Synthesis and Chemically Amplified Photo-Cross-Linking Reaction of a Polyimide Containing an Epoxy Group
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- 作者：Han Sung Yu ; Takashi Yamashita ; and Kazuyuki Horie
- 刊名：Macromolecules
- 出版年：1996
- 出版时间：February 12, 1996
- 年：1996
- 卷：29
- 期：4
- 页码：1144 - 1150
- 全文大小：498K
- 年卷期：v.29,no.4(February 12, 1996)
- ISSN：1520-5835
文摘
A new polyimide, PI(6FDA/ep-AHHFP), containing an epoxygroup was synthesized bythe reaction of epichlorohydrin with PI(6FDA/AHHFP), which wasprepared from 4,4'-(1,1,1,3,3,3-hexafluoro-2-propylidene)diphthalic anhydride (6FDA) and2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (AHHFP) in the presence of benzyl(trimethyl)ammoniumchloride at 110-120 
C. Thispolyimide having an epoxy group is highly soluble in most commonsolvents. Photochemical reactivityof PI(6FDA/ep-AHHFP) was examined in the presence ofdiphenyliodonium hexafluoroarsenate as anacid generator. The conversion and the curing rate were determinedby the absorbance change in the IRband at 905 cm-1 for the epoxy group.The activation energy for cross-linking reaction ofPI(6FDA/ep-AHHFP) was found to be ~6 kJ/mol. The reaction radius of an acidin PI(6FDA/ep-AHHFP) containingdiphenyliodonium hexafluoroarsenate as a photoacid generator wasdetermined to be about 19-30 Å inthe chemical amplification process when heated for 5-40 min at50-195 C. The quantum yield forcross-linking of PI(6FDA/ep-AHHFP), 
gel, obtainedfrom the characteristic curve was 3.0. Thesensitivity,Dgel, and contrast, 
, after postcure at 100C for 30 min were 4.8 × 10-10 einsteincm-2 and 5.7, respectively.The quantum yield for cross-linking, GPC, wasdetermined to be 2.6 from gel permeation chromatographymeasurements.
C. Thispolyimide having an epoxy group is highly soluble in most commonsolvents. Photochemical reactivityof PI(6FDA/ep-AHHFP) was examined in the presence ofdiphenyliodonium hexafluoroarsenate as anacid generator. The conversion and the curing rate were determinedby the absorbance change in the IRband at 905 cm-1 for the epoxy group.The activation energy for cross-linking reaction ofPI(6FDA/ep-AHHFP) was found to be ~6 kJ/mol. The reaction radius of an acidin PI(6FDA/ep-AHHFP) containingdiphenyliodonium hexafluoroarsenate as a photoacid generator wasdetermined to be about 19-30 Å inthe chemical amplification process when heated for 5-40 min at50-195 C. The quantum yield forcross-linking of PI(6FDA/ep-AHHFP), gel, obtainedfrom the characteristic curve was 3.0. Thesensitivity,Dgel, and contrast, , after postcure at 100C for 30 min were 4.8 × 10-10 einsteincm-2 and 5.7, respectively.The quantum yield for cross-linking, GPC, wasdetermined to be 2.6 from gel permeation chromatographymeasurements.