Four-Dimensional Imaging of ZnO-Coated Alumina Aerogels by Scanning Transmission X-ray Microscopy and Ptychographic Tomography
Abstract
Functional porous materials are of mounting significance 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 Al2O3 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 Al2O3 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 Al2O3 and ZnO, were extracted from the reconstructed 3D data. This pioneering soft X-ray spectro-ptycho-tomography research will anchor further studies of functional porous materials.
- Authors:
-
- Brockhouse Institute for Materials Research, McMaster University, Hamilton, Ontario L8S 4M1 Canada
- Advanced Light Source, Berkeley Lab, Berkeley, California 94720, United States
- Lawrence Livermore National Laboratory, Livermore, California 94550 United States
- Publication Date:
- Research Org.:
- Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Materials Sciences & Engineering Division; Natural Sciences and Engineering Research Council of Canada (NSERC); Canadian Institutes of Health Research
- OSTI Identifier:
- 1656474
- Alternate Identifier(s):
- OSTI ID: 1544493
- Report Number(s):
- LLNL-JRNL-748333
Journal ID: ISSN 1932-7447; ark:/13030/qt9s13x766
- Grant/Contract Number:
- AC02-05CH11231; AC52-07NA27344
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Journal of Physical Chemistry. C
- Additional Journal Information:
- Journal Volume: 122; Journal Issue: 44; Journal ID: ISSN 1932-7447
- Publisher:
- American Chemical Society
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 77 NANOSCIENCE AND NANOTECHNOLOGY; 36 MATERIALS SCIENCE; X-rays; oxides; atomic layer deposition; aerogels; materlais
Citation Formats
Wu, Juan, Zhu, Xiaohui, Shapiro, David A., Lee, Jonathan I., Van Buuren, Tony, Biener, Monika M., Gammon, Stuart A., Li, Tian T., Baumann, Theodore F., and Hitchcock, Adam P. Four-Dimensional Imaging of ZnO-Coated Alumina Aerogels by Scanning Transmission X-ray Microscopy and Ptychographic Tomography. United States: N. p., 2018.
Web. doi:10.1021/acs.jpcc.8b07363.
Wu, Juan, Zhu, Xiaohui, Shapiro, David A., Lee, Jonathan I., Van Buuren, Tony, Biener, Monika M., Gammon, Stuart A., Li, Tian T., Baumann, Theodore F., & Hitchcock, Adam P. Four-Dimensional Imaging of ZnO-Coated Alumina Aerogels by Scanning Transmission X-ray Microscopy and Ptychographic Tomography. United States. https://doi.org/10.1021/acs.jpcc.8b07363
Wu, Juan, Zhu, Xiaohui, Shapiro, David A., Lee, Jonathan I., Van Buuren, Tony, Biener, Monika M., Gammon, Stuart A., Li, Tian T., Baumann, Theodore F., and Hitchcock, Adam P. Tue .
"Four-Dimensional Imaging of ZnO-Coated Alumina Aerogels by Scanning Transmission X-ray Microscopy and Ptychographic Tomography". United States. https://doi.org/10.1021/acs.jpcc.8b07363. https://www.osti.gov/servlets/purl/1656474.
@article{osti_1656474,
title = {Four-Dimensional Imaging of ZnO-Coated Alumina Aerogels by Scanning Transmission X-ray Microscopy and Ptychographic Tomography},
author = {Wu, Juan and Zhu, Xiaohui and Shapiro, David A. and Lee, Jonathan I. and Van Buuren, Tony and Biener, Monika M. and Gammon, Stuart A. and Li, Tian T. and Baumann, Theodore F. and Hitchcock, Adam P.},
abstractNote = {Functional porous materials are of mounting significance 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 Al2O3 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 Al2O3 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 Al2O3 and ZnO, were extracted from the reconstructed 3D data. This pioneering soft X-ray spectro-ptycho-tomography research will anchor further studies of functional porous materials.},
doi = {10.1021/acs.jpcc.8b07363},
journal = {Journal of Physical Chemistry. C},
number = 44,
volume = 122,
place = {United States},
year = {Tue Oct 16 00:00:00 EDT 2018},
month = {Tue Oct 16 00:00:00 EDT 2018}
}
Web of Science
Figures / Tables:
Works referenced in this record:
Advanced carbon aerogels for energy applications
journal, January 2011
- Biener, Juergen; Stadermann, Michael; Suss, Matthew
- Energy & Environmental Science, Vol. 4, Issue 3, p. 656-667
Quantitative Phase Composition of TiO 2 -Coated Nanoporous Au Monoliths by X-ray Absorption Spectroscopy and Correlations to Catalytic Behavior
journal, February 2014
- Bagge-Hansen, Michael; Wichmann, Andre; Wittstock, Arne
- The Journal of Physical Chemistry C, Vol. 118, Issue 8
Nanoporous Gold Disks Functionalized with Stabilized G-Quadruplex Moieties for Sensing Small Molecules
journal, October 2016
- Qiu, Suyan; Zhao, Fusheng; Zenasni, Oussama
- ACS Applied Materials & Interfaces, Vol. 8, Issue 44
ALD Functionalized Nanoporous Gold: Thermal Stability, Mechanical Properties, and Catalytic Activity
journal, August 2011
- Biener, Monika M.; Biener, Juergen; Wichmann, Andre
- Nano Letters, Vol. 11, Issue 8
Structural Optimization of 3D Porous Electrodes for High-Rate Performance Lithium Ion Batteries
journal, December 2014
- Ye, Jianchao; Baumgaertel, Andreas C.; Wang, Y. Morris
- ACS Nano, Vol. 9, Issue 2
Atomic Layer Deposition-Derived Ultra-Low-Density Composite Bulk Materials with Deterministic Density and Composition
journal, December 2013
- Biener, Monika M.; Biener, Juergen; Wang, Yinmin M.
- ACS Applied Materials & Interfaces, Vol. 5, Issue 24
Nanoporous Metal Enhanced Catalytic Activities of Amorphous Molybdenum Sulfide for High-Efficiency Hydrogen Production
journal, February 2014
- Ge, Xingbo; Chen, Luyang; Zhang, Ling
- Advanced Materials, Vol. 26, Issue 19
Galvanic exchange-formed ultra-low Pt loading on synthesized unique porous Ag-Pd nanotubes for increased active sites toward oxygen reduction reaction
journal, February 2018
- Zhao, Zhi Liang; Wang, Qi; Zhang, Lian Ying
- Electrochimica Acta, Vol. 263
Electrodeposition of porous graphene networks on nickel foams as supercapacitor electrodes with high capacitance and remarkable cyclic stability
journal, January 2014
- Yang, Shaolin; Deng, Bingchen; Ge, Ruijing
- Nanoscale Research Letters, Vol. 9, Issue 1
Ultralow Loading Pt Nanocatalysts Prepared by Atomic Layer Deposition on Carbon Aerogels
journal, August 2008
- King, Jeffrey S.; Wittstock, Arne; Biener, Juergen
- Nano Letters, Vol. 8, Issue 8, p. 2405-2409
3D Visualization of the Iron Oxidation State in FeO/Fe 3 O 4 Core–Shell Nanocubes from Electron Energy Loss Tomography
journal, July 2016
- Torruella, Pau; Arenal, Raúl; de la Peña, Francisco
- Nano Letters, Vol. 16, Issue 8
Three-Dimensional Valency Mapping in Ceria Nanocrystals
journal, October 2014
- Goris, Bart; Turner, Stuart; Bals, Sara
- ACS Nano, Vol. 8, Issue 10
STEM-EDX tomography of bimetallic nanoparticles: A methodological investigation
journal, March 2016
- Slater, Thomas J. A.; Janssen, Arne; Camargo, Pedro H. C.
- Ultramicroscopy, Vol. 162
Four-dimensional STEM-EELS: Enabling nano-scale chemical tomography
journal, March 2009
- Jarausch, Konrad; Thomas, Paul; Leonard, Donovan N.
- Ultramicroscopy, Vol. 109, Issue 4
Biomineralization at Titanium Revealed by Correlative 4D Tomographic and Spectroscopic Methods
journal, May 2018
- Wang, Xiaoyue; Langelier, Brian; Shah, Furqan A.
- Advanced Materials Interfaces, Vol. 5, Issue 14
Soft X-ray spectromicroscopy and ptychography
journal, April 2015
- Hitchcock, Adam P.
- Journal of Electron Spectroscopy and Related Phenomena, Vol. 200
Quantitative Evaluation of Radiation Damage to Polyethylene Terephthalate by Soft X-rays and High-energy Electrons
journal, February 2009
- Wang, Jian; Botton, Gianluigi A.; West, Marcia M.
- The Journal of Physical Chemistry B, Vol. 113, Issue 7
Evaluating focused ion beam and ultramicrotome sample preparation for analytical microscopies of the cathode layer of a polymer electrolyte membrane fuel cell
journal, April 2016
- de A. Melo, Lis G.; Hitchcock, Adam P.; Berejnov, Viatcheslav
- Journal of Power Sources, Vol. 312
Individual Titanate Nanoribbons Studied by 3D-Resolved Polarization Dependent X-ray Absorption Spectra Measured with Scanning Transmission X-ray Microscopy
journal, October 2015
- Zhu, Xiaohui; Hitchcock, Adam P.; Bittencourt, Carla
- The Journal of Physical Chemistry C, Vol. 119, Issue 42
Correlative Nanoscale 3D Imaging of Structure and Composition in Extended Objects
journal, November 2012
- Xu, Feng; Helfen, Lukas; Suhonen, Heikki
- PLoS ONE, Vol. 7, Issue 11
3d chemical mapping of toners by serial section scanning transmission X-ray microscopy
journal, March 2003
- Hitchcock, A. P.; Araki, T.; Ikeura-Sekiguchi, H.
- Journal de Physique IV (Proceedings), Vol. 104
Ultrahigh-Resolution X-ray Tomography
journal, November 1994
- Haddad, W. S.; McNulty, I.; Trebes, J. E.
- Science, Vol. 266, Issue 5188
Chemical composition mapping with nanometre resolution by soft X-ray microscopy
journal, September 2014
- Shapiro, David A.; Yu, Young-Sang; Tyliszczak, Tolek
- Nature Photonics, Vol. 8, Issue 10
Measuring spectroscopy and magnetism of extracted and intracellular magnetosomes using soft X-ray ptychography
journal, December 2016
- Zhu, Xiaohui; Hitchcock, Adam P.; Bazylinski, Dennis A.
- Proceedings of the National Academy of Sciences, Vol. 113, Issue 51
Beyond crystallography: Diffractive imaging using coherent x-ray light sources
journal, April 2015
- Miao, J.; Ishikawa, T.; Robinson, I. K.
- Science, Vol. 348, Issue 6234
Probe retrieval in ptychographic coherent diffractive imaging
journal, March 2009
- Thibault, Pierre; Dierolf, Martin; Bunk, Oliver
- Ultramicroscopy, Vol. 109, Issue 4
X-ray ptychographic computed tomography at 16 nm isotropic 3D resolution
journal, January 2014
- Holler, M.; Diaz, A.; Guizar-Sicairos, M.
- Scientific Reports, Vol. 4, Issue 1
Quantitative biological imaging by ptychographic x-ray diffraction microscopy
journal, December 2009
- Giewekemeyer, K.; Thibault, P.; Kalbfleisch, S.
- Proceedings of the National Academy of Sciences, Vol. 107, Issue 2
Soft X‐ray Ptychographic Imaging and Morphological Quantification of Calcium Silicate Hydrates (C–S–H)
journal, August 2015
- Bae, Sungchul; Taylor, Rae; Shapiro, David
- Journal of the American Ceramic Society, Vol. 98, Issue 12
Nanoscale Chemical Imaging of an Individual Catalyst Particle with Soft X-ray Ptychography
journal, February 2016
- Wise, Anna M.; Weker, Johanna Nelson; Kalirai, Sam
- ACS Catalysis, Vol. 6, Issue 4
Dependence on Crystal Size of the Nanoscale Chemical Phase Distribution and Fracture in Li x FePO 4
journal, June 2015
- Yu, Young-Sang; Kim, Chunjoong; Shapiro, David A.
- Nano Letters, Vol. 15, Issue 7
Progress in Soft X-ray Microscopy Characterization of PEM Fuel Cell Catalyst Layers
journal, July 2016
- Hitchcock, A. P.; Wu, J.; Lee, V.
- Microscopy and Microanalysis, Vol. 22, Issue S3
(Plenary) Doing More with Less: Challenges for Catalyst Layer Design
journal, August 2016
- Putz, A. M. V.; Susac, D.; Berejnov, V.
- ECS Transactions, Vol. 75, Issue 14
Three-dimensional localization of nanoscale battery reactions using soft X-ray tomography
journal, March 2018
- Yu, Young-Sang; Farmand, Maryam; Kim, Chunjoong
- Nature Communications, Vol. 9, Issue 1
Electronic Structures of Well-Aligned Er-Doped ZnO Nanorod Arrays
journal, December 2011
- Chen, Cheng-Ying; Lai, Kun-Yu; Lo, Jian-Wei
- Journal of Nanoscience and Nanotechnology, Vol. 11, Issue 12
Influence of the oxygen partial pressure and post-deposition annealing on the structure and optical properties of ZnO films grown by dc magnetron sputtering at room temperature
journal, December 2011
- Yuste, M.; Escobar Galindo, R.; Caretti, I.
- Journal of Physics D: Applied Physics, Vol. 45, Issue 2
N Doping to ZnO Nanorods for Photoelectrochemical Water Splitting under Visible Light: Engineered Impurity Distribution and Terraced Band Structure
journal, August 2015
- Wang, Meng; Ren, Feng; Zhou, Jigang
- Scientific Reports, Vol. 5, Issue 1
Spectroscopic evidence for limited carrier hopping interaction in amorphous ZnO thin film
journal, December 2009
- Cho, Deok-Yong; Kim, Jeong Hwan; Na, Kwang Duk
- Applied Physics Letters, Vol. 95, Issue 26
Quantification of aluminium coordinations in alumina and silica–alumina by Al K-edge XANES
journal, January 2001
- Kato, Yuko; Shimizu, Ken-ichi; Matsushita, Norimitsu
- Physical Chemistry Chemical Physics, Vol. 3, Issue 10
Full multiple-scattering calculations on silicates and oxides at the Al K edge
journal, May 1996
- Cabaret, Delphine; Sainctavit, Philippe; Ildefonse, Philippe
- Journal of Physics: Condensed Matter, Vol. 8, Issue 20
X-Ray Interactions: Photoabsorption, Scattering, Transmission, and Reflection at E = 50-30,000 eV, Z = 1-92
journal, July 1993
- Henke, B. L.; Gullikson, E. M.; Davis, J. C.
- Atomic Data and Nuclear Data Tables, Vol. 54, Issue 2, p. 181-342
Nanoscale Morphological and Chemical Changes of High Voltage Lithium–Manganese Rich NMC Composite Cathodes with Cycling
journal, July 2014
- Yang, Feifei; Liu, Yijin; Martha, Surendra K.
- Nano Letters, Vol. 14, Issue 8
Near-edge X-ray refraction fine structure microscopy
journal, February 2017
- Farmand, Maryam; Celestre, Richard; Denes, Peter
- Applied Physics Letters, Vol. 110, Issue 6
Fourier ring correlation as a resolution criterion for super-resolution microscopy
journal, September 2013
- Banterle, Niccolò; Bui, Khanh Huy; Lemke, Edward A.
- Journal of Structural Biology, Vol. 183, Issue 3
BoneJ: Free and extensible bone image analysis in ImageJ
journal, December 2010
- Doube, Michael; Kłosowski, Michał M.; Arganda-Carreras, Ignacio
- Bone, Vol. 47, Issue 6
Nucleation and Growth Modes of ALD ZnO
journal, October 2012
- Baji, Zsófia; Lábadi, Zoltán; Horváth, Zsolt E.
- Crystal Growth & Design, Vol. 12, Issue 11
Soft X-ray spectromicroscopy beamline at the CLS: Commissioning results
journal, November 2007
- Kaznatcheev, K. V.; Karunakaran, Ch.; Lanke, U. D.
- Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 582, Issue 1
Soft X-ray spectroscopy from image sequences with sub-100 nm spatial resolution
journal, February 2000
- Jacobsen,
- Journal of Microscopy, Vol. 197, Issue 2
Ptychographic Imaging of Nano-Materials at the Advanced Light Source with the Nanosurveyor Instrument
journal, June 2017
- Shapiro, David A.; Celestre, Rich; Denes, Peter
- Journal of Physics: Conference Series, Vol. 849
A pyramid approach to subpixel registration based on intensity
journal, January 1998
- Thevenaz, P.; Ruttimann, U. E.; Unser, M.
- IEEE Transactions on Image Processing, Vol. 7, Issue 1
Works referencing / citing this record:
Oxygen-diffusion-driven oxidation behavior and tracking areas visualized by X-ray spectro-ptychography with unsupervised learning
journal, April 2019
- Hirose, Makoto; Ishiguro, Nozomu; Shimomura, Kei
- Communications Chemistry, Vol. 2, Issue 1
Figures / Tables found in this record: