Colorless Polyimides Derived from an Alicyclic Tetracarboxylic Dianhydride, CpODA

• Published in: Polymers Vol. 13; no. 16; p. 2824
• Main Authors: Ozawa, Hiroki, Ishiguro, Eriko, Kyoya, Yuri, Kikuchi, Yasuaki, Matsumoto, Toshihiko
• Format: Journal Article
• Language: English
• Published: Basel MDPI AG 22.08.2021; MDPI
• Subjects: alicyclic polyimides; colorless polyimides; Cosmic rays; CPI; CpODA; Dianhydrides; Dielectric properties; Dipole interactions; high Tg; Low temperature; Molecular structure; Molecular weight; Nitrogen; Optical properties; polyalicyclic structure; Polyimide resins; Polymerization; Polymers; Temperature; Vacuum distillation; Viscosity; Japan
• ISSN: 2073-4360; 2073-4360
• DOI: 10.3390/polym13162824

An alicyclic tetracarboxylic dianhydride having cyclopentanone bis-spironorbornane structure (CpODA) was polycondensated with aromatic dianhydrides to form the corresponding poly(amic acid)s which possessed logarithmic viscosities in the range 1.47–0.54 dL/g. The poly(amic acid) was imidized by three methods: a chemical, a thermal, and a combined chemical and thermal process. In a thermal method, imidization temperature markedly influenced the film quality and molecular weight of the polyimide. When the poly(amic acid) was cured over the Tg of the corresponding polyimide, the flexible polyimide films were obtained and the molecular weights increased several times, which means that the post-polymerization took place. In spite of low-temperature cure below Tg flexible films with the imidization ratio of 100% were fabricated by a combined chemical and thermal imidization technique. The films possessed the decomposition temperatures in a range of 475–501 °C and Tgs over 330 °C. The high Tg results from a dipole–dipole interaction between the keto groups of the polymer chains as well as development of the rigid polyalicyclic unit. The polyimide films exhibited CTE between 17 and 57 ppm/K. All the films fabricated were entirely colorless and possessed the λcut-offs shorter than 337 nm. Notably, the films prepared by a chemical method exhibited outstanding optical properties.