High-pressure single-crystal neutron diffraction to 10 GPa by angle-dispersive techniques

Bull, Craig L.; Guthrie, Malcolm; Archer, J.; Fernandez-Diaz, M. T.; Loveday, J. S.; Komatsu, Kazuki; Hamidov, Hayrullo; Nelmes, R. J.

doi:10.1107/s0021889811021819

Cited by 18 publications

(13 citation statements)

References 17 publications

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“…Paris-Edinburgh presses with a very restricted access to the reciprocal space are too cumbersome to be easily operated during the measurements of single-crystal intensities (Fang et al, 2010). Nevertheless, they can give data suitable for structure refinement at short neutron wavelengths (Bull et al, 2011). Because of the large volumes required for neutron single-crystal diffraction up to now (>1 mm 3 ), panoramic opposed-anvil cells with large anvils made of sapphire (Kuhs et al, 1989(Kuhs et al, , 1996McMahon et al, 1990) or moissanite (Xu et al, 2002;McIntyre et al, 2005) have been employed to collect data for full structure refinement.…”

Section: Introductionmentioning

confidence: 99%

Single-crystal neutron diffraction in diamond anvil cells with hot neutrons

2018

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It is demonstrated that it is possible to perform single-crystal measurements in diamond anvil cells (DACs) with a monochromatic beam at modern hot neutron sources that offer the benefit of short neutron wavelengths with high fluxes. A piston-cylinder DAC with conical Boehler-Almax diamonds that allows for a wide accessibility of the reciprocal space has been developed. The diffraction data collected in this cell using hot neutrons are of very good quality and can be used for a full and reliable structure refinement.

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Section: Introductionmentioning

confidence: 99%

Single-crystal neutron diffraction in diamond anvil cells with hot neutrons

2018

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“…Despite the relatively low intensity of neutron sources, the design and development of the Paris-Edinburgh (P-E) pressure cell has enabled powder neutron diffraction to routinely reach pressures of $10 GPa (Besson et al, 1992), and, through the use of more specialized equipment, pressures as high as $30 GPa can be achieved (Klotz et al, 1995). At present, single-crystal neutron diffraction using the P-E press is limited to 16 GPa (Bull, Bocian et al, 2011;Bull, Guthrie et al, 2011). Techniques for powder and single-crystal neutron diffraction at higher pressures than those currently accessible using a P-E press are still undergoing rapid development (Klotz, 2012;Binns et al, 2016).…”

Section: Introductionmentioning

confidence: 99%

Neutron total scattering of crystalline materials in the gigapascal regime

2017

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Neutron total scattering of disordered crystalline materials provides direct experimental access to the local (short-range) structure. The ways in which this local structure agrees (or disagrees) with the long-range crystal structure can provide important insight into structure-property relationships. High-pressure neutron diffraction using a Paris-Edinburgh (P-E) pressure cell allows experimenters to explore the ways in which materials are affected by pressure, can reveal new synthetic routes to novel functional materials and has important applications in many areas, including geology, engineering and planetary science. However, the combination of these two experimental techniques poses unique challenges for both data collection and analysis. In this paper it is shown that, with only minor modifications to the standard P-E press setup, high-quality total scattering data can be obtained from crystalline materials in the gigapascal pressure regime on the PEARL diffractometer at ISIS. The quality of the data is assessed through the calculation of coordination numbers and the use of reverse Monte Carlo refinements. The time required to collect data of sufficient quality for detailed analysis is assessed and is found to be of the order of 8 h for a quartz sample. Finally, data from the perovskite LaCo 0.35 Mn 0.65 O 3 are presented and reveal that PEARL total scattering data offer the potential of extracting local structural information from complex materials at high pressure.

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“…Bull et al [1] used the Paris-Edinburgh press, a widely-used press for its easiness of handling [2], for single-crystal neutron diffraction of KD2PO4 and squaric acid (D2C4O4) at 5, 7.5 GPa. Further high-pressure data were collected on squaric acid at 3.5 and 10 GPa [3]. The sample space in the PE-press is surrounded by two-opposed anvils and two or four supporting pillars which limit the accessible reciprocal space only in a horizontal plane perpendicular to the compression axis.…”

Section: Introductionmentioning

confidence: 99%

A nano-polycrystalline diamond anvil cell with bulk metallic glass cylinder for single-crystal neutron diffraction

Yamashita

Komatsu

Klotz

et al. 2019

High Pressure Research

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A nano-polycrystalline diamond anvil cell with bulk metallic glass cylinder for singlecrystal neutron diffraction. A nano-polycrystalline diamond anvil cell with bulk metallic glass cylinder for single-crystal neutron diffraction A nano-polycrystalline diamond anvil cell with bulk metallic glass cylinder for single-crystal neutron diffractionAbstract A high-pressure cell for in-situ single-crystal neutron diffraction was developed. The cell uses nano-polycrystalline diamond anvils in a tubular load frame made of bulk metallic glass which is highly transparent to neutrons and does not produce Bragg reflections. Diffraction peaks from a sample can be measured from almost any direction and the simple geometry of the cell allows accurate attenuation corrections. We demonstrate the operation of the cell by ambientpressure experiment using a single-crystal of NaCl on the D9 diffractometer at the Institute-Laue-Langevin. A high-pressure experiment was also carried out on a single crystal of ice VII at 2.35GPa showing the potential to detect weak diffraction spots. The correct integration of weak reflections together with the simple attenuation correction will help to carry out precise structure analysis and address new scientific problems using neutron diffraction.

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High-pressure single-crystal neutron diffraction to 10 GPa by angle-dispersive techniques

Cited by 18 publications

References 17 publications

Single-crystal neutron diffraction in diamond anvil cells with hot neutrons

Single-crystal neutron diffraction in diamond anvil cells with hot neutrons

Neutron total scattering of crystalline materials in the gigapascal regime

A nano-polycrystalline diamond anvil cell with bulk metallic glass cylinder for single-crystal neutron diffraction

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