Palladium-gallium based catalysts are highly active for the hydrogenation of CO2 to methanol. Using in situ X-ray absorption spectroscopy (XAS), we have recently determined that an alloying and de-alloying dynamic may play a key role in the catalytic performance of these materials. However, detailed atomic scale insights into the working catalysts have not been fully realised. Here, we propose to use differential pair distribution function (d-PDF) analysis to obtain further insight into the atomic to nanoscale structure of the as-synthesized material, the dynamics of the alloy formation, and the how the material evolves under reaction conditions. The goals of this study are to (i) gain insight into the catalyst structure and changes thereof under reaction conditions; and (ii) explore how the alloy is formed during synthesis.