Synthesis of New Multiple Layered Dion-Jacobson Perovskites

2014 ◽  
Vol 1655 ◽  
Author(s):  
Léa Gustin ◽  
Jérôme Lefebvre ◽  
Clare Davis-Wheeler ◽  
Amy K. Pressley ◽  
John B. Wiley
Keyword(s):  
Solid State ◽  
Alkali Metals ◽  
Layered Compound ◽  
Direct Reaction ◽  
Exchange Reactions ◽  
Metal Chlorides ◽  
Ceramic Method ◽  
X Ray ◽  
New Compounds ◽  
Layered Perovskites

ABSTRACTNew multiple layered perovskites with general formula RbLaNaxNb2+xO7+3x, x = 1 and 2, were synthesized via a ceramic method. While the triple layered compound could be obtained by simple direct reaction, the quadruple layered one was synthesized using a two-step solid state approach. The compounds were characterized by X-ray powder diffraction; the newly obtained compounds appear to be isostructural with the previously reported RbCa2Nb3O10 and RbCa2NaNb4O13 for RbLaNaNb3O10 and RbLaNa2Nb4O13, respectively. Preliminary results show that the new compounds can undergo ion exchange reactions involving alkali metals and transition metal chlorides.

Compounds of Complex Halo and Pseudohalo Acids of the Group IIB Metals, Part V [1] Preparative and Spectroscopic Studies of the [Hg2I5]-, [Hg2I6]2- and [Hg3I8]2- Ions

1982 ◽  
Vol 37 (5) ◽  
pp. 646-648 ◽  
Author(s):  
S. P. Perlepes ◽  
Th. F. Zafiropoulos ◽  
A. K. Anagnostopoulos ◽  
A. G. Galinos
Keyword(s):  
Solid State ◽  
Spectroscopic Studies ◽  
Molar Conductance ◽  
X Ray ◽  
New Compounds ◽  
Complex Anions

The preparations of new compounds, containing the complex anions [Hg2l5]-, [Hg2l6]2- and [Hg3I8]2-, are reported.Distorted iodine-bridged configurations are proposed for the complexes in the solid state, utilising analyses, X-ray powder patterns, molar conductance measurements and spectral (IR, UV) data

Multinuclear NMR and Powder X-ray Diffraction Studies of Si and Sn Clathrates of Alkali Metals: Vacancies, Disorder and Knight Shifts

2001 ◽  
Vol 691 ◽  
Author(s):  
Michael J. Ferguson ◽  
Igor L. Moudrakovski ◽  
Christopher I. Ratcliffe ◽  
John S. Tse
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Nmr Spectra ◽  
Alkali Metals ◽  
Rietveld Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Binary Metal ◽  
Knight Shifts

ABSTRACTThe Structure I type binary metal clathrates of K/Si, Rb/Si and Cs/Sn have been synthesised and studied by powder X-ray diffraction and solid state NMR. Rietveld analysis shows that in all three materials some of the cages are empty, and that in the Cs/Sn clathrate there are vacancies in the Sn framework. The NMR results yield Knight shifts for 29Si and 39K and confirm that the Cs/Sn clathrate is not conducting. Many of the features of the NMR spectra can be understood in terms of the distributions of atom vacancies.

Neue Verbindungen Ag2HgMX4 mit Wurtzstannitstruktur / New Compounds Ag2HgMX4 with the Wurtzstannite Type Structure

1989 ◽  
Vol 44 (9) ◽  
pp. 1035-1036 ◽  
Author(s):  
H. Haeuseler ◽  
M. Himmrich
Keyword(s):  
Solid State ◽  
Type Structure ◽  
Solid State Reactions ◽  
Similar Composition ◽  
X Ray ◽  
Unknown Structure ◽  
New Compounds

Three new compounds, Ag2HgGeS4, Ag2HgSnS4, and Ag2HgSnSe4, crystallizing in the wurtzstannite type structure have been prepared by solid state reactions at 700°C and characterized by X-ray powder methods. A fourth compound of similar composition Ag2HgGeSe4, with an hitherto unknown structure crystallizes cubically with a = 10.796 A.

Crystal Structures of New Compounds Na0.5Sm4.5Ti4O15 and Na0.5Eu4.5Ti4O15

2011 ◽  
Vol 415-417 ◽  
pp. 468-471
Author(s):  
Qiao Hong Yu ◽  
Zheng Fa Li ◽  
Yong Xiang Li ◽  
Ping Zhan Si ◽  
Jiang Ying Wang ◽  
...  
Keyword(s):  
Solid State ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Diffraction Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ordinary Temperature ◽  
Europium Titanate ◽  
New Compounds

New compounds of sodium samarium titanate Na0.5Sm4.5Ti4O15and sodium europium titanate Na0.5Eu4.5Ti4O15were synthesized successfully by solid state reaction at 1300 oC and 1200 oC, respectively. The lattice parameters of Na0.5Sm4.5Ti4O15and Na0.5Eu4.5Ti4O15were determined at ordinary temperature by using X-ray powder diffraction method. Their Lattice types were determined, and their patterns were indexed. Polycrystalline X-ray diffraction data of sodium samarium titanate were listed. Differences of their crystal structures were analyzed and discussed.

Hydrogen Desorption Reactions of the Na-Mg-B-H System

2010 ◽  
Vol 72 ◽  
pp. 164-169 ◽  
Author(s):  
Daphiny Pottmaier ◽  
Sebastiano Garroni ◽  
Maria Dolors Barò ◽  
Marcello Baricco
Keyword(s):  
Solid State ◽  
Research And Development ◽  
Ball Milling ◽  
Powder Diffraction ◽  
Hydrogen Desorption ◽  
X Ray ◽  
New Compounds ◽  
Desorption Reaction

Hydrogen storage in the solid state has shown increasing research and development, and recently an approach in mixing two hydride systems together by ball milling (reactive hydride composites) has been investigated in more detail, e.g. NaBH4 plus MgH2. Thermodynamic destabilization may occur by new compounds formation during dehydrogenation, e.g. MgB2. A study of the the role of O2/H2O contamination for the reaction 2NaBH4 + MgH2 ↔ 2NaH + MgB2 + 4H2 was conducted using in-situ X-ray powder diffraction. Desorption reaction is observed to begin by a competition of MgH2 and NaBH4 decomposition due to higher reactivity promoted by ball milling processing summed to O2/H2O contamination. Oxidation of NaBH4 into NaBO2 is observed to happen in higher degree than MgH2/Mg into MgO for the Na-Mg-B-H system.

scholarly journals Single Crystal X-ray Structure Analyses of Thallides: Halide Incorporation and Mixed Alkali Sites in A8Tl11X (A = K, Rb, Cs; X = Cl, Br)

Proceedings ◽  
2018 ◽  
Vol 2 (14) ◽  
pp. 1124
Author(s):  
Stefanie Gärtner ◽  
Susanne Tiefenthaler
Keyword(s):  
Single Crystal ◽  
Alkali Metals ◽  
Data Sets ◽  
Moisture Sensitivity ◽  
Metal Compounds ◽  
X Ray ◽  
Mixed Alkali ◽  
Extra Electron ◽  
Alkali Metal Compounds ◽  
New Compounds

A8Tl11 (A = alkali metal) compounds have been known since the investigations of Corbett et al. in 1995 and still are matter of current discussions as the compound includes one extra electron referred to the charge of the Tl117− cluster. Attempts to substitute the charge by incorporation of a halide atom succeeded for the lightest homologue of the group, Cs8Ga11Cl, and powder diffraction experiments for the heavier homologues also suggested the formation of analogous compounds. However, X-ray single crystal studies on A8Tl11X to prove this substitution and to provide a deeper insight into the influence on the thallide substructure have not yet been performed, probably due to severe absorption combined with air and moisture sensitivity for this class of compounds. In our contribution we present single crystal X-ray analyses of the new compounds Cs8Tl11Cl0.8, Cs8Tl11Br0.9 and Cs5Rb3Tl11Cl0.5. It is shown that a (partial) incorporation of halide can also be indirectly determined by examination of the Tl-Tl distances for low resolved data sets, e.g., for Cs5.7K2.3Tl11Cl?. Mixed occupied sites by two different alkali metals indicate a dependence on the cesium content, the systems K/Rb–Tl–Br and K/Rb–Tl–Cl only gave rise to the formation of the higher reduced (K/Rb)8Tl11 and the less reduced by-product (K/Rb)15Tl27. We have not been able to prove the formation of halide including thallides in the absence of cesium.

New Synthesis of Solid-Solution Lead Hydroxyapatite (PbHAP) by Ceramic and Semi-Ceramic Methods

2020 ◽  
Vol 42 (3) ◽  
pp. 363-363
Author(s):  
Mohammed A B Abdul jabar and Ignatov A V Mohammed A B Abdul jabar and Ignatov A V
Keyword(s):  
Solid State ◽  
Solid State Reaction ◽  
Solid State Reaction Method ◽  
Precipitation Method ◽  
Ceramic Method ◽  
Reaction Method ◽  
X Ray ◽  
New Synthesis ◽  
Lead Hydroxyapatite ◽  
Micro Analysis

The synthesis of solid solutions lead hydroxyapatite, Pb10(PO4)6*y(OH)2, were successfully synthesized by solid-state reaction (ceramic method) (y= 0.95; 0.96; 0.97; 0.98; 0.99 and 1.00) and precipitation (semi ceramic method) (y= 0.97; 0.98; 0.99 and 1.00) methods at 800 and#186;C for 50 hours. The X-ray powder diffraction (DRON-3m diffractometer), electron microscopy scanning (SEM) and energy dispersive X-ray micro-analysis which characterized all samples. It has been established that Pb10(PO4)5.82(OH)2 and Pb10(PO4)5.88(OH)2 are the best synthesis for lead hydroxyapatite in the solid-state reaction method, and Pb10(PO4)5.88(OH)2 is the precipitation method.

scholarly journals Solid state interactions in the systems CaO(CaCO3)-Fe2O3 and CuFe2O4-CaO

2005 ◽  
Vol 41 (1) ◽  
pp. 67-77 ◽  
Author(s):  
B.S. Boyanov
Keyword(s):  
Sulfuric Acid ◽  
Solid State ◽  
Acid Solution ◽  
Diffraction Analysis ◽  
Sulfuric Acid Solution ◽  
Formation Process ◽  
X Ray Diffraction ◽  
Exchange Reactions ◽  
X Ray ◽  
Ferrite Formation

The solid state interactions in the systems CaO(CaCO3)-Fe2O3 and CuFe2O4-CaO have been studied using X-ray diffraction analysis. The influence of the temperature on the ferrite formation process has been investigated in the range of 900-1200 oC and duration up to 360 min. It has been shown that a mixture of ferrites forms at 1000 oC and interaction of 240 min. The exchange reactions in the systems CuFe2O4-CaO and Cu0.5Zn0.5Fe2O4-CaO have been studied, too. It has been established that Ca2+ ions exchange Cu2+ and Zn2 partially and the solubility of copper and zinc in a 7 % sulfuric acid solution increases 10-15 times.

Preparation and X-Ray Crystal Structures of Tetrahydrofuran-Complexed Rare Earth Chlorides — a Structurally Rich Series

1998 ◽  
Vol 51 (1) ◽  
pp. 75 ◽  
Author(s):  
Glen B. Deacon ◽  
Tiecheng Feng ◽  
Peter C. Junk ◽  
Brian W. Skelton ◽  
Alexander N. Sobolev ◽  
...  
Keyword(s):  
Oxygen Atom ◽  
Crystal Structures ◽  
Ion Pairs ◽  
Far Infrared ◽  
Prolonged Treatment ◽  
Direct Reaction ◽  
Metal Powders ◽  
Metal Chlorides ◽  
X Ray ◽  
Linear Chains

Anhydrous lanthanoid metal chlorides LnCl3(thf)n (Ln = La, Ce, Nd, Sm, n = 2; Ln = Tb, Ho, n = 2·5; Ln = Dy, Tm, n= 2·7; Ln = Gd, Yb, Lu, n = 3; Ln = Er, n = 3·5) have been prepared in excellent yield by the direct reaction of the lanthanoid metal powders with hexachloroethane in tetrahydrofuran (thf), and (Ln = Eu, n = 0·8; Ln = La, n = 1·7; Ln = Pr, n = 2; Ln = Gd, n = 2·5; Ln = Er, n = 3) in good yield except for EuCl3(thf)0·8 from bulk metal. [YbCl3(thf)2]2 was prepared by prolonged treatment of solid YbCl3(thf)3 with pentane. The X-ray crystal structures of [LnC3(thf)2] (Ln = La, Ce or Pr), [LnCl3(thf)3.5] (Ln = Gd or Er), [YbCl3(thf)3] and [LaCl3(thf)(H2O)] have been determined. For [LaCl3(thf)2], a square antiprismatic single-stranded polymer, ... La(-Cl)3(thf)3La(-Cl)3(thf)2 ..., is the first eight-coordinate LnCl3(thf)n complex. The metal is surrounded by two sets of three bridging chlorines and cis thf oxygens. [LnCl3(thf)2] (Ln = Ce, Pr) have seven-coordinate structures with doubly chloride-bridged linear chains, ... LnCl(µ-Cl)3(thf)2LnCl(µ-Cl)2(thf)2 ... where the lanthanoid atom exists in a pentagonal bipyramidal environment, the pentagonal bipyramidal plane being defined by four chloride atoms and one oxygen atom of the thf ligand, and the axial positions being occupied by a chloride and a thf oxygen atom. [LnCl3(thf)3.5] (Ln = Gd, Er) crystallize as discrete ion pairs, [LnCl2(thf)5]+ [LnCl4(thf)2]¯. The lanthanoid atom in the cation displays pentagonal bipyramidal geometry with two apical chloride atoms and five equatorial thf ligands while the anion has quasi-regular octahedral stereochemistry with trans thf ligands. [LaCl3(thf)(H2O)] displays an eight-coordinate two-dimensional polymeric array with six bridging chlorides per lanthanum atom. Far-infrared spectra have been recorded for a number of products and used as a basis for structural proposals, particularly for products with fractional thf.

HREM in solid-state chemistry and crystallography

1992 ◽  
Vol 50 (1) ◽  
pp. 104-105
Author(s):  
Lars Kihlborg ◽  
Margareta Sundberg ◽  
Gunnar Svensson
Keyword(s):  
Solid State ◽  
High Temperature Superconductors ◽  
High Resolution Electron Microscopy ◽  
Atomic Resolution ◽  
Solid State Chemistry ◽  
X Ray ◽  
Solid State Ionics ◽  
Resolution Electron ◽  
New Compounds

High-resolution electron microscopy has had a great impact on solid state chemistry. The possibility it offers of directly imaging the structure of solids has made it an unvaluable complement to conventional diffraction methods. Disorder and extended effects have become accessible to observation, superstructures, structural modulations and microphases can be identified and particles down to nanometer size can be studied. Combined with electron diffraction and x-ray microanalysis it is a powerful tool for phase analysis, giving guidance to synthesis of new compounds. Under certain conditions even chemical reactions can be studied in situ at atomic resolution. Numerous examples in be found in the fields of high-temperature superconductors, zeolites, ferroelectrics and solid state ionics.

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