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Metal nano-aerogels combine a large surface area, a high structuralstability, and a high catalytic activity towards a variety of chemicalreactions. The performance of such nanostructures is underpinned by theatomic-level distribution of their constituents. Yet monitoring theirsub-nanoscale structure and composition to guide property optimization remainsextremely challenging. Here, we synthesized Pd nano-aerogels from a K2PdCl4precursor and two different NaBH4 reductant concentrations in distilled water.Atom probe tomography reveals that the aerogel is poly-crystalline and thatimpurities (Na, K) are integrated from the solution into grain boundaries. Abinitio calculations indicate that these impurities preferentially bound to thePd-metal surface and are ultimately found in grain boundaries forming as theparticles coalesce during synthesis, with Na atoms thermodynamicallyequilibrating with the surrounding solution and K atoms remaining betweengrowing grains. If controlled, impurity integration, i.e. grain boundarydecoration, may offer opportunities for designing new nano-aerogels.

Understanding alkali contamination in colloidal nanomaterials to unlock grain boundary impurity engineering