New chelate complexes of copper and iron: Synthesis and impregnation into a polymer matrix from solution in supercritical carbon dioxide

New chelate complexes of copper diiminate and iron diiminate were synthesized. Their physical characteristics have been studied. The diffusion of supercritical carbon dioxide (scCO(2)) into polyarylate (PAR) films and their impregnation with diiminates were investigated. The equilibrium degree of PAR swelling in scCO(2) is about 10%. The conditions of impregnation (45 degreesC, 8 MPa, 1.5 h) were determined. The impregnation was confirmed by the FT-IR spectroscopic data. Thermal reduction of metal ions was investigated. Transformations of the chelate complexes on the polymer-film surface were studied by ESCA. The value of the Auger factor indicates that, after thermal reduction, the copper ion is in a nearly univalent state. The copper content in films is as large as 6.3 wt %; the iron content is 4.5 wt %. The FT-IR and ESCA spectroscopic studies showed that, in the course of impregnation, chelate complexes interact with functional groups of the polymer. Subsequent thermal reduction of metal in air results in diiminate evaporation and thermooxidative degradation with ligand decomposition and enrichment of the surface with metal, atoms. According to the SAXS data, the size distribution of metal-containing particles ranges from 20 to 60 nm with a maximum at 34 nm.