ChemInform Abstract: In situ Neutron Powder Diffraction on Intermediate Hydrides of MgPd3in a Novel Sapphire Gas Pressure Cell.

ChemInform ◽  
2010 ◽  
Vol 41 (9) ◽  
Author(s):  
Holger Kohlmann ◽  
Nadine Kurtzemann ◽  
Richard Weihrich ◽  
Thomas Hansen
Keyword(s):  
Powder Diffraction ◽  
Neutron Powder Diffraction ◽  
Gas Pressure ◽  
Pressure Cell

scholarly journals Design and use of a sapphire single-crystal gas-pressure cell for in situ neutron powder diffraction

2021 ◽  
Vol 54 (3) ◽  
Author(s):  
Raphael Finger ◽  
Nadine Kurtzemann ◽  
Thomas C. Hansen ◽  
Holger Kohlmann
Keyword(s):  
Single Crystal ◽  
Powder Diffraction ◽  
Neutron Powder Diffraction ◽  
Gas Pressure ◽  
Sample Holder ◽  
Pressure Cell ◽  
Hydrogen Deuterium ◽  
Sapphire Single Crystal ◽  
Deuterium Gas

A sapphire single-crystal gas-pressure cell without external support allowing unobstructed optical access by neutrons has been developed and optimized for elastic in situ neutron powder diffraction using hydrogen (deuterium) gas at the high-intensity two-axis diffractometer D20 at the Institut Laue-Langevin (Grenoble, France). Given a proper orientation of the single-crystal sample holder with respect to the detector, parasitic reflections from the sample holder can be avoided and the background can be kept low. Hydrogen (deuterium) gas pressures of up to 16.0 MPa at 298 K and 8.0 MPa at 655 K were tested successfully for a wall thickness of 3 mm. Heating was achieved by a two-sided laser heating system. The typical time resolution of in situ investigations of the reaction pathway of hydrogen (deuterium) uptake or release is on the order of 1 min. Detailed descriptions of all parts of the sapphire single-crystal gas-pressure cell are given, including materials information, technical drawings and instructions for use.

Metal hydride formation in palladium and palladium rich intermetallic compounds studied by in situ neutron diffraction

2013 ◽  
Vol 28 (S2) ◽  
pp. S242-S255 ◽  
Author(s):  
H. Kohlmann ◽  
N. Kurtzemann ◽  
T. C. Hansen
Keyword(s):  
Intermetallic Compounds ◽  
Powder Diffraction ◽  
Neutron Powder Diffraction ◽  
Gas Pressure ◽  
Type Structure ◽  
Sapphire Crystal ◽  
Direct Reaction ◽  
Β Phase ◽  
In Situ Neutron Diffraction

In order to investigate the hydrogenation of intermetallic compounds, a gas pressure cell for in situ neutron powder diffraction based on a sapphire crystal tube was constructed. By proper orientation of the single crystal Bragg peaks of the container material can be avoided, resulting in a very low diffraction background. Using a laser heating and gas pressure controller, the hydrogenation (deuteration) of palladium and palladium rich intermetallics was studied in real time up to 8 MPa gas pressure and 700 K. Crystal structure parameters of palladium deuterides could be obtained under various deuterium gas pressures, corresponding to compositional ranges of 0.04≤x≤0.11 for the α-phase and 0.52≤x≤0.72 for the β-phase at 446 K. In situ neutron powder diffraction of the deuteration of a thallium lead palladium intermetallic Tl1-xPbxPd3 shows two superstructures of the cubic closest packing (ccp) to transform independently into a AuCu3 type structure. This proves a direct reaction to the deuterium filled AuCu3 type structure instead of a reaction cascade involving different ccp superstructures and thus gives new insights into the reaction pathways of palladium rich intermetallic compounds.

In Situ Neutron Powder Diffraction Study of Ti3SiC2 Synthesis

2004 ◽  
Vol 84 (10) ◽  
pp. 2281-2288 ◽  
Author(s):  
Erdong Wu ◽  
Erich H. Kisi ◽  
Shane J. Kennedy ◽  
Andrew J. Studer
Keyword(s):  
Diffraction Study ◽  
Powder Diffraction ◽  
Neutron Powder Diffraction

Oxygen Ordered Phases in LaxSr1−xMnOy(0 ≤x≤ 0.2, 2.5 ≤ y ≤ 3): An In situ Neutron Powder Diffraction Study

2008 ◽  
Vol 20 (4) ◽  
pp. 1636-1645 ◽  
Author(s):  
Leopoldo Suescun ◽  
Bogdan Dabrowski ◽  
James Mais ◽  
Steven Remsen ◽  
James W. Richardson ◽  
...  
Keyword(s):  
Diffraction Study ◽  
Powder Diffraction ◽  
Neutron Powder Diffraction ◽  
Ordered Phases

Mn-Mg disordering in cummingtonite: a high-temperature neutron powder diffraction study

2000 ◽  
Vol 64 (2) ◽  
pp. 255-266 ◽  
Author(s):  
J. J. Reece ◽  
S. A. T. Redfern ◽  
M. D. Welch ◽  
C. M. B. Henderson
Keyword(s):  
Crystal Structure ◽  
Phase Transition ◽  
New York ◽  
High Temperature ◽  
Powder Diffraction ◽  
Elevated Temperatures ◽  
Neutron Powder Diffraction ◽  
Site Preference ◽  
A Site

AbstractThe crystal structure of a manganoan cummingtonite, composition [M4](Na0.13Ca0.41Mg0.46Mn1.00) [M1,2,3](Mg4.87Mn0.13)(Si8O22)(OH)2, (Z = 2), a = 9.5539(2) Å, b = 18.0293(3) Å, c = 5.2999(1) Å, β = 102.614(2)° from Talcville, New York, has been refined at high temperature using in situ neutron powder diffraction. The P21/m to C2/m phase transition, observed as spontaneous strains +ε1 = −ε2, occurs at ˜107°C. Long-range disordering between Mg2+ and Mn2+ on the M(4) and M(2) sites occurs above 550°C. Mn2+ occupies the M(4) and M(2) sites preferring M(4) with a site-preference energy of 24.6±1.5 kJ mol−1. Disordering induces an increase in XMnM2 and decrease in XMnM4 at elevated temperatures. Upon cooling, the ordered states of cation occupancy are ‘frozen in’ and strains in lattice parameters are maintained, suggesting that re-equilibration during cooling has not taken place.

Performance of Cu-coated vanadium cans forin situneutron powder diffraction experiments on hydrogen storage materials

2012 ◽  
Vol 45 (5) ◽  
pp. 902-905 ◽  
Author(s):  
Roxana Flacau ◽  
Jim Bolduc ◽  
Thomas Bibienne ◽  
Jacques Huot ◽  
Helmut Fritzsche
Keyword(s):  
Hydrogen Storage ◽  
High Temperatures ◽  
Powder Diffraction ◽  
Neutron Powder Diffraction ◽  
Simple Design ◽  
Hydrogen Storage Materials ◽  
High Quality ◽  
Handling System ◽  
Storage Materials

In situneutron powder diffraction (NPD) measurements of hydrogenation processes taking place at high temperatures pose difficulties related to the choice of sample can material. This article describes a simple design for a copper-coated vanadium can and its connection to the gas-handling system, tested up to 523 K. High-quality NPD patterns of TiV1.2Mn0.8body-centred cubic alloy, as-cast and partially hydrogenated, were collected at 373 K and deuterium pressures up to 2 bar (200 kPa).

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