scholarly journals Monitoring of FES2 reactions using high-temperature XRD coupled with gas chromatography

2019 ◽  
Vol 34 (2) ◽  
pp. 90-96
Author(s):  
K.-A. M. Stirrup ◽  
M. A. Rodriguez ◽  
E. N. Coker ◽  
J. J. M. Griego ◽  
T. M. Anderson
Keyword(s):  
Gas Chromatography ◽  
High Temperature ◽  
Simultaneous Thermal Analysis ◽  
Gas Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Iron Disulfide ◽  
Thermal Batteries ◽  
High Temperature Xrd

High-temperature X-ray diffraction with concurrent gas chromatography (GC) was employed in the study of iron disulfide (FeS2) cathode pellets disassembled from thermal batteries. When FeS2 cathode materials were analyzed in an air environment, reaction of the KCl and LiCl salt phases led to the formation of Li2(SO4) and KFe2S3 phases beginning at ~230 °C. These phases subsequently reacted to generate various forms of potassium iron sulfates in the 280–500 °C range, with the final products resulting in a β-Fe2O3 phase and K2(SO4). Independent simultaneous thermal analysis coupled with mass spectroscopy (MS) augmented the diffraction results and supported the overall picture of FeS2 decomposition. Both gas analysis measurements (i.e. GC and MS) from the independent experiments confirmed the formation of SO2 off-gas species during the breakdown of the FeS2. In contrast, characterization of the same cathode material under inert conditions showed the persistence of the initial FeS2 phase throughout the entire temperature range of analysis.

scholarly journals Monitoring of CoS2 reactions using high-temperature XRD coupled with gas chromatography (GC)

2016 ◽  
Vol 31 (2) ◽  
pp. 90-96 ◽  
Author(s):  
Mark A. Rodriguez ◽  
Eric N. Coker ◽  
James J. M. Griego ◽  
Curtis D. Mowry ◽  
Adam S. Pimentel ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
High Temperature ◽  
Gas Analysis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Thermal Batteries ◽  
Cobalt Disulfide ◽  
High Temperature Xrd ◽  
Salt Phase

High-temperature X-ray diffraction with concurrent gas chromatography (GC) was used to study cobalt disulfide cathode pellets disassembled from thermal batteries. When CoS2 cathode materials were analyzed in an air environment, oxidation of the K(Br, Cl) salt phase in the cathode led to the formation of K2SO4 that subsequently reacted with the pyrite-type CoS2 phase leading to cathode decomposition between ~260 and 450 °C. Independent thermal analysis experiments, i.e. simultaneous thermogravimetric analysis/differential scanning calorimetry/mass spectrometry (MS), augmented the diffraction results and support the overall picture of CoS2 decomposition. Both gas analysis measurements (i.e. GC and MS) from the independent experiments confirmed the formation of SO2 off-gas species during breakdown of the CoS2. In contrast, characterization of the same cathode material under inert conditions showed the presence of CoS2 throughout the entire temperature range of analysis.

Rhombohedral-cubic phase transition characterization of (Pb,Ge)Te using high-temperature XRD

2008 ◽  
Vol 23 (2) ◽  
pp. 137-140 ◽  
Author(s):  
J. Sariel ◽  
I. Dahan ◽  
Y. Gelbstein
Keyword(s):  
High Temperature ◽  
Cylindrical Specimen ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
Continuous Transformation ◽  
X Ray ◽  
High Temperature Xrd ◽  
Powder Samples ◽  
Powder Metallurgy Approach

Rhombohedral-cubic transformation in Bi2Te3 doped-Pb1−xGexTe alloys is presented. Samples of Bi2Te3 doped Pb1−xGexTe were prepared by powder metallurgy approach. These powder samples were examined by high-temperature X-ray diffraction (XRD) and scanning electron microscopy/energy dispersive spectroscopy. A bulk (pressed powder) cylindrical specimen was used for dilatometery characterizations. According to the XRD examinations it seems that upon increasing the temperatures a continuous transformation occurs from the rhombohedral to the cubic phase, accompanied by the formation of a small amount of the phase Ge0.74Pb3.26Te4.

scholarly journals High-pressure synthesis and characterization of the non-centrosymmetric scandium borate ScB6O9(OH)3

2020 ◽  
Vol 75 (6-7) ◽  
pp. 597-603
Author(s):  
Birgit Fuchs ◽  
Hubert Huppertz
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Pressure High Temperature ◽  
Structure Solution ◽  
Temperature Experiment ◽  
Pressure Synthesis

AbstractThe non-centrosymmetric scandium borate ScB6O9(OH)3 was obtained through a high-pressure/high-temperature experiment at 6 GPa and 1473 K. Single-crystal X-ray diffraction revealed that the structure is isotypic to InB6O9(OH)3 containing borate triple layers separated by scandium layers. The compound crystallizes in the space group Fdd2 with the lattice parameters a = 38.935(4), b = 4.4136(4), and c = 7.6342(6) Å. Powder X-ray diffraction and vibrational spectroscopy were used to further characterize the compound and verify the proposed structure solution.

High pressure growth and characterization of SrCrO3 single crystal

2015 ◽  
Vol 29 (25n26) ◽  
pp. 1542025 ◽  
Author(s):  
L. P. Cao ◽  
L. Q. Pan ◽  
W. M. Li ◽  
X. C. Wang ◽  
Q. Q. Liu ◽  
...  
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Single Crystal ◽  
Perovskite Structure ◽  
Resistivity Measurement ◽  
X Ray Diffraction ◽  
X Ray ◽  
Measurement Results

Single crystal [Formula: see text] was prepared under high pressure and high temperature. Single crystal X-ray diffraction (XRD) result shows a cubic perovskite structure. The magnetic and resistivity measurement results indicate that [Formula: see text] is a paramagnetic semiconductor.

scholarly journals In situ characterization of the effects of Nb and Sn on the anatase–rutile transition in TiO2 nanotubes using high-temperature X-ray diffraction

2014 ◽  
Vol 307 ◽  
pp. 372-381 ◽  
Author(s):  
Nathália C. Verissimo ◽  
Alessandra Cremasco ◽  
Christiane A. Rodrigues ◽  
Rodnei Bertazzoli ◽  
Rubens Caram
Keyword(s):  
High Temperature ◽  
Tio2 Nanotubes ◽  
X Ray Diffraction ◽  
In Situ Characterization ◽  
X Ray

Synthesis and structural characterization of Li3Y(BO3)2

2017 ◽  
Vol 72 (2) ◽  
pp. 153-158 ◽  
Author(s):  
Sebastian Bräuchle ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Temperature ◽  
Solid State ◽  
Boric Acid ◽  
Structural Characterization ◽  
Diffraction Data ◽  
Lithium Carbonate ◽  
X Ray Diffraction ◽  
X Ray

AbstractLi3Y(BO3)2 was prepared by high-temperature solid state synthesis at 900°C in a platinum crucible from lithium carbonate, boric acid, and yttrium(III) oxide. The compound crystallizes monoclinically in the space group P21/c (no. 14) (Z=4) isotypically to Li3Gd(BO3)2. The structure was refined from single-crystal X-ray diffraction data: a=8.616(3), b=6.416(3), c=10.014(2) Å, β=116.6(2)°, V=494.9(3) Å3, R1=0.0211, and wR2=0.0378 for all data. The crystal structure of Li3Y(BO3)2 consists of [Y2O14] dinuclear units, which are interconnected to each other by planar B(1)O3 groups and LiO4 tetrahedra via common edges and corners along the a axis.

Preparation and characterization of a novel solid solution of aluminum in tungsten carbide by mechanically activated high-temperature reaction

2006 ◽  
Vol 21 (7) ◽  
pp. 1700-1703 ◽  
Author(s):  
Junmin Yan ◽  
Xianfeng Ma ◽  
Wei Zhao ◽  
Huaguo Tang ◽  
Changjun Zhu ◽  
...  
Keyword(s):  
Solid Solution ◽  
High Temperature ◽  
Substitutional Solid Solution ◽  
Phase Identification ◽  
Temperature Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
High Temperature Reaction

In this work, a novel substitutional solid solution (W0.8Al0.2)C was synthesized by mechanically activated high-temperature reaction. X-ray diffraction was used for phase identification during the whole reaction process. Environment scanning electronic microscopy–field emission gun and energy dispersive x-ray were used to investigate the microstructure and the quantitative material composition of the specimen. (W0.8Al0.2)C was found to crystallize in the WC-type, and the cell parameters were a = 2.907(1) Å and c = 2.837(1) Å. The hardness of (W0.8Al0.2)C was tested to be 19.3 ± 1 GPa, and the density was 13.19 ± 0.05 g cm−3.

Synthesis and characterization of robust three-dimensional chiral metal sulfates

RSC Advances ◽  
2014 ◽  
Vol 4 (92) ◽  
pp. 50435-50442 ◽  
Author(s):  
J. N. Behera ◽  
Joydeep Bhattacharjee ◽  
Satoshi Horike ◽  
Subba R. Marri ◽  
Prem P. Dahiya
Keyword(s):  
Thermal Decomposition ◽  
High Temperature ◽  
First Principles ◽  
Three Dimensional ◽  
Ammonium Ion ◽  
Synthesis And Characterization ◽  
First Principles Calculations ◽  
X Ray Diffraction ◽  
X Ray

Chiral three-dimensional Mg(ii) and Mn(ii) sulfates have been synthesized, well characterized and studied from first-principles calculations. High temperature X-ray diffraction, thermogravimetric analysis and DFT calculations reveal that the structures of both the compounds remain intact even after the thermal decomposition of the ammonium ion.

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