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.

Hydrothermal synthesis of spherical and hollow Gd2O3 : Eu3+ phosphors

Spherical and submicrometer-sized hollow Gd2O3:Eu3+ phosphors were prepared by homogeneous precipitation and hydrothermal method by varying the concentrations of reactants and changing the synthesis conditions. In the precipitation step, the spherical nucleus was formed and grew to large particles. In the hydrothermal step, the large particles crystallized to solid or hollow spheres. At last, Gd2O3:Eu3+ phosphors were obtained by annealing at the temperature more than 600 degrees C. The deduced mechanics of forming the solid and hollow spheres was proposed. And the obtained spherical Gd2O3:Eu3+ phosphors had better red luminescence properties. The relative luminescence intensity and the lifetime increased with increasing annealing temperatures.

Hydrothermal synthesis of Fe and Mn doped SnO2 and its magnetic structures

The dilute magnetic semiconductor of Sn1-x-yMnxFeyO2 (0 <= x <= 0.10, 0 <= y <= 0.10) Were syhthesized with the hydrothermal method using SnCl4, Mn(CH3COO)(2) center dot 4H(2)O and FeCl3 center dot 6H(2)O as the raw materials. The structure, morphologies and magnetic properties of the sample were characterized via X-ray powder diffractometer(XRD), transmission electron microscopy(TEM), Raman spectrum and superconducting and quantum interference device(SQUIT), and Mossbeaur spectrum. No secondary phase was found in the XRD spectrum. The morphology of the samples is affected by the kind or the mount of transition metal. The local vibrating model-of Mn Positioned SnO2 sites was found in Raman spectrum. The measured magnetic results indicate that when x = 0.10, y = 0, the sample exhibits strong magnetization in low-temperature (5 K), but the magnetization decrease rapidly at room. temperature; In contrast, when x = 0, y = 0.1, the sample's magnetization and coercivity are both small, but being temperature independent. Mossbeaur spectra indicates that part of the Fe is ferromagnetic coupled, and the simulating results indicate that the ferromagnetic character is intrinsic.

Hydrothermal synthesis, structure characterization of a new mixed Mo/V metal-oxygen cluster compound: [Co(phen)(3)](2)[HPMo4V (Mo4V6IV)-V-VI M2O44]center dot 4H(2)O, (M=0.78Mo(V)+0.22V(IV))

A new polyoxometalate [Co(phen)(3)](2)[HPMo4V Mo-4(VI) V-6(IV) M2O44]center dot 4H(2)O (M = 0.78Mo(V)+ 0.22V(IV)) 1 was hydrothermally synthesized and characterized by IR, elemental analyses, X-ray photoelectron spectrum, ESR and single crystal X-ray diffraction. The title compound is in the triclinic space group P (1) over bar with a = 12.0953(7) angstrom, b = 14.0182(6) angstrom, c = 14.6468(7) angstrom, V=2402.55(18) angstrom(3), alpha = 105.134(2), beta = 91.841(3), gamma = 91.401(2), Z = 1, and R-1 (wR(2)) = 0.0617 (0.1701). The compound was prepared from tetra-capped pseudo-Kepin with phosphorus-centered polyoxoanions [PMo8V6M2O44](5-) , [Co(phen)(3)](2+) cations and linked through hydrogen bonds and pi-pi stacking interaction into three-dimensional supramolecular framework. Astudy of the magnetic properties of 1 demonstrates that it exhibits antiferromagnetic coupling interactions.

Hydrothermal synthesis of ZrW2O8 nanorods

Negative thermal expansion ZrW2O8 nanorods were synthesized by a rapid low-temperature hydrothermal route, followed with a heat treatment at 500 degrees C for 6h. Acidity of the HCl addition to the mixed solution in the hydrothermal condition strongly affects the formation of the precursor ZrW2O7(OH)(2)(H2O)(2). High acidity of HCl in the range of 5-10 N facilitates the nucleation of ZrW2O7(OH)(2)(H2O)(2), but constrains its growth. Low acidity of HCl addition (< 5 N) only obtained the products ZrO2 and WO3 by firing the precursors. FE-SEM images revealed that the shape and size of ZrW2O8 were modeled after its precursor ZrW2O7(OH)(2)(H2O)(2).

The first discrete mixed-valence hexadecavanadate host shell cluster anions: hydrothermal synthesis, structure and characterization of [V16O38(Cl)](8-)

A new compound, [NH4](2)[Zn(phen)(3)](2)[Zn(phen)(2)(H2O)(2)][V16O38(Cl)] (.) 5H(2)O (1), was synthesized in the hydrothermal condition. The "naked" [V16O38(Cl)](8-) is the first observation with host shell structure in polyoxovanadate chemistry.

Hydrothermal synthesis and crystal structure of a sulfur-bridged binuclear copper(II) coordination polymer generated by a spontaneous reduction

A simultaneous reduction SO42- to S2- by 2,5-pyridinedicarboxylate under hydrothermal conditions produced a new binuclear copper(II) coordination polymer [CuS(4,4'-bipy)](n) (4,4-bipy = 4,4'-bipyridine) (1). Single crystal X-ray analysis revealed that compound I consisted of sulfur-bridged binuclear copper(II) units with Cu-Cu bonding which were combined with 4,4-bipy to generate a three-dimensional network constructed from mutual interpenetration of two-dimensional (6,3) nets. Crystal data for 1:C10H8CuN2S, tetragonal 14(1)/acd, a = 14.0686(5) Angstrom, b = 14.0686(5) Angstrom, c = 38.759(2) Angstrom, Z = 32. Other characterizations by elemental analysis, IR, EPR and TGA analysis were also described in this paper.

Vaterite-type YBO3 : Eu3+ crystals: hydrothermal synthesis, morphology and photoluminescence properties

Vaterite-type YBO3:Eu3+ crystals with interesting flower and hedgehog fungus-like structures composed of nanosheets were obtained by controlled crystallization of Y2O3 and Eu2O3 in H3BO3 solutions under acidic hydrothermal (HT) conditions. Nanosheets of uniform thicknesses were formed by preferential crystal growth along the (100) crystallographic plane and specific three-dimensional structures were further developed through a homocentric growth mechanism. Optical emission measurements showed that the HT-grown nanosheet crystals exhibited a higher ratio of the emitted red-to-orange light ratio than crystals grown from solid-state reactions. The photoluminescence intensity and emission lifetimes were also studied as a function of the Eu3+ dopant concentration and the HT synthesis temperature. The effect of some additives: a chelating ligand, a surfactant and a polymer, on the YBO3:Eu3+ crystals morphology was also investigated.

In(OH)(3) and In2O3 nanorod bundles and spheres: Microemulsion-mediated hydrothermal synthesis and luminescence properties

Indium hydroxide, In(OH)(3), nano-microstructures with two kinds of morphology, nanorod bundles (around 500 nm in length and 200 nm in diameter) and caddice spherelike agglomerates (around 750 - 1000 nm in diameter), were successfully prepared by the cetyltrimethylammonium bromide (CTAB)/water/cyclohexane/n-pentanol microemulsion-mediated hydrothermal process. Calcination of the In(OH)(3) crystals with different morphologies (nanorod bundles and spheres) at 600 degrees C in air yielded In2O3 crystals with the same morphology. X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and photoluminescence (PL) spectra as well as kinetic decays were used to characterize the samples. The pH values of microemulsion play an important role in the morphological control of the as-formed In(OH)(3) nano-microstructures from the hydrothermal process. The formation mechanisms for the In( OH) 3 nano- microstructures have been proposed on an aggregation mechanism. In2O3 nanorod bundles and spheres show a similar blue emission peaking around 416 and 439 nm under the 383-nm UV excitation, which is mainly attributed to the oxygen vacancies in the In2O3 nano-microstructures.

Hydrothermal synthesis, structure, and characterization of two one-dimensional chainlike hybrid complexes [(CuX)(2)(o-phen)](infinity) (X = Br, Cl; o-phen = o-phenanthroline)

Two novel organic-inorganic hybrid complexes [(CuX)(2)(o-phen)](infinity) (X = Br (1), Cl (2); o-phen = o-phenanthroline) have been synthesized hydrothermally and characterized structurally by elemental analyses, IR, ESR, XPS spectrum, TG analyses and single-crystal X-ray diffraction. Both title compounds exhibit novel one-dimensional chainlike copper halide scaffolding constructed by the unusual [Cu3X3] hexagon motifs by sharing opposite edges, where a single Cu site of each [Cu3X3] hexagon is chelated with N donors of o-phen group. To our knowledge, such basic o-phen-copper halide skeleton has not been reported hitherto. Moreover, TG analyses indicate that both title compounds possess high thermal stability.

A two-dimensional molybdenum (V) phosphate with covalently bonded transition metal coordination complexes: hydrothermal synthesis and structure characterization of Na-2[{Mn(phen)(2)(H2O)}{Mn(phen)(2)}(3){Mn (Mo12O24)-O-V (HPO4)(6)(PO4)(2)(OH)(6)}] center dot 4H(2)O (phen=1,10-phenanthroline)

An organic-inorganic hybrid molybdenum phosphate, Na-2[{Mn(phen)(2)(H2O)} {Mn(phen)(2)}(3){(MnMo12O24)-O-v (HPO4)(6)(PO4)(2) (OH)(6)}] . 4H(2)O (phen=1,10-phenanthroline), involving molybdenum present in V oxidation state and covalently bonded transition metal coordination complexes, has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. Deep brown-red crystals are formed in the triclinic system, space group P (1) over bar, a=16.581(l)Angstrom, b=18.354(1)Angstrom, c=24.485(2)Angstrom, alpha=80.589(l)degrees, beta=71.279(1)degrees, gamma=67.084(1)degrees, V=6493.8(8)Angstrom(3), Z=2, lambda(MoKalpha)=0.71073Angstrom (R(F)=0.0686 for 29,053 reflections). Data were collected on a Bruker Smart Apex CCD diffractometer at 293 K in the range of 1.76 < theta < 28.06degrees using omega-2theta scans technique. The structure of the title compound may be considered to be based on {Mo6O12(HPO4)(3)(PO4)(OH)(3)} units bonded together with {Mn(phen)(2)} subunits into a two-dimensional network. Two types of tunnels are observed in the solid of the title compound.

Hydrothermal synthesis and structure of [Ni(en)(2)V6O14](n)

A new complex [Ni (en)(2)V6O14](n) was hydrothermally synthesized and characterized by 2-dimensional vanadium oxide framework pillared by Ni(en)(2)group. Single crystal X-ray analysis indicates that this compound crystallizes in monoclinic system, space group P2(1)/c with a=0. 892 17(18) nm, b = 1. 711 1(3) nm, c=0. 662 73(13) nm, beta=111. 58(3)degrees, V=0.940 8(3) nm(3), Z=2, D-c=2.501 g/cm(3), R=0. 042 3, omegaR=0. 060 9, S=1. 006.

Hydrothermal synthesis and structural characterization of a novel P-V-O layered compound [H(2)en](2)[H3O](6)[Co(H2O)(2)(VO)(8)(OH)(4)(PO4)8]

A new compound [H(2)en](2)[H3O](6)[Co(H2O)(2)(VO)(8)(OH)(4)(PO4)(8)] has been hydrothermally synthesized. Single crystal X-ray analysis indicates that this compound crystallizes in a monoclinic system, space group P2(1)/n with a=1.438 5(3) nm, b=1.012 2(2) nm, c=1.832 5(4) nm, beta=90.21degrees, V=2.668 2 (9) nm(3), Z = 2, D-c = 2.112 g/cm(3), R = 0.055, wR = 0.149 7, S = 1.037. The structure of [H(2)en](2)[H3O](6)[Co(H2O)(2)(VO)(8)(OH)(4)(PO4)(8)] is characterized by P-V-O layers constructed by [(VO)4 (OH)(2)(PO4)(4)](6-) non-symmetric units. The P-V-O layers are pillared by [Co(H2O)(2)](2+) group, resulting in the channels within which the protonated diaminoethane and H3O+ are located.