Hydrothermal preparation of Ba(Ti,Zr)O3 fine powders

Fine powders consisting of aggregated submicron crystallites of Ba(Ti,Zr)O3 in the complete range of Ti/Zr ratios are prepared at 85–130°C by hydrothermal method, starting from TiO2 + ZrO2 · xH2O mixed gel and Ba(OH)2 solution. The products obtained below 110°C incorporate considerable amounts of H2O and OH− within the lattice. As-prepared BaTiO3 is cubic and converts to tetragonal phase after the heat treatment at 1200°C, accompanied by the loss of residual hydroxyl ions. TEM investgations of the growth features show a transformation of the gel to the crystallite. Ba2+ ions entering the gel produce chemical changes within the gel, followed by dehydration, resulting in a cubic perovskite phase irrespective of Ti/Zr. The sintering properties of these powders to fine-grained, high density ceramics and their dielectric properties are presented.

Hydrothermal synthesis of Ba(Ti, Sn)O3 fine powders and dielectric properties of the corresponding ceramics

Fine powders of submicron-sized crystallites of BaTiO3 were prepared at 85–130°C by the hydrothermal method, starting from TiO2.ξH2O gel and Ba(OH)2 solution. The products obtained below 110°C incorporated considerable amounts of H2O and OH− in the lattice. As-prepared BaTiO3 is cubic and converts to the tetragonal phase after heat treatment at 1200°C, accompanied by the loss of residual OH− ions. Hydrothermal reaction of SnO2.ξH2O gel with Ba(OH)2 at 150–260°C gives rise to the hydrated phase, BaSn(OH)6.3H2O, due to the amphoteric nature of SnO2.ξH2O which stabilises Sn(OH)62− anions in basic media. On heating in air or releasing the pressure in situ at 260°C, BaSn(OH)6.3H2O converts to BaSnO3 through an intermediate, BaSnO(OH)4. Solid solutions of Ba(Ti,Sn)O3 are directly formed from (TiO2 + SnO2)..ξH2O gel up to 35 mol% SnO2. At higher Sn contents, the hydrothermal products are mixtures of BaSn(OH)6.3H2O and BaTiO3, which on annealing at 1000°C result in monophasic Ba(Ti,Sn)O3. The sintering characteristics and the dielectric properties of the ceramics prepared out of these fine powders are presented. The dielectric properties of fine-grained Ba(Ti,Sn)O3 ceramics are explained on the basis of the prevailing diffuse phase transition behaviour.

In-situ one-step hydrothermal synthesis of a lead germanate-graphene composite as a novel anode material for lithium-ion batteries

Lead germanate-graphene nanosheets (PbGeO3-GNS) composites have been prepared by an efficient one-step, in-situ hydrothermal method and were used as anode materials for Li-ion batteries (LIBs). The PbGeO3 nanowires, around 100–200 nm in diameter, are highly encapsulated in a graphene matrix. The lithiation and de-lithiation reaction mechanisms of the PbGeO3 anode during the charge-discharge processes have been investigated by X-ray diffraction and electrochemical characterization. Compared with pure PbGeO3 anode, dramatic improvements in the electrochemical performance of the composite anodes have been obtained. In the voltage window of 0.01–1.50 V, the composite anode with 20 wt.% GNS delivers a discharge capacity of 607 mAh g−1 at 100 mA g−1 after 50 cycles. Even at a high current density of 1600 mA g−1, a capacity of 406 mAh g−1 can be achieved. Therefore, the PbGeO3-GNS composite can be considered as a potential anode material for lithium ion batteries.

Hydrothermal synthesis and characterization of CaSO4 pseudomicrorods

Calcium sulphate (CaSO4) pseudomicrorods have been synthesized by alow-temperature hydrothermal method using CaSO4 powder as a precursor and hexadecylamine as a surfactant at 180 degrees C for at different intervals of time. The powder X-ray diffraction pattern indicates that the as-formed pseudomicrorods are of orthorhombic phase with lattice parameters a = 7.0023(4) angstrom, b = 6.9939(5) angstrom and c = 6.2434(4) angstrom. Scanning electron microscopy images show that the pseudomicrorods have diameters of about 0.2-2.5 mm and lengths of about 2-10 mm. Fourier transform infrared spectroscopy shows a strong doublet near 609 and 681 cm(-1) arising from nu(4) (SO42) bending vibrations. The strongest band observed at 1132 cm(-1) is associated with nu(3) (SO42-) stretching vibrations. The band near 420-450 cm(-1) is attributed to nu(2) (SO42-) bending vibrations. The Raman spectrum exhibits an intense peak at 1008 cm(-1) associated with the SO42- mode. The photoluminescence spectrum exhibits UV bands (330, 350 nm), strong green bands (402, 436 nm) and weak blue bands (503 nm). A widening of the optical band gap was observed as the particle size decreased.

Hydrothermal synthesis, characterization and Raman studies of Eu3+ activated Gd2O3 nanorods

Eu3+ (8 mol%) activated gadolinium oxide nanorods have been prepared by hydrothermal method without and with surfactant, cityl trimethyl ammonium bromide (CTAB). Powder X-ray diffraction (PXRD) studies reveal that the as-formed product is in hexagonal Gd(OH)(3):Eu phase and subsequent heat treatment at 350 and 600 degrees C transforms the sample to monoclinic GdOOH:Eu and cubic Gd2O3:Eu phases, respectively. The structural data and refinement parameters for cubic Gd2O3:Eu nanorods were calculated by the Rietveld refinement. SEM and TEM micrographs show that as-obtained Gd(OH)(3):Eu consists of uniform nanorods in high yield with uniform diameters of about 15 nm and lengths of about 50-150 nm. The temperature dependent morphological evolution of Gd2O3:Eu without and with CTAB surfactant was studied. FTIR studies reveal that CTAB surfactant plays an important role in converting cubic Gd2O3:Eu to hexagonal Gd(OH)(3):Eu. The strong and intense Raman peak at 489 cm(-1) has been assigned to A(g) mode, which is attributed to the hexagonal phase of Gd2O3. The peak at similar to 360 cm(-1) has been assigned to the combination of F-g and E-g modes, which is mainly attributed to the cubic Gd2O3 phase. The shift in frequency and broadening of the Raman modes have been attributed to the decrease in crystallite dimension to the nanometer scale as a result of phonon confinement. (C) 2010 Elsevier B.V. All rights reserved.

Hydrothermal synthesis of Gd2O3:Eu3+ nanophosphors: Effect of surfactant on structural and luminescence properties

Various morphologies of Eu3+ activated gadolinium oxide have been prepared by hydrothermal method using hexadecylamine (HDA) as surfactant at different experimental conditions. The powder X-ray diffraction studies reveal as-formed product is hexagonal Gd(OH)(3):Eu3+ phase and subsequent heat treatment at 350 and 600 degrees C transforms to monoclinic GdOOH:Eu3+ and cubic Gd2O3:Eu3+ phases respectively. SEM pictures of without surfactant show irregular shaped rods along with flakes. However, in the presence of HDA surfactant, the particles are converted into rods of various sizes. The temperature dependent morphological evolution of Gd2O3:Eu3+ without and with HDA surfactant is studied. TEM micrographs of Gd(OH)(3):Eu3+ sample with HDA confirms smooth nanorods with various diameters in the range 20-100 nm. FTIR studies reveal that HDA surfactant plays an important role in conversion of cubic to hexagonal phases. Among these three phases, cubic phase Gd2O3:Eu3+ (lambda(ex) = 254 nm) show red emission at 612 nm corresponding to D-5(0)-> F-7(2) and is more efficient host than the monoclinic counterpart. The band gap for hexagonal Gd(OH)(3):Eu3+ is more when compared to monoclinic GdOOH:Eu3+ and cubic Gd2O3:Eu3+. (C) 2013 Elsevier B. V. All rights reserved.

Hydrothermal growth and characterization of ZnO crystals

ZnO crystals with dimensions of 30 x 38 x 8 turn 3 have been grown by the hydrothermal method using a mixed solution of KOH, LiOH and H2O2. The growing rates for +c(0001) and -c(000 (1) over bar) were 0.17 and 0.09 mm/day, respectively. The crystal color was very light green for +c sector and dark brown for -c sector. For the +c sector, the resistivity at room temperature was 80 0 cm, the carrier concentration was about 10(4)/cm(3), and the mobility was about 100 cm(2)/Vs. The full-width at half-maximum (FWHM) of double axis X-ray rocking curve for the polished Zn face cut from +c sector was 45 arcsec. The photoluminescence (PL) spectrum and the absorption spectrum of +c part of the crystals at room temperature were also reported and discussed in this paper. (c) 2008 Elsevier B.V. All rights reserved.

Growth of ZnO single crystal by chemical vapor transport method

ZnO crystals were grown by CVT method in closed quartz tube under seeded condition. Carbon was used as a transport agent to enhance the chemical transport of ZnO in the growth process. ZnO single crystals were grown by using GaN/sapphire and GaN/Si wafer as seeds. The property and crystal quality of the ZnO single crystals was studied by photoluminescence spectroscopy and X-ray diffraction technique.

Hydrothermal synthesis of lanthanide fluorides LnF(3) (Ln = La to Lu) nano-/microcrystals with multiform structures and morphologies

Lanthanide fluoride LnF(3) (Ln = La to Lu) nano-/microcrystals with multiform crystal structures (hexagonal and orthorhombic) and morphologies (separated elongated nanoparticles, aggregated nanoparticles, polyhedral microcrystals) were successfully synthesized by a facile, effective, and environmentally friendly hydrothermal method. X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, high-resolution transmission electron microscopy, and photoluminescence spectra were used to characterize the samples. The experimental results indicated that the use of NaBF4 is indispensable for obtaining LnF(3) crystal structures.

Hydrothermal synthesis and luminescent properties of Y2O3:Tb3+ and Gd2O3:Tb3+ microrods

One-dimensional (1D) Y2O3:Tb3+ and Gd2O3:Tb3+ microrods have been successfully prepared through a large-scale and facile hydrothermal method followed by a subsequent calcination process in N-2/H-2 mixed atmosphere. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (IR), thermogravimetric analysis (TGA), energy-dispersive X-ray spectra (EDX). scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), photoluminescence (PL) and cathodoluminescence (CL) spectra as well as kinetic decays were used to characterize the samples. The as-formed products via the hydrothermal process could transform to cubic Y2O3:Tb3+ and Gd2O3:Tb3+ with the same morphology and slight shrinking in size after a postannealing process.

Self-assembled 3D flowerlike Lu2O3 and Lu2O3 : Ln(3+) (Ln = Eu, Tb, Dy, Pr, Sm, Er, Ho, Tm) microarchitectures: Ethylene glycol-mediated hydrothermal synthesis and luminescent properties

Three-dimensional flowerlike Lu2O3 and Lu2O3:Ln(3+) (Ln = Eu, Th, Dy, Pr, Sm, Er, Ho, Tm) microarchitectures have been successfully synthesized via ethylene glycol (EG)-mediated hydrothermal method followed by a subsequent heat treatment process. X-ray diffraction, Fourier transform infrared spectroscopy, energy-dispersive X-ray spectra, thermogravimetric and differential thermal analysis, elemental analysis, inductively coupled plasma atomic absorption spectrometric analysis, ion chromatogram analysis, X-ray photoelectron spectra, scanning electron microscopy, transmission electron microscopy, photoluminescence spectra as well kinetic decays, and cathodoluminescence spectra were used to characterize the samples. Hydrothermal temperature, EG, and CH3COONa play critical roles in the formation of the lutetium oxide precursor microflowers. The reaction mechanism and the self-assembly evolution process have been proposed. The as-formed lutetium oxide precursor could transform to Lu2O3 With their original flowerlike morphology and slight shrinkage in the size after postannealing process.

Facile Hydrothermal Synthesis and Luminescent Properties of Large-Scale GdVO4:Eu3+ Nanowires

Large-scale GdVO4:Eu3+ nanowires with diameters of about 15 nm and lengths of several micrometers were achieved by a facile hydrothermal method in the presence of disodium ethylenediamine tetraacetate (Na2H2L). The influences of several parameters, such as pH value, reaction temperature, and molar ratio of Na2H2L to Gd3+ on the final products were investigated. The formation mechanism of the as-obtained GdVO4:Eu3+ nanowires is proposed on the basis of time-dependent experiments. It is found that the organic additive Na2H2L, which acts as a shape modifier, has a dynamic effect by adjusting the growth rates of different facets, resulting in the formation of the GdVO4:Eu3+ nanowires. The luminescent spectrum of GdVO4:Eu3+ nanowires shows the strong characteristic dominant emission of the Eu3+ ions at 614 nm.

Hydrothermal Synthesis and Luminescent Properties of Novel Ordered Sphere CePO4 Hierarchical Architectures

The ordered-sphere CePO4 hierarchical architectures have been successfully synthesized by a simple hydrothermal method through the controlled growth of the CePO4 nanorods and self-assemble hierarchical structure under various reaction conditions. The evolution of the morphology of the samples has been investigated in detail. It was found that the coexistence of citric acid and cetaltrimethylammonium bromide in the reaction system plays an important role in the formation of the spherical CePO4 hierarchical architectures. A possible mechanism of the formation and growth of the hierarchical structure was suggested according to the experimental results and analysis. The effects of the reaction time as well as the variation of the morphologies on the luminescent properties of the products were also studied.

Facile synthesis of highly uniform octahedral LuVO4 microcrystals by a facile chemical conversion method

Uniform octahedral LuVO4 microcrystals have been successfully prepared through a designed two-step hydrothermal method. One-dimensional lutetium precursor was first prepared through a simple hydrothermal route. Subsequently, a well-shaped octahedral LuVO4 sample was synthesized at the expense of the wirelike precursors during the hydrothermal process. The whole process in this method was carried out in aqueous conditions without the use of any organic solvents, surfactant, or catalyst. The conversion process from nanowire precursor to octahedral product has been investigated in detail. The LuVO4 : Ln(3+) (Ln Eu, Dy, Sm, and Er) phosphors show strong light emissions with different colors coming from different activator ions under ultraviolet light excitation or low-voltage electron beam excitation. Furthermore, this general and facile method may be of much significance in the synthesis of many other lanthanide compounds with polyhedral morphology.

Hydrothermal synthesis of SrCO3 : Eu3+/Tb3+ microneedles and their luminescence properties

SrCO3:Eu3+ /Tb3+ microneedles that grow along the a-axis were successfully prepared through a large-scale and facile hydrothermal method without any template and further annealing treatment. X-ray diffraction (XRD), scanning electron microscopy (SEM), and photoluminescence (PL) spectra as well kinetic decays, were used to characterize the samples. The preferential growth along a-axis for SrCO3:Eu3+/Tb3+ microneedles has been proposed through analysis of the XRD patterns of samples obtained at different hydrothermal treatment time. Under ultraviolet excitation, the SrCO3:Eu3+ and SrCO3:Tb3+ microncedle samples show a strong red and green emission corresponding to the D-5(0)-F-7(j) (J = 1, 2, 3, 4) transitions of Eu3+ and the D-5(4)-(7) F-j (J = 6, 5, 4, 3) transitions of Tb3+, respectively, which have potential applications in lighting fields.