Synthesis and optical properties of CuS nanoplate-based architectures by a solvothermal method

The controlled synthesis of copper sulfide (CuS) nanoplate-based architectures in different solvents has been realized at low cost by simply reaction of Cu(NO₃)₂·3H₂O and S under solvothermal conditions without the use of any template. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis spectrometer and fluorescence measurement were used to characterize the products. The products were all in hexagonal phase with high crystallinity and the morphology was significantly influenced by the solvents. The CuS products synthesized in dimethylformamide (DMF) were nanoplates and the samples prepared in ethanol were flower-like morphology composed of large numbers of nanoplates, but those synthesized in ethylene glycol (EG) were CuS architectures with high symmetry made up of several nanoplates arranged in a certain mode. The optical properties were investigated and the growth mechanisms of these CuS crystals were also proposed.     

Simple routes to synthesis and characterization of nanosized tin telluride compounds

Nanosized tin telluride compounds were prepared by chemical reduction process and hydrothermal methods. The nanosized SnTe compounds were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The SnTe nanoalloy prepared by chemical reduction process presented quasi-spherical morphology with aggregation. The sizes of particle were 40-50 nm. The powder prepared by hydrothermal process was nearly nanospheres, and the particle sizes were 30-40 nm with narrow distribution. The effect of capping agent, reductant sort, and reaction temperature on the morphology, the particle sizes and the phase of SnTe alloys have been investigated. Experimental results indicated that N₂H₄·H₂O plays a crucial role in the formation of nanosized rode-like SnTe compounds.     

Hydrothermal preparation and characterization of Cd0.9Mn0.1S nanorods

Cd_0.9Mn_0.1S semiconductor nanorods were successfully prepared by the hydrothermal reaction of CdCl₂·2.5H₂O and MnCl₂·5H₂O with (NH₄)₂S in aqueous solution. Atomic absorption spectrometry (AAS) and energy dispersive spectroscopy (EDS) were used to determine the Mn contents of these complex nanorods. The samples were characterized by scanning electron microscopy (SEM-EDS), X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-vis absorption spectra, photoluminescence (PL) and compared with the undoped CdS nanorods. The results showed that nanostructured multiplex compounds with high aspect ratio were obtained via hydrothermal method. The products showed almost totally rod-like morphology with approximately identical diameter about 20 nm and the maximal length up to 200 nm.     

Characterizations of octahedral zinc oxide synthesized by sonochemical method

The ultrasonic reaction of zinc nitrate hexahydrate (Zn(NO₃)₂·6H₂O) and hexamethylenetetramine (C₆H₁₂N₄) was investigated by varying the concentration of the reactants, the irradiation time, and the type of sonicator. The morphology, composition, and phase structure of the products were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) and ultraviolet-visible (UV-vis) spectroscopy. Octahedral zinc oxide (ZnO) micropowders were formed at low concentrations, 0.05 M, of Zn(NO₃)₂·6H₂O and C₆H₁₂N₄ in both lab-made sonicator and commercial ultrasonic bath. However, at concentrations between 0.1 and 1.0 M Zn(NO₃)₂-C₆H₁₂N₄ mainly plate-like zinc hydroxide nitrate hydrate (Zn₅(OH)₈(NO₃)₂(H₂O)₂) resulted with only a small fraction of ZnO, irrespective of the irradiation time employed, highlighting the sensitivity of the system to the concentration of the starting materials. Heat treatment of Zn₅(OH)₈(NO₃)₂(H₂O)₂ at 350 °C in air affords a ZnO phase of irregular morphology. Octahedral ZnO is found to exhibit slightly lower IR absorption and similar UV absorption to that of commercial prismatic hexagonal ZnO, although an extra peak due to small quantities of Zn₅(OH)₈(NO₃)₂(H₂O)₂ is observed.     

Preparation and characterization of SnO nanowhiskers

In this paper, some single-crystalline Stannous oxide (SnO) nanowhiskers were successfully prepared by a wet method using SnCl₂·2H₂O as raw material and cetyltrimethylammoniumbromide (CTAB) as surfactant. The morphologies, purity and sizes of the products were characterized by transmission electron microscopy, powder X-ray diffractmetry and standard selected area electron diffraction. The results showed that the diameter and the length of the particles were 10-30 and 200-400 nm, respectively. The influence of some reaction parameters, including the pressure, the temperature, the surfactant and the reaction duration, on the formation, morphology and particle size of SnO crystallite is discussed.     

Chondroitin sulfate template-mediated biomimetic synthesis of nano-flake hydroxyapatite

By Ca(NO₃)₂·4H₂O and (NH₄)₃PO₄·3H₂O as reagents and chondroitin sulfate (ChS) as a template, nano-flake hydroxyapatite (HA) is synthesized using a biomimetic method according to the biomineralization theory. HA crystals obtained are characterized in crystalline phase, microstructure, chemical composition and morphology by X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), transmission electron microscopy (TEM) and elemental analysis respectively. UV-vis spectrum is adopted to investigate interactions between functional groups ChS and HA. The results show that HA crystal nucleation and growth take place in chemical interactions between HA crystals and ChS as a template. And elemental analysis indicates that obtained HA contains a small amount of ChS. Furthermore, ChS concentration significantly affects the morphology of HA crystals. Staple-fiber-like HA crystals can be obtained at a low concentration in ChS, and flake-like HA crystals synthesized at a high concentration (≥0.5 wt.%) of ChS as a template.     

Hydrothermal synthesis and characterization of nanocrystalline Zn-Mn spinel

Hydrothermal method had been used to successfully synthesize the nanocrystalline spinel zinc manganese oxide (ZnMn₂O₄) directly from Zn(CH₃COO)₂·2H₂O, NaOH, Mn(NO₃)₂ and H₂O₂ at 170 °C for the reaction time of 48 h. The effects of the synthesis conditions, such as the Zn/Mn molar ratio, the reaction temperature, the reaction time, the zinc source and the concentrations of NaOH and H₂O₂, on the formation of the Zn-Mn spinel were investigated. The products were characterized by means of X-ray diffraction (XRD), inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The results indicated that the compositions of the Zn-Mn spinel with the tetragonal structure were Zn_1.14Mn_1.86O₄. Scanning electron microscope (SEM) and transmission electron microscopy (TEM) images showed that the products at 170 °C were with square-shaped nanocrystalline spinel with the particle size of about 20-50 nm. The thermal behaviors of the products were investigated by thermogravimetric analysis (TG).     

Synthesis of quasi-1D cuprous oxide nanostructure and its structural characterizations

A wealth of superfine polycrystalline cuprous oxide (Cu₂O) nanowires have been synthesized with hydrazine hydrated (N₂H₄·H₂O), act as the reducing agent, and Cu(OH)₂ nanowires, act as a soft template and surfactant, at room temperature. Two methods were employed for the synthesis of these nanowires, i.e. with and without capping agent (polyethylene glycol Mw 8000). Techniques of powder X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED) pattern, electron diffraction X-ray (EDX) spectroscopy, and UV-visible (UV-vis) spectroscopy have been used to characterize the morphology, structure, crystallinity, purity, and composition of nanowires. The average diameters of Cu₂O nanowires, prepared with and without capping agent, were observed to be 8-10 and 12-15 nm and lengths of several microns, respectively. It is found that capping agent (PEG) confines the dimensions of synthesized nanowires. In addition, the observed optical band gap of products show blue-shift effect compared to the bulk Cu₂O (E_g=2.17 eV), which ascribe it as a promising material for the conversion between solar energy and electrical or chemical energy.     

Synthesis of basic magnesium carbonate microrods with a “house of cards” surface structure using rod-like particle template

Basic magnesium carbonate (Mg₅(CO₃)₄(OH)₂·4H₂O) microrods with a surface structure of “house of cards” have been synthesized without any alkaline reagent, using rod-like particles, magnesium carbonate trihydrate, as templates. The product was characterized by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM). The transformation process from rod-like MgCO₃·3H₂O particles to Mg₅(CO₃)₄(OH)₂·4H₂O microrods with a surface structure of “house of cards” was recorded. Preliminary discussions on possible growth mechanisms of Mg₅(CO₃)₄(OH)₂·4H₂O microrods are also proposed in this paper.     

Direct synthesis of beta gallium oxide nanowires, nanobelts, nanosheets and nanograsses by microwave plasma

In this study, beta-gallium oxide (β-Ga₂O₃) nanowires, nanobelts, nanosheets, and nanograsses were synthesized through microwave plasma of liquid phase gallium containing H₂O in Ar atmosphere using silicon as the substrate. The nanowires with diameters of about 20-30 nm were several tens of microns long and the nanobelts with thickness of about 20-30 nm were tens to hundreds of microns long. The morphology and structure of products were analyzed by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM) and X-ray diffraction (XRD). These results showed that multiple nucleation and growth of β-Ga₂O₃ nanostructures could easily occur directly out of liquid gallium exposed to appropriate H₂O and Ar in the gas phase. The growth process of β-Ga₂O₃ nanostructures may be dominated by VS (vapor-solid) mechanism.     

A facile method to the cube-like MnSe2 microcrystallines via a hydrothermal process

A convenient hydrothermal process was applied to prepare the cube-like MnSe₂ microcrystallines through the reaction of MnSO₄·H₂O with Se and NaH₂PO₂·H₂O in aqueous solution at 160 °C for 12 h. Powder X-ray diffraction (XRD) analysis confirmed that the product was the cubic phase of MnSe₂ with cell parameter a=6.440 Å. The chemical composition of the MnSe₂ was determined by XPS. The Raman spectrum of MnSe₂ presented the peaks of the Se-Se stretching mode at 232.44 and 266.58 cm⁻¹. The images of scanning electron microscope (SEM) and transmission electron microscope (TEM) showed the cube-like morphology of the product with the edge length ranging from 20 to 30 μm. The formation mechanism of the MnSe₂ microcrystallines was discussed as well.     

Room temperature synthesis of Cu2O nanocubes and nanoboxes

Monodisperse Cu₂O nanocubes are synthesized by reducing freshly prepared Cu(OH)₂ with N₂H₄·H₂O in water at room temperature. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations show that most of these nanocubes are uniform in size, with the average edge length of ∼500 nm. Selected area electron diffraction (SAED) investigation reveals that these nanocubes are single crystalline. Further, Cu₂O nanoboxes are obtained by etching Cu₂O nanocubes with acetic acid solution at room temperature. The nanoboxes retain the size and external morphology of the nanocubes.     

Structural characterization of nanocrystalline CrOOH·2H2O aerogel by X-ray diffraction

The nanostructured powder prepared by critical CO₂ extraction of the urea-assisted wet chromia gel mixture at 373 K in vacuum was studied by X-ray diffraction techniques. Thermoanalytical methods showed the presence of the lattice water molecules in the resulting phase corresponding to a chemical formula CrOOH·2H₂O. The CrOOH·2H₂O nanocrystals of 3-5 nm in diameter were observed in transmission electron microscopy and their structure was derived from the Rietveld analysis in which the disorder contribution to the X-ray scattering was implemented. The structural model shows that the hexagonal unit cell of α-CrOOH undergoes monoclinic distortion with half of the O⁻² anions and OH⁻ groups being replaced by bonded water molecules in the three-dimensional packing resulting in half of the sites in regular Cr⁺³ octahedra being vacant. Further examination of the quasi-crystalline disordered state of the CrOOH·2(H₂O) nanocrystals was performed by model independent method of Radial Distribution Function (RDF). This complementary technique is sensitive to the molecular composition and allows to assess the average atomic (or electron) density distribution and the spacings of the atomic arrangements in the nearest neighbor shells comprising the range of the crystalline order in the structure of this material.     

Surface of Zn-Mn-O and its role in room temperature ferromagnetism: An XPS analysis

The existence of ferromagnetism in Zn-Mn-O semiconductor samples and dependence on the preparation condition were investigated. We systematically examined the samples with manganese concentration ranging from 0 to 10 at.%, prepared by a solid state reaction route using (ZnC₂O₄·2H₂O)_1−x and (MnC₂O₄·2H₂O)_x as precursors. Thermal treatment was carried out in air at temperatures ranging from 400 to 900 °C. The samples were investigated by X-ray diffraction, transmission electron microscopy, magnetization measurements and XPS spectroscopy. XPS surface composition, chemical analysis and depth profiling were successfully employed on powder revealing the chemical composition at the surface of the grains and underneath. The present investigation suggests that physical properties and observed room temperature ferromagnetism might be due to grain surface effects. It seems that the ferromagnetic phase is correlated with oxygen build up at the surface.     

Formation of self-assembled quantum dots of iron oxide thin films by spray pyrolysis from non-aqueous medium

Quantum dots (QDs) of iron oxide have been deposited onto ITO coated glass substrates by spray pyrolysis technique, using ferric chloride (FeCl₃·7H₂O) in non-aqueous medium as a starting material. The non-aqueous solvents namely methanol, ethanol, propanol, butanol and pentanol were used as solvents. The effect of solvents on the film structure and morphology was studied. The structural, morphological, compositional and optical properties were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive analysis of X-rays (EDAX), and optical absorption measurement techniques.     

Facile synthesis of calcium silicate hydrate using sodium dodecyl sulfate as a surfactant assisted by ultrasonic irradiation

Calcium silicate hydrate (CSH) consisting of nanosheets has been successfully synthesized assisted by a tip ultrasonic irradiation (UI) method using calcium nitrate (Ca(NO₃)·4H₂O), sodium silicate (Na₂SiO₃·9H₂O) and sodium dodecyl sulfate (SDS) in water. Systematic studies found that reaction time of ultrasonic irradiation and concentrations of surfactant (SDS) in the system were important factors to control the crystallite size and morphologies. The products were characterized by X-ray power diffraction (XRD), field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectrometry (FTIR). The size–strain plot (SSP) method was used to study the individual contributions of crystallite sizes and lattice strain on the peak broadening of the CSH. These characterization techniques revealed the successful formation of a crystalline phase with an average crystallite size of about 13 nm and nanosheet morphology at a reaction time of 10 min UI with 0.2 g SDS in solvent which were found to be optimum time and concentrations of SDS for the synthesis of CSH powders.     

Temperature controlled synthesis of SrCO3 nanorods via a facile solid-state decomposition rout starting from a novel inorganic precursor

Strontium carbonate nanorods have been successfully synthesized via solid-state decomposition of a new precursor, [Sr(Pht)(H₂O)₂]. The obtained nanorods were found to be orthorhombic with the length of 70-100 nm and the diameter of about 10-15 nm. The Effect of calcinations temperature on morphology and purity of the products has been investigated. Strontium carbonate nanorods were formed at 500 °C. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transform infrared (FT-IR) spectroscopy. In addition, further evidence for the purity and stoichiometry of the product was obtained by XPS (X-ray photoelectron spectroscopy) spectrum.     

Synthesis and characterization of CdS nanoparticles in the presence of oleic acid as solvent and stabilizer

Oleic acid (OA)-capped CdS nanoparticles (NPs) have been successfully synthesized via the direct reaction of Cd(CH₂COO)₂·2H₂O with S powder in OA solvent at 230 °C under nitrogen flow, which was a kind of clean and air-stable solvent. The morphologies and structures of the as-synthesized CdS NPs are examined by transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), X-ray diffractometer (XRD), and Fourier transform infrared (FTIR) spectroscopy, and the typical Ostwald ripening growth mechanism is concluded. Moreover, the collected ultraviolet–visible (UV–vis) absorption spectroscopy and photoluminescence (PL) spectroscopy demonstrate good optical properties of CdS NPs.     

PAA-assisted synthesis of CaCO3 microcrystals and affecting factors under microwave irradiation

In the present paper, we described a polyacrylic acid (PAA)-assisted microwave irradiation route for synthesis of Calcium carbonate (CaCO₃) microcrystals. CaCl₂·2H₂O and NaHCO₃ were used as the starting reactants. Researches showed that the presence of PAA could strongly affect the phase and morphology of CaCO₃ crystals. X-ray powder diffraction (XRD) analyses showed that the product prepared from the system with/without PAA corresponded to Vaterite/Calcite, respectively. Scanning electron microscopy (SEM) observations showed that the hierarchical CaCO₃ microcrystals were obtained in the presence of PAA. Some factors influencing the morphology of the as-synthesized CaCO₃ crystals were systematically investigated.     

Synthesis and electrochemical properties of Ni doped titanate nanotubes for lithium ion storage

Ni doped titanate nanotubes were synthesized by hydrothermal method using Ni doped rutile TiO₂ nanopowders as a starting material. The electrochemical properties were investigated by cyclic voltammmetric methods. The microstructure and morphology of the synthesized powders were characterized by XRD (X-ray diffraction), and HRTEM (high resolution transmission electron microscopy). Ni doped nanotubes were composed of H₂Ti₂O₅·H₂O with outer and inner diameter of ∼10 nm and 6 nm and showed a initial discharge capacity of 305 mAh/g with poor cycling performance. However, after firing, the Ni doped nanotubes revealed better cycling performance due to lower reaction with hydrate and smaller diameter of the tubes.