Structure, electrochemical, magnetic and resonance properties of new layered antimonate Li(4)FeSbO(6) were comprehensively studied using powder X-ray diffraction, cyclic voltammetry, magnetic susceptibility, heat capacity, electron spin resonance and Mössbauer spectroscopy. In the crystal structure the iron ions form the triangular network within (LiFeSbO(6))(3-) layers alternating with nonmagnetic lithium layers. The electrochemical activity studied implies an Fe(3+)/Fe(4+) redox couple at 4.3 V (ox.) and 3.9 V (red.) thereby revealing that Li can be reversibly extracted. The long-range antiferromagnetic order was found to occur at the Néel temperature, T(N) ≈ 3.6 K, confirmed both by the magnetic susceptibility data and specific heat ones. The effective magnetic moment is estimated to be 5.93 μ(B)/f.u. and satisfactorily agrees with theoretical estimations assuming high-spin configuration of Fe(3+) (S = 5/2). In the magnetically ordered state, though, the magnetization demonstrates rather peculiar behavior. An additional anomaly on the M(T) curves appears at T(2) < T(N) in moderate magnetic field. The positions of transitions at T(N) and T(2) separate increasingly with increasing external field. Multiple measurements consistently demonstrated field-sensitive moving of magnetic phase boundaries constituting a unique phase diagram for the compound under study. The complex low-dimensional (2D) nature of magnetic coupling was confirmed by the dynamic magnetic properties study. Electron spin resonance from Fe(3+) ions in paramagnetic phase is characterized by a temperature independent effective g-factor of 1.99 ± 0.01. However, the distortion and broadening of the ESR line were found to take place upon approaching the magnetically ordered state from above. The divergence of the temperature-dependent linewidth is analyzed in terms of both critical behavior close to long-range magnetic order and the Berezinskii-Kosterlitz-Thouless (BKT)-type transition. Heat capacity measurements even at zero field manifested an appearance of the additional anomaly at temperatures below the Néel temperature. The temperature dependence of ESR intensity, linewidth and shift of the resonant field imply an extended region of short-range order correlations in the compound studied. The rich variety of the anomalies in magnetic and resonance properties makes this new antimonate a very interesting system to investigate the multiple phase transitions and competing exchange interaction due to the critical role of the layered structure organization accompanied by the frustration effects in triangular antiferromagnets.

Single crystalline ammonium trivanadate NH4V3O8 with variable morphologies, including shuttles, flowers, belts, and plates, was synthesized by the hydrothermal treatment of NH4VO3 with acetic acid. The crystals optimally grow under gentle conditions of 140 °C for 48 h. The resulting NH4V3O8 microcrystals were characterized by means of X-ray diffraction, scanning electron microscopy, infrared and Raman spectroscopy, static magnetization studies, and thermal analysis. The key factors to control the size and morphology of the crystals are the pH value and the vanadium concentration. A tentative microscopic growth mechanism is proposed and it is demonstrated how shape and morphology of the resulting microcrystalline material can be tuned by appropriate synthesis parameters.

Anatase TiO 2 nanotubes were synthesized via the hydrothermal method followed by annealing at 500 °C in argon for 1 h. The phase structure, morphology, and composition were investigated in detail by means of X-ray diffraction, scanning and highresolution transmission electron microscopy, infrared spectroscopy, and thermal analysis. The material consists of nanotubes with diameter of 10−15 nm and lengths of several hundred nanometers. The electrochemical properties were investigated by cyclic voltammetry and galvanostatic cycling. The data imply a first cycle irreversible capacity of 385 mAh/g, and capacities of 307 and 265 mAh/g after the second and 50th cycle, respectively, at C/10. The Coulombic efficiency of about 99% after cycle 50 implies excellent cycling stability. Hence anatase TiO 2 nanotubes evidence great potential for usage in highpower lithium-ion batteries.