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Overview: Diffractive optical element (DOE) is an important part of the large aperture spatial diffractive optical system. Materials of DOE with the characteristics of high optical transmittance, satisfactory optical homogeneity, and good dimensional stability are urgently required. As a kind of engineering polymer with high performance, polyimides (PIs) are widely used in the aerospace field, owing to their inherent good mechanical properties, resistance to chemicals, desirable dielectric permittivity, and high-temperature stability. However, the preparation of PI films on the market mostly adopts a biaxial stretching forming process, which is equivalent to pre-orienting the film and will introduce errors in beam control. In order to obtain PI with optical homogeneity, it is necessary to improve the existing preparation process. Nevertheless, there are few reports on the improvement of film forming process for optical imaging application. The forming process parameters of the optical imaging quality films: viscosity, rotation speed, spin coating time and precuring temperature are 105 p, 900 rpm, 120 s and 70 ℃, respectively. According to the film-forming process parameters, the optical homogeneity results of PI film with 100 mm aperture are obtained: PV≤1/4λ and RMS≤1/20λ. Moreover, the process has good stability, therefore, we can stably prepare PI film with large aperture (100 mm) which meet the Rayleigh criterion, which is the basis of the subsequent preparation of Fresnel film lens. The characteristic peak at 1366 cm-1 is due to the peak in amide bond. At 2900 cm-1~3200 cm-1, the broad absorption peaks of - COOH group and - NH group corresponding to the polyamic acid disappear, indicating that the polyimide film has been completely imidized. The temperature Td of 5% is 582 ℃. The carbon yield of the BPDA-DABA type PI at 800 ℃ is about 62.7%. The glass transition temperature Tg of BPDA-DABA PI is 359 ℃. The thermal expansion coefficient of PI film is about 3.2 ppm·K-1, which makes the deformation of PI film itself under the condition of temperature change have the lowest influence on the beam control. It can basically meet the requirements of optical PI for dimensional stability. The tensile strength of the BPDA-DABA type PI is ~285 MPa due to the hydrogen bond between molecular chains. The transparency of both the BPDA-DABA PI and PMDA-ODA PI films are more than 80% at 550 nm. In summary, BPDA-DABA PI has excellent mechanical strength and good thermal properties, and these basic indices can meet the design requirements of optical PI film. In this paper, the spin coating method is used to solve the problem that the low thermal expansion coefficient tensile PI film with 100 mm aperture meets Rayleigh criterion, which lays the foundation for solving the optical homogeneity of diffractive optical elements on the ground or in the synchronous orbit environment.
Synthetic route of PI film
Infrared spectrum of PI film
TGA curve of PI film
tanδ curve of PI film
Comparison of tensile strength and elongation at break of two different types of PI films
Transmittance curves of PI films
Optical homogeneity of PI films