samples were investigated with a SQUID magnetometer which shows that the magnetic properties are strongly dependent on the size as well as shape of the iron oxide.     

Formation and characterization of nanoparticles based CuInS2 absorbing layer for solar cell

CuInS2 powders have been successfully prepared by simple heating a mixture of copper nitrate, indium nitrate and thiourea in ethylene glycol. The prepared powders were fully characterized by SEM, XRD and UV-Vis spectroscopy. The particle shape of the powders obtained with an optimal condition showed spherical shape with about 50 nm in size. The XRD results showed more enhanced crystallized CuInS2 with chalcopyrite structure with increasing reaction time. The values in band-gap energy of nano-sized CuInS2 powders would be estimated 1.63 eV, blue-shifted from that of micron-sized powders due to size quantization effect.     

One-pot sonochemical synthesis of dendron-stabilized gold nanoparticles as promising nano-hybrid with potential impact in biological application

Dihydroxy fatty acid-based (DF) dendron-stabilized gold nanoparticles (AuNps) were synthesized without adding any external reducing or stabilizing agent. Each DHA base dendron (G1, G2, or G3) possesses a single thiol at the focal point and free -OH groups at the other terminal and as a result can be used to reduce AuCl₄⁻ to Au⁰ and stabilize the nascent AuNps by the thiol group. The size and distribution of the AuNp produced can also be correlated with the rate of Au (III) reduction. TEM images vividly demonstrate the specific morphology of gold nanoparticles with different sizes and shapes obtained by using different generations of DF dendrons.     

In situ one-step synthesis of CuInS2 thin films with different morphologies and their optical properties

Journal of Materials Science: Materials in Electronics - CuInS2 (CIS) thin films with petal-like nanostructures were synthesized in situ on copper substrates through a facile, one-step solvothermal...     

Combining thermolysis of molecular precursor with sol-gel process to zinc gallate nanoparticles

Zinc gallate nanoparticles were prepared by combining thermolysis of single molecular precursor with sol-gel method in the presence of a capping agent. The size and shape of zinc gallate nanoparticles could be controlled by changing the reaction temperature. Single molecular precursor with alkyl and alkoxide ligand was used for zinc gallate nanoparticles to ensure the correct stoichiometry of the product.     

One-pot synthesis and characterization of poly(alkoxysilane)s promoted by silver colloidal nanoparticles

Si-Si/Si-O dehydrocoupling of hydrosilanes with alcohols (1:1.5 mole ratio), catalyzed by AgNO3 which converted to Ag(0) colloidal nanoparticles, gave poly(alkoxysilane)s in one-pot in moderate to high yield. The hydrosilanes include p-X-C6H4SiH3 (X = H, CH3, OCH3, F), PhCH2SiH3, and (PhSiH2)2. The alcohols include MeOH, EtOH, (i)PrOH, PhOH, and CF3(CF2)2CH2OH. The weight average molecular weight and polydispersity of the poly(alkoxysilane)s were in the range of 1,600 approximately 8,000 Dalton and 1.4 approximately 3.5. The dehydrocoupling reactions of phenylsilane with ethanol (1:3 mole ratio) in the presence of the silver nanocolloid catalyst produced only triethoxyphenylsilane as product.     

Rapid preparation of CuInS2 microparticles via a solution-chemical synthesis route and its characterization

CuInS₂ microparticles were synthesized successfully by a facile solution-chemical method in a mixed solvent of triethylenetetramine–ethylene glycol (1:1, v/v) under the open-air condition using copper chloride, indium chloride and sulfur as starting materials. The factors including the temperature and reaction time which might affect the purity of the product during the synthesis were discussed. Phase constituents, morphology, structure and optical properties of the as-prepared CuInS₂ powders were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), Energy Dispersive Spectrometer (EDS), and ultraviolet–visible (UV–vis) spectrophotometry. It's found that the products were significantly affected by the temperature and reaction time. A possible formation mechanism was put forward and briefly discussed.     

Thermal decomposition studies of CuInS2

Single crystals of copper indium disulphide (CuInS₂) have been successfully grown by the chemical vapour transport (CVT) technique using iodine as the transporting agent. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were carried out for the CVT grown CuInS₂ single crystals. It was revealed that the crystals are thermally stable between the ambient temperature (300 K) and 845 K and that the decomposition occurs sequentially in three steps. The kinetic parameters, e.g., activation energy, order of reaction, and frequency factor were evaluated using non-mechanistic equations for thermal decomposition.