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

Shapiro, David A.; Babin, Sergey; Celestre, Richard; Chao, Weilun; Conley, Ray; Denes, P.; Enders, Bjoern; Enfedaque, Pablo; James, Susan; Joseph, J.; Krishnan, Harinarayan; Marchesini, Stefano; Muriki, Krishna; Nowrouzi, Kasra; Oh, Sharon; Padmore, Howard; Warwick, Tony; Yang, Luyi; Yashchuk, Valeriy V.; Yu, Young‐Sang; Zhao, Jiangtao

doi:10.1126/sciadv.abc4904

Cited by 58 publications

(44 citation statements)

References 42 publications

(57 reference statements)

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“…The reactor temperature was fixed at 250 °C. A total of 1000 deposition cycles were achieved to deposit 58…”

Section: Supporting Informationmentioning

confidence: 99%

“…The reactor temperature was fixed at 250 °C. A total of 1000 deposition cycles were achieved to deposit 58 Methods for Planar and 3D Electrochemical Testing: Electrochemical impedance spectroscopy (EIS) measurements were conducted with a Biologic VMP3 equipment over a frequency range from 10 Hz up to 500 KHz on T-Nb 2 O 5 films. Cyclic voltammetry (CV) and galvanostatic charge and discharge plots were investigated on the VMP3 potentiostat/ galvanostat equipment using a homemade Teflon like a flat cell with Li metal used as the counter and reference electrode.…”

Section: (10 Of 11)mentioning

confidence: 99%

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Fast X‐ray Nanotomography with Sub‐10 nm Resolution as a Powerful Imaging Tool for Nanotechnology and Energy Storage Applications

et al. 2021

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nano-computed-tomography (nano-CT). They have emerged in many synchrotrons worldwide [1][2][3][4][5][6] and have been widely used in energy science where typical spatial resolutions of 30-60 nm and respective field of view (FOV) of about 40-70 μm are ideal for the ex situ or in situ characterization of different type of lithium-ion batteries. [7][8][9][10][11][12] However, they can be also utilized to characterize any type of materials like alloys, [13,14] rocks, [15] single minerals in solution, [16,17] polymers, [18] liquids, [19] biological tissues, [20] etc. While 19 nm spatial resolution has been reported in 2D on gold test patterns with long exposure, [21,22] existing TXMs operating with high brightness synchrotron sources currently provide a maximum resolution of 30 nm. [23] Projection microscopy, another full-field nano-CT technique, has the potential of achieving sub-20 nm spatial resolution. However, the best 3D resolution reported so far is 55 nm. [24] The constant and rapid development of manufactured nanomaterials and the societal and economic stakes associated with them are important drivers for improving the resolving power of X-ray microscopes.In the last decade, transmission X-ray microscopes (TXMs) have come into operation in most of the synchrotrons worldwide. They have proven to be outstanding tools for non-invasive ex and in situ 3D characterization of materials at the nanoscale across varying range of scientific applications. However, their spatial resolution has not improved in many years, while newly developed functional materials and microdevices with enhanced performances exhibit nanostructures always finer. Here, optomechanical breakthroughs leading to fast 3D tomographic acquisitions (85 min) with sub-10 nm spatial resolution, narrowing the gap between X-ray and electron microscopy, are reported. These new achievements are first validated with 3D characterizations of nanolithography objects corresponding to ultrahigh-aspect-ratio hard X-ray zone plates. Then, this powerful technique is used to investigate the morphology and conformality of nanometer-thick film electrodes synthesized by atomic layer deposition and magnetron sputtering deposition methods on 3D silicon scaffolds for electrochemical energy storage applications.

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“…The reactor temperature was fixed at 250 °C. A total of 1000 deposition cycles were achieved to deposit 58…”

Section: Supporting Informationmentioning

confidence: 99%

Section: (10 Of 11)mentioning

confidence: 99%

Fast X‐ray Nanotomography with Sub‐10 nm Resolution as a Powerful Imaging Tool for Nanotechnology and Energy Storage Applications

et al. 2021

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“…For instance, sub-10 nm resolutions are now achieved by cryo-soft X-ray ptychography. [190] For EELS, recent advances concerning STEM monochromators and direct detectors have increased the energy resolution below 5 meV together with the sensitivity of the analysis. [191] Concerning 3D-imaging, FIB-SEM is undeniably the method of choice to image very large volumes, up to 10 7 µm 3 with a high isotropic resolution (voxel sizes of 8 × 8 × 8 nm) compatible with the imaging of the smallest cellular organelles.…”

Section: Perspectivesmentioning

confidence: 99%

“…For instance, sub‐10 nm resolutions are now achieved by cryo‐soft X‐ray ptychography. [ 190 ] For EELS, recent advances concerning STEM monochromators and direct detectors have increased the energy resolution below 5 meV together with the sensitivity of the analysis. [ 191 ]…”

Section: Perspectivesmentioning

confidence: 99%

Deciphering the Structure and Chemical Composition of Drug Nanocarriers: From Bulk Approaches to Individual Nanoparticle Characterization

Chaupard

Frutos

Gref

2021

Part & Part Syst Charact

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payload's pharmacokinetics and contributed to achieve the desired pharmacological response at the target. They are now widely exploited for therapeutic purposes, including the treatment of severe diseases such as cancer and infections. [1] A plethora of natural and synthetic materials have been engineered at a nanoscopic level and explored for drug delivery (Figure 1). Liposomes, the first nanotechnology-based drug delivery system, were discovered early in the 1960s. [2] The first Food and Drug Administration (FDA)-approved nanotechnology was the liposomal Doxil formulation designed for the treatment of Kaposi's sarcoma and since then, more than twenty liposomal and lipid-based formulations have been approved by regular authorities. [3] Many other types of drug nanocarriers have been developed, including polymeric, hybrid or metal nanoparticles (NPs), nanogels, dendrimers, quantum dots, carbon nanotubes (CNTs), and micelles (Figure 1). Several nanotechnologies containing an active molecule or a drug combination, such as Onpattro and Vyxeos, were FDA-approved in recent years, demonstrating the potential of nanomedicine and the growing interest in this field. [4,5] Moreover, the FDA-approved NP-based vaccines represent a giant step in the fight against the COVID-19 pandemic. [6] Nowadays, a large variety of materials is used to prepare drug nanocarriers: i) organic compounds (lipids, synthetic or natural polymers, biomolecules); ii) inorganic materials (silica, carbon networks, metals, or metal oxides) and iii) hybrid organic-inorganic networks combining the properties of both their organic and inorganic counterparts. Generally, drug nanocarriers have a core-shell structure: i) the cores incorporate the drugs and release them in a controlled manner and ii) the shells govern the interactions with the living media (control protein adsorption, avoid recognition by the immune system, allow targeting diseased tissues and organs, confer bio-adhesion properties). Organic compounds remain the most employed materials for drug incorporation and for engineering multifunctional shells. Additionally, the presence of metals in drug nanocarriers' composition offers new functionalities, such as antibacterial or antifungal properties, [7] radioenhancement [8] or imaging abilities for personalized therapies. [9] More recently, nanoscale hybrid metal-organic frameworks (MOFs) emerged as versatile Drug nanocarriers (NCs) with sizes usually below 200 nm are gaining increasing interest in the treatment of severe diseases such as cancer and infections. Characterization methods to investigate the morphology and physicochemical properties of multifunctional NCs are key in their optimization and in the study of their in vitro and in vivo fate. Whereas a variety of methods has been developed to characterize "bulk" NCs in suspension, the scope of this review is to describe the different approaches for the NC characterization on an individual basis, for which fewer techniques are available. The accent is put on methods devoid of labelling, whi...

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“…ptychographic CDI, with both a wide field of view and a high spatial resolution, is applicable to various samples (Rodenburg et al, 2007;Pfeiffer, 2018). Thus far, ptychographic CDI measurement systems have been developed at synchrotron radiation facilities, especially for use in the soft (Shapiro et al, 2020) and hard (Takahashi et al, 2011;Holler et al, 2014;Deng et al, 2019;Schropp et al, 2020) X-ray regions, and have been applied to the structural imaging of biological specimens (Deng et al, 2015) and functional materials (Ihli et al, 2020). Ptychographic CDI has also been extended to the visualization of chemical states using X-ray absorption edges (Shapiro et al, 2014;Hirose et al, 2018), which is called spectro-ptychography or the ptychographic X-ray absorption fine structure (XAFS) method.…”

Section: Introductionmentioning

confidence: 99%

Development and application of a tender X-ray ptychographic coherent diffraction imaging system on BL27SU at SPring-8

Abe¹,

Kaneko²,

Ishiguro³

et al. 2021

J Synchrotron Rad

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Ptychographic coherent diffraction imaging (CDI) allows the visualization of both the structure and chemical state of materials on the nanoscale, and has been developed for use in the soft and hard X-ray regions. In this study, a ptychographic CDI system with pinhole or Fresnel zone-plate optics for use in the tender X-ray region (2–5 keV) was developed on beamline BL27SU at SPring-8, in which high-precision pinholes optimized for the tender energy range were used to obtain diffraction intensity patterns with a low background, and a temperature stabilization system was developed to reduce the drift of the sample position. A ptychography measurement of a 200 nm thick tantalum test chart was performed at an incident X-ray energy of 2.500 keV, and the phase image of the test chart was successfully reconstructed with approximately 50 nm resolution. As an application to practical materials, a sulfur polymer material was measured in the range of 2.465 to 2.500 keV including the sulfur K absorption edge, and the phase and absorption images were successfully reconstructed and the nanoscale absorption/phase spectra were derived from images at multiple energies. In 3 GeV synchrotron radiation facilities with a low-emittance storage ring, the use of the present system will allow the visualization on the nanoscale of the chemical states of various light elements that play important roles in materials science, biology and environmental science.

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

Cited by 58 publications

References 42 publications

Fast X‐ray Nanotomography with Sub‐10 nm Resolution as a Powerful Imaging Tool for Nanotechnology and Energy Storage Applications

Fast X‐ray Nanotomography with Sub‐10 nm Resolution as a Powerful Imaging Tool for Nanotechnology and Energy Storage Applications

Deciphering the Structure and Chemical Composition of Drug Nanocarriers: From Bulk Approaches to Individual Nanoparticle Characterization

Development and application of a tender X-ray ptychographic coherent diffraction imaging system on BL27SU at SPring-8

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