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Preparation of low thermal expansion coefficient thermoplastic polyimide film

A technology of polyimide film and low thermal expansion coefficient, which is applied in the field of hybrid film preparation, can solve the problems of poor thermal processing performance of the film, and achieve good heat resistance, low device requirements, and good uniformity

Inactive Publication Date: 2009-04-15
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The research results show that the enhancement and decline of molecular chain mobility depends on the content of silica, the molecular weight of polyimide and the relaxation temperature region. The thermal expansion coefficient of the hybrid film decreases significantly with the addition of silica, but the two films Poor thermal processing performance
[0009] The polyimide / silicon dioxide (PI / SiO2) prepared by Cao Feng et al. 2 ) hybrid film for detection of PI / SiO 2 The properties of the hybrid films were found to increase with the SiO 2 With the addition of the hybridization factor, the heat resistance of the PI film is improved, and the CTE of the pure PI film is 65.9×10 -6 K -1 39.9×10 at 30% -6 K -1 , but there is still a relatively large gap with the CTE of copper foil for FCCL
When measuring the adhesion of hybrid materials to glass substrates, it was found that with SiO 2 As the content increases, the bonding ability of the material to the substrate is gradually enhanced. At the same time, Gao Shengqiang et al. believe that the introduction of silicon-containing functional groups into the polyimide main chain structure can significantly improve the bonding of the metal, single crystal silicon and semiconductor surfaces of the material. performance, but there is still a lot of room for improvement in improving the CTE of the material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 8.5g of DMAc, add 16.1ml of tetraethyl orthosilicate (TEOS), stir for 40min, add 5.2ml of water, continue stirring for 1.5h until the solution is uniform and transparent, add 5.0ml of glacial acetic acid (HAc) until the solution is clear, and age at room temperature 22h, standby.

[0033] Weigh 1.3944g of p-phenylenediamine (rigid diamine), 1.1168g of DAMI (flexible diamine) (molar ratio 5:1) and join in 42.5g of DMAc solvent simultaneously, after it dissolves completely, add in 2 batches with two kinds of diamine BTDA in an equimolar amount of amine, so that the solid content (mass fraction) is 15%, and stirred for 3 hours to prepare a PAA solution. Take 5.3019g of pre-aged silica sol, add it to PAA solution, and continue stirring for 3h to obtain PAA / SiO 2 Preparation of hybridization solution.

[0034] PAA / SiO 2 The solution was dip-coated on a glass plate, placed in a vacuum oven and heated stepwise (100°C×1h, 200°C×1h, 280°C×1h), and the dehydration and cy...

Embodiment 2

[0037] Weigh 8.6g of DMAc, add 16.1ml of tetraethyl orthosilicate (TEOS), stir for 30min, add 5.2ml of water, continue stirring for 1h until the solution is uniform and transparent, add 5.0ml of hydrochloric acid (HCl) until the solution is clear, and age at room temperature for 24h. spare.

[0038] Weigh 2.5847g ODA (rigid diamine), 1.3957gDAMI (flexible diamine) (molar ratio 4: 1) and join in 42.5gDMAc solvent at the same time, after it dissolves completely, add in batches equimolar amounts of two diamines PMDA, so that its solid content (mass fraction) was 14.5%, stirred for 4 hours to prepare a PAA solution. Take 5.8909g of pre-aged silica sol, add it to the PAA solution, and continue stirring for 4h to obtain PAA / SiO 2 Preparation of hybridization solution.

[0039] PAA / SiO 2 The solution was dip-coated on a glass plate, placed in a vacuum oven and heated stepwise (100°C×1h, 200°C×1h, 280°C×1h), and the dehydration and cyclization of PI / SiO 2 hybrid film.

[0040] Th...

Embodiment 3

[0042] Weigh 8.4g of DMF, add 16.1ml of tetraethyl orthosilicate (TEOS), stir for 50min, add 5.2ml of water, continue to stir for 1h until the solution is uniform and transparent, add 5.0ml of glacial acetic acid (HAc) until the solution is clear, and age at room temperature for 24h ,spare.

[0043] Weigh 1.9410g ODA (rigid diamine), 1.3974g BAPP (flexible diamine) (molar ratio 3:1) and add them to 42.5g DMF solvent at the same time. BTDA so that its solid content (mass fraction) was 15.1%, and stirred for 4.5 hours to prepare a PAA solution. Take 5.8909g of pre-aged silica sol, add it to PAA solution, and continue stirring for 4.5h to obtain PAA / SiO 2 Preparation of hybridization solution.

[0044] PAA / SiO 2 The solution was dip-coated on a glass plate, placed in a vacuum oven and heated stepwise (100°C×1h, 200°C×1h, 280°C×1h), and the dehydration and cyclization of PI / SiO 2 hybrid film.

[0045] The coefficient of thermal expansion (CTE) of the film measured by a static...

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Abstract

The invention relates to a preparation method of a thermoplastic polyimide film with low coefficient of thermal expansion, which obtains an objective product by copolymerization, sol-gel process and condensation. Two different diamine and dianhydride are added into copolyreaction to generate polyreaction. A sol-gel in situ method is adopted, the reaction process is easy to control, the purity of the product is good and the uniformity is good; and the obtained solution is heated step by step in a vacuum oven and carries out condensation. The preparation technique is simple and is easy to control; the obtained product has better heat resistance; and the invention is suitable for being used by flexible copper clad laminate and has higher application value in the industry.

Description

technical field [0001] The invention relates to a method for reducing the coefficient of thermal expansion (CTE) of a thermoplastic polyimide film used in FCCL, in particular to the preparation of a hybrid film with two different diamine raw materials. Background technique [0002] Since it was first introduced to the market in 1966, polyimide (PI) film has been used as a high-performance insulating material in the aerospace industry and the electrical and electronic industry for its excellent electrical properties, flame retardancy, high temperature resistance and radiation resistance. each field. With the development of application technology, the application field of PI film is expanding day by day, especially in microelectronics and information industry, the original product performance can no longer meet the requirements of new technology. Globally, the current largest application market of polyimide film is flexible printed circuit board (FPC), mainly used for flexibl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L79/08C08K3/36C08G73/10
Inventor 黄培俞娟吕亮
Owner NANJING UNIV OF TECH
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