Homogeneous polyimide films with increased bis(N,N'-disalicylidene-1,2-phenylenediaminato)zirconium(IV) content
Date
1997-12Author
He, Liling
Wagner, Shawn
Illingsworth, Marvin
Jensen, Andrew
Yap, Glenn
Rheingold, Arnold
Metadata
Show full item recordAbstract
To increase the concentration of inorganic component in polyimide films and enhance the materials' resistance to atomic oxygen, the complex (4-amino-N,N'-disalicylidene-1,2-phenylenediaminato)(N,N'-disalicylidene-1,2-phenylenediaminato)zirconium(IV), Zr(adsp)(dsp), was synthesized and allowed to react with poly(maleic anhydride) (PMA). The resulting Zr-PMA pendent polymer was mixed with a commercially available polyamic acid of pyromellitic dianhydride and 4,4'-oxydianiline (PMDA-ODA) in various proportions in NMP. Films were then cast onto glass substrates, and thermally imidized. The new mixed ligand complex and the Zr-PMA polymer were characterized by TLC, IR, 1H NMR, and elemental analysis, along with X-ray crystallography for the former and TGA for the latter. The imidized films of the Zr-PMA polymer blended with PMDA-ODA polyimide were studied by optical examination of multilayer film samples for crack formation, and SEM photography before and after atomic oxygen erosion in a plasma asher. The upper limit of Zr complex incorporation onto prebaked poly(maleic anhydride) was approximately 24% (mol of Zr/mol of repeat units). The upper limit of zirconium complex concentration for the Zr-PMA/PMDA-ODA blends, above which films crack upon imidization, was 8 mol %, compared to 4 mol % for mixtures of Zr(dsp)2 in PMDA-ODA polyimide.