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Polyimide nano-foam and preparation method thereof

A polyimide and nano-foam technology, applied in the field of materials, can solve problems such as reduction, and achieve the effects of increasing molar volume, excellent mechanical properties, and increasing Tg

Active Publication Date: 2016-08-03
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the inorganic particles act as a nucleating agent to make the distribution of pores more uniform, but the porous material obtained by this method is a multi-connected through hole. In the process, the inert gas produces a plasticizing effect on the polyimide matrix, resulting in Material T g reduce

Method used

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  • Polyimide nano-foam and preparation method thereof

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[0032] The invention provides a kind of preparation method of polyimide nano-foam, it is characterized in that, comprises the following steps:

[0033] A) Polymerizing diamine compounds containing adamantyl groups, diamine compounds not containing adamantyl groups, and dianhydride compounds in a solvent to obtain a polyamic acid solution;

[0034] B) mixing the thermally unstable compound with the polyamic acid solution, followed by uniform dispersion, casting, curing and thermal imidization to obtain a polyimide film;

[0035] C) thermally decomposing the polyimide film to obtain polyimide nano foam.

[0036] In the present invention, the adamantane-containing diamine compound, the adamantane-free diamine compound and the dianhydride compound are polymerized in a solvent to obtain a polyamic acid solution.

[0037] In the present invention, the temperature of the polymerization reaction is preferably 20-40°C, more preferably the reaction is carried out at 20-30°C. The solvent...

Embodiment 1

[0079] Add 15.924g (0.05mol) of 2,2'-bis(4-aminophenyl)adamantane (I-1) into 340ml of N,N'-dimethylacetamide solution, stir and dissolve, then add 10.01g ( 0.05mol) 4,4'-diaminodiphenyl ether, stirred and dissolved, then added 31.021g (0.1mol) 3,3',4,4'-diphenyl ether tetracarboxylic dianhydride, and stirred at room temperature for 24 hours to obtain To the polyamic acid solution, 8.543 g of polyethylene glycol (III-10) with an average molecular weight of 600 was added and dispersed uniformly by ultrasonic to obtain a mixed solution with a solid content of 15%. The mixed solution was cast on the substrate, and cured for 10 h at a humidity of 30% and a temperature of 80° C. to obtain a polyamic acid film. The polyamic acid film was placed in a heating device under nitrogen, and the temperature was raised from room temperature to 300° C. at a rate of 3° C. / min, and kept for 1 hour to obtain a polyimide film.

[0080] The above polyimide film was raised from 50°C to 100°C at a h...

Embodiment 2

[0082]Add 15.924g (0.05mol) of 2,2'-bis(4-aminophenyl)adamantane (I-1) into 350ml of N,N'-dimethylacetamide solution, stir and dissolve, then add 10.01g ( 0.05mol) 4,4'-diaminodiphenyl ether, after stirring and dissolving, add 2.907g (III-1) of polyethylene glycol diaminobenzoate (III-1) with an average molecular weight of 750, add 3 , 32.223g (0.1039mol) of 3′,4,4′-diphenyl ether tetracarboxylic dianhydride was stirred at room temperature for 24 hours to obtain a polyamic acid solution. The polyamic acid solution was cast onto a glass sheet, and cured for 10 h at a humidity of 20% and a temperature of 100° C. to obtain a polyamic acid film. The polyamic acid film was placed in a heating device under nitrogen, raised from room temperature to 300°C at a rate of 5°C / min, and kept for 0.5h to obtain a polyimide film.

[0083] The above polyimide film was raised from room temperature to 250°C at a heating rate of 1°C / min in an air atmosphere, and kept for 4 hours, and then raised...

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Abstract

The invention provides polyimide nano-foam and a preparation method thereof .The preparation method includes the following steps that firstly, a diamine compound containing admantyl groups, a diamine compound containing no admantyl group and a dianhydride compound are subjected to a polymerization reaction in a solvent, and a polyamide acid solution is obtained; secondly, a compound with thermal instability and the polyamide acid solution are subjected to uniform dispersion or a polymerization reaction, tape casting, curing and thermal imidization in sequence, and a polyimide film is obtained; thirdly, the polyimide film is subjected to thermal decomposition, and the polyimide nano-foam is obtained .As the admantyl groups are large-size groups, the molar volume of atomic groups is increased, then the dielectric constant of a polyimide matrix is effectively reduced, and accordingly the dielectric constant of the polyimide nano-foam material is reduced; besides, by introducing the admantyl groups, the glass-transition temperature of polyimide is increased, and the thermal stability of the material is improved .Moreover, the polyimide nano-foam has good mechanical properties.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a polyimide nano foam and a preparation method thereof. Background technique [0002] Currently, with the rapid development of the integrated circuit (IC) industry, the number of transistors integrated on a chip is increasing, and at the same time, microelectronic devices are becoming smaller and smaller. Under these dual effects, the density of interconnection wiring on the chip is increasing, and the interconnection resistance and inter-line capacitance increase, resulting in signal transmission time delay and even signal distortion. The "International Semiconductor Technology Development Blueprint" revised by the International Semiconductor Industry Association in 2009 predicts that in order to meet the future development of the IC industry, the dielectric constant of the insulating layer must be <2.0. However, the dielectric constant value of the bulk materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/00C08J5/18C08G73/10C08L79/08
CPCC08G73/1007C08G73/1071C08J5/18C08J9/0061C08J2379/08
Inventor 邱雪鹏吕朋霞董志鑫代学民
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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