Search results for "Diffraction"
showing 10 items of 1584 documents
Crystallite size of kaolinites as indicator of different geochemical types of bauxite
2009
A simple microstructural X-ray diffraction analysis using the Voigt function method reveals differences between bauxite deposits in the Iberian Range Catalanides area (NE, Spain). The highest values of apparent crystallite sizes, measured by volume weighted Dv values from 001 kaolinite reflection, have been found in bauxites of type 1.
Role of the thermal treatment on the microstructure of YAGG nanopowders prepared by urea glass route
2023
Yttrium aluminium gallium garnet (YAGG, Y3Al2Ga3O12) doped with rare-earth ions has drawn large attention owing to its optical properties with applications ranging from persistent luminescent phosphors to nanothermometers. Herein, three different YAGG materials were synthesized via the urea glass route followed by thermal treatment, relatively undoped; doped with Ce3+, Cr3+, and Nd3+; and doped with Ce3+, Cr3+, and Yb3+. The garnet formation was studied in situ upon thermal treatment from 300 to 1000 ◦C using synchrotron powder diffraction. Our results show that with this method, the onset of formation of the garnet is about 860 ◦C, with comparable cell parameters for both undoped and doped…
One‐Pot Synthesis of a New High‐Aluminium‐Content Super‐Microporous Aluminosilicate
2006
A new super-microporous aluminosilicate having a high aluminium content (Si/Al ca. 1) has been prepared through a surfactant-assisted procedure with the use of a commercially available binary precursor (di-sec-butoxyaluminooxytriethoxysilane) as a single source of both Al and Si. The formation of super-micropores is a result of a significant network shrinkage associated with the thermal elimination of the surfactant. This solid has been studied by X-ray powder diffraction, electron microscopy, nuclear magnetic resonance spectroscopy and porosimetry. A preliminary analysis of the acidity and the catalytic activity of the super-microporous solid for the selective catalytic reduction of NOx is…
Crystal Structures and Polymorphism of Nickel and Copper Coordination Polymers with Pyridine Ligands
2014
The crystal structures of a series of pyridine coordination polymers [MIICl2(C5H5N)x]n (M = Ni, Cu), prepared via thermal decomposition are reported. [NiCl2(C5H5N)4] (1) decomposes stepwise via [NiCl2(C5H5N)2]n (2), [NiCl2(C5H5N)]n (3), and [NiCl2(C5H5N)2/3]n (4), to NiCl2 with increasing temperature. The thermal decomposition of [CuCl2(C5H5N)2]n (5), progresses via two polymorphs of [CuCl2(C5H5N)]n (6a and 6b), and [CuCl2(C5H5N)2/3]n (7), to CuCl2. The compounds 3, 4, and 7 were prepared as pure phases. All crystal structures were determined by X-ray powder diffraction. Notably, the crystal structures of the polymorphs 6a and 6b were determined from powder diffraction data of a mixture of …
Interaction of Alkaline Metal Cations with Oxidic Surfaces: Effect on the Morphology of SnO2 Nanoparticles
2010
Reaction pathways to SnO(2) nanomaterials through the hydrolysis of hydrated tin tetrachloride precursors were investigated. The products were prepared solvothermally starting from hydrated tin tetrachloride and various (e.g., alkali) hydroxides. The influence of the precursor base on the final morphology of the nanomaterials was studied. X-ray powder diffraction (XRD) data indicated the formation of rutile-type SnO(2). Transmission electron microscopy (TEM) studies revealed different morphologies that were formed with different precursor base cations. Data from molecular dynamics (MD) simulations provide theoretical evidence that the adsorption of the cations of the precursor base to the f…
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…
Regio- and Stereoselective Synthesis of Spiropyrrolizidines and Piperazines through Azomethine Ylide Cycloaddition Reaction.
2015
A series of original spiropyrrolizidine derivatives has been prepared by a one-pot three-component [3 + 2] cycloaddition reaction of (E)-3-arylidene-1-phenyl-pyrrolidine-2,5-diones, l-proline, and the cyclic ketones 1H-indole-2,3-dione (isatin), indenoquinoxaline-11-one and acenaphthenequinone. We disclose an unprecedented isomerization of some spiroadducts leading to a new family of spirooxindolepyrrolizidines. Furthermore, these cycloadducts underwent retro-1,3-dipolar cycloaddition yielding unexpected regioisomers. Upon treatment of the dipolarophiles with in situ generated azomethine ylides from l-proline or acenaphthenequinone, formation of spiroadducts and unusual polycyclic fused pip…
A microcalorimetric study of the different states of argon and nitrogen adsorbed AT 77 K on silicalite-I and ZSM-5
1992
The adsorption of argon and nitrogen on a series of MFI-type zeolites (silicalite-I (Si/Al>1000) and HZSM-5 (16<Si/Al<120)) was studied by isothermal microcalorimetry, volumetry and neutron diffraction.
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…
Anisotropic chemical etching of semipolar \{10\bar {1}\bar {1}\}\mbox {/} \{10\bar {1}{+}1\} ZnO crystallographic planes: polarity versus dangling bo…
2009
ZnO thin films grown by metal?organic vapor phase epitaxy along the nonpolar direction and exhibiting semipolar facets have been chemically etched with HCl. In order to get an insight into the influence of the ZnO wurtzite structure in the chemical reactivity of the material, Kelvin probe microscopy and convergent beam electron diffraction have been employed to unambiguously determine the absolute polarity of the facets, showing that facets are unstable upon etching in an HCl solution and transform into planes. In contrast, facets undergo homogeneous chemical etching perpendicular to the initial crystallographic plane. The observed etching behavior has been explained in terms of surface oxy…