Synthesis of NH4FePO4·H2O nano-plates via solid-state reaction at low temperature and its thermochemistry properties

Ammonium-iron(II) phosphate monohydrate was synthesized via solid-state reaction at low temperature and characterized by X-ray diffraction, infrared spectroscopy, chemical analysis and scanning electron microscope. Thermochemical study was performed by an isoperibol solution calorimeter at 298.15 K. The results show that the obtained product is NH₄FePO₄·H₂O with plate shape of nanometer measure. According to Hess's law, a new thermochemical cycle was designed, and the standard enthalpy of formation of the titled complex at 298.15 K is .     

Structural characterization and AC conductivity of bis tetrapropylammonium hexachlorado-dicadmate, [N(C3H7)4]2Cd2Cl6

Synthesis, crystal structure, vibrational study, ¹³C, ¹¹¹Cd CP-MAS-NMR analysis and electrical properties of the compound [N(C₃H₇)₄]₂Cd₂Cl₆, are reported. The latter crystallizes in the triclinic system (space group , Z = 2) with the following unit cell dimensions: a = 9.530(1) Å, b = 11.744(1) Å, c = 17.433(1) Å, α = 79.31(1)°, β = 84.00(1)° and γ = 80.32(1)°. Besides, its structure was solved using 6445 independent reflections down to R = 0.037. The atomic arrangement can be described by alternating organic and inorganic layers parallel to the plan, made up of tetrapropylammonium groups and Cd₂Cl₆ dimers, respectively. In crystal structure, the inorganic layer, built up by Cd₂Cl₆ dimers, is connected to the organic ones through van der Waals interaction in order to build cation-anion-cation cohesion. Impedance spectroscopy study, reported in the sample, reveals that the conduction in the material is due to a hopping process. The temperature and frequency dependence of dielectric constants of the single crystal sample has been investigated to determine some related parameters to the dielectric relaxation.     

Spectroscopic and glass transition investigations on Nd-doped NaF-Na2O-B2O3 glasses

New developments in photonic technology need new materials for various applications. In the present report, Nd³⁺-doped NaF-Na₂O-B₂O₃ glasses were prepared and the spectroscopic and glass transition properties were analysed. The Fourier transform infrared spectral studies reveal that the glass contains BO₃ and BO₄ units as the local structures and the Na⁺ ions as the network modifiers. The absorption studies were carried out by using Judd-Ofelt theory, the experimental and theoretical oscillator strengths were also calculated. The emission spectral study was done for the 1 mol% Nd-doped glass and the spontaneous emission probability and stimulated emission cross-sections for the , transitions were calculated using the J-O parameters.     

Thermochemical studies on SrFe12O19(s)

The citrate-nitrate gel combustion route was used to prepare SrFe₁₂O₁₉(s) powder sample and the compound was characterized by X-ray diffraction analysis. A solid-state electrochemical cell of the type: (−)Pt, O₂(g)/{CaO(s) + CaF₂(s)}//CaF₂(s)//{SrFe₁₂O₁₉(s) + SrF₂(s) + Fe₂O₃(s)}/O₂(g), Pt(+) was used for the measurement of emf as a function of temperature from 984 to 1151 K. The standard molar Gibbs energy of formation of SrFe₁₂O₁₉(s) was calculated as a function of temperature from the emf data and is given by: (SrFe₁₂O₁₉, s, T)/kJ mol⁻¹ (±1.3) = −5453.5 + 1.5267 × (T/K). Standard molar heat capacity of SrFe₁₂O₁₉(s) was determined in two different temperature ranges 130-325 K and 310-820 K using a heat flux type differential scanning calorimeter (DSC). A heat capacity anomaly was observed at 732 K, which has been attributed to the magnetic order-disorder transition from ferrimagnetic state to paramagnetic state. The standard molar enthalpy of formation, (298.15 K) and the standard molar entropy, (298.15 K) of SrFe₁₂O₁₉(s) were calculated by second law method and the values are −5545.2 kJ mol⁻¹ and 633.1 J K⁻¹ mol⁻¹, respectively.     

Synthesis and characterization of a new organic dihydrogenomonophosphate [3,5-(CH3O)2C6H3NH3]2(H2PO4)2

Chemical preparation, crystal structure, calorimetric studies and spectroscopic investigation are given for a new organic cation dihydrogenomonophosphate [3,5-(CH₃O)₂C₆H₃NH₃]₂(H₂PO₄)₂. This compound is triclinic with the following unit cell parameters: a=9.030(6) Å, b=16.124(5) Å, c=8.868(3) Å, α=75.04(3)°, β=110.71(4)°, γ=104.61(1)°, Z=4, V=1148.0(1) Å³, Z=2 and ρ_cal.=1.454 g cm⁻³. Crystal structure was solved and refined to R=0.04, 2752 independent reflections. The atomic arrangement can be described as inorganic layers of H₂PO₄⁻ anions parallel to planes, between which are located the organic groups. Solid-state and MAS-NMR spectroscopies are in agreement with the X-ray structure. Ab initio calculations allow the attribution of the phosphorous and carbon signals to the independent crystallographic sites and to the various atoms of the organic groups.     

Effect of AlF3, CaF2 and MgF2 on hot-pressed hydroxyapatite-nanophase alpha-alumina composites

Nanophase alpha-alumina and hydroxyapatite composites (with and without 5 wt% AlF₃, CaF₂ or MgF₂, added separately) were hot pressed at 1100 °C and 1200 °C to investigate their mechanical properties and phase stability. Hydroxyapatite slightly decomposed to tri-calcium-phosphate when there was no F⁻ present. With the addition of AlF₃, CaF₂ or MgF₂ into the composite, it improved its thermal stability and mechanical properties. Substitution of OH⁻ by F⁻ ions in hydroxyapatite was verified by the change in hydroxyapatite's hexagonal lattice parameters and unit cell volume. A fracture toughness of 2.8 MPa  and μ-hardness of 8.25 GPa were calculated for the composite containing CaF₂ after the hot pressing at 1200 °C.     

Synthesis and characterization of nanocrystalline ferroelectric Sr0.8Bi2.2Ta2O9 by conventional and microwave sintering: A comparative study

In recent years mechanical activation technique has been utilized to synthesize the nanocrystalline form of compounds resulting in enhancement in the properties. Also, microwave sintering is being preferred over conventional sintering due to rapid processing and uniform temperature distribution throughout the specimen. In the present work, nanocrystalline non-stoichiometric strontium bismuth tantalate (SBT) of the composition Sr_0.8Bi_2.2Ta₂O₉ ferroelectric ceramics were synthesized by microwave sintering process (with sintering temperatures of 1000 °C and 1100 °C) and conventional solid state reaction process (with sintering temperature of 1100 °C) with an objective of comparing the properties of the synthesized specimens by the two processes. X-ray diffraction analysis shows the formation of single phase layered perovskite structure formation by both the processes. Scanning electron microscopy reveals the formation of a finer granular microstructure in the specimen synthesized by microwave sintering compared to that in the specimen prepared by conventional sintering. The specimen prepared by microwave sintering process exhibits improved electrical properties with higher dielectric constant, higher piezoelectric and pyroelectric coefficients and lower dielectric loss.     

Structural transition in the normal state of the superconductor Mo3Sb7

Low-temperature X-ray diffraction measurements on a correlated-electron superconductor Mo₃Sb₇ revealed that the high-temperature cubic state with the Ir₃Ge₇ type structure (space group ) transforms to tetragonal below T_S=53 K, at which spin-gap formation was recently suggested. The effect of electron correlations to the structural instability is briefly discussed in connection with the condensation of the high-temperature local moments to the spin-singlet-like state.     

Crystal structures and phase transitions in Ba2HoTaO6

The structure of the cation-ordered double perovskite Ba₂HoTaO₆ was examined using synchrotron X-ray powder diffraction at fine temperature intervals over the range of 90-300 K. Ba₂HoTaO₆ has a cubic structure in space group at room temperature. A proper ferroelastic phase transition to I4/m tetragonal symmetry occurs near approximately 260 K. Analysis of the spontaneous tetragonal strain versus temperature indicated that the phase transition is second order in nature.     

Dielectric, electrical and magnetoelectric characterization of (x)Ni0.8Zn0.2Fe2O4 + (1 − x)Pb0.93La0.07(Zr0.60Ti0.40)O3 composites

The structural, electrical, dielectric, magnetic and magnetoelectric properties of (x)Ni_0.8Zn_0.2Fe₂O₄ + (1 − x)Pb_0.93La_0.07(Zr_0.60Ti_0.40)O₃ (x = 0, 0.15, 0.30, 0.45 and 1) have been studied by means of various experimental techniques. Polycrystalline samples of this series have been prepared by the double sintering ceramic method. X-ray diffraction data analysis revealed purity of the composites. Microstructural analysis using scanning electron microscopy mode depicts the presence of two phases in contact with each other. Dielectric properties were studied at and well above room temperature. Temperature dependent variation of the dielectric constant show diffused phase transition which can be well described by fitting the Lorentz-type relation, . Observation of well-saturated ferroelectric hysteresis loop and magnetic hysteresis loop for composites indicates that ferroelectric and magnetic ordering exist simultaneously at room temperature. The static value of magneto electric voltage coefficient (α_E) has been studied as a function of magnetic field at room temperature for all the composites. The maximum value of α_E is 7.53 mV/(cm Oe) for 85% PLZT-15% NZFO composites.