Synthesis and characterization of Manganese doped ferroxane nanoparticles
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AA9.4.1
Synthesis and characterization of Manganese doped ferroxane nanoparticles Maria M. Cortalezzi1, Jerome Rose2, Eliza Tsui1, Andrew R. Barron3, Jean-Yves Bottero2, Mark Wiesner1. 1 Department of Civil and Environmental Engineering, Rice University, 6100 Main Street MS317, Houston, Texas, USA. 2 Centre Européen de Recherche et d'Enseignement de Géosciences de l'Environnement (CEREGE), UMR 6535 CNRS-Université Aix-Marseille III, Europole de l'arbois - BP 80, 13545 AIX-EN-PROVENCE CEDEX 4, FRANCE. 3 Department of Chemistry, Rice University, 6100 Main Street MS-60, Houston, Texas, USA.
ABSTRACT Ferroxane nanoparticles are precursors to iron oxide ceramic porous membranes. The ferroxane-derived ceramics have an average pore size of 24 nm and a surface area of 80 m2/g. Previous work has shown that these membranes have a molecular weight cut off of 180,000 dalton and their permeability is comparable to commercially available membranes. The ferroxane nanoparticles were reacted with manganese acetyl acetonate and then applied to the fabrication of mixed metal oxides. The nanoparticles were dried to form a ceramic chip. Upon sintering, asymmetric mixed metal oxide ceramic membranes were obtained. The materials were characterized by EXAFS, EDAX imaging and IDX mapping. EXAFS showed that the atomic environment of the iron and dopant material was different from those in the initial compounds, thus confirming that the reaction took place. The concentration of dopant metal was between 7% and 10%, with uniform concentration throughout the material.
INTRODUCTION Ferroxane are nanoparticles with an iron oxide core surrounded by organic groups 1. The ferroxane particles can be used to fabricate porous ceramics and ceramic membranes 1 2 in the ultrafiltration range. Previous work in our laboratory showed that the ferroxane membranes have an average pore size of 24 nm and a BET surface area of 80 m2/g 2. Iron oxide has been recognized as a catalytic material for the decomposition of organic compounds such as quinoline and benzoic acid through Fenton type reactions 3,4; thus, the ferroxane nanoparticles can be applied to the fabrication of reactive membranes for pollution abatement 5. Metal doped ceramics can be prepared by a traditional ceramic powder approach, which involves physically mixing the separate oxides, sintering at high temperature for extended times, grinding and sintering again 6. The microstructure, grain size and grain size distribution, and consequently, pore size and pore size distribution, are not easily reproducible with this method, and physical mixing is limited to the micrometer scale 7. Also, this approach is limited to power processing, while fabrication of thin films and coatings as needed in the fabrication of asymmetric membranes, require solution processing, as in the sol gel synthesis. However, sol-gel presents several difficulties in the processing steps and its environmental impact is not negligible
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8 9. One method has been proposed in the fabrication of metal doped aluminates that ove
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