The vibrational spectra of NbBO4, TaBO4, NaNb3O8 and NaTa3O8

The infrared and Raman spectra of NbBO₄ have been interpreted in terms of the zircon structure in space group I4₁/amd (D¹⁷_4h). Frequency shifts were observed in the Raman bands upon isotopic substitution of the boron atoms and when Nb was replaced by Ta in the crystal lattice. NaTa₃O₈ contains TaO₈ dodecahedra which are almost identical to the ones in TaBO₄ and its Raman spectra are compared with those of NaNb₃O₈ and of NbBO₄ amd TaBO₄ in order to assign metal—oxygen bands. The BO⁵⁻₄ vibrational bands resemble those of the SiO⁴⁻₄ groups rather than the B(OH)⁻₄ ones. However, the BO stretching force constant is much lower than the corresponding SiO one in SiO⁴⁻₄ and it appears as if the metal—oxygen interactions are much stronger in NbBO₄ and TaBO₄ than in ZrSiO₄ and HfSiO₄, respectively.     

Na3Al2Nb34O64 und Na (Si,Nb) Nb10O19: Clusterverbindungen mit isolierten Nb6-Oktaedern

Na₃Al₂Nb₃₄O₆₄ and Na (Si, Nb) Nb₁₀O₁₉. Cluster Compounds with Isolated Nb₆-Octahedra Hexagonal ormolu coloured plates of the new compounds Na₃Al₂Nb₃₄O₆₄ ( I ) and Na(Si, Nb)Nb₁₀O₁₉ ( II ) were prepared by heating pellets of NaF, Al₂O₃, NbO₂ and NbO (3:1:8:2) and NaF, NbO₂ and NbO (1:4:2), respectively, at approx. 850°C. I was contained in a sealed gold capsule, II in a silica tube. The Si incorporated in II originates from the container material. Both compounds crystallize in R 3 , I with a = 784.4(1), c = 7065(1) pm, Z = 3 and II with a = 784.1(1), c = 4221.8(5) pm, Z = 6. I and II represent new structure types. They contain the same characteristic structural units, namely discrete Nb₆O₁₂ clusters (d_Nb–Nb = 283 ± 4 pm) and Nb₂O₁₀ units with Nb–Nb dumbells (d_Nb–Nb ≈? 269 pm) in edgesharing coordination octahedra. In addition NbO₆ octahedra containing Nb in the oxidation state + 5 and NaO₁₂ cube-octahedra occur in both compounds besides AlO₄ and SiO₄ tetrahedra in I and II , respectively. The structures can be described in terms of a common closepacking of O and Na atoms together with Nb₆ octahedra.     

Specific thermal and thermodynamic properties of the tellurites Fe2(TeO3)3, Fe2TeO5 and Fe2Te4O11

The temperature dependence of the molar heat capacities of the tellurites Fe₂(TeO₃)₃, Fe₂TeO₅ and Fe₂Te₄O₁₁ were determined. By statistical manipulation of the values obtained, the parameters in the equations for the corresponding compounds showing this dependence were determined using the least-squares method. These equations together with the standard molar entropies were used to determine the thermodynamic functions Δ₀^T S _m⁰, Δ_T^T,H _m⁰ and (Φ_m⁰ + Δ₀^T’ H _m⁰ / T) for T’=298.15 K.     

Anionic templating: synthesis,structure, and characterization of novel three-dimensional mixed-metal oxychlorides Te(4)M(3)O(15).Cl (M = Nb(5+) or Ta(5+))

Two new three-dimensional oxychlorides are reported, Te(4)M(3)O(15).Cl (M = Nb(5+) or Ta(5+)). The isostructural materials were synthesized by chemical transport reactions utilizing TeO(2), M(2)O(5), and MCl(5) (M = Nb(5+) or Ta(5+)) as reagents. The compounds exhibit a three-dimensional cationic tunnel framework, with Cl(-) anions occupying the tunnels. Crystal data: monoclinic, space group C2/c, a = 18.9944(7) A, b = 7.8314(3) A, c = 21.1658(8) A, beta = 116.6400(10) degrees, Z = 8 (T = 295 K).     

Synthesis, structural characterization, and thermal stability of a new layered germanate structure, Na4Ge16O28(OH)12

The new layered germanate structure Na4Ge16O28(OH)12 has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction, FTIR, and SEM. The crystal lattice parameters are a = 7.3216(6) A, b = 14.3986(9) A, c = 7.7437(6) A, alpha = 90.0 degrees, beta = 100.179(7) degrees, gamma = 90.0 degrees, and V = 803.5(1) A3. The space group is C2/m with Z = 1. The germanium oxide sheets are connected non-covalently via electrostatic interactions with the sodium cations and H-bridging. At temperatures above 400 degrees C, the structure starts decomposing into sodium enneagermanate (Na4Ge9O20), germanium dioxide, and water as determined by powder X-ray diffraction, TGA, DTA, DSC, and GCMS.     

K2[Te4O8(OH)10]: synthesis,crystal structure and thermal behavior

Dipotassium octaoxodecahydroxotetratellurate, K₂[Te₄O₈(OH)₁₀], has been prepared hydrothermally in acidic medium under autogenous pressure. It crystallizes in space group P2₁/c of the monoclinic system with Z=2 in a cell of dimensions a=5.592(1) Å, b=8.283(2) Å, c=16.255(3) Å, and β=99.62(3)°. The outstanding feature of the structure is a tetrameric [Te₄O₈(OH)₁₀]^2– anion built up from edge and corner sharing TeO₆ octahedra. These anions and K⁺ cations are held together by electrostatic interactions and by hydrogen bonds. The compound decomposes in two steps at 350 and 420 °C, corresponding to a water and an oxygen loss, respectively, and affording the mixed valence oxide K₂Te^VI₃Te^IVO₁₂.     

Oxyfluorotitanophosphate cluster [Ti10P4O16F44]16-: synthesis and characterization of K16[Ti10P4O16F44

One oxyfluorotitanophosphate cluster compound, K16[Ti10P4O16F44], has been synthesized and structurally characterized. As far as we know, it is the first cluster compound for titanophosphate.     

Low temperature synthesis and characterization of Mn3O4 nanoparticles

Heating hydrous manganese (II) hydroxide gel at 85 °C for 12 hours produces Mn₃O₄ nanoparticles. They were characterized by X-ray powder diffraction (XRD) and infrared spectroscopy (FTIR). The particle size estimated from the SEM and X-ray peak broadening is approximately 32 nm, showing them to be nanocrystalline. EPR measurements confirm a typical Mn²⁺signal with a highly resolved hyperfine structure.      

Microwave-assisted synthesis and characterization of hexagonal Fe3O4 nanoplates

Hexagonal magnetite (Fe₃O₄) nanoplates with an average edge length of 80 nm were successfully prepared in large quantities by a facile microwave-assisted route. The influences of experiment parameters such as reaction time, microwave power, and concentration of NaOH and other additive agents on the morphology and size of final products were investigated in detail. Phase structure, morphology and magnetic properties of products were carefully studied by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution transmission electron microscope (HRTEM), and vibrating sample magnetometer (VSM). Magnetic studies revealed that hexagonal Fe₃O₄ nanoplates have low saturation magnetization of 36.4 emu/g and the possible reason has been proposed.     

Synthesis,structure and ionic conductivity of the molybdenum arsenate: Ag12.4Na1.6Mo18As4O71

The syntheses, structure and ionic conductivity of Ag_12.4Na_1.6Mo₁₈As₄O₇₁ are reported. Crystals and polycrystalline powders are synthesized by solid state reaction. It crystallized in the monoclinic space group C2/c with a = 20.032 Å, b = 16.872 Å, c = 19.373 Å and β = 112.14°. The structure can be described by the assemblage of Mo₈As₂O₃₄ ribbons interconnected through Mo₂O₇ groups. Monovalent cations are located around these ribbons. The ionic conductivities have been measured, on pellets of polycrystalline powders, between 423 and 663 K in the frequency range 1–13000 Hz, using diagrams of complex impedance. Impedance analysis suggests the presence of a dependent electrical relaxation temperature process in the material. Activation energy was obtained from Arrhenius plots (log σT versus 1000/T) and found to be 0.6 eV. The activation energies obtained from impedance and loss spectra are close. It suggests that the ionic transport in the elaborated material is due to a hopping mechanism. The dependence in frequency of the ac conductivity is found to obey Jonsher's relation.