Search results for " diffraction"

Physical properties of (1−x)Ba0.95Pb0.05TiO3+xCo2O3 (x=0, 0.1, 0.3, 0.5, 1.0, 2.0wt%) ceramics

2015

The paper reports studies of the (1−x)Ba0.95Pb0.05TiO3 – xCo2O3 (x≤0.02) ceramics. Results of X-ray powder diffraction, dielectric, magnetic and IR measurements, as well as ab initio simulations are presented. The Co-doping induces small decrease of the (c/a) tetragonality of the perovskite lattice and leads to the gradual shift of the ferroelectric transition temperature from 398 K for x=0 down to 357 K for x=0.02. The conductivity activation energies are in the range 0.8–0.9 eV in agreement with the calculations. The high-temperature conductivity can be ascribed by the migration of oxygen vacancies introduced to compensate the charge deficiency due to Co3+ valence at the B-site of the per…

Organic solvent vapor effects on phase transition of α and β tegafur upon grinding with solvent additives.

2012

Abstract Solvent effects on α tegafur (5-fluoro-1-(tetrahydro-2-furyl)uracil) phase transition to β tegafur during grinding with solvent additive, as well as phase transition in samples exposed to 95% relative solvent vapor pressure has been studied in this research. Samples containing 0.5% and 0.1% of β tegafur in α and β tegafur mixture, as well as samples of pure α tegafur were ground with different solvent additives, and conversion degrees depending on the solvent were determined using PXRD method. Samples with α and β tegafur weight fraction of 1:1 were exposed to 95% relative solvent vapor pressure, and phase transition rates were determined. Solubility of α tegafur, solvent sorption …

Polymorphism and solvates of flecainide base

2013

Flecainide base is pharmaceutically active substance used for production of flecainide acetate which is known in market as Tambacor, Almarytm, Apocard, Ecrinal or Flecaine. It is determined that flecainide base forms four polymorphic forms abbreviated as Ib, IIb, IIIb and IVb. Flecainide base form Ib is thermodynamically stable form at laboratory temperature while form IIIb is stable at higher temperatures. Flecainide form Ib absorbs water in its structure between layers and forms non-stoichiometric hydrate. Flecainide base binds with organic solvents and form monosolvates. Flecainide base form Ib crystallizes in orthorhombic crystals with lattice parameters a = 27.88 Å, b = 13.78 Å, c = 9.…

Wavelength compensation of broadband light diffraction

1998

A tangent formula derived from Patterson-function arguments. VII. Solution of inorganic structures from powder data with accidental overlap

2000

Accidental overlap constitutes one of the principal limitations for the solution of crystal structures from powder diffraction data, since it reduces the number of available intensities for direct-methods application. In this work, the field of application of the direct-methods sum function is extended to cope with powder patterns with relatively large amounts of accidental overlap. This is achieved by refining not only the phases of the structure factors but also the estimated intensities of the severely overlapped peaks during the structure solution process. This procedure has been specifically devised for inorganic compounds with uncertain cell contents and with probable severe atomic di…

From Mannose to Small Amphiphilic Polyol: Perfect Linearity Leads To Spontaneous Aggregation

2016

Terminally unsaturated and diastereochemically pure polyol derived from d-mannose shows spontaneous aggregation behavior in water solution. In order to study and clarify this unforeseen phenomenon, a conformational study based on NMR spectroscopy combined with ab initio structure analysis using the COSMO-solvation model was pursued. The results, together with X-ray diffraction studies, suggest a low energy linear conformation for this particular substrate both in solid states and in solution. For such small-sized acyclic carbohydrate derivatives, the linear conformation appears to be a key prerequisite for the unusual molecular self-assembly reported herein. peerReviewed

Polystyrene nanoparticle-templated hollow titania nanosphere monolayers as ordered scaffolds

2018

We report a novel multi-step method for the preparation of ordered mesoporous titania scaffolds and show an illustrative example of their application to solar cells. The method is based on (monolayer) colloidal nanosphere lithography that makes use of polystyrene nanoparticles organised at a water–air interface and subsequently transferred onto a solid substrate. A titania precursor solution (titanium(IV) isopropoxide in ethanol) is then drop-cast onto the monolayer and left to “incubate” overnight. Surprisingly, instead of the expected inverse monolayer-structure, a subsequent calcination step of the precursor yields an ordered monolayer of hollow titania nanospheres with a wall thickness …

Study of the structural phase transformation of iron oxide nanoparticles from an Fe2+ ion source by precipitation under various synthesis parameters …

2015

Abstract Magnetite nanoparticles were precipitated from a pure aqueous ferrous salt solution in an air atmosphere. The influence of the solution molarity, the rate of precipitator agent addition, stirring time and annealing temperature was studied. The morphology, crystalline phase purity and magnetic properties of the obtained powders were studied by X-Ray powder diffraction (XRD), Scanning electron microscopy (SEM), Differential thermal analysis (DTA), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS) and Vibrating sample magnetometer (VSM). The synthesis conditions were seen to have an effect on phase composition. It was possible to obtain near stoichiometric Fe…

Use of alkylarsonium directing agents for the synthesis and study of zeolites

2019

[EN] Expanding the previously known family of -onium (ammonium, phosphonium, and sulfonium) organic structure-directing agents (OSDAs) for the synthesis of zeolite MFI, a new member, the arsonium cation, is used for the first time. The new group of tetraalkylarsonium cations has allowed the synthesis of the zeolite ZSM-5 with several different chemical compositions, opening a route for the synthesis of zeolites with a new series of OSDA. Moreover, the use of As replacing N in the OSDA allows the introduction of probe atoms that facilitate the study of these molecules by powder X-ray diffraction (PXRD), solid-state nuclear magnetic resonance (MAS NMR), and X-ray absorption spectroscopy (XAS)…

X-ray absorption spectroscopy study of local dynamics and thermal expansion in ReO3

2015

The thermal expansion of polycrystalline ${\mathrm{ReO}}_{3}$ is studied in vacuum by x-ray diffraction from 300 to 600 K and by extended x-ray absorption fine structure (EXAFS) at the Re ${L}_{3}$ edge from 30 to 600 K. A detailed EXAFS analysis is presented up to the sixth coordination shell around Re. The crystal thermal expansion is weak throughout the explored range, negative below 100 K, positive from 150 to 500 K, and negative again above 500 K. The analysis of mean square relative displacements obtained by EXAFS and of mean square displacements available from x-ray and neutron diffraction measurements confirms the presence of significant static disorder in the investigated samples. …