ABSTRACT:The effects of thermal curing method on degree of imidization, molecular orientation, and chain ordering of the 4,4-oxydiphenylene pyromellitimide (PMDA--ODA) were investigated. Three different thermal curing methods were chosen in this study; two casts of polyamic acid on silicon wafer were isothermally cured at 200°C for 3 h (l-200) and 300°C for 3 h (l-300) respectively, and the other one was cured in step manner (S-300): I00°C for 1 h, 200°C for 1 h, and finally 300°C for I h. The degree of imidization was highest in the 1-300 and lowest in the S-300, demonstrating that the amount of solvent and degree of imidization at each stage of the curing cycles significantly affect the final degree of imidization. The degree of in-plane orientation was found highest for the S-300 and lowest for the 1-300. This suggests that the in-plane orientation decreases with increase of the chain immobilization. This chain ordering was found to be easily induced for the 1-300 among the three cured films. In the 1-300, the chains in the film are sparsely packed and ordering by the diffusion of polymer chians occurs most easily.KEY WORDS 4,4-Oxydiphenylene Pyromellitimide / Degree of Imidization / Molecular Orientation / Chain Ordering / In recent years, much attention has been directed to aromatic polyimide films, widely used as high-temperature insulators and dielectric coatings, adhesives, matrices, and alignment layer films for liquid crystal display. 1 • 2 The traditional synthetic route for these materials is two steps, the synthesis of poly(amic acid) (PAA) and subsequent thermal or chemical imidization (curing) of the PAA. 1 In preparation of the polyimide films, thermal imidization is generally used as the second step. Thermal imidization involves the simultaneous loss of solvent, cyclization of amic acid group to form imide, and both intra-and inter-molecular structure evolution. 3 • 7 -12 Regulation of the conditions on thermal imidization provides a wide spectrum of properties. Thus, understanding the effects of thermal curing method on the structure of the resulting polyimide film is very important to control the microstructure of the polyimide formed and to ensure final properties. However, a comparison of the degree of imidization, molecular orientation, and chain ordering among the polyimide films prepared by thermally different curring methods has not been made.This article studies the effects of thermal curing method on the structure of the polyimide films interfaced with silicon substrate. Three different curing methods were taken as follows; (i) isothermal curing at 200°C for 3 h (1-200), (ii) isothermal curing at 300°C for 3 h (1-300), and (iii) step curing (S-300) which consists of three steps: isothermal heating at 100°C for 1 h followed by isothermal heating at 200°C for 1 h, and then isothermal heating at 300°C for l h.
EXPERIMENTAL
MaterialsPyralin (Du Pont), a mixture of polyamic acid (4,4'-oxydiphenylene pyromellitamic acid), l-methyl-2-pyrrot To whom all correspondence should be addressed.lido...