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Oliveira et al., Expanding the Mechanochemical Toolbox_XAS-XRD.pdf (1.51 MB)
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Expanding the Mechanochemical Toolbox: Combining X-Ray Absorption Spectroscopy and Scattering for in Situ Time-Resolved Monitoring of Gold Nanoparticle Mechanosynthesis

preprint
submitted on 12.05.2020 and posted on 15.05.2020 by Paulo F M de Oliveira, Adam Michalchuk, Ana de Oliveira Guilherme Buzanich, Ralf Bienert, Roberto M. Torresi, Pedro H. C. Camargo, Franziska Emmerling
The development of time-resolved in situ approaches for monitoring mechanochemical
transformations has revolutionized the field of mechanochemistry. Currently, the established in
situ approaches greatly limit the scope of investigations that are possible. Here we develop a new
approach to simultaneously follow the evolution of bulk atomic and electronic structure during a
mechanochemical synthesis. This is achieved by coupling two complementary synchrotron-based
X-ray methods: X-ray absorption spectroscopy and X-ray diffraction. We apply this method to
investigate the bottom-up mechanosynthesis of technologically important Au nanoparticles in the
presence of three different reducing agents. Moreover, we demonstrate how X-ray absorption
spectroscopy offers unprecedented insight into the early stage generation of growth species (e.g.
monomers and clusters), which lead to the subsequent formation of nanoparticles. These
processes are beyond the detection capabilities of diffraction methods. The approach is general,
and not limited to monitoring NP mechanosynthesis. This combined X-ray approach paves the
way to new directions in mechanochemical research of advanced electronic materials.

Funding

FAPESP 2019/01619-0

FAPESP 2015/26308-7

Jane and Aatos Erkko foundation

History

Email Address of Submitting Author

paulofmo@usp.br

Institution

Universidade de São Paulo - Instituto de Química

Country

Brazil

ORCID For Submitting Author

0000-0003-4854-5352

Declaration of Conflict of Interest

There are no conflicts of intererest

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