Search results for "Powder diffraction"
showing 10 items of 243 documents
Thermally highly stable amorphous zinc phosphate intermediates during the formation of zinc phosphate hydrate.
2015
The mechanisms by which amorphous intermediates transform into crystalline materials are still poorly understood. Here we attempt to illuminate the formation of an amorphous precursor by investigating the crystallization process of zinc phosphate hydrate. This work shows that amorphous zinc phosphate (AZP) nanoparticles precipitate from aqueous solutions prior to the crystalline hopeite phase at low concentrations and in the absence of additives at room temperature. AZP nanoparticles are thermally stable against crystallization even at 400 °C (resulting in a high temperature AZP), but they crystallize rapidly in the presence of water if the reaction is not interrupted. X-ray powder diffract…
The comparison of seven different methods to quantify the amorphous content of spray dried lactose
2006
The purpose of this work was to verify the usefulness, advantages and disadvantages of seven methods that are widely used to detect, and quantify the amorphous contents in pharmaceutical solids. Here, StepScan DSC, a type of modulated temperature calorimetry method, was applied for the first time to quantify amorphicity. The comparison of the analytical methods was undertaken with real (non-artificial) test samples, i.e. spray-dried lactose samples with various degrees of crystallinity. In these samples, it was essential that the amorphous and the crystalline portions are not present as separate particles, which is the case when physical (artificial) mixtures of totally amorphous and totall…
X-ray powder diffraction data for five lanthanoid chromates [Ln2(CrO4)3(H2O)5]·2H2O (Ln=La,Pr,Nd,Sm,Eu)
1994
X-ray powder diffraction data are reported for a series of isomorphous compounds of [Ln2(CrO4)3(H2O)5]·2H2O, where Ln=La, Pr, Nd, Sm, or Eu. The compounds crystallize in monoclinic space group P21/c (No: 14) with Z=4. Refined unit cell parameters and indexed powder diffraction patterns are given.
Thermal expansion and magnetic properties of benzoquinone-bridged dinuclear rare-earth complexes.
2017
The synthesis and structural characterization of two benzoquinone-bridged dinuclear rare-earth complexes [BQ(MCl2·THF3)2] (BQ = 2,5-bisoxide-1,4-benzoquinone; M = Y (1), Dy (2)) are described. Of these reported metal complexes, the dysprosium analogue 2 is the first discrete bridged dinuclear lanthanide complex in which both metal centres reside in pentagonal bipyramidal environments. Interestingly, both complexes undergo significant thermal expansion upon heating from 120 K to 293 K as illustrated by single-crystal X-ray and powder diffraction experiments. AC magnetic susceptibility measurements reveal that 2 does not show the slow relation of magnetization in zero dc field. The absent of …
Synthesis, crystal structure, optical, thermal and magnetic studies of a new organic-inorganic hybrid based on tetrachloroferrate (III)
2021
Abstract A new organic metal halide hybrid, benzyltrimethylammonium tetrachloroferrate (III), 1, ((BzMe3N)FeCl4) was synthesized by slow evaporation. The single crystal X-ray diffraction reveals that 1, crystallizes in the P-1 triclinic space group with the parameters a = 7.158 (5), b = 8.814 (8), c = 12.922 (4) A, α = 82.44 (5), β = 86.14 (4), γ = 87.13 (7)°, V = 805.7 (10) A3 and Z = 2. The structure packing exhibits a cationic and anionic layers alternation linked by means of C─H⋯Cl hydrogen interactions. The Hirshfeld surface and the lattice energy of 1 were calculated. The material purity was verified using X-ray powder diffraction and Rietveld refinements. The TG-DTA a…
Ball-milling and AlB2 addition effects on the hydrogen sorption properties of the CaH2 + MgB2 system
2011
Abstract Among the borohydrides proposed for solid state hydrogen storage, Ca(BH 4 ) 2 is particularly interesting because of its favourable thermodynamics and relatively cheap price. Composite systems, where other species are present in addition to the borohydride, show some advantages in hydrogen sorption properties with respect to the borohydrides alone, despite a reduction of the theoretical storage capacity. We have investigated the milling time influence on the sorption properties of the CaH 2 + MgB 2 system from which Ca(BH 4 ) 2 and MgH 2 can be synthesized by hydrogen absorption process. Manometric and calorimetric measurements showed better kinetics for long time milled samples. …
Dissolution behavior of co-amorphous amino acid-indomethacin mixtures: The ability of amino acids to stabilize the supersaturated state of indomethac…
2017
Article
Proton sponge lead halides containing 1D polyoctahedral chains
2021
Hybrid one-dimensional lead halides, containing the protonated 1,8-bis(dimethylamino)naphthalene moiety (C14H19N2, monoprotonated "proton sponge"), were prepared by simple one-pot methods and investigated in terms of crystal structure, morphology, thermal stability and electronic properties. The as-precipitated (C14H19N2)PbBr3 and (C14H19N2)PbI3 species are isostructural and crystallize in the orthorhombic Pbca space group, resulting in 1D crystal phases with ([PbX3](-))(infinity) chains (built by face-sharing [PbX6] octahedra; X = Br, I), among which the (C14H19N2)(+) cations are inserted. The two compounds display complete miscibility in the solid state: both (C14H19N2)PbI2Br and (C14H19N…
THz nanocrystal acoustic vibrations from ZrO2 3D supercrystals
2013
International audience; We report sharp low-frequency Raman spectral features of supercrystals synthesized via the "benzyl alcohol route" and consisting of either yttrium-stabilized or pure zirconia (ZrO2) nanocrystals. In situ formed benzoate species control the nanocrystal growth and act as organic glue leading to the assembly of the nanocrystals in highly ordered 3D supercrystals. We attribute some Raman peaks to THz acoustic vibrations of individual nanocrystals which are only weakly coupled due to the strong acoustic mismatch between the capping ligands and the nanocrystals. Peak positions are consistent with nanocrystal sizes estimated from transmission electron microscopy and X-ray p…
Influence of Axial Pressure on the Electrical Properties of Li0.06Na0.94NbO3 Ceramic
2011
Lead-free ceramic Li0.06Na0.94NbO3 was synthesized using a conventional solid-state processing. The single-phase perovskite structure was identified by X-ray powder diffraction technique. The values of lattice parameters of Li0.06Na0.94NbO3 are lower than those for pure NaNbO3. The EDS analysis shows the fairly homogeneous distribution of all elements throughout the grains. An axial pressure significantly influences electric properties. With increasing pressure the peak intensity in the ϵ(T) curve decreases, the peak becomes diffused and shifts to a lower temperature. The value of tanδ increases with increasing axial pressure and its local maximum shifts towards lower temperatures.