Publication date: 17th July 2025
Along with their prolonged lifetime and regenerability, what distinguishes the exsolution catalysts from conventional ones is the homogeneous distribution and tailorable size of the metallic particles. These features can be precisely controlled by tuning intrinsic parameters (such as perovskite defect chemistry and dopant concentration) as well as extrinsic parameters (such as time, temperature, and oxygen partial pressure) during the exsolution process.
Electron microscopy has proven to be a powerful tool for monitoring the morphological evolution of exsolved particles [1]. However, complementary techniques are required to obtain volumetric information on changes in nanoparticle size, population, and distribution. For this purpose, small-angle X-ray scattering (SAXS) offers a valuable opportunity [2,3]. Taking advantage of the electron density contrast between the metallic particles and the host oxide, SAXS provides a unique and direct method to monitor the evolution of both surface (i.e., exogenous) and internal (i.e., endogenous) particles.
In this contribution, I will present the growth behavior of exogeneous and endogeneous nickel nanoparticles exsolved from nanoporous and sintered matrices, as studied via SAXS. Particular focus will be placed on the effects of exsolution temperature and nickel dopant concentration on nanoparticle morphology evolution. The development of in situ SAXS experiments for studying nickel nanoalloys will also be discussed.
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