Highly dispersed Pd nanoparticles within silica: Synthesis and characterization: Fid-Bau Portal

Highly dispersed Pd nanoparticles within silica: Synthesis and characterization

Ramakrishnan, Ayyappan / Dumbuya, Karifala / Ofili, Jimmy / Steinrück, Hans-Peter / Gottfried, J. Michael / Schwieger, Wilhelm

Abstract

Abstract Well dispersed and homogeneously distributed Pd nanoparticles within a silica matrix were synthesized by a two stage process: (1) intercalation of palladium tetrammine ions into the layered aluminium-free silicate Na ilerite followed by (2) a self-reduction of the complex through decomposition of the tetrammine ligands by calcination at 550°C for 5h under N2 or air. Samples calcined in N2 predominantly contained nanoparticles of metallic Pd, while calcination in air led largely to the formation of PdO, as confirmed by XPS and supported by XRD and TGA. Thus, the Pd/PdO loading in the silica can be selectively tuned through this method. The intercalates were characterized by standard methods such as XRD, TGA, ICP and TEM. TGA of the intercalates indicated that the stabilization of the palladium tetrammine complex was enhanced by intercalation into Na ilerite. Based on ICP analysis, the Pd loadings in the intercalates were estimated to be about 18mass-%, which was also in agreement with the results from TGA. TEM revealed that the Pd/PdO nanoparticles were well dispersed in the silica matrix with an average particle size of approximately 8–10nm after calcination in air.

Research Highlights ► Method to synthesize metal nanoparticles within silica matrix by an intercalation of Palladium tetrammine cations into Na ilerite. ► Tuning the Pd / PdO content in the intercalates by selectively changing the calcination medium (N2 or air). ► High Pd loadings (up to 18 mass %) and well dispersed nanoparticles of particle size 8-10 nm are realized.