Synthesis and redox behaviors of copper oxide and manganese oxide nanoparticles

Chapter 1. A general introduction to the field of transition metal oxide nanoparticles is presented, highlighting the industrial applications and research interest in copper oxide and manganese oxide nanoparticles in particular. A background of x-ray diffraction and transition electron microscopy used in this research is presented.Chapter 3. An aqueous method for synthesizing 20--40 nm Mn3O4 nanoparticles from manganese nitrate and HMT at temperatures between 25°C and 80°C is described and results of nanoparticle characterization are presented. The effects of nitrate concentration, synthesis temperature, and reaction time on the Mn3O4 nanoparticle size, size distribution, and morphology are evaluated. The activation energy for the formation of Mn3O4 nanoparticles is calculated from the synthesis yield.Chapter 4. The behavior of copper oxide nanoparticles in reduction experiments is evaluated synchrotron radiation and in-situ time-resolved x-ray diffraction (TR-XRD) are used to monitor phase changes during reduction. CuO reduction experiments in CO and H 2 gases using ramping temperature and isothermal conditions are presented.Chapter 5. Reduction of Mn3O4 nanoparticles and oxidation of MnO nanoparticles using synchrotron radiation and in-situ TR-XRD is presented. Redox temperature decreases with decreases nanoparticle size. The formation of the intermediate phase Mn5O8 with further oxidation of MnO, observed in MnO nanoparticles, is discussed.Chapter 2. An aqueous method for producing 5--18 nm wide copper oxide (CuO) nanoparticles at 36°C to 50°C using copper nitrate and hexamethylenetetramine (HMT) is presented. HMT quality and concentration is used to control CuO nanoparticle size. A decrease in nanoparticle size with increasing HMT concentration indicates that HMT acts as a surfactant in the reaction. Activation energy for formation of CuO is calculated from the reaction rate.Chapter 6. Measurements of lattice parameter in nanoparticles of MnO and Cu2O formed by reducing Mn3O4 and CuO nanoparticles are presented. Lattice contraction in MnO nanoparticles is evaluated with emphasis on effect of manganese ion valence. Dilation of the Cu2O lattice is discussed.