X-ray studies bridge the molecular and macro length scales during the emergence of CoO assemblies

Lukas Grote, Cecilia A. Zito, Kilian Frank, Ann-Christin Dippel, Patrick Reisbeck, Krzysztof Pitala, Kristina O. Kvashnina, Stephen Bauters, Blanka Detlefs, Oleh Ivashko, Pallavi Pandit, Matthias Rebber, Sani Y. Harouna-Mayer, Bert Nickel and Dorota Koziej ()
Additional contact information
Lukas Grote: Center for Hybrid Nanostructures
Cecilia A. Zito: Center for Hybrid Nanostructures
Kilian Frank: Ludwig-Maximilians-Universität München, Faculty of Physics and Center for NanoScience (CeNS)
Ann-Christin Dippel: Deutsches Elektronen-Synchrotron DESY
Patrick Reisbeck: Ludwig-Maximilians-Universität München, Faculty of Physics and Center for NanoScience (CeNS)
Krzysztof Pitala: AGH, University of Science and Technology, Faculty of Physics and Applied Computer Science
Kristina O. Kvashnina: The Rossendorf Beamline at the European Synchrotron Radiation Facility ESRF
Stephen Bauters: The Rossendorf Beamline at the European Synchrotron Radiation Facility ESRF
Blanka Detlefs: European Synchrotron Radiation Facility ESRF
Oleh Ivashko: Deutsches Elektronen-Synchrotron DESY
Pallavi Pandit: Deutsches Elektronen-Synchrotron DESY
Matthias Rebber: Center for Hybrid Nanostructures
Sani Y. Harouna-Mayer: Center for Hybrid Nanostructures
Bert Nickel: Ludwig-Maximilians-Universität München, Faculty of Physics and Center for NanoScience (CeNS)
Dorota Koziej: Center for Hybrid Nanostructures

Nature Communications, 2021, vol. 12, issue 1, 1-12

Abstract: Abstract The key to fabricating complex, hierarchical materials is the control of chemical reactions at various length scales. To this end, the classical model of nucleation and growth fails to provide sufficient information. Here, we illustrate how modern X-ray spectroscopic and scattering in situ studies bridge the molecular- and macro- length scales for assemblies of polyhedrally shaped CoO nanocrystals. Utilizing high energy-resolution fluorescence-detected X-ray absorption spectroscopy, we directly access the molecular level of the nanomaterial synthesis. We reveal that initially Co(acac)3 rapidly reduces to square-planar Co(acac)2 and coordinates to two solvent molecules. Combining atomic pair distribution functions and small-angle X-ray scattering we observe that, unlike a classical nucleation and growth mechanism, nuclei as small as 2 nm assemble into superstructures of 20 nm. The individual nanoparticles and assemblies continue growing at a similar pace. The final spherical assemblies are smaller than 100 nm, while the nanoparticles reach a size of 6 nm and adopt various polyhedral, edgy shapes. Our work thus provides a comprehensive perspective on the emergence of nano-assemblies in solution.

Date: 2021
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DOI: 10.1038/s41467-021-24557-z

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