Preparation of amino-acid-regulated hydroxyapatite particles by hydrothermal method

The hydroxyapatite nanorods (about 80 nm in length and 15 nm in width) with uniform size were achieved by hydrothermal method at 100 °C and pH 10 in the presence of alanine and glutamic acid. A special instillment order was used and the prepared powders were characterized for phase composition by X-ray diffraction and Fourier Transform infrared spectroscopy. The size and morphology of HAP nanoparticles were studied by Transmission electron microscopy. The characterization showed that the amino acid could induce the synthesis of hydroxyapatite nanoparticle and control HAP crystal growth when HAP crystal was formed. An instable monetite phase (CaPO₃OH) was found in the progress of ACP transforming to HAP.     

A hydrothermal method to prepare the spherical ZnS and flower-like CdS microcrystallites

The spherical ZnS and flower-like CdS microcrystallites are prepared by a convenient hydrothermal process through the reactions of Zn(CH₃COO)₂·2H₂O or Cd(CH₃COO)₂·2H₂O with S and NaH₂PO₂·H₂O in aqueous solution at 180 °C for 12 h. Powder X-ray diffraction (XRD) is used to confirm the cubic phases of the ZnS and CdS microcrystallites. Their chemical compositions are characterized by X-ray photoelectron spectroscopy (XPS). Scanning electron microscope (SEM) images show the morphologies of the as-synthesized ZnS and CdS. The photoluminescence spectra (PL) exhibit their optical properties.     

Silver nanoparticles of variable morphology synthesized in aqueous foams as novel templates

In this paper, we describe the synthesis of silver nanocrystals within aqueous foams as a template. More specifically, we show that aqueous Ag⁺ions may be electrostatically complexed with the anionic surfactants aerosol OT (sodiumbis-2-ethylhexyl-sulfosuccinate, (AOT) and sodium dodecyl sulphate (SDS)) in a highly stable liquid foam. After drainage of the foam, the silver ions are reducedin situby introducing sodium borohydride into the foam by capillary flow. This leads to the formation of silver nanoparticles of spherical, tape-and sheet-like morphology in the foam. The structure of the foam is extremely complex and presents reaction sites of different spatial extent. The differences in foam reaction-site geometry are believed to be responsible for the morphology variation in the silver nanoparticles observed. The silver nanoparticles are observed to be extremely stable in solution suggesting that the AOT or SDS molecules stabilize them. This approach appears promising for application in large-scale synthesis of nanoparticles and may be readily extended to other chemical compositions.     

Frequency upconversion of Tm and Yb codoped YLiF4 synthesized by hydrothermal method

In this paper, YLiF₄ codoped with Tm³⁺ and Yb³⁺ ions was synthesized by hydrothermal method. Yb³⁺ concentration is fixed at 1.5%, and Tm³⁺ concentration is changed from 0.1 to 0.4%. Intense upconversion luminescence is observed when the samples are excited by 980 nm. The dependence of upconversion luminescence on Tm³⁺ concentrations is presented. The results show that upconversion luminescence increases with the Tm⁺ concentration and gets its peak at 0.3 mol%. Under the excitation of 980 nm, the blue emission of 479 nm and the red emission of 647 nm are both duo to two photons process, and the UV emission of 361 nm is attributed to the three photons process. We also analyse the upconversion mechanism and process.     

Morphology control of titanium oxides by tetramethylammonium cations in hydrothermal conditions

The effect of tetramethylammonium cations (TMA⁺) on TiO₂ crystal morphology in hydrothermal conditions has been studied. The as-synthesized samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) methods. The morphologies including besom-like particle, nanosheet and nanotube have been observed. The different ways TMA⁺ cations in the hydrothermal bases affect the crystal growth manner are suggested to be responsible for the different morphologies of the as-synthesized samples.     

独特形貌碳酸钙的微波水热合成与表征

以醋酸钙和尿素为原料,在无添加剂的条件下采用微波水热法合成技术,直接制得了高度对称的双头矛状、双头扁平铲形、拉长六边形、拉长四边形、侧表面为六边形的多面体和六瓣花状等奇异形貌的碳酸钙晶体,利用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、傅里叶红外光谱仪(FT-IR)等对样品进行了表征,并对碳酸钙晶体的形成过程进行了分析。结果表明醋酸钙用量、尿素用量和微波辐照能量对碳酸钙晶体的结构与形貌具有重要调控作用。     

Structural and photoluminescence properties of aligned Sb-doped ZnO nanocolumns synthesized by the hydrothermal method

Aligned Sb-doped ZnO nanocolumns were synthesized by a simple hydrothermal method. Based on the analyses of the X-ray diffraction and photoluminescence result, it could be confirmed that the Sb has successfully doped in the ZnO crystal lattices to form an accepter energy level. At 85 K, the recombination of the acceptor-bound exciton was predominant in PL spectrum, which was attributed to the transition of the (Sb_Zn-2V_Zn) complex bound exciton. The acceptor binding energy had been calculated to be 123 meV.     

Photocatalytic oxidation of nitric oxide with immobilized titanium dioxide films synthesized by hydrothermal method

Gas-phase photocatalytic oxidation (PCO) of nitric oxide (NO) with immobilized TiO2 films was studied in this paper. The immobilized TiO2 films were synthesized by hydrothermal method. The characterization for the physicochemical properties of catalysts prepared under different hydrothermal conditions were carried out by X-ray diffraction analysis (XRD), transmission electron microscopy (TEM), high resolution-transmission electron microscopy (HR-TEM), Brunauer-Emmett-Teller measurements (BET) and scanning electron micrograph (SEM). It was found that the PCO efficiency of the catalyst was mainly depended on the hydrothermal conditions. The optimal values of hydrothermal temperature and hydrothermal time were 200 degrees C and 24 h, respectively. Furthermore, it was also known that the photocatalytic efficiency would decrease remarkably when the calcination temperature was over than 450 degrees C. Under the optimal conditions (hydrothermal condition: 200 degrees C for 24 h; calcination temperature: 450 degrees C), the photocatalytic efficiency of catalyst could reach 60% higher than that of Degussa P25.     

Novel hydrothermal synthesis method for tobermorite fibers and investigation on their thermal stability

Tobermorite fibers have been successfully synthesized by hydrothermal reaction at 200°C under the pressure of 2 MPa after 3-10 h using a Ca(II)-EDTA complex precursor. XRD patterns, TG-DTA analysis, and SEM observations show that the products are needle-like tobermorite fibers, which have diameter, length, and aspect ratio in the range of 0.1-10, 40-100, and 20-80 μm, respectively. The fibers can maintain their shapes up to 1150°C during the heat treatment.     

Influence of growth time and annealing on rutile TiO2 single-crystal nanorod arrays synthesized by hydrothermal method in dye-sensitized solar cells

Vertically aligned TiO₂ nanorod (NR) arrays have been grown on the fluorine doped tin oxide (FTO) substrates by hydrothermal methods and the structures were employed to fabricate the dye-sensitized solar cells (DSSCs). The charge transport properties were investigated by the current to voltage curves and the electrochemical impedance spectroscopy. It was found that DSSCs containing the as-prepared and 500 °C annealed TiO₂ NRs exhibit different trends with the growth time (t). The DSSCs assembled with the un-sintered NR arrays showed the highest power conversion efficiency (η) of 1.87%. When DSSCs were assembled with the sintered NR arrays, nearly 400% enhanced efficiency were obtained, and the values (η) showed a positive correlation with t. This behavior may be attributed to the improved adhesion and electric contact between TiO₂ and FTO, as well as the reduced number of recombination sites.     

Phase structure, morphology, and Raman characteristics of NaNbO3 particles synthesized by different methods

NaNbO₃ (NN) particles were synthesized by using conventional mixed-oxide (CMO), molten salt synthesis (MSS) and topochemical micro-crystal conversion methods (TMC), respectively. The effects of preparation methods on the phase structure, morphology and Raman characteristics of the NaNbO₃ particles were investigated. The results show that the NN particles prepared by conventional mixed-oxide and molten salt synthesis methods are all of orthorhombic structure in Pbma space group. Furthermore, those particles have equiaxial morphology. The single-crystal NaNbO₃ particles synthesized by the topochemical micro-crystal conversion method are of pseudocubic structure. Moreover, they are of plate-like shape with a high aspect ratio and a high (h 0 0) degree of orientation, which is very promising as template for texturing (K, Na)NbO₃ (KNN) based ceramics. Besides, all the spectra lines in the Raman spectra can be attributed to the internal modes of NbO₆ octahedron, and they prove that the particles synthesized by the different methods have different structure types.     

Rietveld refinement and spectroscopic studies of sodium lead fluoroapatite lacunaire synthesized by hydrothermal method

The structure of NaPb₉(PO₄)₆F(H₂O)_0.33, isostructural with apatite, was determined by X-ray powder diffraction methods and the result of Rietveld refinement is P6₃/m, a = 9.76396(8) Å and c = 7.27520(9) Å. The final refinement led to R_F = 5.4%, R_B = 6.6%. In the tunnel, the water molecule (O_w) and F⁻ ions appear to be located in 2b and 4e sites, with occupancies of 0.028(6) and 0.075(8), respectively. In the M(1) and M(2) sites the occupancies of Pb and Na are 0.282(3)/0.051(3) and 0.467(5)/0.033(5), respectively. The formula assigned to the compound is [Pb_3.38(4)Na_0.62(4)](1)[Pb_5.60(6)Na_0.40(6)](2)(PO₄)₆F_0.90(10)(H₂O)_0.33(7)□_0.77(17), where □ = vacancy. The assignment of the observed frequencies in the Raman and infrared spectra is discussed on the basis of a unit-cell group analysis and by comparison with fluor and chloroapatite analogs. The result of ³¹P and ²³Na magic angle spinning-nuclear magnetic resonance (MAS-NMR) spectroscopies confirmed the structural results.     

Photoluminescence studies from ZnO nanorod arrays synthesized by hydrothermal method with polyvinyl alcohol as surfactant

Well-aligned ZnO nanorod arrays have been synthesized by a simple hydrothermal method with polyvinyl alcohol as surfactant on F:SnO₂ conductive glasses substrates. Visible violet photoluminescence has been observed at room temperature. A series of annealing treatments in different environments have been made in order to investigate the nature of these emissions. The violet emission shows no change after annealing in air, while shifts to the ultra-violet region after annealing in H₂. It is concluded that the violet emission is due to V_Zn⁻ defect formed at the surface of the ZnO nanorods.     

Facile two-step preparation of polystyrene/anatase TiO2 core/shell colloidal particles and their potential use as an oxidation photocatalyst

Titania and materials containing titania have received considerable attention due to their technological importance in many areas. In this study, anatase crystalline titania (TiO₂) coated polystyrene (PS) colloidal particles were successfully prepared in two easy steps. First, a one pot synthesis of the colloidal particles was produced via an emulsifier-free emulsion copolymerization of styrene (S) and 2-(dimethylamino)ethyl methacrylate (DMA) at pH 4.0. In the second step, the synthesized particles were coated by titania using a sol–gel process in-situ hydrolysis and a condensation reaction of titanium(IV) isopropoxide in an acidic aqueous solution. In this way, anatase crystalline titania, rather than the usual amorphous form, was obtained as a shell on the PS colloidal particles. Both the PS colloidal particles and the polystyrene/anatase titania (PS/TiO₂) core/shell colloidal particles had monodisperse morphology and were characterized using SEM, Zetasizer, FTIR, XRD and TGA techniques or measurements. In addition, the photocatalytic activity of the PS/TiO₂ core/shell particles was tested for the first time in an oxidation reaction, in the oxidation of 4-methoxybenzyl alcohol (MBA) with O₂ in water. Much higher selectivities of the target product, p-anisaldehyde (AA), were obtained with the PS/TiO₂ core/shell particles than with a commercial anatase crystalline TiO₂.     

Influence of fluorine substitution on the morphology and structure of hydroxyapatite nanocrystals prepared by hydrothermal method

Hydroxyapatite (HAp) nanocrystals with different levels of fluorine substitution (P/F = 0, 6, 4 and 2) on the OH sites were produced via hydrothermal method. The fluorine substitution was found to alter the morphology of crystals appreciably. The aspect ratio and the crystallinity of HAp crystals increased with increasing fluorine substitution. The presence of broad ring and hallow ring patterns in electron diffraction suggests the low-crystalline nature of HAp crystals. With increasing fluorine substitution, the diffraction patterns exhibited discrete rings and numerous diffraction spots, implying the increased crystallinity. Raman spectra from the HAp nanoparticles also support the less-crystalline nature of the pristine HAp and the enhanced crystallization by fluorine substitution. In HAp crystals processed with no fluorine substitution, surface energy and planar Ca²⁺ density are less sensitive to the crystallographic orientation because of its low-crystalline nature, favoring equi-axed or slightly elongated particles. The addition of fluorine apparently increased the crystallinity, enhancing the orientation dependent growth and accordingly the aspect ratio. Osteoblast proliferation was observed to be enhanced by fluorine substitution in HAp. In vitro biological data support that the excellent osteoblastic cell viability and functional activity of the fluoridated apatite.     

Atomic scale study of the dehydration/structural transformation in micro and nanostructured brucite (Mg(OH)2) particles: Influence of the hydrothermal synthesis conditions

Micro and nanostructured brucite (Mg(OH₂)) particles synthesized by hydrothermal method from solutions with high content of hydrazine (0.14 M) and nitrate (0.24 g) were compared with samples obtained from low hydrazine content (0.0002 M) and nitrate (0.12 g). The samples were heated at 180 °C for 4 h, 6 h and 12 h. XRD, TEM-HRTEM, SAED and image analysis techniques were used for the morphological and structural characterization. The effect of electron beam irradiation on the brucite dehydration was observed in atomic resolution images at 300 kV. Hexagonal crystals show differences in crystallinity, strains and kinetic of reaction. High hydrazine/nitrate samples have slightly larger crystals with better crystallinity, showing a strong preferential orientation. Rietveld refinements show how unit cell parameters are bigger in samples obtained with higher hydrazine/nitrate content, confirming also the preferential orientation along the 0 0 0 1 plane. Differences in the dehydration process show the rapid formation of a porous surface, the amorphised cortex or the presence of highly oriented strains in samples prepared from higher hydrazine/nitrate content. Conversely, crystals slightly smaller with randomly scattered defect surfaces showing the Mg(OH)₂/MgO interphase in samples prepared with low hydrazine/nitrate content. Significant differences in the kinetic of reaction indicate how the dehydration process is faster in samples prepared with high hydrazine/nitrate content.     

Synthesis and characterizations of polycrystalline walnut-like CdS nanoparticle by solvothermal method with PVP as stabilizer

A wide range of cadmium sulfide (CdS) 3D polycrystalline walnut-like nanocrystals were prepared by solvothermal method with polyvinylpyrrolidone (PVP) as stabilizer. The morphology, structure, and phase composition of the as-prepared CdS nanoparticles were examined by using various techniques (X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), selected-area electron diffraction (SAED)). The optical properties of CdS were characterized by photoluminescence (PL) spectra. The paper showed that when the proper dosage of PVP (0.12 g 50 mL⁻¹) and the temperature of reaction (120 °C) were taken, continuous polycrystalline nanoparticles with regular morphology were obtained. The mechanism for the PVP-assisted synthesis of CdS 3D nanostructures and the growth process of CdS nanoparticles via Ostwald Ripening process under different temperatures with different dosages of PVP were also investigated. A sensitive electrochemical detection device of DNA hybridization using a paste glass carbon electrode (GCE) assembled by the PVP-capped CdS nanoparticles and immobilizing DNA probe was developed as a novel application of nano-semiconductors such as CdS to achieve a notable amplification in sensor response.     

Crystal morphology and growth mechanism of reinforcements synthesized by direct melt reaction in the system Al–Zr–O

In-situ Al₃Zr and Al₂O₃ particulates reinforced aluminum matrix composites were fabricated by the direct melt reaction (DMR) technique in the system Al–Zr–O. Microstructures of the composites and crystal morphology of in-situ formed Al₃Zr and Al₂O₃ particulates were analyzed by scanning-electron microscope (SEM) and transmission electron microscope (TEM). Results indicated that in-situ formed Al₃Zr and Al₂O₃ particles were finer and well distributed in aluminum matrix. Al₃Zr particulates with a tetragonal structure are mainly in the shape of polyhedron. A few of them are rectangular. The length/width ratio of the rectangular Al₃Zr is less than 2.0 and the maximum size is 4 μm. In addition, submicro Al₂O₃ particles with a hexagonal structure were also found in this system. Furthermore, it is found that twin may appear in the Al₃Zr crystal. The twin plane is (1 ). The twinning direction is [2 1].     

Energy transfer and luminescence properties of Eu-doped NaTb(WO4)2 phosphor prepared by a facile hydrothermal method

NaTb_(1−x)Eu_x(WO₄)₂ (x = 0-100%) phosphors have been synthesized via a mild hydrothermal process directly without further sintering treatment. X-ray diffraction (XRD), scanning electron microscope (SEM), photoluminescence excitation and emission spectra and decay curve were used to characterize the samples. Moreover, the luminescence colors of NaTb_(1−x)Eu_x(WO₄)₂ (NTbW:Eu) samples can be tuned from green, green-yellow, and yellow to red by simply adjusting the relative Eu³⁺-doping concentrations under a single wavelength excitation, which might find potential applications in the light displays systems.