<div>The development of time-resolved in situ approaches for monitoring mechanochemical</div><div>transformations has revolutionized the field of mechanochemistry. Currently, the established in</div><div>situ approaches greatly limit the scope of investigations that are possible. Here we develop a new</div><div>approach to simultaneously follow the evolution of bulk atomic and electronic structure during a</div><div>mechanochemical synthesis. This is achieved by coupling two complementary synchrotron-based</div><div>X-ray methods: X-ray absorption spectroscopy and X-ray diffraction. We apply this method to</div><div>investigate the bottom-up mechanosynthesis of technologically important Au nanoparticles in the</div><div>presence of three different reducing agents. Moreover, we demonstrate how X-ray absorption</div><div>spectroscopy offers unprecedented insight into the early stage generation of growth species (e.g.</div><div>monomers and clusters), which lead to the subsequent formation of nanoparticles. These</div><div>processes are beyond the detection capabilities of diffraction methods. The approach is general,</div><div>and not limited to monitoring NP mechanosynthesis. This combined X-ray approach paves the</div><div>way to new directions in mechanochemical research of advanced electronic materials.</div>
Structural Evolution of Ag-LEV Zeolite upon Heating: An In Situ Single-Crystal X-ray Diffraction (SC-XRD) and X-ray Absorption Spectroscopy (XAS) Study