Near-edge X-ray refraction fine structure microscopy

Farmand, Maryam; Celestre, Richard; Denes, P.; Kilcoyne, A. L. D.; Marchesini, Stefano; Padmore, H. A.; Tyliszczak, Tolek; Warwick, Tony; Shi, Xiaowen; Lee, James; Yu, Yi; Cabana, Jordi; Joseph, J.; Krishnan, Harinarayan; Perciano, Talita; Maia, Filipe R. N. C.; Shapiro, David A.

doi:10.1063/1.4975377

Cited by 43 publications

(23 citation statements)

References 30 publications

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“…At each energy point and tilt angle, the camera background signal is measured with the beamline shutter closed, and the background is removed in subsequent data processing. 31,55 Ptychographic images were reconstructed using 500 iterations of the relaxed averaged alternating reflection reconstruction algorithm implemented in the SHARP ptychography code developed by the Center for Applied Mathematics for Energy Research Applications. 66 MethodsFourier Ring Correlation.…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

Four-Dimensional Imaging of ZnO-Coated Alumina Aerogels by Scanning Transmission X-ray Microscopy and Ptychographic Tomography

Zhu

Shapiro

et al. 2018

J. Phys. Chem. C

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Functional porous materials are of increasing importance in energy conversion and catalysis. Improved analysis is needed to guide optimization. Four-dimensional (4D) imaging [chemical mapping in three-dimensional (3D) by spectro-tomography] of an Al 2 O 3 aerogel coated with ZnO by atomic layer deposition was performed using soft X-ray ptychography at the Zn L-edge. A two-dimensional spatial resolution of 14(2) nm was achieved. Visualizations of the 3D chemical structure are provided. The degree of ZnO coverage of the surface of the Al 2 O 3 aerogel framework in two different samples was estimated and found to be both thicker and less homogeneous than expected. Other analyses of the 4D results, including the degree of contact between Al 2 O 3 and ZnO, were extracted from the reconstructed 3D data. This pioneering soft X-ray spectro-ptycho-tomography study will anchor further studies of functional porous materials.

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Section: ■ Experimental Sectionmentioning

confidence: 99%

Four-Dimensional Imaging of ZnO-Coated Alumina Aerogels by Scanning Transmission X-ray Microscopy and Ptychographic Tomography

Zhu

Shapiro

et al. 2018

J. Phys. Chem. C

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“…The FRC calculation is explained in detail in the Supplementary Materials. The quantity analyzed is the scattering contrast,

, where

and

are the reconstructed maps of the optical density and phase and is similarly linear with material thickness ( 22 ). Figure 1B shows that the FRC maintains a high value out to the full NA, which reaches a full-period spatial frequency of 0.17 nm −1 , corresponding to 6-nm oscillation periods.…”

Section: Resultsmentioning

confidence: 99%

“…The overall chemical maps are in qualitative agreement, but the ptychographic chemical map displays nanoscale chemical phases in the particle interior, which are not visible in conventional imaging mode. In this case, the chemical maps are obtained with a linear combination of reference spectra measured from nanoparticles of pure materials ( 22 ); thus, they represent quantitative composition with red being FePO 4 and green being LiFePO 4 . The radiation dose delivered to the sample is estimated in fig.…”

Section: Resultsmentioning

confidence: 99%

An ultrahigh-resolution soft x-ray microscope for quantitative analysis of chemically heterogeneous nanomaterials

et al. 2020

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The analysis of chemical states and morphology in nanomaterials is central to many areas of science. We address this need with an ultrahigh-resolution scanning transmission soft x-ray microscope. Our instrument provides multiple analysis tools in a compact assembly and can achieve few-nanometer spatial resolution and high chemical sensitivity via x-ray ptychography and conventional scanning microscopy. A novel scanning mechanism, coupled to advanced x-ray detectors, a high-brightness x-ray source, and high-performance computing for analysis provide a revolutionary step forward in terms of imaging speed and resolution. We present x-ray microscopy with 8-nm full-period spatial resolution and use this capability in conjunction with operando sample environments and cryogenic imaging, which are now routinely available. Our multimodal approach will find wide use across many fields of science and facilitate correlative analysis of materials with other types of probes.

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“…However, as this work has demonstrated, one major benefit of X-ray linear dichroic ptychography is that strong polarization-dependent phase contrast is also available when imaged at the off-resonant energy. Benefits of off-resonance, dose-efficient imaging have been reported (48,55), in which the large phase shifts and strong energy dependence near atomic resonances play an important role in achieving high spatial resolution. It was observed that the maximum resolution peak falls at the energy of the most negative phase shift relative to vacuum, which yields the maximum phase…”

Section: Discussionmentioning

confidence: 99%

X-ray linear dichroic ptychography

Zhou

Rana

et al. 2021

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

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Biominerals such as seashells, coral skeletons, bone, and tooth enamel are optically anisotropic crystalline materials with unique nanoscale and microscale organization that translates into exceptional macroscopic mechanical properties, providing inspiration for engineering new and superior biomimetic structures. Using Seriatopora aculeata coral skeleton as a model, here, we experimentally demonstrate X-ray linear dichroic ptychography and map the c-axis orientations of the aragonite (CaCO3) crystals. Linear dichroic phase imaging at the oxygen K-edge energy shows strong polarization-dependent contrast and reveals the presence of both narrow (<35°) and wide (>35°) c-axis angular spread in the coral samples. These X-ray ptychography results are corroborated by four-dimensional (4D) scanning transmission electron microscopy (STEM) on the same samples. Evidence of co-oriented, but disconnected, corallite subdomains indicates jagged crystal boundaries consistent with formation by amorphous nanoparticle attachment. We expect that the combination of X-ray linear dichroic ptychography and 4D STEM could be an important multimodal tool to study nano-crystallites, interfaces, nucleation, and mineral growth of optically anisotropic materials at multiple length scales.

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Near-edge X-ray refraction fine structure microscopy

Abstract: See supplementary material for a brief description of the experimental system and data analysis protocol. Soft X-ray ptychographic microscopy was carried out at beamline 5.3.2.

Cited by 43 publications

References 30 publications

Four-Dimensional Imaging of ZnO-Coated Alumina Aerogels by Scanning Transmission X-ray Microscopy and Ptychographic Tomography

Four-Dimensional Imaging of ZnO-Coated Alumina Aerogels by Scanning Transmission X-ray Microscopy and Ptychographic Tomography

An ultrahigh-resolution soft x-ray microscope for quantitative analysis of chemically heterogeneous nanomaterials

X-ray linear dichroic ptychography

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