Search Menu
DOE PAGES title logo U.S. Department of Energy
Office of Scientific and Technical Information
Search Scholarly Publications

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

Journal Article · · Advanced Materials
ORCiD logo [1];  [1];  [1];  [1];  [1];  [1];  [1];  [1];  [1];  [2];  [3];  [1];  [1];  [4];  [5];  [5];  [6];  [1];  [5]
  1. Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
  2. Northwestern Univ., Evanston, IL (United States); SLAC National Accelerator Lab., Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL)
  3. Northwestern Univ., Evanston, IL (United States)
  4. Univ. de Lille (France). Centrale Lille Inst, Institut d’Electronique, de Microélectronique et de Nanotechnologie; Univ. Polytechnique des Hauts de France (UPHF), Lille (France). YNCREA-ISEN; Univ. Paul Sabatier, Toulouse (France). Centre Interuniversitaire de Recherche et d'Ingenierie des Materiaux (CIRIMAT); Reseau sur le Stockage Electrochimique de l'Energie (RS2E), Amiens (France)
  5. Univ. de Lille (France). Centrale Lille Inst, Institut d’Electronique, de Microélectronique et de Nanotechnologie; Univ. Polytechnique des Hauts de France (UPHF), Lille (France). YNCREA-ISEN; Reseau sur le Stockage Electrochimique de l'Energie (RS2E), Amiens (France)
  6. Univ. Paul Sabatier, Toulouse (France). Centre Interuniversitaire de Recherche et d'Ingenierie des Materiaux (CIRIMAT); Reseau sur le Stockage Electrochimique de l'Energie (RS2E), Amiens (France)
+ Show Author Affiliations

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.

Research Organization:
SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States); Argonne National Laboratory (ANL), Argonne, IL (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES); French National Research Agency (ANR)
Grant/Contract Number:
AC02-76SF00515; ANR-16-CE24-0012-01; AC02-06CH11357
OSTI ID:
1780990
Alternate ID(s):
OSTI ID: 1798169
Journal Information:
Advanced Materials, Vol. 33, Issue 21; ISSN 0935-9648
Publisher:
WileyCopyright Statement
Country of Publication:
United States
Language:
English

References (54)

Direct observations of liquid water formation at nano- and micro-scale in platinum group metal-free electrodes by operando X-ray computed tomography journal September 2018
Interlaced zone plate optics for hard X-ray imaging in the 10 nm range journal March 2017
Design, characterization, and performance of a hard x-ray transmission microscope at the National Synchrotron Light Source II 18-ID beamline journal May 2019
Tomosaic : efficient acquisition and reconstruction of teravoxel tomography data using limited-size synchrotron X-ray beams journal August 2018
Three-dimensional alteration of neurites in schizophrenia journal February 2019
Three-dimensional holey-graphene/niobia composite architectures for ultrahigh-rate energy storage journal May 2017
P05 imaging beamline at PETRA III: first results conference September 2014
Microstructural evolution and deformation behavior of Al-Cu alloys: A Transmission X-ray Microscopy (TXM) and micropillar compression study journal February 2018
Synthesis of T-Nb2O5 thin-films deposited by Atomic Layer Deposition for miniaturized electrochemical energy storage devices journal January 2019
Silicon-Microtube Scaffold Decorated with Anatase TiO 2 as a Negative Electrode for a 3D Litium-Ion Microbattery journal January 2014
High-rate electrochemical energy storage through Li+ intercalation pseudocapacitance journal April 2013
Oxygen vacancies enhance pseudocapacitive charge storage properties of MoO3−x journal December 2016
X-ray ptychographic computed tomography at 16 nm isotropic 3D resolution journal January 2014
Safe and recyclable lithium-ion capacitors using sacrificial organic lithium salt journal December 2017
Fabrication of hard x-ray zone plates with high aspect ratio using metal-assisted chemical etching
  • Li, Kenan; Wojcik, Michael J.; Divan, Ralu
  • Journal of Vacuum Science & Technology B, Nanotechnology and Microelectronics: Materials, Processing, Measurement, and Phenomena, Vol. 35, Issue 6 https://doi.org/10.1116/1.4991794
journal November 2017
Three-Dimensional Reconstruction and Analysis of All-Solid Li-Ion Battery Electrode Using Synchrotron Transmission X-ray Microscopy Tomography journal May 2018
Three-dimensional localization of nanoscale battery reactions using soft X-ray tomography journal March 2018
Self-spreading of the wetting ridge during stick-slip on a viscoelastic surface journal January 2017
Distributed Optimization and Statistical Learning via the Alternating Direction Method of Multipliers book January 2011
X-ray Imaging of Functional Three-Dimensional Nanostructures on Massive Substrates journal November 2019
Full-field microimaging with 8 keV X-rays achieves a spatial resolutions better than 20 nm journal January 2011
Imaging of 3D morphological evolution of nanoporous silicon anode in lithium ion battery by X-ray nano-tomography journal October 2018
Cramming more components onto integrated circuits, Reprinted from Electronics, volume 38, number 8, April 19, 1965, pp.114 ff. journal September 2006
Robust Locally Weighted Regression and Smoothing Scatterplots journal December 1979
SciPy 1.0: fundamental algorithms for scientific computing in Python journal February 2020
Definition and Estimation of Resolution in Single-Particle Reconstructions journal July 2010
Atomic Layer Deposition of Functional Layers for on Chip 3D Li-Ion All Solid State Microbattery journal October 2016
A High Resolution, Hard X-ray Bio-imaging Facility at SSRL journal June 2008
TomoPy: a framework for the analysis of synchrotron tomographic data journal August 2014
An ultrahigh-resolution soft x-ray microscope for quantitative analysis of chemically heterogeneous nanomaterials journal December 2020
Zone-Doubling Technique to Produce Ultrahigh-Resolution X-Ray Optics journal December 2007
Fourier shell correlation threshold criteria journal September 2005
The nanotomography endstation at the PETRA III Imaging Beamline journal March 2013
Automated markerless full field hard x-ray microscopic tomography at sub-50 nm 3-dimension spatial resolution journal April 2012
Design and Mechanisms of Asymmetric Supercapacitors journal August 2018
Distributed Optimization for Nonrigid Nano-Tomography journal January 2021
Tunable hard x-ray nanofocusing with Fresnel zone plates fabricated using deep etching journal January 2020
Pb 2+ –Calcite Interactions under Far-from-Equilibrium Conditions: Formation of Micropyramids and Pseudomorphic Growth of Cerussite journal January 2018
Mapping Three-dimensional Dissolution Rates of Calcite Microcrystals: Effects of Surface Curvature and Dissolved Metal Ions journal February 2019
Two-Frame Motion Estimation Based on Polynomial Expansion book January 2003
Trainable Weka Segmentation: a machine learning tool for microscopy pixel classification journal March 2017
Three dimensions, two microscopes, one code: Automatic differentiation for x-ray nanotomography beyond the depth of focus limit journal March 2020
Thick Binder-Free Electrodes for Li-Ion Battery Fabricated Using Templating Approach and Spark Plasma Sintering Reveals High Areal Capacity journal January 2018
Broadband X-ray full field microscopy at a superbend journal September 2009
The Mathematics of Computerized Tomography book January 2001
High Areal Energy 3D-Interdigitated Micro-Supercapacitors in Aqueous and Ionic Liquid Electrolytes journal August 2017
Condenser for Koehler-like illumination in transmission x-ray microscopes at undulator sources journal January 2006
Experimental evidence of reaction-induced fracturing during olivine carbonation: Fracturing During Olivine Carbonation journal September 2016
Soft X-ray microscopy at a spatial resolution better than 15 nm journal June 2005
Quantification and modeling of mechanical degradation in lithium-ion batteries based on nanoscale imaging journal June 2018
Exploring novel deformation mechanisms in aluminum–copper alloys using in situ 4D nanomechanical testing journal September 2019
Fast Electrochemical Storage Process in Sputtered Nb 2 O 5 Porous Thin Films journal April 2019
High-resolution non-destructive three-dimensional imaging of integrated circuits journal March 2017
The ASTRA Toolbox: A platform for advanced algorithm development in electron tomography journal October 2015

Similar Records

Related Subjects

36 MATERIALS SCIENCE
batteries
nanolithography
nanotomography
synchrotrons
transmission x-ray microscopy
x-rays