Metrological characterization of X-ray diffraction methods at different acquisition geometries for determination of crystallite size in nano-scale materials

2013 ◽  
Vol 85 ◽  
pp. 111-123 ◽  
Author(s):  
Vladimir Uvarov ◽  
Inna Popov

2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Mihaela Flondor ◽  
Ioan Rosca ◽  
Doina Sibiescu ◽  
Mihaela-Aurelia Vizitiu ◽  
Daniel-Mircea Sutiman ◽  
...  

In this paper the synthesis and the study of some complex compounds of Fe(III) with ligands derived from: 2-(4-chloro-phenylsulfanyl)-1-(2-hydroxy-3,5-diiodo-phenyl)-ethanone (HL1), 1-(3,5-dibromo-2-hydroxy-phenyl)-2-phenylsulfanyl-ethanone(HL2), and 2-(4-chloro-phenylsulfanyl)-1-(3,5-dibromo-2-hydroxy-phenyl)-ethanone (HL3) is presented. The characterization of these complexes is based on method as: the elemental chemical analysis, IR and ESR spectroscopy, M�ssbauer, the thermogravimetric analysis and X-ray diffraction. Study of the IR and chemical analysis has evidenced that the precipitates form are a complexes and the combination ratio of M:L is 1:2. The central atoms of Fe(III) presented paramagnetic properties and a octaedric hybridization. Starting from this precipitation reactions, a method for the gravimetric determination of Fe(III) with this organic ligands has been possible. Based on the experimental data on literature indications, the structural formulae of the complex compounds are assigned.



1997 ◽  
Vol 30 (4) ◽  
pp. 427-430 ◽  
Author(s):  
F. Sánchez-Bajo ◽  
F. L. Cumbrera

A modified application of the variance method, using the pseudo-Voigt function as a good approximation to the X-ray diffraction profiles, is proposed in order to obtain microstructural quantities such as the mean crystallite size and root-mean-square (r.m.s.) strain. Whereas the variance method in its original form is applicable only to well separated reflections, this technique can be employed in the cases where there is line-profile overlap. Determination of the mean crystallite size and r.m.s. strain for several crystallographic directions in a nanocrystalline cubic sample of 9-YSZ (yttria-stabilized zirconia) has been performed by means of this procedure.



2016 ◽  
Vol 257 ◽  
pp. 147-151 ◽  
Author(s):  
Yi Wang ◽  
Svilen Bobev

Single-crystals of the new compound Ca14NbxIn1–xAs11 have been obtained from a solid-state reaction in a sealed Nb ampoule. The initial experiment had been set up with the aim to investigate the effect of electron doping (via In) on the crystal structure and physical properties of Ca14MnAs11. Subsequent single-crystal X-ray diffraction and elemental analysis work suggested that instead of Ca14MnxIn1–xAs11, the major product of the reaction is the phase Ca14NbxIn1–xAs11. This supposition was corroborated when the title compound was synthesized from a reaction of Ca, In and As in a sealed Nb ampoule, proving that, 1) Mn metal is not included in the structure, and 2) that the inadvertent side reaction of As with the walls of the Nb container is the source of the niobium. The overall structure is isotypic with the tetragonal Ca14AlSb11 structure type (space group I41/acd), although some marked differences between the two must be noted. Current ongoing work is focused on the synthesis of phase pure polycrystalline samples and determination of the physical properties of this unusual transition metal Zintl phase.



1961 ◽  
Vol 10 (8) ◽  
pp. 503-505
Author(s):  
Kazuo NEGORO ◽  
Takashi MATSUOKA


Sign in / Sign up

Export Citation Format

Share Document