2,153 research outputs found
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Artifacts from manganese reduction in rock samples prepared by focused ion beam (FIB) slicing for X-ray microspectroscopic analysis
Abstract. Manganese (Mn)-rich natural rock coatings, so-called rock varnishes, are discussed controversially regarding their genesis. Biogenic and abiogenic mechanisms, as well as a combination of both, have been proposed to be responsible for the Mn oxidation and deposition process. We conducted scanning transmission X-ray microscopy - near edge X-ray absorption fine structure spectroscopy (STXM-NEXAFS) measurements to examine the abundance and spatial distribution of the different oxidation states of Mn within these nano- to micrometer thick crusts. Such microanalytical measurements of thin and hard rock crusts require sample preparation with minimal contamination risk. Focused ion beam (FIB) slicing, a well-established technique in geosciences, was used in this study to obtain 100â200ânm thin slices of the samples for X-ray transmission spectroscopy. However, even though this preparation is suitable to investigate element distributions and structures in rock samples, we observed that, using standard parameters, modifications of the Mn oxidation states occur in the surfaces of the FIB slices. Based on our results, the preparation technique likely causes the reduction of Mn4+ to Mn2+/3+. We draw attention to this issue, since FIB slicing, SEM imaging, and other preparation and visualization techniques operating in the keV range are well-established in geosciences, but researchers are often unaware of the potential for reduction of Mn and possibly other elements in the samplesâ surface layers
Compressive Sensing for Dynamic XRF Scanning
X-Ray Fluorescence (XRF) scanning is a widespread technique of high
importance and impact since it provides chemical composition maps crucial for
several scientific investigations. There are continuous requirements for
larger, faster and highly resolved acquisitions in order to study complex
structures. Among the scientific applications that benefit from it, some of
them, such as wide scale brain imaging, are prohibitively difficult due to time
constraints. However, typically the overall XRF imaging performance is
improving through technological progress on XRF detectors and X-ray sources.
This paper suggests an additional approach where XRF scanning is performed in a
sparse way by skipping specific points or by varying dynamically acquisition
time or other scan settings in a conditional manner. This paves the way for
Compressive Sensing in XRF scans where data are acquired in a reduced manner
allowing for challenging experiments, currently not feasible with the
traditional scanning strategies. A series of different compressive sensing
strategies for dynamic scans are presented here. A proof of principle
experiment was performed at the TwinMic beamline of Elettra synchrotron. The
outcome demonstrates the potential of Compressive Sensing for dynamic scans,
suggesting its use in challenging scientific experiments while proposing a
technical solution for beamline acquisition software.Comment: 16 pages, 7 figures, 1 tabl
Nanoscale X-ray investigation of magnetic metallofullerene peapods
Endohedral lanthanide ions packed inside carbon nanotubes (CNTs) in a
one-dimensional assembly have been studied with a combination of high
resolution transmission electron microscopy (HRTEM), scanning transmission
X-ray microscopy (STXM), and X-ray magnetic circular dichroism (XMCD). By
correlating HRTEM and STXM images we show that structures down to 30 nm are
resolved with chemical contrast and record X-ray absorption spectra from
endohedral lanthanide ions embedded in individual nanoscale CNT bundles. XMCD
measurements of an ErN@C bulk sample and a macroscopic assembly of
filled CNTs indicates that the magnetic properties of the endohedral Er3+ ions
are unchanged when encapsulated in CNTs. This study demonstrates the
feasibility of local magnetic X-ray characterization of low concentrations of
lanthanide ions embedded in molecular nanostructures
Direct visualization of dynamic magnetic coupling in a Co/Py bilayer with picosecond and nanometer resolution
We present a combination of ferromagnetic resonance (FMR) with spatially and
time-resolved X-ray absorption spectroscopy in a scanning transmission X-ray
microscope (STXM-FMR). The transverse high frequency component of the
resonantly excited magnetization is measured with element-specifity in a
Permalloy (Py) disk - Cobalt (Co) stripe bilayer microstructure. STXM-FMR
mappings are snapshots of the local magnetization-precession with nm spatial
resolution and ps temporal resolution. We directly observe the transfer of
angular momentum from Py to Co and vice versa at their respective
element-specific resonances. A third resonance could be observed in our
experiments, which is identified as a coupled resonance of Py and Co.Comment: Version submitted to Physical Review Applied with updated author list
and supplemental information (Ancillary file
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Atomic and nano-scale characterization of a 50-year-old hydrated C3S paste
This paper investigates the atomic and nano-scale structures of a 50-year-old hydrated alite paste. Imaged by TEM, the outer product C-S-H fibers are composed of particles that are 1.5-2 nm thick and several tens of nanometers long. 29Si NMR shows 47.9% Q1 and 52.1% Q2, with a mean SiO4 tetrahedron chain length (MCL) of 4.18, indicating a limited degree of polymerization after 50 years' hydration. A Scanning Transmission X-ray Microscopy (STXM) study was conducted on this late-age paste and a 1.5 year old hydrated C3S solution. Near Edge X-ray Absorption Fine Structure (NEXAFS) at Ca L3,2-edge indicates that Ca2 + in C-S-H is in an irregular symmetric coordination, which agrees more with the atomic structure of tobermorite than that of jennite. At Si K-edge, multi-scattering phenomenon is sensitive to the degree of polymerization, which has the potential to unveil the structure of the SiO44 - tetrahedron chain
A Scanning Transmission X-ray Microscopy Study of Cubic and Orthorhombic CâA and Their Hydration Products in the Presence of Gypsum.
This paper shows the microstructural differences and phase characterization of pure phases and hydrated products of the cubic and orthorhombic (Na-doped) polymorphs of tricalcium aluminate (CâA), which are commonly found in traditional Portland cements. Pure, anhydrous samples were characterized using scanning transmission X-ray microscopy (STXM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) and demonstrated differences in the chemical and mineralogical composition as well as the morphology on a micro/nano-scale. CâA/gypsum blends with mass ratios of 0.2 and 1.9 were hydrated using a water/CâA ratio of 1.2, and the products obtained after three days were assessed using STXM. The hydration process and subsequent formation of calcium sulfate in the CâA/gypsum systems were identified through the changes in the LIII edge fine structure for Calcium. The results also show greater Ca LII binding energies between hydrated samples with different gypsum contents. Conversely, the hydrated samples from the cubic and orthorhombic CâA at the same amount of gypsum exhibited strong morphological differences but similar chemical environments
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