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 synthesiz ed. Their physical characteristics have been studied. The diffusion of supe rcritical carbon dioxide (scCO(2)) into polyarylate (PAR) films and their i mpregnation with diiminates were investigated. The equilibrium degree of PA R swelling in scCO(2) is about 10%. The conditions of impregnation (45 degr eesC, 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 therma l reduction, the copper ion is in a nearly univalent state. The copper cont ent 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 impregnatio n, chelate complexes interact with functional groups of the polymer. Subseq uent thermal reduction of metal in air results in diiminate evaporation and thermooxidative degradation with ligand decomposition and enrichment of th e surface with metal, atoms. According to the SAXS data, the size distribut ion of metal-containing particles ranges from 20 to 60 nm with a maximum at 34 nm.