Femtosecond electronic structure response to high intensity XFEL pulses probed by iron X-ray emission spectroscopy.

We report the time-resolved femtosecond evolution of the K-shell X-ray emission spectra of iron during high intensity illumination of X-rays in a micron-sized focused hard X-ray free electron laser (XFEL) beam. Detailed pulse length dependent measurements revealed that rapid spectral energy shift and broadening started within the first 10 fs of the X-ray illumination at intensity levels between 10 and 10 W cm. We attribute these spectral changes to the rapid evolution of high-density photoelectron mediated secondary collisional ionization processes upon the absorption of the incident XFEL radiation.

Detection of the Chiral Spin Structure in Ferromagnetic SrRuO Thin Film.

SrRuO (SRO) thin films and their heterostructure have attracted much attention because of the recently demonstrated fascinating properties, such as topological Hall effect and skyrmions. Critical to the understanding of those SRO properties is the study of the spin configuration. Here, we conduct resonant soft X-ray scattering (RSXS) at the oxygen K edge to investigate the spin configuration of a four-unit-cell SRO film that was grown epitaxially on a single-crystal SrTiO.

Pressure-induced metathesis reaction to sequester Cs.

We report here a pressure-driven metathesis reaction where Ag-exchanged natrolite (Ag16Al16Si24O80·16H2O, Ag-NAT) is pressurized in an aqueous CsI solution, resulting in the exchange of Ag(+) by Cs(+) in the natrolite framework forming Cs16Al16Si24O80·16H2O (Cs-NAT-I) and, above 0.5 GPa, its high-pressure polymorph (Cs-NAT-II). During the initial cation exchange, the precipitation of AgI occurs.

Atomically engineered metal-insulator transition at the TiO2/LaAlO3 heterointerface.

We demonstrate that the atomic boundary conditions of simple binary oxides can be used to impart dramatic changes of state. By changing the substrate surface termination of LaAlO3 (001) from AlO2 to LaO, the room-temperature sheet conductance of anatase TiO2 films are increased by over 3 orders of magnitude, transforming the intrinsic insulating state to a high mobility metallic state, while maintaining excellent optical transparency.

Irreversible xenon insertion into a small-pore zeolite at moderate pressures and temperatures.

Pressure drastically alters the chemical and physical properties of materials and allows structural phase transitions and chemical reactions to occur that defy much of our understanding gained under ambient conditions. Particularly exciting is the high-pressure chemistry of xenon, which is known to react with hydrogen and ice at high pressures and form stable compounds. Here, we show that Ag16Al16Si24O8·16H2O (Ag-natrolite) irreversibly inserts xenon into its micropores at 1.

Super-hydrated zeolites: pressure-induced hydration in natrolites.

High-pressure synchrotron X-ray powder diffraction studies of a series of alkali-metal-exchanged natrolites, A16Al16Si24O80·nH2O (A=Li, K, Na, Rb, and Cs and n=14, 16, 22, 24, 32), in the presence of water, reveal structural changes that far exceed what can be achieved by varying temperature and chemical composition. The degree of volume expansion caused by pressure-induced hydration (PIH) is inversely proportional to the non-framework cation radius. The expansion of the unit-cell volume through PIH is as large as 20.

Resolving material-specific structures within Fe₃O₄|γ-Mn₂O₃ core|shell nanoparticles using anomalous small-angle X-ray scattering.

Here it is demonstrated that multiple-energy, anomalous small-angle X-ray scattering (ASAXS) provides significant enhancement in sensitivity to internal material boundaries of layered nanoparticles compared with the traditional modeling of a single scattering energy, even for cases in which high scattering contrast naturally exists. Specifically, the material-specific structure of monodispersed Fe₃O₄|γ-Mn₂O₃ core|shell nanoparticles is determined, and the contribution of each component to the total scattering profile is identified with unprecedented clarity. We show that Fe₃O₄|γ-Mn₂O₃ core|shell nanoparticles with a diameter of 8.

Immobilization of large, aliovalent cations in the small-pore zeolite K-natrolite by means of pressure.

High-pressure ion exchange of small-pore zeolite K-natrolite allows immobilization of nominally non-exchangeable aliovalent cations such as trivalent europium. A sample exchanged at 3.0(1) GPa and 250 °C contains about 4.

Pressure- and heat-induced insertion of CO2 into an auxetic small-pore zeolite.

When the small-pore zeolite natrolite is compressed at ca. 1.5 GPa and heated to ca.

High pressure investigation of alpha-form and CH4-loaded beta-form of hydroquinone compounds.

The high pressure compression behaviors of two hydroquinone compounds have been investigated using a combination of in situ synchrotron x-ray powder diffraction and Raman spectroscopy up to ca. 7 GPa. The structural integrity of the alpha-form hydroquinone clathrate is maintained throughout the pressure range, whereas the CH(4)-loaded beta-form hydroquinone clathrate decomposes and transforms to a new high pressure phase near 5 GPa.

Inelastic x-ray scattering of dense solid oxygen: evidence for intermolecular bonding.

The detailing of the intermolecular interactions in dense solid oxygen is essential for an understanding of the rich polymorphism and remarkable properties of this element at high pressure. Synchrotron inelastic x-ray scattering measurements of oxygen K-edge excitations to 38 GPa reveal changes in electronic structure and bonding on compression of the molecular solid. The measurements show that O(2) molecules interact predominantly through the half-filled 1pi(g)* orbital <10 GPa.

Pressure-induced hydration and order-disorder transition in a synthetic potassium gallosilicate zeolite with gismondine topology.

Two high-pressure phases of a potassium gallosilicate with a gismondine framework (K-GaSi-GIS) were characterized using Rietveld refinements of in-situ high-pressure, high-resolution synchrotron X-ray powder diffraction data. The observed response of the K-GaSi-GIS framework under hydrostatic pressure is a gradual flattening of the so-called "double crankshaft" structural chain units. At pressures below 1.

Dehydration-induced water disordering in a synthetic potassium gallosilicate natrolite.

A new potassium gallosilicate zeolite with a natrolite topology (approximate formula K8.2Ga8.2Si11.

Valence band x-ray emission spectra of compressed germanium.

We report measurements of the valence band width in compressed Ge determined from x-ray emission spectra below the Ge K edge. The width of the valence band does not show any pressure dependence in the semiconducting diamond-type structure of Ge below 10 GPa. On the other hand, in the metallic beta-Sn phase above 10 GPa the valence band width increases under compression.

Bonding changes in compressed superhard graphite.

Compressed under ambient temperature, graphite undergoes a transition at approximately 17 gigapascals. The near K-edge spectroscopy of carbon using synchrotron x-ray inelastic scattering reveals that half of the pi-bonds between graphite layers convert to sigma-bonds, whereas the other half remain as pi-bonds in the high-pressure form. The x-ray diffraction pattern of the high-pressure form is consistent with a distorted graphite structure in which bridging carbon atoms between graphite layers pair and form sigma-bonds, whereas the nonbridging carbon atoms remain unpaired with pi-bonds.

Single-element elliptical hard x-ray micro-optics.

Using micro-fabrication techniques, we have manufactured a single element kinoform lens in single-crystal silicon with an elliptical profile for 12.398 keV (1A) x-rays. By fabricating a lens that is optimized at fixed wavelengths, absorption in the lens material can be significantly reduced by removing 2_ phase-shifting regions.