Publication date: 10th April 2024
Since its inception a decade ago, exsolution has proven to be a powerful tool for the design of advanced energy materials. Therefore, the ability to tailor the size, morphology, and composition of the exsolved nanoparticles is critical to implement this technique to further improve the performance of such nanostructured catalysts [1]. Previously, ex-situ techniques had been used to probe this rather complex system, but the growing interest to understand the exsolution processes and the material changes during catalytic operation has paved way for the development of in-situ methods such as XRD, AP-XPS, and TEM [2]. So far however, poor information could be gathered with respect the nanoparticle size evolution during the exsolution process.
In this work, the exsolution of nano alloy with Ru-Ni composition from an A-site deficient double perovskite of the type (La2−xNiRuO6−δ, x = 0.15) [3], was investigated via in-situ X-ray scattering methods. In particular, the exsolution process was studied at 450 and 550°C for 5 h both by in situ XRD and small-angle X-ray scattering (SAXS). This latter method represents a novel approach and offers a direct and highly statistically relevant investigation of the size evolution of exsolved nanoparticles. The analysis of the SAXS) curves gave an insight into the formation of both surface and sub-surface nanoparticles.At 450 °C the particles formed on the surface increased from 0.5 to 2 nm, whereas the buried component grew from 3 to 10 nm in diameter. which agreed with the particle size distribution seen in the TEM images [3]. During the exsolution process over 5 hours we could monitor different nucleation events which corresponded well to the structural changes of the perovskite matrix and the reduction of the metal species monitored by in situ XRD and XANES spectroscopy, respectively.
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