Preparation method for hyperbranched polymide film with low dielectric constant

Abstract

The invention relates to a preparation method for a hyperbranched polymide film with the low dielectric constant. A series of the low-dielectric constant PI films with a hyperbranched structure are synthesized by taking 2,4,6-triaminopyrimidine (TAP) as a branching center through a one-step method. Through introduction of the hyperbranched structure, the dielectric constant of the PI film is significantly lowered, the inherent advantages of PI are better kept, and the good mechanical strength and thermo-oxidative stability are supplied to the film. The hyperbranched structure contains a large quantity of molecular chain end groups, dense packing of molecular chains is effectively inhibited, and therefore the hyperbranched PI film has the excellent dissolution characteristic to be more prone to be processed into a complex device. Compared with a Kapton standard film which is generally used at present, under the same testing conditions, the dielectric constant of the hyperbranched PI film prepared through the method is lowered by 20%-40%, the lowest dielectric constant even gets close to 2.0 and reaches the ultralow dielectric constant level, and the urgent demand for micro-electronic industry development in future can be met.

Description

technical field

[0001] The invention belongs to a method for preparing a hyperbranched polyimide film, in particular to a method for preparing a hyperbranched polyimide film with a low dielectric constant. Background technique

[0002] In today's information age, with the rapid development of science and technology, electronic products are developing in the direction of multi-function, high performance and portability. In order to meet the needs of the microelectronics industry, it is increasingly important to design high-performance VLSIs. With the continuous increase of wiring density in integrated circuits and the continuous shrinking of microprocessors, problems such as signal delay, inter-line interference and power dissipation caused by resistance-capacitance hysteresis (RCdelay) have become increasingly prominent. The feature size of microelectronic devices depends on the dielectric constant (Dk) of the intermetal dielectric in integrated circuits. The smaller the f...

Examples

Embodiment 1

[0041] Add 0.8342g of 2,4,6-triaminopyrimidine (TAP), 2.9422g of BPDA and 15g of o-cresol to the reaction vessel equipped with mechanical stirring successively, protect with argon, turn on the stirring and cool down the system until the temperature of the system drops to 5 ℃, add 0.25g quinoline, continue to stir for 4h, then react at 70℃ for 3h, and then raise the system temperature to 140℃ for 24h; after the reaction, when the system is cooled to 25℃, pour the reaction solution into 140mL methanol A solid product was precipitated in , and the crude product F was obtained after filtration. The crude product F was washed 3 times with 60 mL of methanol to afford the product G. The product G was extracted with 70 mL methanol for 24 h in a Soxhlet extractor to obtain product H. Dry the product H in a vacuum oven for 12 hours with the temperature controlled at 120°C to obtain product J; dissolve 1 g of product J in 19 g of chloroform, filter through a tetrafluoro filter element w...

Embodiment 2

[0043] Add 0.4171g of 2,4,6-triaminopyrimidine (TAP), 2.0526g of BAPP, 2.9422ga-BPDA and 16g of p-cresol to the reaction vessel equipped with mechanical agitation in sequence. When the temperature of the system drops to 1°C, add 0.4g of isoquinoline, continue to stir for 5h, then react at 80°C for 4h, then raise the temperature of the system to 160°C, and react for 30h; after the reaction, when the system is cooled to 25°C The reaction solution was poured into 130 mL of ethanol to precipitate a solid product, and the crude product F was obtained after filtration. The crude product F was washed 4 times with 50 mL of ethanol to obtain product G. Product G was extracted with 65 mL ethanol for 30 h in a Soxhlet extractor to obtain product H. Dry the product H in a vacuum oven for 15 hours with the temperature controlled at 130°C to obtain product J; dissolve 2 g of product J in 32 g of dichloromethane, filter through a tetrafluoro filter element with a pore size of 220 nm, and po...

Embodiment 3

[0045] Add 0.5005g of 2,4,6-triaminopyrimidine (TAP), 1.3371g of 6FBA, 3.1022g of ODPA and 12g of m-cresol in sequence to the reaction vessel equipped with mechanical stirring, protect with argon, turn on the stirring and cool down the system. When the temperature drops to 4°C, add 0.5g of benzoic acid, continue to stir for 7h, then react at 85°C for 5h, then raise the temperature of the system to 180°C, and react for 35h; Pour into 100mL of n-propanol to precipitate a solid product, and obtain the crude product F after filtration. The crude product F was washed 5 times with 40 mL of n-propanol to obtain product G. Product G was extracted with 50 mL n-propanol for 35 h in a Soxhlet extractor to obtain product H. Dry the product H in a vacuum oven for 18 hours with the temperature controlled at 140°C to obtain product J; dissolve 2 g of product J in 45 g of tetrahydrofuran, filter through a tetrafluoro filter element with a pore size of 220 nm, and pour it on a glass plate adj...

technical field

[0001] The invention belongs to a method for preparing a hyperbranched polyimide film, in particular to a method for preparing a hyperbranched polyimide film with a low dielectric constant. Background technique

[0002] In today's information age, with the rapid development of science and technology, electronic products are developing in the direction of multi-function, high performance and portability. In order to meet the needs of the microelectronics industry, it is increasingly important to design high-performance VLSIs. With the continuous increase of wiring density in integrated circuits and the continuous shrinking of microprocessors, problems such as signal delay, inter-line interference and power dissipation caused by resistance-capacitance hysteresis (RCdelay) have become increasingly prominent. The feature size of microelectronic devices depends on the dielectric constant (Dk) of the intermetal dielectric in integrated circuits. The smaller the f...

Examples

Embodiment 1

[0041] Add 0.8342g of 2,4,6-triaminopyrimidine (TAP), 2.9422g of BPDA and 15g of o-cresol to the reaction vessel equipped with mechanical stirring successively, protect with argon, turn on the stirring and cool down the system until the temperature of the system drops to 5 ℃, add 0.25g quinoline, continue to stir for 4h, then react at 70℃ for 3h, and then raise the system temperature to 140℃ for 24h; after the reaction, when the system is cooled to 25℃, pour the reaction solution into 140mL methanol A solid product was precipitated in , and the crude product F was obtained after filtration. The crude product F was washed 3 times with 60 mL of methanol to afford the product G. The product G was extracted with 70 mL methanol for 24 h in a Soxhlet extractor to obtain product H. Dry the product H in a vacuum oven for 12 hours with the temperature controlled at 120°C to obtain product J; dissolve 1 g of product J in 19 g of chloroform, filter through a tetrafluoro filter element w...

Embodiment 2

[0043] Add 0.4171g of 2,4,6-triaminopyrimidine (TAP), 2.0526g of BAPP, 2.9422ga-BPDA and 16g of p-cresol to the reaction vessel equipped with mechanical agitation in sequence. When the temperature of the system drops to 1°C, add 0.4g of isoquinoline, continue to stir for 5h, then react at 80°C for 4h, then raise the temperature of the system to 160°C, and react for 30h; after the reaction, when the system is cooled to 25°C The reaction solution was poured into 130 mL of ethanol to precipitate a solid product, and the crude product F was obtained after filtration. The crude product F was washed 4 times with 50 mL of ethanol to obtain product G. Product G was extracted with 65 mL ethanol for 30 h in a Soxhlet extractor to obtain product H. Dry the product H in a vacuum oven for 15 hours with the temperature controlled at 130°C to obtain product J; dissolve 2 g of product J in 32 g of dichloromethane, filter through a tetrafluoro filter element with a pore size of 220 nm, and po...

Embodiment 3

[0045] Add 0.5005g of 2,4,6-triaminopyrimidine (TAP), 1.3371g of 6FBA, 3.1022g of ODPA and 12g of m-cresol in sequence to the reaction vessel equipped with mechanical stirring, protect with argon, turn on the stirring and cool down the system. When the temperature drops to 4°C, add 0.5g of benzoic acid, continue to stir for 7h, then react at 85°C for 5h, then raise the temperature of the system to 180°C, and react for 35h; Pour into 100mL of n-propanol to precipitate a solid product, and obtain the crude product F after filtration. The crude product F was washed 5 times with 40 mL of n-propanol to obtain product G. Product G was extracted with 50 mL n-propanol for 35 h in a Soxhlet extractor to obtain product H. Dry the product H in a vacuum oven for 18 hours with the temperature controlled at 140°C to obtain product J; dissolve 2 g of product J in 45 g of tetrahydrofuran, filter through a tetrafluoro filter element with a pore size of 220 nm, and pour it on a glass plate adj...

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