Preparation of high modulus, low thermal expansion coefficient polyimide hybridization film

A low thermal expansion coefficient and polyimide technology, which is applied in the field of low thermal expansion polyimide hybrid film to prepare high modulus, can solve the problem of long operation time, and achieve the goal of increasing the density and increasing the amount of doping Effect

Active Publication Date: 2009-04-15
连云港达昇新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Preparation of high modulus, low thermal expansion coefficient polyimide hybridization film
  • Preparation of high modulus, low thermal expansion coefficient polyimide hybridization film

Examples

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Embodiment 1

[0031] Weigh 3.5897g of 4,4'-diaminodiphenyl ether (ODA), dissolve it in 42.5000g of N,N'-dimethylacetamide (DMAc) solvent, stir evenly at room temperature, and then add the equimolar amount of ODA in batches The amount of dianhydride monomer pyromellitic anhydride (PMDA) is a total of 3.9103g, continue to stir, along with the continuous dissolving of dianhydride monomer, the viscosity of polymer also constantly increases, continue to stir at normal temperature after monomer is all dissolved After 4 hours, a PAA solution with a solid content (mass fraction) of 15% was prepared.

[0032] Add 1.3002g tetraethyl orthosilicate (TEOS) to PAA solution, 0.1123gH 2 O, 0.3743g catalyst glacial acetic acid (HAc) and 0.075g coupling agent (KH550), stirring continuously for 4h to form a homogeneous phase, complete the sol reaction and form SiO 2 PAA / SiO with a mass percentage of 4.76% 2 hybrid solution.

[0033] PAA / SiO 2 The solution was dip-coated on a glass plate, placed in a vacuu...

Embodiment 2

[0035] Weigh 1.8837g m-phenylenediamine, dissolve in 42.5000g N,N'-dimethylacetamide (DMAc) solvent, stir evenly at normal temperature, then add the dianhydride monomer 3 in an equimolar amount to ODA in batches , a total of 5.6163g of 3,4,4-benzophenone tetra-acid dianhydride (BTDA), continue to stir, along with the continuous dissolution of the dianhydride monomer, the viscosity of the polymer is also constantly increasing, after all the monomers are dissolved, continue to Stir at room temperature for 3.5 h to prepare a PAA solution with a solid content (mass fraction) of 15%.

[0036] Add 1.3002g tetraethyl orthosilicate (TEOS) to PAA solution, 0.1123gH 2 O, 0.3743g catalyst glacial acetic acid (HAc) and 0.075g coupling agent (KH560), stirring continuously for 4h to form a homogeneous phase, complete the sol reaction and form SiO 2 PAA / SiO with a mass percentage of 4.76% 2 hybrid solution.

[0037] PAA / SiO 2 The solution was dip-coated on a glass plate, placed in a vacu...

Embodiment 6

[0039] Weigh 2.8737g of 4,4'-diaminodiphenyl ether (ODA), dissolve it in 42.2500g of N,N'-dimethylacetamide (DMAc) solvent, stir evenly at room temperature, then add in batches with ODA, etc. The molar amount of dianhydride monomer 3,3,4,4-benzophenonetetraacid dianhydride (BTDA) is a total of 4.6263g, continue to stir, along with the continuous dissolving of dianhydride monomer, the viscosity of polymer also constantly increases After all the monomers are dissolved, continue to stir at room temperature for 3.5 hours to obtain a PAA solution with a solid content (mass fraction) of 15.5%.

[0040] Add 2.6004g tetraethyl orthosilicate (TEOS) to PAA solution, 0.2247gH 2 O, 0.7486g catalyst glacial acetic acid (HAc) and 0.075g coupling agent (KH560), stirring continuously for 4.5h to form a homogeneous phase, complete the sol reaction and form SiO 2 9.1% by mass of PAA / SiO 2 hybrid solution.

[0041] PAA / SiO 2 The solution was dip-coated on a glass plate, placed in a vacuum ov...

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Abstract

The invention relates to a preparation method of thermosetting polyimide film with high modulus and low coefficient of thermal expansion, which obtains an objective product by copolymerization, sol-gel process and condensation. Rigid diamine and dianhydride are adopted in the polyreaction. A sol-gel in situ method is adopted, the reaction process is easy to be controlled, the uniformity is good; the amount of hybridization of inorganic particles can be increased; and the obtained solution is heated step by step to generate condensation reaction. The preparation technique is simple and is easy to be controlled; and the obtained product has higher elastic modulus and low coefficient of thermal expansion; therefore, the invention has higher application value in industry.

Description

technical field [0001] The invention relates to a method for preparing polyimide hybrid film with high modulus and low thermal expansion coefficient, in particular to hybrid modification of thermosetting polyimide by sol-gel blending method. Background technique [0002] As a high-performance special engineering plastic film, polyimide (PI) film has stable and excellent physical properties, chemical properties and electrical properties in a wide temperature range, especially high thermal stability and glass transition temperature. It is widely used in high-tech fields such as aerospace and microelectronics. In the international market, polyimide film is mainly used as the base material of flexible copper clad foil (FCCL) in flexible printed circuit board (FPC). The polyimide film used in FCCL not only requires the good heat resistance and chemical stability of ordinary polyimide, but also requires the film to have higher strength, modulus, low thermal expansion and other pr...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L79/08C08K9/06
Inventor 黄培俞娟
Owner 连云港达昇新材料科技有限公司
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