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.

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 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.

A new dynamic framework with direct in situ visualisation of breathing under CO2 gas pressure

CrystEngComm ◽  
2019 ◽  
Vol 21 (22) ◽  
pp. 3415-3419 ◽  
Author(s):  
Phumile Sikiti ◽  
Charl X. Bezuidenhout ◽  
Dewald P. van Heerden ◽  
Leonard J. Barbour
Keyword(s):  
Single Crystal ◽  
Diffraction Analysis ◽  
Gas Pressure ◽  
X Ray Diffraction ◽  
Co2 Gas ◽  
X Ray ◽  
Dynamic Framework

Structural evidence from in situ single-crystal X-ray diffraction analysis reveals flexibility in a new non-interpenetrated pillared-layer MOF that switches between a wide-pore and a narrow-pore form.

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 High-pressure cell for neutron diffraction with in situ pressure control at cryogenic temperatures

2014 ◽  
Vol 85 (4) ◽  
pp. 043904 ◽  
Author(s):  
Matthew K. Jacobsen ◽  
Christopher J. Ridley ◽  
Artur Bocian ◽  
Oleg Kirichek ◽  
Pascal Manuel ◽  
...  
Keyword(s):  
High Pressure ◽  
Neutron Diffraction ◽  
Pressure Control ◽  
Cryogenic Temperatures ◽  
High Pressure Cell ◽  
Pressure Cell

scholarly journals Creation of new guest accessible space under gas pressure in a flexible MOF: multidimensional insight through combination of in situ techniques

2016 ◽  
Vol 52 (76) ◽  
pp. 11374-11377 ◽  
Author(s):  
Prashant M. Bhatt ◽  
Eustina Batisai ◽  
Vincent J. Smith ◽  
Leonard J. Barbour
Keyword(s):  
Pressure Gradient ◽  
Single Crystal ◽  
Gas Pressure ◽  
Single Crystal Diffraction ◽  
In Situ Techniques

Creation of a new guest accessible space under gas pressure in a flexible MOF studied by in situ single crystal diffraction and Pressure Gradient DSC.

Sign in / Sign up

Export Citation Format

Share Document