scholarly journals Validation of a Sapphire Gas-Pressure Cell for Real-Time In Situ Neutron Diffraction Studies of Hydrogenation Reactions

2021 ◽  
Vol 5 (3) ◽  
pp. 22
Author(s):  
Raphael Finger ◽  
Thomas C. Hansen ◽  
Holger Kohlmann
Keyword(s):  
Neutron Diffraction ◽  
Single Crystal ◽  
Real Time ◽  
Hydrogen Pressure ◽  
Gas Pressure ◽  
Single Crystal Sample ◽  
Sample Holder ◽  
Pressure Cell ◽  
Hydrogenation Reactions

A gas-pressure cell, based on a leuco-sapphire single-crystal, serving as a pressure vessel and sample holder, is presented for real time in situ studies of solid-gas hydrogenation reactions. A stainless steel corpus, coated with neutron absorbing varnish, allows alignment for the single-crystal sample holder for minimizing contributions to the diffraction pattern. Openings in the corpus enable neutron scattering as well as contactless temperature surveillance and laser heating. The gas-pressure cell is validated via the deuteration of palladium powder, giving reliable neutron diffraction data at the high-intensity diffractometer D20 at the Institut Laue-Langevin (ILL), Grenoble, France. It was tested up to 15.0 MPa of hydrogen pressure at room temperature, 718 K at ambient pressure and 584 K at 9.5 MPa of hydrogen pressure.

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.

scholarly journals A double-walled sapphire single-crystal gas-pressure cell (type III) for in situ neutron diffraction

2022 ◽  
Vol 55 (1) ◽  
Author(s):  
Raphael Finger ◽  
Thomas C. Hansen ◽  
Holger Kohlmann
Keyword(s):  
Neutron Diffraction ◽  
Single Crystal ◽  
Ambient Pressure ◽  
Functional Materials ◽  
Gas Pressure ◽  
Elastic Neutron ◽  
Type Iii ◽  
Pressure Cell ◽  
Sapphire Single Crystal

In situ neutron diffraction is an important characterization technique for the investigation of many functional materials, e.g. for hydrogen uptake and release in hydrogen storage materials. A new sapphire single-crystal gas-pressure cell for elastic neutron scattering has been developed and evaluated; it allows conditions of 298 K and 9.5 MPa hydrogen pressure and 1110 K at ambient pressure. The pressure vessel consists of a sapphire single-crystal tube of 35 mm radius and a sapphire single-crystal crucible as sample holder. Heating is realized by two 100 W diode lasers. It is optimized for the D20 diffractometer, ILL, Grenoble, France, and requires the use of a radial oscillating collimator. Its advantages over earlier sapphire single-crystal gas-pressure cells are higher maximum temperatures and lower background at low and high diffraction angles. The deuterium uptake in palladium was followed in situ for validation, proving the potential of the type-III gas-pressure cell for in situ neutron diffraction on solid–gas reactions.

Real-Time In Situ Neutron Diffraction Investigation of Phase-Specific Load Sharing in a Cold-Rolled TRIP Sheet Steel

JOM ◽  
2018 ◽  
Vol 70 (8) ◽  
pp. 1576-1586 ◽  
Author(s):  
Dunji Yu ◽  
Lu Huang ◽  
Yan Chen ◽  
Piyamanee Komolwit ◽  
Ke An
Keyword(s):  
Neutron Diffraction ◽  
Real Time ◽  
Sheet Steel ◽  
Load Sharing ◽  
Specific Load ◽  
Cold Rolled ◽  
In Situ Neutron Diffraction

scholarly journals Tracing Phase Transformation and Lattice Evolution in a TRIP Sheet Steel under High-Temperature Annealing by Real-Time In Situ Neutron Diffraction

Crystals ◽  
2018 ◽  
Vol 8 (9) ◽  
pp. 360 ◽  
Author(s):  
Dunji Yu ◽  
Yan Chen ◽  
Lu Huang ◽  
Ke An
Keyword(s):  
Phase Transformation ◽  
High Temperature ◽  
Neutron Diffraction ◽  
Real Time ◽  
Retained Austenite ◽  
Sheet Steel ◽  
Carbon Diffusion ◽  
Structure Evolution ◽  
In Situ Neutron Diffraction

Real-time in situ neutron diffraction was used to characterize the crystal structure evolution in a transformation-induced plasticity (TRIP) sheet steel during annealing up to 1000 °C and then cooling to 60 °C. Based on the results of full-pattern Rietveld refinement, critical temperature regions were determined in which the transformations of retained austenite to ferrite and ferrite to high-temperature austenite during heating and the transformation of austenite to ferrite during cooling occurred, respectively. The phase-specific lattice variation with temperature was further analyzed to comprehensively understand the role of carbon diffusion in accordance with phase transformation, which also shed light on the determination of internal stress in retained austenite. These results prove the technique of real-time in situ neutron diffraction as a powerful tool for heat treatment design of novel metallic materials.

Quasi-Steady State Principle and In Situ Real-Time Investigation of Transient Strains in 6061-T6 Al Alloy Using Neutron Diffraction

2007 ◽  
Vol 345-346 ◽  
pp. 797-800 ◽  
Author(s):  
W. Woo ◽  
Zhi Li Feng ◽  
X.L. Wang ◽  
Donald W. Brown ◽  
Bjørn Clausen ◽  
...  
Keyword(s):  
Steady State ◽  
Neutron Diffraction ◽  
Real Time ◽  
Al Alloy ◽  
Quasi Steady State

Kinetics Study of Hydrogen Discharge from A Lani4.5AL0.5Dy Electrode by in Situ Real Time Neutron Diffraction

1992 ◽  
Vol 293 ◽  
Author(s):  
Christiane Poinsignon ◽  
Nicole Dalphrase ◽  
Michel Latroche ◽  
Jean Pannetier ◽  
Annick Percheron
Keyword(s):  
Neutron Diffraction ◽  
Real Time ◽  
Potential Range ◽  
Linear Potential ◽  
Discharge Process ◽  
Cell Parameters ◽  
Β Phase ◽  
Α Phase ◽  
Full Capacity

AbstractElectrochemical studies performed by linear potential scan voltamperometry on the monosubstituted intermetallic hydrides LaNi4.5M0.5, with M=AI, Mn or Co, confirm previous observations [ 14, 16, 20] of the influence of the nickel substitute on the rate of hydrogen insertion/desinsertion in solid gaz : the rate of discharge is faster for the Co and Mn substituted hydrides than for the Al one : during a controled discharge process by potential step of 20mV during 10 hours, hydrogen full capacity is desinserted over a potential range of 200mV in 80 hours for LaNi4.5AI0.5, over 130mV in 40 hours for LaNi4.5Mn0.5 and over 50mV in 30 hours for LaNi4.5Co0.5Coupled techniques of real time neutron diffraction and linear potential scan voltammetry applied to the in situ study of the charge/discharge of a LaNi4.5A10.5Dx electrode in a KOD 7N electrolyte gives account for the respective variation of the cell parameters of the α and β phases[ 11] and provides access to the hydogen desinsertion kinetics from both phases. The decrease rate of the unit cell volume of the α phase is found to be 4.8 10−3 A3/hour whereas that of the β phase is 61 10−3 A3/hour. At the end of the discharge process occurence of isolated 13ph ase domains is attributed to the faster rate of hydrogen desinsertion in the β phase than in the (β phase, which is in all likelihood at the origin of the loss of capacity observed during cycling for this electrode.

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