This thesis focuses on synthesis and characterization of palladium-based nanoparticles. Background information of the research in this thesis is provided in Chapter 1. Preparation and characterization of pure palladium nanoparticles are presented in Chapter 2. A fast and convenient method to prepare ultra small Pd nanoparticles via Pluronic P123 reduction is discussed in detail. Impregnation method and poly method are also studied in this chapter. Chapter 3 reports the studies of these methods to prepare ultra small bimetallic (bimetallic means a mixture of two metals) palladium-based nanoparticles. Oleylamine-mediated method used Pd nanoparticles prepared via P123 reduction as precursor. Ultra small palladium-based nanoparticles are prepared in this way. With the assistance of trioctylphosphine complex as precursor, tiny palladium-based bimetallic nanoparticles can be prepared with certain structure. The structure of these bimetallic nanoparticles gives a better electrochemical activity than pure palladium nanoparticles. When loaded on mesoporous carbon, these tiny trioctylphosphine-assisted palladium nanoparticles displayed good thermal stability
