Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction

The first high-pressure neutron diffraction study in a miniature diamond-anvil cell of a single crystal of size typical for X-ray diffraction is reported. This is made possible by modern Laue diffraction using a large solid-angle image-plate detector. An unexpected finding is that even reflections whose diffracted beams pass through the cell body are reliably observed, albeit with some attenuation. The cell body does limit the range of usable incident angles, but the crystallographic completeness for a high-symmetry unit cell is only slightly less than for a data collection without the cell. Data collections for two sizes of hexamine single crystals, with and without the pressure cell, and at 300 and 150 K, show that sample size and temperature are the most important factors that influence data quality. Despite the smaller crystal size and dominant parasitic scattering from the diamond-anvil cell, the data collected allow a full anisotropic refinement of hexamine with bond lengths and angles that agree with literature data within experimental error. This technique is shown to be suitable for low-symmetry crystals, and in these cases the transmission of diffracted beams through the cell body results in much higher completeness values than are possible with X-rays. The way is now open for joint X-ray and neutron studies on the same sample under identical conditions.

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Use of a miniature diamond-anvil cell in a joint X-ray and neutron high-pressure study on copper sulfate pentahydrate

IUCrJ ◽

10.1107/s2052252521010708 ◽

2021 ◽

Vol 9 (1) ◽

Author(s):

Giulia Novelli ◽

Konstantin V. Kamenev ◽

Helen E. Maynard-Casely ◽

Simon Parsons ◽

Garry J. McIntyre

Keyword(s):

High Pressure ◽

Single Crystal ◽

Diffraction Data ◽

Diamond Anvil Cell ◽

Structural Parameters ◽

Structure Refinement ◽

Neutron Data ◽

X Ray ◽

Sulfate Pentahydrate ◽

Diamond Anvil

Single-crystal X-ray and neutron diffraction data are usually collected using separate samples. This is a disadvantage when the sample is studied at high pressure because it is very difficult to achieve exactly the same pressure in two separate experiments, especially if the neutron data are collected using Laue methods where precise absolute values of the unit-cell dimensions cannot be measured to check how close the pressures are. In this study, diffraction data have been collected under the same conditions on the same sample of copper(II) sulfate pentahydrate, using a conventional laboratory diffractometer and source for the X-ray measurements and the Koala single-crystal Laue diffractometer at the ANSTO facility for the neutron measurements. The sample, of dimensions 0.40 × 0.22 × 0.20 mm3 and held at a pressure of 0.71 GPa, was contained in a miniature Merrill–Bassett diamond-anvil cell. The highly penetrating diffracted neutron beams passing through the metal body of the miniature cell as well as through the diamonds yielded data suitable for structure refinement, and compensated for the low completeness of the X-ray measurements, which was only 24% on account of the triclinic symmetry of the sample and the shading of reciprocal space by the cell. The two data-sets were combined in a single `XN' structure refinement in which all atoms, including H atoms, were refined with anisotropic displacement parameters. The precision of the structural parameters was improved by a factor of up to 50% in the XN refinement compared with refinements using the X-ray or neutron data separately.

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High Pressure Behavior of Mascagnite from Single Crystal Synchrotron X-ray Diffraction Data

Crystals ◽

10.3390/cryst11080976 ◽

2021 ◽

Vol 11 (8) ◽

pp. 976

Author(s):

Paola Comodi ◽

Maximiliano Fastelli ◽

Giacomo Criniti ◽

Konstantin Glazyrin ◽

Azzurra Zucchini

Keyword(s):

High Pressure ◽

Single Crystal ◽

Room Temperature ◽

Diamond Anvil Cell ◽

Geometrical Parameters ◽

X Ray Diffraction ◽

Third Order ◽

X Ray ◽

Diamond Anvil ◽

Murnaghan Equation

High-pressure synchrotron X-ray diffraction was carried out on a single crystal of mascagnite, compressed in a diamond anvil cell. The sample maintained its crystal structure up to ~18 GPa. The volume–pressure data were fitted by a third-order Birch–Murnaghan equation of state (BM3-EOS) yielding K0 = 20.4(7) GPa, K’0 = 6.1(2), and V0 = 499(1) Å3, as suggested by the F-f plot. The axial compressibilities, calculated with BM3-EOS, were K0a = 35(3), K’0a = 7.7(7), K0b = 10(3), K’0b = 7(1), K0c = 25(1), and K’0c = 4.3(2) The axial moduli measured using a BM2-EOS and fixing K’0 equal to 4, were K0a = 52(2), K0b = 20 (1), and K0c = 29.6(4) GPa, and the anisotropic ratio of K0a:K0b:K0c = 1:0.4:0.5. The evolution of crystal lattice and geometrical parameters indicated no phase transition until 17.6 GPa. Sulphate polyhedra were incompressible and the density increase of 30% compared to investigated pressure should be attributed to the reduction of weaker hydrogen bonds. In contrast, some of them, directed along [100], were very short at room temperature, below 2 Å, and showed a very low compressibility. This configuration explains the anisotropic compressional behavior and the lowest compressibility of the a axis.

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Combined X-ray and neutron single-crystal diffraction in diamond anvil cells

Journal of Applied Crystallography ◽

10.1107/s1600576719014201 ◽

2020 ◽

Vol 53 (1) ◽

pp. 9-14 ◽

Cited By ~ 1

Author(s):

Andrzej Grzechnik ◽

Martin Meven ◽

Carsten Paulmann ◽

Karen Friese

Keyword(s):

High Pressure ◽

Data Processing ◽

Single Crystal ◽

Diamond Anvil Cell ◽

Crystal Data ◽

Structural Refinement ◽

Single Crystal Diffraction ◽

X Ray ◽

Diamond Anvil ◽

First Time

It is shown that it is possible to perform combined X-ray and neutron single-crystal studies in the same diamond anvil cell (DAC). A modified Merrill–Bassett DAC equipped with an inflatable membrane filled with He gas has been developed. It can be used on laboratory X-ray and synchrotron diffractometers as well as on neutron instruments. The data processing procedures and a joint structural refinement of the high-pressure synchrotron and neutron single-crystal data are presented and discussed for the first time.

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High-pressure single-crystal study on AlPO4 with synchrotron radiation

Journal of Applied Crystallography ◽

10.1107/s0021889890005702 ◽

1990 ◽

Vol 23 (5) ◽

pp. 397-400 ◽

Cited By ~ 7

Author(s):

H. Sowa ◽

K. Reithmayer ◽

J. Macavei ◽

W. Rieck ◽

H. Schulz ◽

...

Keyword(s):

Synchrotron Radiation ◽

Single Crystal ◽

Diamond Anvil Cell ◽

Structural Parameters ◽

X Rays ◽

X Ray ◽

Single Crystal Study ◽

Diamond Anvil ◽

Counting Statistics ◽

Good Agreement

A single-crystal study on AlPO4 was performed at 2.90 (7) GPa with synchrotron radiation using a diamond-anvil cell with a beryllium gasket. For the data collection the radiation wavelength of only 0.54 Å, was chosen to minimize the absorption of X-rays in the pressure cell. The diffracted intensity was high enough to measure even weak reflections with sufficient counting statistics. The refined structural parameters are in good agreement with those determined from data collected with a conventional X-ray tube.

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Momentum-resolved resonant inelastic X-ray scattering on a single crystal under high pressure

Journal of Synchrotron Radiation ◽

10.1107/s1600577513028944 ◽

2013 ◽

Vol 21 (1) ◽

pp. 131-135 ◽

Cited By ~ 3

Author(s):

Masahiro Yoshida ◽

Kenji Ishii ◽

Ignace Jarrige ◽

Tetsu Watanuki ◽

Kazutaka Kudo ◽

...

Keyword(s):

High Pressure ◽

Single Crystal ◽

Diamond Anvil Cell ◽

Ambient Pressure ◽

Electronic Excitations ◽

X Ray ◽

X Ray Scattering ◽

Angle Condition ◽

Diamond Anvil ◽

Ray Scattering

A single-crystal momentum-resolved resonant inelastic X-ray scattering (RIXS) experiment under high pressure using an originally designed diamond anvil cell (DAC) is reported. The diamond-in/diamond-out geometry was adopted with both the incident and scattered beams passing through a 1 mm-thick diamond. This enabled us to cover wide momentum space keeping the scattering angle condition near 90°. Elastic and inelastic scattering from the diamond was drastically reduced using a pinhole placed after the DAC. Measurement of the momentum-resolved RIXS spectra of Sr2.5Ca11.5Cu24O41at the CuK-edge was thus successful. Though the inelastic intensity becomes weaker by two orders than the ambient pressure, RIXS spectra both at the center and the edge of the Brillouin zone were obtained at 3 GPa and low-energy electronic excitations of the cuprate were found to change with pressure.

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Introduction to DAC Techniques. Single Crystal X-ray Diffraction Technique at High Pressure Using Diamond Anvil Cell.

The Review of High Pressure Science and Technology ◽

10.4131/jshpreview.8.10 ◽

1998 ◽

Vol 8 (1) ◽

pp. 10-16

Author(s):

Yasuhiro Kudoh

Keyword(s):

High Pressure ◽

Single Crystal ◽

Diamond Anvil Cell ◽

X Ray Diffraction ◽

X Ray ◽

Diamond Anvil

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PHASE TRANSITION IN LAYERED PEROVSKITE LIKE MANGANATE Ca3Mn2O7 UNDER HIGH PRESSURE

International Journal of Modern Physics B ◽

10.1142/s0217979201007117 ◽

2001 ◽

Vol 15 (18) ◽

pp. 2491-2497 ◽

Cited By ~ 1

Author(s):

J. L. ZHU ◽

L. C. CHEN ◽

R. C. YU ◽

F. Y. LI ◽

J. LIU ◽

...

Keyword(s):

Crystal Structure ◽

High Pressure ◽

Diamond Anvil Cell ◽

The Other ◽

Layered Perovskite ◽

X Ray Diffraction ◽

Two Phase ◽

X Ray ◽

Diamond Anvil

In situ high pressure energy dispersive X-ray diffraction measurements on layered perovskite-like manganate Ca 3 Mn 2 O 7 under pressures up to 35 GPa have been performed by using diamond anvil cell with synchrotron radiation. The results show that the structure of layered perovskite-like manganate Ca 3 Mn 2 O 7 is unstable under pressure due to the easy compression of NaCl-type blocks. The structure of Ca 3 Mn 2 O 7 underwent two phase transitions under pressures in the range of 0~35 GPa. One was at about 1.3 GPa with the crystal structure changing from tetragonal to orthorhombic. The other was at about 9.5 GPa with the crystal structure changing from orthorhombic back to another tetragonal.

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