Ll. He et al., HOMOGENEOUS POLYIMIDE FILMS WITH INCREASED ISALICYLIDENE-1,2-PHENYLENEDIAMINATO)ZIRCONIUM(IV) CONTENT, Chemistry of materials, 9(12), 1997, pp. 3005-3011
To increase the concentration of inorganic component in polyimide film
s and enhance the materials' resistance to atomic oxygen, the complex
salicylidene-1,2-phenylenediaminato)zirconium(rv), Zr(adsp)-(dsp), was
synthesized and allowed to react with poly(maleic anhydride) (PMA). T
he resulting Zr-PMA pendent polymer was mixed with a commercially avai
lable polyamic acid of pyromellitic dianhydride and 4,4'-oxydianiline
(PMDA-ODA) in various proportions in NMP. Films were then cast onto gl
ass substrates, and thermally imidized. The new mixed ligand complex a
nd the Zr-PMA polymer were characterized by TLC, IR, H-1 NMR, and elem
ental analysis, along with X-ray crystallography for the former and TG
A for the latter. The imidized films of the Zr-PMA polymer blended wit
h PMDA-ODA polyimide were studied by optical examination of multilayer
film samples for crack formation, and SEM photography before and afte
r atomic oxygen erosion in a plasma asher. The upper limit of Zr compl
ex incorporation onto prebaked poly(maleic anhydride) was approximatel
y 24% (mel of Zr/mol of repeat units). The upper limit of zirconium co
mplex 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.