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A kind of polyimide resin containing cyano group and its application in preparing copper-clad foil

A technology of polyimide resin and copper clad foil, which is applied in the field of copper clad foil, can solve the problems of low heat resistance and mechanical properties of copper clad foil, large difference in thermal expansion coefficient, small bonding ability, etc., and achieve good size Stability and mechanical properties, extended service life, easily controlled effects

Inactive Publication Date: 2018-03-09
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the polyimide resin used in the 2L-FCCL resin base film layer is divided into thermosetting polyimide resin (PI) and thermoplastic polyimide resin (TPI). The former has excellent thermal stability and mechanical properties, but it is not compatible with metal substrates. The bonding ability between them is small, the adhesion is low and the flexibility is insufficient; the latter has strong adhesion to the metal substrate, but the existence of flexible groups makes the heat resistance and mechanical properties of the prepared copper clad foil relatively low, reports Some people adopt the method of combining thermoplastic and thermosetting polyimide and pressing it into copper clad foil (WO2007083526A1), that is, coating thermoplastic polyimide resin on both sides of thermosetting polyimide, and hot pressing with copper foil on both sides to form a double-sided copper-clad foil. Adhesive flexible copper clad foil, theoretically not only enhances the adhesion between the resin base film and copper foil, but also ensures the heat resistance, mechanical properties and dimensional stability of the resin layer itself, but the combination of PI and TPI The method can only prepare double-sided flexible copper-clad foil, and the coefficient of thermal expansion (CTE) between PI and TPI layers is quite different, and the copper-clad foil will be delaminated and exploded during soldering.

Method used

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  • A kind of polyimide resin containing cyano group and its application in preparing copper-clad foil
  • A kind of polyimide resin containing cyano group and its application in preparing copper-clad foil
  • A kind of polyimide resin containing cyano group and its application in preparing copper-clad foil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] This example is to prepare a two-layer adhesive-free single-sided flexible copper-clad foil. In the general formula of the PI layer structure, when Ar is a biphenyl structure, X is a biphenyl structure, Y is a diphenyl ether structure, and the circled Ar' It is polyamic acid (PAA) and flexible copper clad foil material with 3,3',4,4'-biphenyltetraacid dianhydride structure, a=0.4, b=0.3, c=0.3.

[0033] 1) Pretreat the surface of the copper foil, first soak the copper foil in CH 2 Cl 2 , ultrasonic treatment for 0.5h to remove the surface grease of the copper foil, soak the soaked copper foil in 0.5mol / L dilute sulfuric acid for 4h to remove the oxide on the surface of the copper foil, wash 3 times with distilled water and 3 times with absolute ethanol, drying;

[0034] 2) Preparation of PAA solution

[0035]Weigh 0.8369g (2mmol) of 1,4-bis(4-amino-2cyanophenoxy)biphenyl, 0.2764g (1.5mmol) of benzidine, and 0.3004g (1.5mmol) of diphenyl ether diamine and dissolve it ...

Embodiment 2

[0041] Referring to Example 1, weigh 8.369 g (20 mmol) of 1,4-bis(4-amino-2 cyanophenoxy) biphenyl, 2.764 g (15 mmol) of benzidine, and 3.004 g (15 mmol) of diphenyl ether diamine Dissolve in 174mL of N,N-dimethylacetamide solution at room temperature (DMAC input according to 15% of the solid content of the system mass), stir for 20min until completely dissolved, add 3,3',4,4'- Biphenyltetraic dianhydride 14.711g (50mmol), keep the system in an anhydrous, clean and nitrogen environment, stir at 0°C for 48h, at this time the reaction bottle is a light yellow transparent viscous liquid, dilute and stir with DMAC for 4h After cleaning, drying, and standing at room temperature for 24 hours, a PAA solution with a concentration of 0.074g / ml was obtained.

[0042] The following steps follow the operation of Example 1 to obtain a two-layer adhesive-free single-sided flexible copper-clad foil. The performance parameters of the obtained flexible copper-clad foil and the performance para...

Embodiment 3

[0044] Referring to Example 1, 2) in the step, N,N-dimethylacetamide (DMAC) solution was replaced by N-methylpyrrolidone, and the amount added was 15.9mL (DMAC input according to 15% of the solid content of the system mass), The rest of the operations remain the same. When step 3) is performed, transfer the copper foil coated with PAA solution to a clean, dry and flat environment for drying according to the following procedures: 60°C for 24 hours, 80°C for 24 hours, and 120°C for 2 hours , dried at 150°C for 1 hour, and the rest of the operations were kept the same to obtain a two-layer flexible copper-clad foil with no adhesive on one side. Compared with Example 1, the linear expansion coefficient of the PI resin layer of the flexible copper-clad foil obtained was slightly increased. The CTE value is 33.24ppm / K.

[0045] The above-mentioned two-layer adhesive-free single-sided flexible copper-clad foil resin surface and the flat rolled copper foil with a thickness of 20 μm (e...

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Abstract

The invention discloses a polyimide resin containing cyano groups, and applications thereof in preparing double-layer adhesive-free single-surface (double-surface) flexible copper-clad laminates (FCCL), and belongs to the technical field of copper-clad laminates. A preparation method comprises following steps: a diamine containing side chain cyano groups and rigid-flexible chain structures is mixed with a dianhydride with a different structure at a molar ratio of 1:1; a polyamide acid (PAA) solution is prepared via reaction in an aprotic polar solvent; metal substrates such as copper foil or copper plates are coated with the PAA solution uniformly, and pre-imidization is carried out at 60 to 160 DEG C so as to obtain a polyimide pre-polymer resin film material; the polyimide pre-polymer resin film material is subjected to complete thermal imidization at 180 to 350 DEG C under vacuum conditions so as to obtain the double-layer adhesive-free single-surface flexible copper-clad laminates. The polyimide resin containing side chain cyano groups and rigid-flexible chain structures possesses low linear expansion coefficient, high peel strength with copper substrates, and excellent dimensional stability and flexural endurance. The double-layer adhesive-free single-surface flexible copper-clad laminates are prepared via coating method, so that delamination caused by large difference of CTE (Coefficient Of Thermal Expansion) value among PI (polyimide resin) and TPI (thermoplastic polyimide) layers is avoided.

Description

technical field [0001] The invention belongs to the technical field of copper-clad foil, and in particular relates to a cyano-containing polyimide resin and its application in the preparation of two-layer adhesive-free single-sided or double-sided flexible copper-clad foil. Background technique [0002] Flexible copper clad foil (FCCL) can be divided into three-layer flexible copper clad foil (3L-FCCL) and two-layer flexible copper clad foil (2L-FCCL) according to the structure. 3L-FCCL is composed of copper foil, adhesive and resin The composition of the base film is the earliest commercialized flexible copper-clad foil category, of which the adhesive layer is an important component, which directly affects the performance and service life of the product. Currently, the adhesive in the 3L-FCCL industry is mainly divided into acrylic There are two major schools of adhesives and epoxy resin adhesives, but whether it is acrylic adhesives or epoxy resin adhesives, the long-term ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10B32B15/08B32B15/20B32B27/06B32B27/28
CPCB32B15/08B32B15/20B32B27/06B32B27/281C08G73/1007C08G73/1042C08G73/1071
Inventor 刘佰军沈艳超李晓白刘振超姜振华
Owner JILIN UNIV
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