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| Naji, M. |
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| Petrov, R. H. | Madrid |
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| Azam, Siraj |
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| Ospanova, Alyiya |
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| Ali, M. A. |
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| Popa, V. |
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| Rančić, M. |
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| Azevedo, Nuno Monteiro |
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Cakir, Cafer T.
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article
Dispersive x-ray absorption spectroscopy for time-resolved in situ monitoring of mechanochemical reactions
Abstract
ABSTRACT<br/>X-ray absorption spectroscopy (XAS) provides a unique, atom-specific tool to probe the electronic structure of solids. By surmounting long-held limitations of powder-based XAS using a dynamically averaged powder in a Resonant Acoustic Mixer (RAM), we demonstrate how time-resolved <i>in situ</i> (TRIS) XAS provides unprecedented detail of mechanochemical synthesis. The use of a custom-designed dispersive XAS (DXAS) set-up allows us to increase the time resolution over existing fluorescence measurements from <i>ca.</i> 15 min to 2 sec, for a complete absorption spectrum. Hence, we here establish TRIS-XAS as a viable method for studying mechanochemical reactions and sampling reaction kinetics. The generality of our approach is demonstrated through RAM-induced (i) bottom-up Au nanoparticle mechanosynthesis, and (ii) synthesis of a prototypical metal organic framework, ZIF-8. Moreover, we demonstrate that our approach also works with the addition of a stainless steel milling ball, opening the door to using TRIS-DXAS for following conventional ball milling reactions. We expect our TRIS-DXAS approach will become an essential part of the mechanochemical tool box.