A kind of polyimide nano-foam and preparation method thereof

A polyimide and nano-foam technology, applied in the field of polyimide, can solve the problems of lower glass transition temperature of materials, disordered distribution of product pores, unstable performance of various properties, etc. Polarizability, the effect of reducing the dielectric constant

Active Publication Date: 2019-12-27
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the former uses highly corrosive HF, and the process is difficult; while the latter replaces highly corrosive HF with dilute hydrochloric acid, although its operability is increased, but most of the pores of the porous polyimide film are obtained by etching. Unicom, and the material prepared by this method has more defects, resulting in a larger water absorption
The Chinese patent application number 201220023402.X obtains different composite polyimide resin solutions by adding porogens of different particle sizes to polyimide resins respectively, and then composites them into multi-layer films. Wash off the porogen with acid to obtain a multi-layer structure porous polyimide film; however, the distribut

Method used

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  • A kind of polyimide nano-foam and preparation method thereof
  • A kind of polyimide nano-foam and preparation method thereof
  • A kind of polyimide nano-foam and preparation method thereof

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preparation example Construction

[0048] The invention provides a kind of preparation method of polyimide nano-foam, comprises the following steps:

[0049] a) react after diamine compound, dianhydride compound and heat unstable substance are mixed in a solvent to obtain a polyimide film; the diamine compound includes diamine containing adamantane group and polysiloxane di amine;

[0050] b) thermally decomposing the polyimide film obtained in step a) to obtain polyimide nano foam.

[0051] In the invention, the diamine compound, the dianhydride compound and the thermally unstable substance are mixed in a solvent and then reacted to obtain a polyimide film. In the present invention, the diamine compound includes adamantane group-containing diamine and polysiloxane diamine. In the present invention, the diamine containing adamantane group is preferably selected from one or more of the structures shown in formula (I-1) to formula (I-9);

[0052]

[0053]

[0054] The present invention has no special lim...

Embodiment 1

[0091] (1) 15.92g (0.05mol) of diamine containing adamantyl groups having a structure shown in formula (I-1), 10.01g (0.05mol) of 4,4'-diaminodiphenyl ether and 5.69g ( 0.0057mol) polysiloxane diamine having a structure shown in formula (II-1) with an average molecular weight of 1000g / mol was added to 250mL DMAc and 150mL DMF mixed solution, stirred and dissolved, and then 34.05g (0.1057mol)3 was added , 3', 4, 4'-benzophenone tetracarboxylic dianhydride, stirring at room temperature for 24h, to obtain a polyamic acid solution with a solid content of 15%; The thermally unstable substance with the structure shown in IV-10) is added to the above polyamic acid solution to disperse evenly to obtain a mixed solution; then the above mixed solution is cast on the substrate and cured at a humidity of 28% and a temperature of 80°C After 10 hours, a polyamic acid film was obtained; then, the polyamic acid film was raised from room temperature to 300° C. at a rate of 5° C. / min under a ni...

Embodiment 2

[0100] (1) 17.52g (0.05mol) of diamine containing adamantyl groups having a structure shown in formula (I-4), 5.00g (0.025mol) of 3,4'-diaminodiphenyl ether, 6.56g ( 0.025mol) 2,5-bis (4-aminophenyl) pyrimidine, 2.91g (0.0039mol) average molecular weight is the thermolabile substance with structure shown in formula (IV-6) and 5.69g (0.00285 mol) The polysiloxane diamine having the structure shown in formula (II-1) with an average molecular weight of 2000g / mol was added to 350mL NMP and 200mL DMF mixed solution, stirred and dissolved, and then added 33.12g (0.10675mol) 3, 3', 4, 4'-diphenyl ether tetracarboxylic dianhydride, stirred at room temperature for 24 hours to obtain a polyamic acid solution with a solid content of 11%; then cast the above polyamic acid solution on a substrate, and 20% at 100°C for 12 hours to obtain a polyamic acid film; then raise the above polyamic acid film from room temperature to 300°C at a rate of 5°C / min under nitrogen atmosphere and keep it for...

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Abstract

The invention provides a polyimide nano foam and a preparation method thereof. The preparation method comprises the following steps: a) reacting a diamine compound, a dianhydride compound and a thermally unstable substance in a solvent to obtain a polyimide nano foam imide film; the diamine compound includes diamine and polysiloxane diamine containing adamantane groups; b) thermally decomposing the polyimide film obtained in step a) to obtain polyimide nano Foam. The present invention adopts the diamine compound including diamine containing adamantane group and polysiloxane diamine as raw material to prepare polyimide nano foam, innovatively introduces polysiloxane structure into polyimide containing adamantane group In the imide molecular chain, the introduced polysiloxane soft segment and the polyimide rigid segment containing adamantane group produce microphase separation, thereby increasing the free volume of the molecule, reducing the polarizability of the molecule, and effectively reducing The dielectric constant and water absorption of the product; increasing the surface tension of the system is conducive to the formation of cells.

Description

technical field [0001] The invention relates to the technical field of polyimide, and more specifically, relates to a polyimide nano-foam and a preparation method thereof. Background technique [0002] At present, with the rapid development of integrated circuits in the field of microelectronics, especially VLSI, microelectronic devices are becoming smaller and smaller, and the number of transistors integrated on a chip is increasing. Therefore, the density of interconnection wiring on the chip is increasing, and the interconnection resistance, inter-line capacitance, and line power consumption increase, resulting in signal transmission delays and even signal distortions such as crosstalk. According to the formula (1) (R is the wire resistance, C is the intralayer and interlayer capacitance, L is the wire length, P is the metal spacing, T is the metal thickness, ρ is the metal resistivity, and k is the dielectric constant of the insulating layer; Dielectric films for advanc...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08G73/10C08J9/00C08J5/18
CPCC08G73/1078C08G73/1085C08J5/18C08J9/00C08J2379/08C08L79/08
Inventor 邱雪鹏吕朋霞董志鑫代学民矫龙
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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