10 resultados para HYDROTHERMAL SYNTHESES

em Deakin Research Online - Australia


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A novel one-step hydrothermal coating process was used to produce nanohydroxyapatite (nano-HA) coating on a titanium–niobium (TiNb) alloy substrate in a newly designed solution containing calcium and phosphate ions. The morphology of the coating was studied using scanning electron microscopy. The phase identification of the coating was carried out using X-ray diffraction, attenuated total reflectance Fourier transform infrared spectroscopy and transmission electron microscopy. The reaction between the surface of TiNb alloy and the solution during the hydrothermal process was studied by Xray photoelectron spectroscopy. Results show that the coating formed on the surface of TiNb alloy was composed of nano-HA particles. During the hydrothermal process, TiO2 and Nb2O5 formed on the TiNb alloy surface and hydrated to Ti(OH)4 and Nb(OH)5, respectively. Calcium phosphate nucleated and grew into a layer of nano-HA particles on the surface of TiNb alloy under the hydrothermal conditions. The crystallinity of the nano-HA coating was improved with the increase in hydrothermal treatment temperature and time duration. Nano-HA coating with good crystallinity was produced on the TiNb alloy via the hydrothermal process at a temperature of 200 ºC for 12 h.

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This study reports a facile hydrothermal method for the synthesis of monodispersed hematite (α-Fe2O3) nanodiscs under mild conditions. The method has features such as no use of surfactants, no toxic precursors, and no requirements of high-temperature decomposition of iron precursors in non-polar solvents. By this method, α-Fe2O3 nanodiscs were achieved with diameter of 50 ± 10 nm and thickness of ~6.5 nm by the hydrolysis of ferric chloride. The particle characteristics (e.g., shape, size, and distribution) and functional properties (e.g., magnetic and catalytic properties) were investigated by various advanced techniques, including TEM, AFM, XRD, BET, and SQUID. Such nanodiscs were proved to show unique magnetic properties, i.e., superparamagnetic property at a low temperature (e.g., 20 K) but ferromagnetic property at a room temperature (~300 K). They also exhibit low-temperature (<623 K) catalytic activity in CO oxidation because of extremely clean surfaces due to non-involvement of surfactants, compared with those spheres and ellipsoids capped by PVP molecules.

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The feasibility of devising a solid support mediated approach to multimodal Ru(II)-peptide nucleic acid (PNA) oligomers is explored. Three Ru(II)-PNA-like monomers, [Ru(bpy)2(Cpp-L-PNA-OH)]2+ (M1), [Ru(phen)2(Cpp-L-PNA-OH)]2+ (M2), and [Ru(dppz)2(Cpp-L-PNA-OH)]2+ (M3) (bpy = 2,2′-bipyridine, phen = 1,10-phenanthroline, dppz = dipyrido[3,2-a:2′,3′-c]phenazine, Cpp-L-PNA-OH = [2-(N-9-fluorenylmethoxycarbonyl)aminoethyl]-N-[6-(2-(pyridin-2yl)pyrimidine-4-carboxamido)hexanoyl]-glycine), have been synthesized as building blocks for Ru(II)-PNA oligomers and characterized by IR and 1H NMR spectroscopy, mass spectrometry, electrochemistry and elemental analysis. As a proof of principle, M1 was incorporated on the solid phase within the PNA sequences H-g-c-a-a-t-a-a-a-a-Lys-NH2 (PNA1) and H-P-K-K-K-R-K-V-g-c-a-a-t-a-a-a-a-lys-NH2 (PNA4) to give PNA2 (H-g-c-a-a-t-a-a-a-a-M1-lys-NH2) and PNA3 (H-P-K-K-K-R-K-V-g-c-a-a-t-a-a-a-a-M1-lys-NH2), respectively. The two Ru(II)-PNA oligomers, PNA2 and PNA3, displayed a metal to ligand charge transfer (MLCT) transition band centered around 445 nm and an emission maximum at about 680 nm following 450 nm excitation in aqueous solutions (10 mM PBS, pH 7.4). The absorption and emission response of the duplexes formed with the cDNA strand (DNA: 5′-T-T-T-T-T-T-T-A-T-T-G-C-T-T-T-3′) showed no major variations, suggesting that the electronic properties of the Ru(II) complexes are largely unaffected by hybridization. The thermal stability of the PNA·DNA duplexes, as evaluated from UV melting experiments, is enhanced compared to the corresponding nonmetalated duplexes. The melting temperature (Tm) was almost 8 °C higher for PNA2·DNA duplex, and 4 °C for PNA3·DNA duplex, with the stabilization attributed to the electrostatic interaction between the cationic residues (Ru(II) unit and positively charged lysine/arginine) and the polyanionic DNA backbone. In presence of tripropylamine (TPA) as co-reactant, PNA2, PNA3, PNA2·DNA and PNA3·DNA displayed strong electrochemiluminescence (ECL) signals even at submicromolar concentrations. Importantly, the combination of spectrochemical, thermal and ECL properties possessed by the Ru(II)-PNA sequences offer an elegant approach for the design of highly sensitive multimodal biosensing tools.

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V2O5·nH2O nanosheets are fabricated hydrothermally with the acidified peroxovanadate solution at 200 °C for 12 h. The X-ray diffraction suggests that V2O5·nH2O nanosheets display lamellar ordering along c-axis direction. Transmission electron microscopy, field-emission scanning electron microscopy, and selected area electron diffraction indicate that V2O5·nH2O nanosheets are very thin in thickness and micron-sized in lateral dimension, and they are two-dimensional crystallites. X-ray photoelectron spectroscopy and thermogravimetric analysis are utilized to confirm the elemental composition of nanosheets. The formation process of nanosheets is also discussed in terms of time- and temperature-controlled experiments.

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Hexagonal V0.13Mo0.87O2.935 nanowires were hydrothermally synthesized at 220 °C for the first time. X-ray diffraction and field-emission scanning electron microscopy were utilized to characterize the phase and morphology of the nanowires, respectively. Transmission electron microscopy and selected area electron diffraction indicate that the nanowires are single crystalline, growing along the [001] direction. Interestingly, the nanowires easily become amorphous under the electron irradiation. The comparative hydrothermal experiments show that the molar ratio between the starting reagents of Mo and NH4VO3 plays a vital role in the anisotropic growth of nanowires. The photoluminescence measurement demonstrates that these nanowires exhibit two strong emission peaks at 420 and 438 nm, which are probably related to the intrinsic oxygen vacancies.

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Primary research in education and social sciences is marked by a diversity of methods and perspectives. How can we accommodate and reflect such diversity at the level of synthesizing research? What are the critical methodological decisions in the process of a research synthesis, and how do these decisions open up certain possibilities, while closing down others?

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The reaction of the group 14 tetrachlorides MCl4 (M = Si, Ge, Sn) with oleum (65 % SO3) at elevated temperatures led to the unique anionic complexes [M(S2O7)3]2– that show the central M atoms in coordination of three chelating S2O72– groups. The mean distances M–O within the complexes increase from 175 pm (M = Si) via 186 pm (M = Ge) up to 200 pm (M = Sn). The charge balance for the [M(S2O7)3]2– anions is achieved by alkaline metal ions A+ (A = Li, Na, K, Rb, Cs) which were implemented in the syntheses in form of their sulfates. The size of the A+ ions, i.e. their coordination requirement causes the crystallographic differences in the crystal structures, while the structure of the complex [M(S2O7)3]2– anions remains essentially unaffected. Furthermore, we were able to characterize the unique germanate Hg2[Ge(S2O7)3]Cl2 which forms when HgCl2 is added as a source for the counter cation. The Hg2+ and the Cl– ions form infinite cationic chains according to 1∞[HgCl2/2]+ which take care for the charge compensation. For selected examples of the compounds the thermal behavior has been monitored by means of thermal analyses and X-ray powder diffraction. For A being an alkaline metal the decomposition product is a mixture of the sulfates A2SO4 and the dioxides MO2, whereas Hg2[Ge(S2O7)3]Cl2 shows a more complicated decomposition. The tris-(disulfato)-silicate Na2[Si(S2O7)3] has additionally been examined by solid state 29Si and 23Na NMR spectroscopic measurements.