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Abstract
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.
