Laser-heating system for high-pressure X-ray diffraction at the Extreme Conditions beamline I15 at Diamond Light Source

Anzellini, Simone; Kleppe, Annette K.; Daisenberger, Dominik; Wharmby, Michael T.; Giampaoli, Ruggero; Boccato, Silvia; Baron, M. A.; Miozzi, Francesca; Keeble, Dean S.; Ross, Allan M.; Gurney, Stuart; Thompson, J. A.; Knap, Giles; Booth, Mark; Hudson, L.; Hawkins, D.; Walter, Michael J.; Wilhelm, H.

doi:10.1107/s1600577518013383

Cited by 26 publications

(31 citation statements)

References 46 publications

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“…In this work, two series of AD-XRD experiments were performed: one at the Materials Science and Powder Diffraction beamline BL04 at the ALBA synchrotron 49 , and one at the Extreme Conditions beamline I15 at the Diamond Light Source (DLS) synchrotron 50 . For the experiment performed at DLS, two membrane DACs were equipped with diamonds with culet sizes ranging from 200 to 100 μ m. Whereas for the experiments performed at ALBA, four membrane DACs were equipped with diamonds with culet sizes ranging from 300 to 200 μ m. In both cases, gaskets where prepared from pre-indented and sparkle-erosion drilled Re foils.…”

Section: Methodsmentioning

confidence: 99%

Thermal equation of state of ruthenium characterized by resistively heated diamond anvil cell

Anzellini

Errandonea

Cazorla

et al. 2019

Sci Rep

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The high-pressure and high-temperature structural and chemical stability of ruthenium has been investigated via synchrotron X-ray diffraction using a resistively heated diamond anvil cell. In the present experiment, ruthenium remains stable in the hcp phase up to 150 GPa and 960 K. The thermal equation of state has been determined based upon the data collected following four different isotherms. A quasi-hydrostatic equation of state at ambient temperature has also been characterized up to 150 GPa. The measured equation of state and structural parameters have been compared to the results of ab initio simulations performed with several exchange-correlation functionals. The agreement between theory and experiments is generally quite good. Phonon calculations were also carried out to show that hcp ruthenium is not only structurally but also dynamically stable up to extreme pressures. These calculations also allow the pressure dependence of the Raman-active E2g mode and the silent B1g mode of Ru to be determined.

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Section: Methodsmentioning

confidence: 99%

Thermal equation of state of ruthenium characterized by resistively heated diamond anvil cell

Anzellini

Errandonea

Cazorla

et al. 2019

Sci Rep

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“…In-situ XRD experiments were conducted at beamline I15 (Anzellini et al 2018) at the Diamond Light Source synchrotron facility, UK, using monochromatic X-rays with a wavelength of 0.4246 Å. The X-ray beam size at the sample position was 9 µm x 6 µm (fullwidth at half maximum, FWHM).…”

Section: Methodsmentioning

confidence: 99%

Static compression of Fe4N to 77 GPa and its implications for nitrogen storage in the deep Earth

Breton

Komabayashi

Thompson

et al. 2019

American Mineralogist

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Compression and decompression experiments on face-centered cubic (fcc) γ′-Fe4N to 77 GPa at room temperature were conducted in a diamond-anvil cell with in situ X-ray diffraction (XRD) to examine its stability under high pressure. In the investigated pressure range, γ′-Fe4N did not show any structural transitions. However, a peak broadening was observed in the XRD patterns above 60 GPa. The obtained pressure-volume data to 60 GPa were fitted to the third-order Birch-Murnaghan equation of state (EoS), which yielded the following elastic parameters: K0 = 169 (6) GPa, K′ = 4.1 (4), with a fixed V0 = 54.95 Å at 1 bar. A quantitative Schreinemakers' web was obtained at 15–60 GPa and 300–1600 K by combining the EoS for γ′-Fe4N with reported phase stability data at low pressures. The web indicates the existence of an invariant point at 41 GPa and 1000 K where γ′-Fe4N, hexagonal closed-packed (hcp) ε-Fe7N3, double hexagonal closed-packed β-Fe7N3, and hcp Fe phases are stable. From the invariant point, a reaction γ′-Fe4N = β-Fe7N3 + hcp Fe originates toward the high-pressure side, which determines the high-pressure stability of γ′-Fe4N at 56 GPa and 300 K. Therefore, the γ′-Fe4N phase observed in the experiments beyond this pressure must be metastable. The obtained results support the existing idea that β-Fe7N3 would be the most nitrogen-rich iron compound under core conditions. An iron carbonitride Fe7(C,N)3 found as a mantle-derived diamond inclusion implies that β-Fe7N3 and Fe7C3 may form a continuous solid solution in the mantle deeper than 1000 km depth. Diamond formation may be related to the presence of fluids in the mantle, and dehydration reactions of high-pressure hydrous phase D might have supplied free fluids in the mantle at depths greater than 1000 km. As such, the existence of Fe7(C,N)3 in diamond can be an indicator of water transportation to the deep mantle.

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“…The high P-T experiment were performed using the beamline LH-system 42 , following the procedure described in Anzellini et al 25 . Before each heating ramp, the sample was brought to the target pressure.…”

Section: Methodsmentioning

confidence: 99%

“…Once coupled together, their relative positions were adjusted to obtain a uniform hot spot over about 40 µ m in diameter. Before and after each heating ramp the relative alignment of the X-rays with the lasers and the temperature reading was checked following the procedure described in Anzellini et al 42 .…”

Section: Methodsmentioning

confidence: 99%

Melting line of calcium characterized by in situ LH-DAC XRD and first-principles calculations

Anzellini

Pozzo

Errandonea

2021

Sci Rep

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In this work, the melting line of calcium has been characterized both experimentally, using synchrotron X-ray diffraction in laser-heated diamond-anvil cells, and theoretically, using first-principles calculations. In the investigated pressure and temperature range (pressure between 10 and 40 GPa and temperature between 300 and 3000 K) it was possible to observe the face-centred phase of calcium and to confirm (and characterize for the first time at these conditions) the presence of the body-centred cubic and the simple cubic phase of calcium. The melting points obtained with the two techniques are in excellent agreement. Furthermore, the present results agree with the only existing melting line of calcium obtained in laser-heated diamond anvil cells, using the speckle method as melting detection technique. They also confirm a flat slope of the melting line in the pressure range between 10 and 30 GPa. The flat melting curve is associated with the presence of the solid high-temperature body-centered cubic phase of calcium and to a small volume change between this phase and the liquid at melting. Reasons for the stabilization of the body-centered face at high-temperature conditions will be discussed.

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Laser-heating system for high-pressure X-ray diffraction at the Extreme Conditions beamline I15 at Diamond Light Source

Cited by 26 publications

References 46 publications

Thermal equation of state of ruthenium characterized by resistively heated diamond anvil cell

Thermal equation of state of ruthenium characterized by resistively heated diamond anvil cell

Static compression of Fe4N to 77 GPa and its implications for nitrogen storage in the deep Earth

Melting line of calcium characterized by in situ LH-DAC XRD and first-principles calculations

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