Abstract:Abstract. Facilities for studying gas-solid interactions on beamline I11 at the Diamond Light Source are described. Sample evolution in low and high gas pressure capillary cells (1×10 −7 to 100 bar) with noncontact cooling and heating (80 to 1273 K) can be monitored structurally (X-rays) and spectroscopically (Raman). First results on the dehydration of MgSO4.7H2O, the formation of CO2 clathrate hydrate and the reaction of amorphous CaSiO3 grains with CO2 gas to form CaCO3 are presented to demonstrate the appl… Show more
“…Time-resolved in situ synchrotron X-ray powder diffraction (SXPD) of the first charge was performed at beamline I11 (Diamond Light Source, U.K.) using the position sensitive detector (PSD), an in-house-developed battery cell with additional ports for gas analysis and an electrolyte reservoir, I11 ’s gas analysis system, and the in-house-developed flow panel. The energy of the X-ray beam was tuned to 25 keV, and the calibrated wavelength was 0.489951(10) Å.…”
Reversible and irreversible
charge exchange reactions of Li- and
Mn-rich layered oxides (Li1.15Ni0.2Co0.1Mn0.55O2, LLO) are investigated with bulk and
surface-sensitive near-edge X-ray absorption fine structure spectroscopy
(NEXAFS) at the Ni L
2,3, Co L
2,3, Mn L
2,3, and O K edges;
mass spectrometry (MS); and operando synchrotron
X-ray powder diffraction (SXPD). The present work shows the relation
between O–O formation in the bulk and Ni, Co, and Mn reduction/oxidation
processes, which in turn deliver outstanding capacities of Li-rich
layered oxides (LLO). Moreover, the reversibility of charge compensation
reactions is discussed and differences between O–O formation
and oxygen release, both occurring mainly upon the first charge (so-called
activation), are identified.
“…Time-resolved in situ synchrotron X-ray powder diffraction (SXPD) of the first charge was performed at beamline I11 (Diamond Light Source, U.K.) using the position sensitive detector (PSD), an in-house-developed battery cell with additional ports for gas analysis and an electrolyte reservoir, I11’s gas analysis system, and the in-house-developed flow panel. The energy of the X-ray beam was tuned to 25 keV, and the calibrated wavelength was 0.489951(10) Å.…”
Reversible and irreversible
charge exchange reactions of Li- and
Mn-rich layered oxides (Li1.15Ni0.2Co0.1Mn0.55O2, LLO) are investigated with bulk and
surface-sensitive near-edge X-ray absorption fine structure spectroscopy
(NEXAFS) at the Ni L
2,3, Co L
2,3, Mn L
2,3, and O K edges;
mass spectrometry (MS); and operando synchrotron
X-ray powder diffraction (SXPD). The present work shows the relation
between O–O formation in the bulk and Ni, Co, and Mn reduction/oxidation
processes, which in turn deliver outstanding capacities of Li-rich
layered oxides (LLO). Moreover, the reversibility of charge compensation
reactions is discussed and differences between O–O formation
and oxygen release, both occurring mainly upon the first charge (so-called
activation), are identified.
“…An alternative pathway that leads to the direct conversion of ACC to calcite with no vaterite intermediate can occur through doping of the initial ACC with Mg [ 86 ] ( figure 5 f ). Recent studies [ 87 , 88 ] have extended this work (using XAS on beamline I18 and high-resolution XRD on beamline I11) to show that the presence of organic molecules is key to controlling the ACC crystallization pathway and to describing the high temperature/pressure transformation of ACC to vaterite in systems equivalent to extraterrestrial environments [ 89 , 90 ]. Figure 5.…”
Section: Characterizing Mineral Precipitation and Weathering Reactionmentioning
Diamond Light Source Ltd celebrated its 10th anniversary as a company in December 2012 and has now accepted user experiments for over 5 years. This paper describes the current facilities available at Diamond and future developments that enhance its capacities with respect to the Earth and environmental sciences. A review of relevant research conducted at Diamond thus far is provided. This highlights how synchrotron-based studies have brought about important advances in our understanding of the fundamental parameters controlling highly complex mineral–fluid–microbe interface reactions in the natural environment. This new knowledge not only enhances our understanding of global biogeochemical processes, but also provides the opportunity for interventions to be designed for environmental remediation and beneficial use.
Aims. We study the formation of calcium carbonate, through the solid-gas interaction of amorphous Ca-silicate with gaseous CO 2 , at elevated pressures, and link this to the possible presence of calcium carbonate in a number of circumstellar and planetary environments. Methods. We use in-situ synchrotron X-ray powder diffraction to obtain detailed structural data pertaining to the formation of the crystalline calcium carbonate phase vaterite and its evolution with temperature. Results. We found that the metastable calcium carbonate phase vaterite was formed alongside calcite, at elevated CO 2 pressure, at room temperature and subsequently remained stable over a large range of temperature and pressure. Conclusions. We report the formation of the calcium carbonate mineral vaterite whilst attempting to simulate carbonate dust grain formation in astrophysical environments. This suggests that vaterite could be a mineral component of carbonate dust and also presents a possible method of formation for vaterite and its polymorphs on planetary surfaces.
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