Automated markerless full field hard x-ray microscopic tomography at sub-50 nm 3-dimension spatial resolution

Wang, Jun; Chen, Yu-chen Karen; Qin, Yuan; Tkachuk, Andrei; Erdonmez, Can K.; Hornberger, Benjamin; Feser, Michael

doi:10.1063/1.3701579

Cited by 109 publications

(95 citation statements)

References 21 publications

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“…In this study, we used a recently developed full-field hard X-ray ultrahigh-resolution (∼30-50 nm without binning pixels) synchrotron-based transmission X-ray microscope (TXM) (14) with a field of view of 20 μm × 20 μm to study magnetite and other iron-rich minerals in bulk CIE clay (AN560.1 from 165.5 m depth of the Ancora core) from just above the onset of the CIE and the coincident high-magnetization layer (5,6). In the front and side views of the TXM image of a submillimeter bulk CIE clay dust (AN560.1-X1) mounted on a tungsten carbide (WC) pin ( Fig.…”

Section: Resultsmentioning

confidence: 99%

“…Although the spatial resolution of the TXM is ∼30-50 nm without binning pixels for a 20-μm × 20-μm field of view (14), the X-ray absorption from an individual ∼50-to ∼100-nm-sized nanoparticle is still too weak to produce a clear contrast to show the magnetosome chains produced by MTB or nonbiogenic isolated magnetite nanoparticles (Fig. 2).…”

Section: Resultsmentioning

confidence: 99%

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Quantified abundance of magnetofossils at the Paleocene–Eocene boundary from synchrotron-based transmission X-ray microscopy

Wang

Chen‐Wiegart

et al. 2015

Proc. Natl. Acad. Sci. U.S.A.

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The Paleocene–Eocene boundary (∼55.8 million years ago) is marked by an abrupt negative carbon isotope excursion (CIE) that coincides with an oxygen isotope decrease interpreted as the Paleocene–Eocene thermal maximum. Biogenic magnetite (Fe3O4) in the form of giant (micron-sized) spearhead-like and spindle-like magnetofossils, as well as nano-sized magnetotactic bacteria magnetosome chains, have been reported in clay-rich sediments in the New Jersey Atlantic Coastal Plain and were thought to account for the distinctive single-domain magnetic properties of these sediments. Uncalibrated strong field magnet extraction techniques have been typically used to provide material for scanning and transmission electron microscopic imaging of these magnetic particles, whose concentration in the natural sediment is thus difficult to quantify. In this study, we use a recently developed ultrahigh-resolution, synchrotron-based, full-field transmission X-ray microscope to study the iron-rich minerals within the clay sediment in their bulk state. We are able to estimate the total magnetization concentration of the giant biogenic magnetofossils to be only ∼10% of whole sediment. Along with previous rock magnetic studies on the CIE clay, we suggest that most of the magnetite in the clay occurs as isolated, near-equidimensional nanoparticles, a suggestion that points to a nonbiogenic origin, such as comet impact plume condensates in what may be very rapidly deposited CIE clays.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Quantified abundance of magnetofossils at the Paleocene–Eocene boundary from synchrotron-based transmission X-ray microscopy

Wang

Chen‐Wiegart

et al. 2015

Proc. Natl. Acad. Sci. U.S.A.

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“…TXM is a non-destructive, nanoscale resolution, highly penetrative hard X-ray imaging technique in which the sample environment can be easily controlled via the development and implementation of in situ environmental apparatuses. 26 In situ imaging was done at an X-ray energy of 8 keV with a large 40 × 40 μm (1600 μm 2 ) field of view and an exposure time of 20 seconds for each image. The moderate exposure time made it possible to generate a clear image by binning a 2 × 2 pixel region using the 2k × 2k CCD camera, resulting in a pixel size of 39 nm.…”

Section: Methodsmentioning

confidence: 99%

In Situ Transmission X-Ray Microscopy of the Lead Sulfate Film Formation on Lead in Sulfuric Acid

Knehr

Eng

Chen‐Wiegart

et al. 2014

J. Electrochem. Soc.

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Transmission X-ray microscopy is utilized to monitor, in real time, the behavior of the PbSO 4 film that is formed on Pb in H 2 SO 4 . Images collected from the synchrotron x-rays are coupled with voltammetric data to study the initial formation, the resulting passivation, and the subsequent reduction of the film. It is concluded with support from quartz-crystal-microbalance experiments that the initial formation of PbSO 4 crystals occurs as a result of acidic corrosion. In addition, the film is shown to coalesce during the early stages of galvanostatic oxidation and to passivate as a result of morphological changes in the existing film. Finally, it is observed that the passivation process results in the formation of large PbSO 4 crystals with low area-to-volume ratios, which are difficult to reduce under both galvanostatic and potentiostatic conditions.

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“…We use newly developed fullfield transmission X-ray microscopy (TXM) at nanoscale resolution combined with X-ray absorption near-edge spectroscopy (XANES) at the National Synchrotron Light Source 28,29 . With this unique in operando TXM-XANES approach and the direct map of the inhomogeneous phase distribution for the multi-particle LiFePO 4 system, we disclose the rate dependent inhomogeneity behaviour, which provides more insight into developing high-rate battery technology.…”

mentioning

confidence: 99%

In operando tracking phase transformation evolution of lithium iron phosphate with hard X-ray microscopy

2014

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The delithiation reaction in lithium ion batteries is often accompanied by an electrochemically driven phase transformation process. Tracking the phase transformation process at nanoscale resolution during battery operation provides invaluable information for tailoring the kinetic barrier to optimize the physical and electrochemical properties of battery materials. Here, using hard X-ray microscopy-which offers nanoscale resolution and deep penetration of the material, and takes advantage of the elemental and chemical sensitivity-we develop an in operando approach to track the dynamic phase transformation process in olivine-type lithium iron phosphate at two size scales: a multiple-particle scale to reveal a rate-dependent intercalation pathway through the entire electrode and a single-particle scale to disclose the intraparticle two-phase coexistence mechanism. These findings uncover the underlying twophase mechanism on the intraparticle scale and the inhomogeneous charge distribution on the multiple-particle scale. This in operando approach opens up unique opportunities for advancing high-performance energy materials.

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Automated markerless full field hard x-ray microscopic tomography at sub-50 nm 3-dimension spatial resolution

Abstract: Hard Xray Focusing less than 50nm for Nanoscopy/spectroscopy AIP Conf.

Cited by 109 publications

References 21 publications

Quantified abundance of magnetofossils at the Paleocene–Eocene boundary from synchrotron-based transmission X-ray microscopy

Quantified abundance of magnetofossils at the Paleocene–Eocene boundary from synchrotron-based transmission X-ray microscopy

In Situ Transmission X-Ray Microscopy of the Lead Sulfate Film Formation on Lead in Sulfuric Acid

In operando tracking phase transformation evolution of lithium iron phosphate with hard X-ray microscopy

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