Synthesis of β-Ga2O3 nanowires through microwave plasma chemical vapor deposition

In this study, we demonstrate the large-scale synthesis of beta gallium oxide (β-Ga₂O₃) nanowires through microwave plasma chemical vapor deposition (MPCVD) of a Ga droplet in the H₂O and Ar atmosphere at 600 W. Unlike the commonly used MPCVD method, the H₂O, not mixture of gas, was employed to synthesize the nanowires. The ultra-long β-Ga₂O₃ nanowires with diameters of about 20-30 nm were several tens of micrometers long. The morphology and structure of products were analyzed by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscope (HRTEM). The growth of β-Ga₂O₃ nanowires was controlled by vapor-solid (VS) crystal growth mechanism.     

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.     

Mesoporous TiO2-B nanowires synthesized from tetrabutyl titanate

Ultralong mesoporous TiO₂-B nanowires were synthesized via a hybrid hydrothermal-ion exchanging-thermal treatment using tetrabutyl titanate (TBOT) as a raw material. The phase transformations and porous structures of TiO₂-B nanowires were characterized and studied by X-ray diffraction (XRD), transmission electron microscopy (TEM) and N₂ adsorption-desorption measurement. Mesoporous TiO₂-B nanowires showed a length of several micrometers and diameter of about 25 nm. The porous structures of obtained TiO₂-B nanowires were demonstrated by BJH pore distribution measurement. The wirelike morphologies and porous structures of monodisperse nanowires calcined at 600 °C showed little change, which indicated that such nanowires possessed high thermal stability. The formation mechanism of TiO₂-B nanowires with mesoporous structures were also discussed based on our experimental results.     

Fabrication and characterization of CuO-core/TiO2-shell one-dimensional nanostructures

We have fabricated CuO-core/TiO₂-shell one-dimensional nanostructures by coating the CuO nanowires with MOCVD-TiO₂. The structure of the core/shell nanowires has been investigated by using scanning electron microscopy, transmission electron microscopy, and X-ray diffraction analysis techniques. The CuO-cores and the TiO₂-shells of the as-synthesized nanowires have been found to have crystalline monoclinic CuO and crystalline tetragonal anatase TiO₂ structures, respectively. The CuO-core/TiO₂-shell nanowires are winding and has rougher surface, whereas the CuO nanowires are straight and have smoother surface.Influence of the substrate temperature and the growth time on the structure such as the morphology, size, and crystallographic orientation of CuO nanowires synthesized by thermal oxidation of Cu foils have also been investigated. All the nanowires have only the CuO phase synthesized at 600 °C, whereas those synthesized at 400 °C have both CuO and Cu₂O phases. The highest density of CuO nanowires with long thin straight morphologies can be obtained at 600 °C. In addition, the growth mechanism of the CuO nanowires has been discussed.     

Synthesis, crystal structure, Cu doped EPR, thermal and voltammetric studies of [Ni(isonicotinamide)2(H2O)4]·(sac)2 single crystal

The single crystal of [Ni(ina)₂(H₂O)₄]·(sac)₂, (NINS), (ina is isonicotinamide and sac is saccharinate) complex has been prepared and its structural, spectroscopic and thermal properties have been determined. The title complex crystallizes in monoclinic system with space group P2₁/c, Z=2. The octahedral Ni(II) ion, which rides on a crystallographic centre of symmetry, is coordinated by two monodentate ina ligands through the ring nitrogen and four aqua ligands to form discrete [Ni(ina)₂(H₂O)₄] unit, which captures two saccharinate ions in up and down positions, each through intermolecular hydrogen bands. The magnetic environment of copper(II) doped NINS crystal has also been identified by electron paramagnetic resonance (EPR) technique. The g and A values of Cu²⁺ doped NINS single crystal were calculated from the EPR spectra recorded in three mutually perpendicular planes. These values indicated that the paramagnetic centre has a rhombic symmetry with the Cu²⁺ ion having distorted octahedral environment. The complex exhibits only metal centred electroactivity in the potential range of −2.00, 1.25 V versus Ag/AgCl reference electrode.     

Synthesis of In-doped Ga2O3 zigzag-shaped nanowires and optical properties

In-doped Ga₂O₃ zigzag-shaped nanowires and undoped Ga₂O₃ nanowires have been synthesized on Si substrate by thermal evaporation of mixed powders of Ga, In₂O₃ and graphite at 1000 °C without using any catalyst via a vapor-solid growth mechanism. The morphologies and microstructures of the products were characterized by field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS) and photoluminescence spectroscopy (PL). The nanowires range from 100 nm to several hundreds of nanometers in diameter and several tens of micrometers in length. A broad emission band from 400 to 700 nm is obtained in the PL spectrum of these nanowires at room temperature. There are two blue-emission peaks centering at 450 and 500 nm, which originate from the oxygen vacancies, gallium vacancies and gallium-oxygen vacancy pairs.     

A novel precursor for synthesis of metallic copper nanocrystals by thermal decomposition approach

[Bis(2-hydroxy-1-naphthaldehydato)copper(II)] complex, as a novel precursor, was employed in thermal decomposition process to synthesize metallic copper nanoparticles using oleylamine (C₁₈H₃₇N) as capping agent. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and ultraviolet-visible (UV-vis) spectroscopy. The synthesized copper nanoparticles have a fcc structure with average size 20-35 nm.     

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.     

GMR in multilayered nanowires electrodeposited in track-etched polyester and polycarbonate membranes

Commercially available track-etched polyester membranes were used as templates to electrodeposit Co–Ni–Cu/Cu multilayered nanowires, giving room-temperature current perpendicular to plane (CPP) giant magnetoresistance (GMR) values of up to ∼12%. In contrast to similar nanowires electrodeposited in track-etched polycarbonate membranes, the GMR obtained in multilayered nanowires electrodeposited in the polyester membranes increased with decreasing Cu-layer thickness t_Cu, for t_Cu in the 2–7 nm range, indicating a lack of ferromagnetic coupling through pinholes, etc. Transmission electron micrographs showed clear evidence for smooth, parallel layer interfaces in the nanowires.     

Preparation and optical properties of Cu2O hollow microsphere film and hollow nanosphere powder via a simple liquid reduction approach

In this work, we report a simple liquid reduction approach to prepare Cu₂O hollow microsphere film and hollow nanosphere powder with Cu(OH)₂ nanorods as precursor and ascorbic acid as the reductant at 60 °C. When Cu(OH)₂ nanorod array film grown on a copper foil is used as the precursor, Cu₂O thin film made up of hollow microspheres with average diameter of 1.2 μm is successfully prepared. When the Cu(OH)₂ nanorods are scraped from the copper foil and then used as the precursor, Cu₂O hollow nanosphere powder with the average diameter of 270 nm is obtained. The samples are characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and ultraviolet-vis light (UV-vis) absorption spectra. A possible formation mechanism of Cu₂O hollow spheres is discussed.     

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.     

Preparation and characterization of polymer coated superparamagnetic magnetite nanoparticle agglomerates

In order to produce magnetic microparticles (agglomerates), magnetite (Fe₃O₄) particles were synthesized using coprecipitation of FeSO₄·7H₂O and FeCl₃·6H₂O with the presence of poly(methacrylic acid) (PMAA) in aqueous solution.. Transmission electron microscopy (TEM), X-ray diffraction, and vibrating sample magnetometry (VSM) methods were used to characterize the PMAA coated superparamagnetic agglomerates. The influences of various processing parameters such as the process temperature, PMAA content, and the addition of surfactant on the agglomerate size and size distribution of produced magnetic microparticles were investigated. The particle size and size distribution characteristics, (the volume weighted mean size (D[4,3], surface weighted mean size D[3,2], the geometric standard deviation, and span value) of the magnetic agglomerates were determined using the laser diffraction technique. The PMAA coated magnetic agglomerates with surface weighted mean sizes ranging from 1.5 to 3 μm were produced successfully.     

Density functional theory calculations of surface properties and H2 adsorption on the Cu2O (1 1 1) surface

First-principles calculation on the basis of the density functional theory (DFT) and generalized gradient approximation have been applied to study the adsorption of H₂ on the stoichiometric O-terminated Cu₂O (1 1 1), Cu₂O (1 1 1)-Cu_CUS and Cu-terminated Cu₂O (1 1 1) surfaces. The optimal adsorption position and orientation of H₂ on the stoichiometric O-terminated Cu₂O (1 1 1) surface and Cu-terminated Cu₂O (1 1 1) surface were determined and electronic structural changes upon adsorption were investigated by calculating the Local Density of States (LDOS) of the Cu_CUS 3d and Cu_CUS 4s of stoichiometric O-terminated Cu₂O (1 1 1) surface. These results showed that H₂ molecule adsorption on Cu_CUS site parallel to stoichiometric O-terminated Cu₂O (1 1 1) surface and H₂ molecule adsorption on Cu₂ site parallel to Cu-terminated Cu₂O (1 1 1) surface were the most favored, respectively. The presence of surface copper vacancy has a little influence on the structures when H₂ molecule adsorbs on Cu_CSA, O_CUS and O_CSA atoms and the H₂ molecule is only very weakly bound to the Cu₂O (1 1 1)-Cu_CUS surface. From the analysis of stoichiometric O-terminated Cu₂O (1 1 1) Local Density of States, it is observed that Cu_CUS 3d orbital has moved to a lower energy and the sharp band of Cu_CUS 4s is delocalized when compared to that before H₂ molecule adsorption, and overlapped substantially with bands due to adsorbed H₂ molecule. The Mulliken charges of H₂ adsorption on Cu_CUS site showed that H₂ molecule obtained electron from Cu_CUS which was consistent with the calculated electronic structural changes upon H₂ adsorption.     

Effect of surface roughness on nucleation and growth of vanadium pentoxide nanowires

The effect of surface roughness on subsequent growth of vanadium pentoxide (V₂O₅) nanowires is examined. With increasing surface roughness, both the number density and aspect ratio of V₂O₅ nanowires increase. Structures and morphology of obtained nanowires were characterized by field emission scanning electron microscopy (FE-SEM) and X-ray diffraction (XRD). The nanowires are approximately 40-90 nm in diameter and 2 μm in length. X-ray diffraction (XRD) analysis indicates that the obtained nanowires are orthorhombic structure with (0 0 1) out-of-plane orientation. The luminescence property of V₂O₅ nanowires has been investigated by photoluminescence (PL) at 150 K and 300 K. PL results show intense visible emission, which is attributed to different inter-band transitions between the V 3d and O 2p band. This simple fabrication approach might be useful for fabrication of large area V₂O₅ nanowires arrays with high density.     

Optical and photoconductivity studies of Cu2O nanowires synthesized by solvothermal method

The solvothermal method has been employed to synthesize cuprous oxide (Cu₂O) nanowires using a precursor of cupric acetate monohydrate (CuAc₂) and ethylene glycol (EG) as the solvent. By optimizing the reaction temperature and reaction time, we have prepared Cu₂O nanowires with a diameter of approximately 7 nm and a length of several nanometers. The UV-visible absorption spectrum of the nanowires shows obvious blueshift compared to the bulk Cu₂O, which arises from the quantum confinement effect of the excitonic transition expected for Cu₂O nanowires. Here we also report the role of different excitation energies on the photoluminescence (PL) properties of the Cu₂O nanowires by steady-state and time-resolved PL spectroscopy. The decay times vary from nanoseconds to picoseconds. Decay kinetics indicates that the average lifetime 〈τ〉 of the nanowires increases with increasing excitation energy. The current-voltage (I-V) curves of the nanowires give the photocurrent density 16 times larger than the dark current density.     

Synthesis of crystalline SrMoO4 nanowires from polyoxometalates

Crystalline SrMoO₄ nanowires were synthesized via a facile hydrothermal process at 180 °C for 10 h. α-(NH₄)₆-P₂Mo₁₈O₆₂·nH₂O, one of polyoxometalates with Dawson structure, was employed as the source of molybdates. The diameter and length of the obtained SrMoO₄ nanowires are about 20 nm and 5-10 μm, respectively. HRTEM results show that the SrMoO₄ nanowires are of high crystallinity with rough surface. However, when Na₂MoO₄·2H₂O was used, there are only SrMoO₄ nanorods with smaller aspect ratio (200/70 nm) in the similar hydrothermal process. The probable growth mechanism was discussed.     

Fabrication and characterization of Mn-doped Cu2O thin films grown by RF magnetron sputtering

Two series of Mn-doped Cu₂O diluted-magnetic-semiconductor thin films were prepared by radio-frequency (RF) magnetron sputtering. One is prepared at different deposition temperature with the same Mn doping concentration; the other is deposited at the same temperature but with varying Mn concentration. They were used to find out the ferromagnetic-order zone for the Mn-doped Cu₂O systems. Most of the samples show high (1 1 1) orientation, except low doping concentration (<6 at%). No impurities were found by X-ray diffraction and electron diffraction measurement. The doped Mn ions substituted Cu ions in the Cu₂O lattice and there were about 1.5% cation vacancies. The grains shown in the transmission electron microscopy (TEM) images for all the samples were tiny, i.e. just 5 nm in diameter. A rough phase diagram for the ferromagnetic order existing in the Mn-doped Cu₂O thin films was given with varying Mn doping concentration and deposition temperature.     

Structural characterisation of [Cu2(bptd) (H2O) Cl4] and [Ni2(bptd)2(H2O)4] Cl4·3H2O; evidence of null intramolecular exchanges by EPR and magnetic measurements

Using the 2,5-bis(2-pyridyl)-1,3,4-thiadiazole (bptd), we recently prepared [Cu₂(bptd) (H₂O) Cl₄] and [Ni₂(bptd)₂ (H₂O)₄] Cl₄, 3H₂O in which the magnetic centres are connected through one diazine+one chloro and two diazine ligand bridges, respectively. These two compounds are the first examples that show null intramolecular magnetic interactions despite M-M distances close to 3.7 Å within perfectly planar edifices:Down to , [Cu₂(bptd)Cl₄(H₂O)] is paramagnetic while, below T_t, half of the Cu²⁺ions interact, leading to residual paramagnetism of one Cu²⁺/f.u. Magnetic susceptibility measurements, EPR and pulsed EPR study indicate the original intermolecular nature of AF exchanges.[Ni₂(bptd)₂(H₂O)₄]Cl₄·3H₂O susceptibility obeys a Curie-law involving pure paramagnetism. Moreover, its EPR spectrum can be interpreted on the basis of virtual S=1 monomers. Below 70 K, Zero Field Splitting (D∼275 G) due to dipolar interactions without magnetic exchanges could be responsible for the LT spectra splitting. For both compounds, the thia role is suggested as partially responsible for the null-in-plane magnetic exchanges.     

Electrical conduction and magnetoelectric effect of (x) BaTiO3 + (1−x) Ni0.92Co0.03Cu0.05Fe2O4 composites in ferroelectric rich region

Particulate composites with composition (x)BaTiO₃+(1−x)Ni_0.92Co_0.03Cu_0.05Fe₂O₄ in which x varies as 1, 0.85, 0.70, 0.55 and 0 (in mol%) were prepared by the conventional double sintering ceramic technique. The presence of two phases viz. ferromagnetic (Ni_0.92Co_0.03Cu_0.05Fe₂O₄) and ferroelectric (BaTiO₃) was confirmed by X-ray diffraction analysis. The dc resistivity and thermo-emf measurements were carried out with variation of temperature. The ac conductivity (σ_ac) measurements investigated in the frequency range 100 Hz to 1 MHz conclude that the conduction in these composites is due to small polarons. The variation of dielectric constant and loss tangent with frequency (20 Hz to 1 MHz) was studied. The static magnetoelectric conversion factor, i.e. dc (dE/dH)_H was measured as a function of intensity of applied magnetic field. The changes were observed in electrical properties as well as in magnetoelectric voltage coefficient as the molar ratio of the constituent phases was varied. A maximum value of magnetoelectric conversion factor of 536.06 μV/cm Oe was observed for the composite with 70% BaTiO₃+30% Ni_0.92Co_0.03Cu_0.05Fe₂O₄ at a dc magnetic field of 2.3 K Oe. The maximum magnetoelectric conversion output has been explained in terms of ferrite-ferroelectric content, applied static magnetic field and resistivity.     

Controlled synthesis of cuprous oxide nanospheres and copper sulfide hollow nanospheres

Uniform Cu₂O nanospheres have been successfully synthesized by reducing CuSO₄ with ascorbic acid in sucrose solution at room temperature. The diameter of the Cu₂O nanospheres can be tuned from 90 to 280 nm by adding different amounts of sucrose in the solution. Furthermore, CuS hollow nanospheres with different diameters have been obtained based on the Kirkendall effect using the as-prepared Cu₂O nanospheres as sacrificial templates. Cu₂O/Cu_7.2S₄ core/shell nanospheres and Cu_7.2S₄ hollow nanospheres are obtained as the intermediate products at different stages of the conversion process. Through the post-treatment of sodium citrate solution, Cu_7.2S₄ hollow nanospheres can be changed into CuS hollow nanospheres. The products are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and field-emission scanning electron microscopy (FESEM). Optical properties of the products have also been studied.