Solvothermal synthesis of In(OH)3 nanorods and their conversion to In2O3

In this work, we demonstrate that monodisperse indium hydroxide (In(OH)₃) nanorods constructed with parallel wire-like subunits have been fabricated via a acrylamide-assisted synthesis route without any template. NH₃ from the hydrolysis of acrylamide acts as the OH⁻ provider. The structure and morphology of as-prepared products have been characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM) and thermogravimetric analysis (TG). A detailed mechanism has been proposed on the basis of time-dependent experimental results. Furthermore, by annealing In(OH)₃ precursors at 500 °C for 3 h in air, In₂O₃ samples were obtained with the designed morphology.     

Characterization of Bi2S3 nanorods and nano-structured flowers prepared by a hydrothermal method

Bismuth sulfide nanorods and nano-structured flowers were synthesized by hydrothermal reaction of bismuth nitrate pentahydrate and thiourea solutions, containing 1 and 2 ml of 65% HNO₃, respectively. By using X-ray diffraction (XRD), selected area electron diffraction (SAED), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution TEM (HRTEM), the products were specified as orthorhombic Bi₂S₃ in the shapes of nanorods and flower-like clusters of nanorods, with the growth of nanorods in the [001] direction. A diffraction pattern was also simulated, and was in good accordance with the SAED pattern obtained from the experiment.     

Photoluminescence properties of the In2O3 octahedrons synthesized by carbothermal reduction method

In₂O₃ octahedrons were synthesized by carbothermal reduction method. The products were characterized by X-ray diffraction (XRD), energy dispersive X-ray (EDX), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electron diffraction analysis (SAED) and room-temperature photoluminescence (PL) spectra. The results show that the products are single-crystalline In₂O₃ octahedrons with the arrises length in the range of 400-3000 nm. The PL spectra displays blue and green emission peaks which can be indexed to default and oxygen vacancies; blue-shift and intensity decrease was observed when excitation wavelength decreases from 380 nm to 325 nm. The growth mechanism of the In₂O₃ octahedrons is discussed.     

Synthesis of (K, Na)NbO3 particles by high temperature mixing method under hydrothermal conditions

In order to prepare the pure (K, Na)NbO₃(KNN) particles with higher crystallinity, the high temperature mixing method (HTMM) under hydrothermal conditions was carried out in this work. The obtained samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and high-resolution transmission electron microscopy (HRTEM). The results indicate that the KNN particles size decrease gradually with the increase of mineralization concentration in the starting solution. The ratio of K⁺/(K⁺ + Na⁺) in the starting solution has a great effect on the phase of the products, and several phases coexist in the product when the ratio of K⁺/(K⁺ + Na⁺) in the starting solution is 0.7.     

Template-free hydrothermal synthesis and high photocatalytic activity of ZnWO4 nanorods

ZnWO₄ nanorods are successfully synthesized by a template-free hydrothermal method, and are characterized in detail by X-ray diffractometer (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED). The results show that the ZnWO₄ nanorods with wolframite structure are well-crystallized single crystallites. The crystallinity of the products is influenced by the pH value of initial precursor suspension. The width and length of the synthesized samples increase with hydrothermal reaction temperature. The photocatalytic efficiency of the ZnWO₄ nanorods for degradation of methylene blue (MB) in aqueous solution under UV light irradiation declines greatly with increasing crystallinity. The ZnWO₄ nanorods prepared at pH of 4 have the best activity in photo-degradation of MB. After six recycles, photocatalytic activity loss of the catalyst is not obvious.     

Preparation and characterization of CuO nanorods by thermal decomposition of CuC2O4 precursor

Synthesis of copper oxide (CuO) nanorods was achieved by thermal decomposition of the precursor of CuC₂O₄ obtained via chemical reaction between Cu(CH₃COO)₂·H₂O and H₂C₂O₄·2H₂O in the presence of surfactant nonyl phenyl ether (9)/(5) (NP-9/5) and NaCl flux. Transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), selected-area electron diffraction (SAED) and high-resolution TEM (HRTEM) were used to characterize the structure features and chemical compositions of the as-made nanorods. The results showed that the as-prepared nanorods is composed of CuO with diameter of 30-100 nm, and lengths ranging from 1 to 3 μm. The mechanism of formation of CuO nanorods was also discussed.     

Synthesis of GaN nanorods by ammoniating Ga2O3 films on TiO2 (rutile) layer deposited on Si(111) substrates

GaN nanorods have been synthesized by ammoniating Ga₂O₃ films on a TiO₂ middle layer deposited on Si(111) substrates. The products were characterized by X-Ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transformed infrared spectra (FTIR) and high-resolution transmission electron microscopy (HRTEM). The XRD analysis indicates that the crystallization of GaN film fabricated on TiO₂ middle layer is rather excellent. The FTIR, SEM and HRTEM demonstrate that these nanorods are hexagonal GaN and possess a rough morphology with a diameter ranging from 200 nm to 500 nm and a length less than 10 μm, the growth mechanism of crystalline GaN nanorods is discussed briefly.     

Facile one-pot synthesis and luminescence of hexagonal TbPO4·nH2O hollow spheres

Monodisperse hexagonal TbPO₄·nH₂O hollow spheres were successfully obtained by utilizing Tb(OH)CO₃ colloidal spheres as the precursor and NH₄H₂PO₄ as the phosphorus source through the hydrothermal process. The obtained hollow spheres were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), respectively. They have the average diameter of 200 nm. There are a number of tiny nanorods with the length of about 60 nm on the surface of the spheres. The obtained TbPO₄ hollow spheres exhibit green color emission from ⁵D₄ − ⁷F_J (J = 6, 5, 4, 3) transitions of the Tb³⁺ ions, which are expected to be applied in display applications and biological applications.     

Large-scale synthesis and characterization of fan-shaped rutile TiO2 nanostructures

Large-scale fan-shaped rutile TiO₂ nanostructures have been synthesized by means of a simple hydrothermal method using only TiCl₄ as titanium source and chloroform/water as solvents. The physicochemical features of the fan-shaped TiO₂ nanostructures are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), nitrogen absorption-desorption, diffuse reflectance ultraviolet-visible spectroscopy (UV-vis) and Fourier transform infrared spectroscopy (FTIR). Structural characterization indicates that the fan-shaped TiO₂ nanostructures are composed of several TiO₂ nanorods with diameters of about 5 nm and lengths of 300-350 nm. The average pore size and BET surface area of the fan-shaped TiO₂ nanostructures are 6.2 nm and 59 m²/g, respectively. Optical adsorption investigation shows that the fan-shaped TiO₂ nanostructures possess optical band gap energy of 3.11 eV.     

Hydrothermal synthesis of monodisperse CeO2 nanocubes

Monodisperse CeO₂ nanocubes have been fabricated via an acrylamide-assisted hydrothermal route. NH₃ and acrylic acid from the hydrolysis of acrylamide act as OH⁻ provider and capping reagent, respectively. The structure and morphology of the products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), field-emission scanning electron microscopy (FE-SEM) and Fourier transformed infrared (FT-IR). The products have a cubic morphology with a mean size of 200 nm. The possible formation mechanism has been discussed based on the experimental results.     

Self-assembly growth of BiFeO3 powders prepared by microwave-hydrothermal method

With FeCl₃·6H₂O and Bi(NO₃)₃·5H₂O powder as raw materials and KOH as a mineralizer, the pure phase BiFeO₃ (BFO) powder was synthesized by microwave-hydrothermal (MH) method at 200 °C, with the reaction time as little as 30 min. The range of preparing the BFO powders had been summarized. The field emission scanning electron microscopy (FE-SEM) images revealed that the little BFO plate grew together forming rock sugar-like BFO powders, and then they grew further to form the mussel-like BFO powders. The transmission electron microscope (TEM) images also improved the self-assembly growth of BFO powders. The X-ray diffraction (XRD), the high resolution transmission electron microscopy (HRTEM) and the selected area electron diffraction (SAED) results indicated that the BFO powders grew along the [110] and [104] crystal orientation. The B-H loops of BFO indicated that the weak magnetism existed in the pure phase BFO powders.     

Synthesis and characterization of bundle-like structures consisting of single crystal Ce(OH)CO3 nanorods

Bundle-like structures consisting of single crystal cerium hydroxide carbonate (Ce(OH)CO₃) nanorods have been synthesized successfully by a hydrothermal method at 100 °C using cerium nitrate (Ce(NO₃)₃·6H₂O) as the cerium source, aqueous carbamide both as an alkaline and carbon source and cetyltrimethylammonium bromide (CTAB) as surfactant. X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) were used to characterize such bundle-like structures. SEM and TEM images show that Ce(OH)CO₃ bundle-like structures were composed of nanorods with diameters of ∼ 100 nm. The XRD pattern and electron diffraction (ED) pattern indicate that Ce(OH)CO₃ has a pure orthorhombic single crystal structure.     

PEG-300 assisted hydrothermal synthesis of 4ZnO·B2O3·H2O nanorods

4ZnO·B₂O₃·H₂O is commonly used as a flame-retardant filler in composite materials. The microstructure of the powder is of importance in its applications. In our study, for the first time, one-dimensional (1D) nanostructure of 4ZnO·B₂O₃·H₂O with rectangle rod-like shape has been synthesized by a hydrothermal route in the presence of surfactant polyethylene glycol-300 (PEG-300). The nanorods have been characterized by X-ray powder diffraction (XRD), inductively coupled plasma with atomic emission spectroscopy (ICP-AES), thermogravimetry (TG) and differential thermal analysis (DTA), scanning electron microscopy (SEM), transmission electron microscopy (TEM) equipped with selected area electron diffraction (SAED) as well as high-resolution transmission electron microscopy (HRTEM). These nanorods are about 70 nm in thickness, 150-800 nm in width and have lengths up to a few microns. 4ZnO·B₂O₃·H₂O nanorods crystallize in the monoclinic space group P2₁/m, a = 6.8871(19) Å, b = 4.9318(10) Å, c = 5.7137(16) Å, β = 98.81(21)° and V = 191.779(71) Å³.     

Hydrothermal synthesis and characterization of CePO4/C core-shell nanorods

The CePO₄/C nanocomposite with core-shell nanostructure has been successfully synthesized using glucose and CePO₄ by a facile and simple hydrothermal method at 160 °C for 24 h. The new material consists of a monoclinic CePO₄ core and an amorphous-C shell. The TEM micrograph indicated that the CePO₄/C nanocomposite was core-shell nanorods. The effects of glucose concentration on the C shells and luminescent intensity of CePO₄/C nanocomposite were investigated. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS) and photoluminescence (PL). This method is simple, low-cost and does not need any surfactant.     

Hydrothermal synthesis, characterization, photocatalytic activity and dye-sensitized solar cell performance of mesoporous anatase TiO2 nanopowders

Mesoporous anatase TiO₂ nanopowder was synthesized by hydrothermal method at 130 °C for 12 h. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), HRTEM, and Brunauer-Emmett-Teller (BET) surface area. The as-synthesized sample with narrow pore size distribution had average pore diameter about 3-4 nm. The specific BET surface area of the as-synthesized sample was about 193 m²/g. Mesoporous anatase TiO₂ nanopowders (prepared by this study) showed higher photocatalytic activity than the nanorods TiO₂, nanofibers TiO₂ mesoporous TiO₂, and commercial TiO₂ nanoparticles (P-25, JRC-01, and JRC-03). The solar energy conversion efficiency (η) of the cell using the mesoporous anatase TiO₂ was about 6.30% with the short-circuit current density (Jsc) of 13.28 mA/cm², the open-circuit voltage (Voc) of 0.702 V and the fill factor (ff) of 0.676; while η of the cell using P-25 reached 5.82% with Jsc of 12.74 mA/cm², Voc of 0.704 V and ff of 0.649.     

Polymer-assisted synthesis of Co2P nanocrystals

Co₂P nanocrystals were successfully synthesized by a polymer-assisted hydrothermal method. The reaction was carried out at 190 °C-220 °C using cobalt chloride hexahydrate (CoCl₂·6H₂O) as Co-source and yellow phosphorous as P-source. Polyacrylamide (PAM) was used as surfactant. By controlling the experiment parameters such as the reaction temperature and the amount of polyacrylamide (PAM), Co₂P nanocrystals with the rod-like or flower-like morphology could be prepared successfully. The phase and the morphology of the samples were characterized by X-ray diffraction (XRD), transmission electron microscopes (TEM), electron diffraction pattern (ED) and high resolution transmission electron microscope (HRTEM). Furthermore, based on the results of the TEM observation, the possible formation processes of the Co₂P nanorods or nanoflowers were also discussed.     

Characterization of cadmium sulfide nanorods prepared by the solvothermal process

Cadmium sulfide nanorods were successfully prepared from cadmium nitrate tetrahydrate and thiourea in ethylenediamine by 200 °C solvothermal reactions using hydroxyethyl cellulose (HEC) as a capping material. X-ray diffraction (XRD), selected area electron diffraction (SAED), and Raman spectroscopy showed that the products were hexagonal wurtzite CdS with the 1st and 2nd harmonic modes at 303.5 and 593.0 cm^− 1, respectively. The intensity ratios of the 2nd to 1st harmonic modes were increased with their aspect ratios, due to the great strength of exciton-phonon coupling. By using scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution TEM (HRTEM) and fast Fourier transformation (FFT), the products were in the shape of nanoparticles in the HEC-free solution, and became nanorods with higher aspect ratios in the HEC-added solutions — especially with longer reaction time. These nanorods were single crystals with growth in the [001] direction.     

Synthesis RMn2O5 (R = Gd and Sm) nano- and microstructures by a simple hydrothermal method

Single-phase RMn₂O₅ (R = Gd and Sm) nano- and microstructures have been successfully synthesized via a simple hydrothermal process at 250 °C for 24 h using NaOH as mineralizer. X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and selective area electron diffraction patterns (SAED) were used to characterize the as-synthesized GdMn₂O₅ and SmMn₂O₅ samples. The effect of NaOH concentration and the molar ratio of Mn²⁺/Mn⁷⁺ on the morphology and size of the final products was studied, and a possible formation mechanism of RMn₂O₅ (R = Gd and Sm) nanoplates and nanorods under hydrothermal conditions was proposed.     

Facile synthesis and electrochemical properties of Mn3O4 nanoparticles with a large surface area

Mn₃O₄ nanoparticles were prepared by a novel oxidation-precipitation method at a low temperature. The crystal phase, microstructure, surface area and electrochemical properties of the products were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), N₂ adsorption-desorption isotherms and cyclic voltammetry (CV). The results indicate that the addition of citric acid and tartaric acid remarkably reduced the particle size and increased the specific surface area of Mn₃O₄ nanoparticles. The samples prepared by the addition of citric acid and tartaric acid have a narrow particle size distribution of 5-10 nm, a surface area of 119 and 122 m²/g, and a capacitance of 171 and 172 F g⁻¹, respectively.     

A green hydrothermal route to GaOOH nanorods

GaOOH nanorods were synthesized by a green hydrothermal method at 200 °C using nanocrystalline Ga₂O₃ powders and distilled water as the starting materials, and characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and thermogravimetric and differential scanning calorimetry (TG-DSC) analysis.