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Polyimide resin, its midbody, preparation method and application thereof

A technology of polyimide resin and polyamic acid, which is applied in the field of polyimide resin, can solve the problems of low glass transition temperature, unsuitable processing and application requirements, and high Tg of polyimide

Active Publication Date: 2009-01-14
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Can be processed at 200-235°C, the disadvantage is that the glass transition temperature is low
In 2006, CN 1718428A announced a laminate made of fusible polyimide, nanometer and / or ultrafine powder, and alkali-free glass cloth. The laminate has a high glass transition temperature, but Its final pressing temperature is close to 400°C, which puts higher requirements on the production equipment and cannot be completed without updating the equipment
However, in general, the Tg of polyimide used in high-density packaging substrates is mostly too high or too low, which is not suitable for current processing and application requirements

Method used

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  • Polyimide resin, its midbody, preparation method and application thereof
  • Polyimide resin, its midbody, preparation method and application thereof
  • Polyimide resin, its midbody, preparation method and application thereof

Examples

Experimental program
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preparation example Construction

[0059] Preparation of the first part polyimide resin

[0060] The polyimide resin provided by the invention is obtained by chemical imidization or thermal imidization of polyamic acid (PAA). Specifically, under the protection of an inert gas, in a three-necked flask equipped with a thermometer and a condenser tube, dissolve the diamine monomer in an organic solvent, stir at 20-50°C, and add tetracarboxylic dianhydride mono If necessary, add an end-capping agent, and finally add the required organic solvent. The amount of organic solvent should be controlled so that the solid content of the resin is between 10-30%. Stir for 0.5-24 hours to obtain PAA . Polyimide can be obtained from PAA through the following three methods:

[0061] 1) Add dehydrating agent and catalyst to the PAA reaction system, at 5-70°C, the preferred reaction temperature is 10-60°C; the reaction time is 1-25 hours, the preferred reaction time is 2-20 hours. Pour this solution into a large amount of poor ...

Embodiment 1

[0065] Embodiment 1, prepare polyimide resin

[0066] Under the protection of nitrogen, add 214.17g (0.5mol) p-6FAPB, 2.5L NMP into a 5L three-neck flask equipped with mechanical stirring, thermometer and condenser, and stir at 25°C. After 6FAPB is completely dissolved, slowly Add 212.50g (0.47mol) 3FDA, react at 20 ℃, add 8.89g (0.06mol) phthalic anhydride (PA) after forming homogeneous solution, continue to stir for 2 hours, obtain homogeneous polyimide precursor solution polyamic acid (PAA ). Add 100mL of acetic anhydride and 50mL of triethylamine into the reaction system, raise the temperature to 60°C, continue stirring for 10 hours, pour the obtained polyimide solution into a large amount of methanol, wash thoroughly, and dry the obtained precipitate at 150°C To constant weight, the chemically imidized polyimide is obtained. The measured intrinsic viscosity is 0.60dL / g, and the glass transition temperature Tg is 258°C.

[0067] The diamine p-6FAPB used in this example ...

Embodiment 2

[0068] Embodiment 2, prepare polyimide resin

[0069] Under nitrogen protection, add 214.17g (0.5mol) m-6FAPB and 2.5L m-cresol into a 5L three-necked flask equipped with mechanical stirring, a thermometer and a condenser, and stir at 25°C. After 6FAPB is completely dissolved, divide Slowly add 164.81g (0.46mol) DSDA in batches, react at 20°C to form a uniform solution, add 11.85g (0.08mol) phthalic anhydride (PA), and continue stirring for 2 hours to obtain a uniform polyimide precursor solution polyamic acid (PAA). Add 100mL of acetic anhydride and 50mL of triethylamine into the reaction system, raise the temperature to 50°C, continue stirring for 12 hours, pour the obtained polyimide solution into a large amount of methanol, wash thoroughly, and dry the obtained precipitate at 150°C To constant weight, the chemically imidized polyimide is obtained. The measured intrinsic viscosity is 0.54dL / g, and the glass transition temperature Tg is 246°C.

[0070] The diamine m-6FAPB...

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Abstract

The invention discloses polyamide resin and intermediate compound thereof as well as the preparation method and the application. The polyamide resin is provided with the chemical structure shown in formula II, wherein, X1 and X2 can be identical or different, representing quadrivalent aryl; Ar represents bivalent aryl, and T represents end capping reagent. The polyamide resin is obtained by polyamic acid shown in formula I structure general formula through chemical imidization or thermal imidization. The polyamide resin is dipped through prosomatic polyamic acid solution or polyamic acid solution being obtained after being dissolved with solvent with a low-boiling point, the basal body is strengthened, and the prepreg is obtained. After the heat-press forming operation is performed, a metal foil layer is covered, and a metal foil layer pressing plate is obtained. The polyamide resin provided by the invention has the advantages of excellent heat resisting property, high mechanical property, low dielectric constant and dissipation, high electrical insulation property and low water absorbing capacity, thereby being especially suitable for manufacturing core plates of packaging subsctrates for packaging super large-scale integrated circuits.

Description

technical field [0001] The invention relates to a polyimide resin and its intermediates, their preparation method and application, in particular to a polyimide resin suitable for manufacturing ultra large scale integrated circuit packaging substrates. Background technique [0002] At present, ultra-large-scale integrated circuits (ULSI) are rapidly developing in accordance with Moore's law. The characteristic line width is getting thinner and the wafer diameter is getting bigger and bigger. The current mainstream production technology is 0.25-0.35 microns, the advanced production technology is 0.13-0.10 microns, and the 60-90 nanometer technology has begun mass production; it is expected to develop to 45 nanometers in 2010, and to 2016 and 2018 respectively. 22nm and 18nm. At the same time, the corresponding VLSI packaging technology is also developing rapidly in the direction of high performance, multi-function, lightweight, thin, miniaturization, and low cost. At present,...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08G73/12B32B15/08B32B27/04B32B17/04B32B37/06B32B38/08
Inventor 杨士勇徐红岩杨海霞范琳
Owner INST OF CHEM CHINESE ACAD OF SCI
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