998 resultados para hydrothermal crystal growth


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Oriented crystallization of CUSO4 center dot 5H(2)O on a Langmuir-Blodgett (LB) film of stearic acid has been studied in the temperature ranges of 73-68 degrees C and 53-20 degrees C, respectively. This is the first time that the LB film at temperature above its melting point has been served as a template to induce nucleation and growth of crystals. The experimental results demonstrated that the LB film in the liquid state has the ability of directing the nucleation and growth of crystals. Moreover, X-ray diffraction patterns of the as prepared crystals revealed that the orientation of the attached crystals on the LB film is affected by temperature greatly.

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Nearly monodisperse Pd nanocubes with controllable sizes were synthesized through a seed-mediated growth approach. By using Pd nanocubes of 22 nm in size as seeds, the morphology of the as-grown nanostructures was fixed as single-crystalline, which enabled us to rationally tune the size of Pd nanocubes. The formation mechanism of initial 22 nm nanocubes was also discussed. The size-dependent surface plasmon resonance properties of the as-synthesized Pd nanocubes were investigated. Compared with previous methods, the yield, monodispersity, perfection of the shape formation, and the range of size control of these nanocubes are all improved.

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Uniform octahedral YVO4:Eu3+ microcrystals have been successfully prepared through a designed two-step hydrothermal conversion method. One-dimensional precursor Y4O(OH)(9)NO3 was first prepared through a simple hydrothermal process without using any surfactant, catalyst or template. Subsequently, well-defined octahedral YVO4 was synthesized at the expense of the precursor during a hydrothermal conversion process. XRD results demonstrate that the diffraction peaks of the final product can be well indexed to the pure tetragonal phase of YVO4.

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Seven supramolecular compounds comprising p-sulfonatocalix[6]arene and transition metals, {[Cu(Imz)-(phen)(H2O)](4)[C6AS]}center dot 10H(2)O (1), {[Cu(Imz)(2)(phen)](2)[Cu(Imz)(phen)(H2O)(2)](2)[C6AS]}center dot 13.3H(2)O (2), {[M(phen)(2)(H2O)]-[(M(phen)(2)](2)[C6AS]}center dot nH(2)O (3 and 4) (3: M = Co and n = 29.6; 4: M = Zn and n = 29.9), {[Cu(phen)(2)](4)[C6AS]}(2)center dot 13H(2)O (5), [H3O](2)[Co(phen)(3)](2)[C6AS]center dot 10.7H(2)O(6), and [Cu(phen)(2)(H2O)](2){[Cu(phen)(2)](2)[C6AS]}center dot 8H(2)O(7)(phen = 1,10-phenanthroline, C6AS = p-sulfonatocalix[6]arene, Imz = imidazole), have been synthesized by a hydrothermal method and structurally characterized by IR spectroscopy, thermogravimetric-differential thermal analysis (TG-DTA), and single crystal X-ray diffraction.

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Large-scale arrays consist of dendritic single-crystalline Ag/Pd alloy nanostructures are synthesized for the first time. A simple galvanic replacement reaction is introduced to grow these arrays directly on Ag substrates. The morphology of the products strongly depended on the reaction temperature and the concentration of H2PdCl4 solution. The mechanism of the formation of alloy and the dendritic morphology has been discussed. These alloy arrays exhibit high surface-enhanced Raman scattering (SERS) activity and may have potential applications in investigation of "in situ" Pd catalytic reactions using SERS. Moreover, electrocatalytic measurements suggest that the obtained dendritic Ag/Pd alloy nanostructures exhibit electrocatytic activity toward the oxidation of formic acid.

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Monodisperse hexagonal Ln(OH)(3) (Ln = Eu, Sm) submicrospindles with uniform morphology and size have been Successfully synthesized in a large scale via a Facile aqueous solution route from the mixture of aqueous solutions or LnCl(3) and NaOH at 5 degrees C without using any surfactant or template. The as-synthesized products are characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA), energy-dispersive X-ray (EDX) spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). The SEM and TEM images show that the as-formed Ln(OH)(3) samples have a spindlelike shape with an equatorial diameter of 80-200 nm and a length of 500-900 nm, which are aggregates of even smaller nanoparticles.

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Hydroxyapatite (Ca-5(PO4)(3)OH) nano- and microcrystals with multiform morphologies (separated nanowires, nanorods, microspheres, microflowers, and microsheets) have been successfully synthesized by a facile hydrothermal process. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), photoluminescence (PL) spectra, kinetic decay, and electron paramagnetic resonance (EPR) were used to characterize the samples. The experimental results indicate that the obtained Ca-5(PO4)(3)OH samples show an intense and bright blue emission under long-wavelength UV light excitation. This blue emission might result from the CO2 center dot- radical impurities in the crystal lattice.

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A general and facile ultrasonic irradiation method has been established for the synthesis of the lanthanide orthovanadate LnVO(4) (Ln = La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) nanoparticles from an aqueous solution of Ln(NO3)(3) and NH4VO3 without any surfactant or template. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and photoluminescence (PL) spectra as well as kinetic decays were employed to characterize the as-prepared products. Ultrasonic irradiation has a strong effect on the morphology of the LnVO(4) nanoparticles. The SEM and TEEM images illustrate that the as-formed LnVO(4) particles have a spindle-like shape with an equatorial diameter of 30-70 nm and a length of 100-200 am, which are the aggregates of even.

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Y2O3 : Eu3+ microspheres, with an average diameter of 3 mu m, were successfully prepared through a large-scale and facile solvothermal method followed by a subsequent heat treatment. X-ray diffraction, Fourier transform infrared spectroscopy, energy-dispersive X-ray spectra, thermogravimetric and differential thermal analysis, inductive coupled plasma atomic absorption spectrometric analysis, scanning electron microscopy, transmission electron microscopy, photoluminescence spectra, as well kinetic decays, and cathodoluminescence spectra were used to characterize the samples. These microspheres were actually composed of randomly aggregated nanoparticles. The formation mechanisms for the Y2O3 : Eu3+ microspheres have been proposed on an isotropic growth mechanism. The Y2O3 : Eu3+ microspheres show a strong red emission corresponding to D-5(0) -> F-7(2) transition (610 nm) of Eu3+ under ultraviolet excitation (259 nm) and low-voltage electron beams excitation (1-5 kV), which have potential applications in fluorescent lamps and field emission displays.

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Highly crystalline CaMoO4:Tb3+ phosphor layers were grown on monodisperse SiO2 particles through a simple sol-gel method, resulting in formation of core-shell structured SiO2@CaMoO4:Tb3+ submicrospheres. The resulting SiO2@CaMoO4: Tb3+ core-shell particles were fully characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDS), transmission electron microscopy (TEM), photoluminescence (PL), low-voltage cathodoluminescence (CL), and kinetic decays. The XRD results demonstrate that the CaMoO4:Tb3+ layers begin to crystallize on the SiO2 spheres after annealing at 400 degrees C and the crystallinity increases with raising the annealing temperature. SEM and TEM analysis indicates that the obtained submicrospheres have a uniform size distribution and obvious core-shell structure. SiO2@CaMoO4:Tb3+ submicrospheres show strong green emission under short ultraviolet (260 nm) and low-voltage electron beam (1-3 kV) excitation, and the emission spectra are dominated by a D-5(4) -F-7(5) transition of Tb3+(544 nm, green) from the CaMoO4:Tb3+ shells.

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Control of crystal polymorph and size is very important in many application fields. Herein we demonstrate that Langmuir-Blodgett (LB) films of stearic acid (SA) and octadecylamine (ODA) can serve as templates and generate different polymorphs of glycine crystals. In the neutral aqueous solutions, gamma-glycine crystallizes on LB films of ODA while the polymorphic outcome becomes the (x-form on LB films of SA. These observed results could be explained by the electrostatic interactions and geometric lattice matching at the LB film/crystal interfaces, respectively. By keeping the appropriate supersaturation, we have successfully controlled the number of crystals grown on LB films; for example, in some certain cases, only one piece of crystal was grown on LB films in solution. Therefore, large crystals of centimeter size could be prepared. These experimental results suggest a new approach to produce an organic crystal with bulk scale.

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A series of Eu3+-doped ZnO films have been prepared by a sol-gel method. These films were characterized by X-ray diffraction (XRD) and photoluminecent spectra (PL). Effects of synthetic parameters, such as annealing atmosphere, temperature and concentration of doped ions, on the highly oriented crystal growth were studied in detail. The crystalline structures of films annealed in vacuum have a wurtzite symmetry with highly c-axis orientation. A characteristic D-5(0) -> F-7(J)(J = 1, 2, 3 and 4) red emission is observed due to energy transfer from the ZnO host to the doped Eu3+ in the c-oriented ZnO films.

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A single-crystalline EuF3 nanoflower with a novel three-dimensional (3D) nanostructure has been successfully synthesized via a facile, fast, efficient, and mild ultrasonic irradiation solution route employing the reaction of Eu(NO3)(3) and KBF4 under ambient conditions without any template or surfactant. The ultrasonic irradiation plays an important role and is necessary for the synthesis of EuF3 with the complex structure. The formation mechanism of this complex nanostructure is proposed in this paper. No template or surfactant is used in this method, which avoids the subsequent complicated workup for the removal of the template or surfactant. Furthermore, a substantial reduction in the reaction time as well as the reaction temperature is observed compared with the hydrothermal process.

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The reaction of Cu(BF4)(2) with pyridine-2,6-dicarboxylic acid (H(2)pydc) and trans-1,2-bis(4-pyridyl)ethylene (bpe) under hydrothermal conditions afforded a porous mixed-valence (CuCuII)-Cu-I coordination polymer. Coexistence of tetrameric and decameric water clusters within the channels of the complex leads to a novel water chain. The metal-organic framework provides both hydrophilic and hydrophobic environments for stabilizing the clusters and retains its integrity upon dehydration and rehydration.

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The crystallization behaviors of the poly(ethylene glycol)-poly(epsilon-caprolactone) diblock copolymer with the PEG weight fraction of 0.50 (PEG(50)-PCL50) was studied by DSC, WAXD, SAXS, and FTIR. A superposed melting point at 58.5 degrees C and a superposed crystallization temperature at 35.4 degrees C were obtained from the DSC profiles running at 10 degrees C/min, whereas the temperature-dependent FTIR measurements during cooling from the melt at 0.2 degrees C/min showed that the PCL crystals formed starting at 48 degrees C while the PEG crystals started at 45 degrees C. The PEG and PCL blocks of the copolymer crystallized separately and formed alternating lamella regions according to the WAXD and SAXS results. The crystal growth of the diblock copolymer was observed by polarized optical microscope (POM). An interesting morphology of the concentric spherulites developed through a unique crystallization behavior. The concentric spherulites were analyzed by in situ microbeam FTIR, and it was determined that the morphologies of the inner and outer portions were mainly determined by the PCL and PEG spherulites, respectively. However, the compositions of the inner and outer portions were equal in the analysis by microbeam FTIR.