scholarly journals Barium titanate via thermal decomposition of Ba,Ti-precursor complexes: The nature of the intermediate phases

2019 ◽  
Author(s):  
Roberto Köferstein
Keyword(s):  
Thermal Decomposition ◽  
Organic Ligands ◽  
X Ray Diffraction ◽  
X Ray ◽  
Barium Titanates ◽  
Intermediate Phases ◽  
Source Preparation ◽  
Low Crystalline ◽  
Electron Energy Loss ◽  
High Temperature Modification

The thermal decomposition of Ba,Ti-precursor complexes, containing organic ligands and suitable for the single-source preparation of nanocrystalline BaTiO3, leads firstly to the segregation of specific Ba-rich and Ti-rich phases. Quantitative electron energy loss spectroscopy and powder X-ray diffraction data indicated that the (i) Ba-rich phase is a BaO-stabilised variant of the calcite-type high-temperature modification of BaCO3 and (ii) Ti-rich phases are represented by low crystalline barium titanates with the general Ba:Ti ratio close to 1:4. The subsequent solid state reaction between these phases results then in the formation of BaTiO3.

Electron Microscopy/Diffraction Study of the Ternary Mn-Er-S System

1990 ◽  
Vol 48 (1) ◽  
pp. 76-77
Author(s):  
A. R. Landa Canovas ◽  
L.C. Otero Diaz ◽  
T. White ◽  
B.G. Hyde
Keyword(s):  
Electron Microscopy ◽  
Gas Flow ◽  
Graphite Crucible ◽  
Nominal Composition ◽  
X Ray Diffraction ◽  
Alumina Crucible ◽  
X Ray ◽  
Intermediate Phases ◽  
Twin Band ◽  
Ar Gas

X-Ray diffraction revealed two intermediate phases in the system MnS+Er2S3,:MnEr2S4= MnS.Er2S3, and MnEr4S7= MnS.2Er2S3. Their structures may be described as NaCl type, chemically twinned at the unit cell level, and isostructural with CaTi2O4, and Y5S7 respectively; i.e. {l13} NaCl twin band widths are (4,4) and (4,3).The present study was to search for structurally-related (twinned B.) structures and or possible disorder, using the more sensitive and appropiate technigue of electron microscopy/diffraction.A sample with nominal composition MnEr2S4 was made by heating Mn3O4 and Er2O3 in a graphite crucible and a 5% H2S in Ar gas flow at 1500°C for 4 hours. A small amount of this material was thenannealed, in an alumina crucible, contained in sealed evacuated silica tube, for 24 days at 1100°C. Both samples were studied by X-ray powder diffraction, and in JEOL 2000 FX and 4000 EX microscopes.

New Coordination Compounds of Fe(III) with Organic Ligands

2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Mihaela Flondor ◽  
Ioan Rosca ◽  
Doina Sibiescu ◽  
Mihaela-Aurelia Vizitiu ◽  
Daniel-Mircea Sutiman ◽  
...  
Keyword(s):  
Chemical Analysis ◽  
Complex Compounds ◽  
Organic Ligands ◽  
X Ray Diffraction ◽  
X Ray ◽  
Elemental Chemical Analysis ◽  
Structural Formulae ◽  
Paramagnetic Properties

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.

scholarly journals A Facile Method to Construct MXene/CuO Nanocomposite with Enhanced Catalytic Activity of CuO on Thermal Decomposition of Ammonium Perchlorate

Materials ◽  
2018 ◽  
Vol 11 (12) ◽  
pp. 2457 ◽  
Author(s):  
Haifeng Zhao ◽  
Jing Lv ◽  
Junshan Sang ◽  
Li Zhu ◽  
Peng Zheng ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Catalytic Activity ◽  
Ammonium Perchlorate ◽  
Photoelectron Spectra ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Improved Performance ◽  
Calcination Method

In this work, a mixing-calcination method was developed to facilely construct MXene/CuO nanocomposite. CuO and MXene were first dispersed in ethanol with sufficient mixing. After solvent evaporation, the dried mixture was calcinated under argon to produce a MXene/CuO nanocomposite. As characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), and X-ray photoelectron spectra (XPS), CuO nanoparticles (60–100 nm) were uniformly distributed on the surface and edge of MXene nanosheets. Furthermore, as evaluated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the high-temperature decomposition (HTD) temperature decrease of ammonium perchlorate (AP) upon addition of 1 wt% CuO (hybridized with 1 wt% MXene) was comparable with that of 2 wt% CuO alone, suggesting an enhanced catalytic activity of CuO on thermal decomposition of AP upon hybridization with MXene nanosheets. This strategy could be further applied to construct other MXene/transition metal oxide (MXene/TMO) composites with improved performance for various applications.

Synthesis, structure and selective luminescence sensing for iron(III) ions of a three-dimensional zinc(II) (4,6)-connected coordination network

2019 ◽  
Vol 75 (2) ◽  
pp. 141-149 ◽  
Author(s):  
Feng Su ◽  
Cheng-Yong Zhou ◽  
Lin-Tao Wu ◽  
Xi Wu ◽  
Chun Han ◽  
...  
Keyword(s):  
Three Dimensional ◽  
Electronic Configuration ◽  
Organic Ligands ◽  
Tetracarboxylic Acid ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Groups ◽  
Dimensional Network ◽  
Solvent Stability ◽  
Solvothermal Conditions

Coordination polymers constructed from conjugated organic ligands and metal ions with a d 10 electronic configuration exhibit intriguing properties for chemical sensing and photochemistry. A ZnII-based coordination polymer, namely poly[aqua(μ6-biphenyl-3,3′,5,5′-tetracarboxylato)(μ2-4,4′-bipyridine)dizinc(II)], [Zn2(C16H6O8)(C10H8N2)(H2O)2] n or [Zn2(m,m-bpta)(4,4′-bipy)(H2O)2] n , was synthesized from a mixture of biphenyl-3,3′,5,5′-tetracarboxylic acid [H4(m,m-bpta)], 4,4′-bipyridine (4,4′-bipy) and Zn(NO3)2·6H2O under solvothermal conditions. The title complex has been structurally characterized by IR spectroscopy, elemental analysis, single-crystal X-ray diffraction and powder X-ray diffraction analysis, and features a μ6-coordination mode. The ZnII ions adopt square-pyramidal geometries and are bridged by two syn–syn carboxylate groups to form [Zn2(COO)2] secondary buildding units (SBUs). The SBUs are crosslinked by (m,m-bpta)4− ligands to produce a two-dimensional grid-like layer that exhibits a stair-like structure along the a axis. Adjacent layers are linked by 4,4′-bipy ligands to form a three-dimensional network with a {44.610.8}{44.62} topology. In the solid state, the complex displays a strong photoluminescence and an excellent solvent stability. In addition, the luminescence sensing results indicate a highly selective and sensitive sensing for Fe3+ ions.

Beobachtungen von Stapelfehlordnungen bei der Oxydation der zweiten zur ersten Stufe des Graphithydrogensulfats / Observation of stacking disorder during the oxidation of second stage to first stage graphite hydrogensulfate

1984 ◽  
Vol 39 (8) ◽  
pp. 768-777 ◽  
Author(s):  
Ko Young Shin ◽  
Hanns-Peter Boehm
Keyword(s):  
Interlayer Spacing ◽  
X Ray Diffraction ◽  
X Ray ◽  
First Order ◽  
Second Stage ◽  
Intermediate Phases ◽  
Degree Of Oxidation ◽  
Stage 1 ◽  
Kinetics Of ◽  
Stacking Disorder

Graphite has been oxidized to graphite hydrogensulfate with (NH4)2S2Og in concentrated H2SO4. The stage 2 compound formed very rapidly, but further oxidation to stage 1 could be followed conveniently. X-ray diffraction of the intermediate phases showed nonintegral (00l)-reflections indicative of partial interstratification disorder. The interlayer spacing of the stage 1 compound increased with continued oxidation. The degree of oxidation as function of oxidation time has been determined from the position of the minima in the reflectance spectra. The density of the compounds and the ratio of acid molecules to anions in the intercalated layers has been estimated using these data and those of buoyancy measurements. There is a minimum in packing density early in the formation of the first stage. The kinetics of intercalation seems to be first order with respect to the free interlayer spaces.

Structural Characterization and Thermal Decomposition of Lime Binders Allow Accurate Radiocarbon Age Determinations of Aerial Lime Plaster

Radiocarbon ◽  
2020 ◽  
Vol 62 (3) ◽  
pp. 633-655 ◽  
Author(s):  
Michael B Toffolo ◽  
Lior Regev ◽  
Eugenia Mintz ◽  
Ifat Kaplan-Ashiri ◽  
Francesco Berna ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Isotopic Signature ◽  
Secondary Phases ◽  
X Ray Diffraction ◽  
Lime Mortar ◽  
X Ray ◽  
Radiocarbon Age ◽  
Carbon Recovery ◽  
Lime Plaster ◽  
Thin Section Petrography

ABSTRACTRadiocarbon (14C) dating of anthropogenic carbonates (CaCO3) such as ash, lime plaster and lime mortar, has proven a difficult task due to the occurrence of a number of contaminants embedded within the CaCO3 pyrogenic binder. These include 14C-free geologic components and/or secondary phases bearing an unknown amount of 14C, and thus the alteration of the original pyrogenic isotopic signature of the material results in major age offsets when carbon recovery is performed through acid hydrolysis. Here we present a characterization/quantification approach to anthropogenic carbonates that includes Fourier transform infrared spectroscopy (FTIR), X-ray diffraction, thin section petrography, thermogravimetric analysis and scanning electron microscopy coupled with high-resolution cathodoluminescence, with which we identified the pyrogenic CaCO3 fraction in an aerial lime plaster and two hydraulic mortars. The preserved pyrogenic component was then isolated by density separation and its purity checked again using FTIR. Carbon was recovered through thermal decomposition in vacuum. The resulting 14C age matches the expected age of the lime plaster, whereas hydraulic mortars are slightly offset due to the carbonation of calcium hydroxide lumps. This approach highlights the importance of a dedicated characterization strategy prior to dating and may be applied to aerial lime plasters to obtain accurate ages.

scholarly journals Ceramic-Reinforced γ-TiAl-Based Composites: Synthesis, Structure, and Properties

Materials ◽  
2019 ◽  
Vol 12 (4) ◽  
pp. 629 ◽  
Author(s):  
Daria Lazurenko ◽  
Andreas Stark ◽  
Maksim Esikov ◽  
Jonathan Paul ◽  
Ivan Bataev ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Compressive Strength ◽  
Creep Behavior ◽  
Longitudinal Direction ◽  
Max Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intermediate Phases ◽  
Plasma Sintering ◽  
The Matrix

In this study, new multilayer TiAl-based composites were developed and characterized. The materials were produced by spark plasma sintering (SPS) of elemental Ti and Al foils and ceramic particles (TiB2 and TiC) at 1250 °C. The matrix of the composites consisted of α2-TiAl and γ-TiAl lamellas and reinforcing ceramic layers. Formation of the α2 + γ structure, which occurred via a number of solid–liquid and solid–solid reactions and intermediate phases, was characterized by in situ synchrotron X-ray diffraction analysis. The combination of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy dispersive X-ray (EDX) analysis revealed that an interaction of TiC with Ti and Al led to the formation of a Ti2AlC Mn+1AXn (MAX) phase. No chemical reactions between TiB2 and the matrix elements were observed. The microhardness, compressive strength, and creep behavior of the composites were measured to estimate their mechanical properties. The orientation of the layers with respect to the direction of the load affected the compressive strength and creep behavior of TiC-reinforced composites. The compressive strength of samples loaded in the perpendicular direction to layers was higher; however, the creep resistance was better for composites loaded in the longitudinal direction. The microhardness of the composites correlated with the microhardness of reinforcing components.

Structural and ferromagnetic properties of Cu-doped GaN

2007 ◽  
Vol 22 (5) ◽  
pp. 1396-1405 ◽  
Author(s):  
B. Seipel ◽  
R. Erni ◽  
Amita Gupta ◽  
C. Li ◽  
F.J. Owens ◽  
...  
Keyword(s):  
Quantum Interference ◽  
Electron Gun ◽  
Superconducting Quantum Interference Device ◽  
X Ray Diffraction ◽  
Calcination Process ◽  
X Ray ◽  
Lattice Constants ◽  
Gan Crystal ◽  
Electron Energy Loss ◽  
Atomic And Electronic Structure

The wurtzite polymorph of GaN was calcined with CuO in flowing nitrogen. As a result of this processing, both superconducting quantum interference device magnetometry and ferromagnetic resonance studies showed ferromagnetism in these samples at room temperature. These magnetic results are qualitatively consistent with very recent first-principle calculations [Wu et al., Appl. Phys. Lett.89, 062505 (2006)] that predict ferromagnetism in Cu-doped GaN. We focus in this paper on analyzing changes in the GaN atomic and electronic structure due to calcination with CuO using multiple analytical methods. Quantitative powder x-ray diffraction (XRD) showed changes in the lattice constants of the GaN due to the incorporation of copper (and possibly oxygen). Energy-dispersive x-ray spectroscopy proved the incorporation of copper into the GaN crystal structure. Electron-gun monochromated electron energy loss spectroscopy showed CuO calcinations-induced GaN band gap changes and indicated changes in the atomic arrangements due to the calcination process. The fine structure of the N K-edge showed differences in the peak ratios with respect to higher nominal CuO contents, corresponding to an increase in the c-lattice constant as confirmed by XRD.

Accelerated Thermal Decomposition of Graphene Oxide Films in Air via in Situ X-ray Diffraction Analysis

2016 ◽  
Vol 120 (27) ◽  
pp. 14984-14990 ◽  
Author(s):  
Qin Pan ◽  
Ching-Chang Chung ◽  
Nanfei He ◽  
Jacob L. Jones ◽  
Wei Gao
Keyword(s):  
Thermal Decomposition ◽  
Graphene Oxide ◽  
Diffraction Analysis ◽  
Oxide Films ◽  
X Ray Diffraction ◽  
X Ray
Sign in / Sign up

Export Citation Format

Share Document