Preparation method for low-dielectric-constant ordered porous polyimide thin film

A polyimide film, low dielectric constant technology, applied in the field of preparation of low dielectric constant ordered porous polyimide film, can solve the problem of SiO2 size, uniformity, dispersion control, air in PI film The problem of uneven pore size distribution, affecting the mechanical properties of PI films, etc., achieves the effect of reducing the linear thermal expansion coefficient, reducing the linear thermal expansion coefficient, and uniform pore size distribution.

Active Publication Date: 2017-05-31
HANGZHOU FIRST APPLIED MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method does not affect the SiO 2 The size, uniformity, and dispersion of the PI film are controlled, and the air hole pore size distribution in the PI film is not uniform, which affects the mechanical properties of the PI film.

Method used

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  • Preparation method for low-dielectric-constant ordered porous polyimide thin film
  • Preparation method for low-dielectric-constant ordered porous polyimide thin film
  • Preparation method for low-dielectric-constant ordered porous polyimide thin film

Examples

Experimental program
Comparison scheme
Effect test

Synthetic example 1

[0045] Silica microspheres with a diameter of 100 nm (named SiO 2 -100), prepared according to the following experimental steps:

[0046] In 90ml ethanol solution, add 28.5wt% concentrated ammonia water and deionized water in turn, keep the temperature at 25°C, and stir for 0.5-2h to ensure the uniform dispersion of the solute in the ethanol solution and the uniform temperature. Then add a certain amount of tetraethyl orthosilicate (TEOS) into the solution, and continue to stir rapidly for 6-12 hours to form a white translucent colloidal solution. The molar ratio of each substance in the synthetic mother liquor is TEOS:NH 3 :H 2 O:EtOH=1:4.4:16:100. After the stirring is completed, centrifuge with a high-speed centrifuge, and wash the precipitate with ethanol three times. Dry the obtained solid in an oven at 65-80°C for 12-24h, and grind it into powder to obtain SiO 2 -100. After testing, its diameter is 100nm.

Synthetic example 2-4

[0048] Silica microspheres with diameters of 200nm, 50nm and 30nm (named as SiO 2 -200, SiO 2 -50 and SiO 2 -30), prepared according to the experimental procedure in [Synthesis Example 1]; but the synthesis temperature in ethanol solution was changed to 20°C, 27°C and 35°C.

Synthetic example 5

[0050] Aminopropyl-modified silica microspheres with a diameter of 100 nm (named APro-SiO 2 -100), made of SiO 2 -100 was obtained by surface modification with amino functional groups. The specific processing steps are as follows:

[0051] In 60ml of toluene, add 1g of SiO synthesized in [Synthesis Example 1] 2 -100, stir well. Add aminopropyltrimethoxysilane (APS), concentrated hydrochloric acid and glacial acetic acid successively, and the molar ratio of each substance in the synthesis mother liquor is: SiO 2 :APS:HCl:HAc:H 2 O: Toluene=1:0.15:0.072:0.24:0.25:34; SiO 2 The molar mass of -100 is 60 g mol -1 . The above solution was stirred at reflux at 110°C for 12-24h. Then cool down to room temperature, centrifuge on a high-speed centrifuge, and wash the precipitate three times with ethanol. Dry the obtained solid in an oven at 65-80°C for 12-24h, and then age it in a muffle furnace at 250°C for 3-6h to obtain APro-SiO 2 -100. After testing, its diameter is 100nm...

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Abstract

The invention discloses a preparation method for a low-dielectric-constant ordered porous polyimide thin film. The method comprises the steps that amino-modified silicon dioxide microspheres are prepared, then, polyimide is grafted onto the surfaces of the amino-modified silicon dioxide microspheres in the form of chemical bonds, a polyimide compound thin film is prepared, silicon dioxide is etched away in a hydrofluoric acid etchant, washing and drying are conducted, and then the low-dielectric-constant ordered porous polyimide thin film is obtained. According to the method, air holes which have the hole diameters ranging from 30 nm to 200 n, are uniform in size distribution and are uniformly distributed in the thin film are introduced into the polyimide thin film, the dielectric constant of the polyimide thin film is lowered, and meanwhile due to the fact that the hole diameters are small, and distribution of the air holes inside the thin film is uniform, the polyimide thin film keeps the high mechanical property and breakdown voltage. The preparation method has the advantages of being low in dielectric constant, high in breakdown voltage, good in mechanical property and capable of lowering the thermal expansion coefficient, and has potential application value and good application prospects in a high-frequency, high-speed and high-density integrated circuit.

Description

technical field [0001] The invention belongs to the field of polymer materials, and relates to a method for preparing a low dielectric constant ordered porous polyimide film used in high-frequency, high-speed, high-density integrated circuits. Background technique [0002] High-speed, high-frequency, and high-density have become the main directions for the development of printed circuit boards (PCBs), flexible printed circuit boards (FPCs) and large-scale integrated circuits. In this context, in integrated circuits with polyimide film as the insulating base layer, since the dielectric constant of conventional polyimide (PI) film remains high above 3.4, signal capacitance delay and signal transmission delay , enhanced interference, increased power loss and other issues have become increasingly prominent, limiting the high-speed and high-frequency transmission performance of signals in electronic components. In order to meet the high-speed signal transmission and further impr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08J9/26C08G73/10C01B33/18C08L79/08
CPCC01B33/18C01P2004/32C01P2004/62C01P2004/64C08G73/105C08G73/1053C08G73/1064C08G73/1067C08G73/1071C08J5/18C08J9/26C08J2379/08
Inventor 周慧曹肖李奇琳童荣柏周光大林建华
Owner HANGZHOU FIRST APPLIED MATERIAL CO LTD
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