TWI758954B - Polyimide thick film and method for manufacturing the same - Google Patents

Abstract

A method for manufacturing a thick polyimide film includes: providing and heating a first stacked structure, the first stacked structure including a first supporting film and a first polyamic acid coating film coated on the first supporting film; providing and heating a second stacked structure, the second stacked structure including a second supporting film and a second polyamic acid coating film; rewinding the heated first and second stacked structures to obtain a third stacked structure, wherein a first polyamic acid gel film and a second polyamic acid gel film are bonded together to form a third polyamic acid gel film; rewinding two third stacked structures, wherein two third polyamic acid gel films of the two third stacked structures are bonded together to form a fourth polyamic acid gel film; imidizing the fourth acid gel film by heating to obtain the polyimide thick film. The application also provides a polyimide thick film prepared by the above-mentioned preparation method of the polyimide thick film. A polyimide thick film manufactured by the above method is also disclosed.

Description

Polyimide thick film and preparation method thereof

The present application relates to the field of polyimide films, in particular to a thick polyimide film and a preparation method thereof.

The polyimide film is generally obtained by casting polyimide onto a steel belt for drying to form a semi-solid film, and then peeling the semi-solid film from the steel belt, pulling the film, imidizing and winding. Among them, polyamide needs to be dried for a certain period of time before forming a semi-solid film. When the thickness of the polyimide film exceeds 200 μm, in order to allow the polyimide to be dried, the winding speed of the polyimide film needs to be reduced to less than 1 m/min, which reduces the processing efficiency; and the existing equipment cannot manufacture the thickness Polyimide films over 400μm.

In view of this, it is necessary to provide a method for preparing a thick polyimide film that solves the above technical problems.

The present application provides a method for preparing a thick polyimide film, including the following steps: providing a first laminated structure and heating the first laminated structure, wherein the first laminated structure includes a first carrier film and a coating to form a the first polyamic acid coating film on the first carrier film, the first polyamic acid coating film is heated to form a first polyamic acid adhesive film; a second laminated structure is provided and the first polyamic acid coating film is heated; The two laminated structure is heated, wherein the second laminated structure includes a second carrier film and a second polyamide coating film coated and formed on the second carrier film, the second polyamide coating film heated to form the dimerized urethane adhesive film; rewinding the heated first laminate structure and the heated second laminate structure to obtain a third laminate structure, wherein the first urethane adhesive film and the second urethane adhesive The films are adhered to form a third polyamic acid film; the two and third laminated structures are rewound, wherein the two and third polyamic acid films are adhered to form a fourth polyamic acid film; The fourth polyimide adhesive film is imidized to obtain the polyimide thick film.

The present application also provides a polyimide thick film prepared by the above-mentioned preparation method of the polyimide thick film.

In the method for preparing a thick polyimide film provided by the present application, a third polyimide film is obtained by rewinding the first polyimide film and the second polyimide film, and then a plurality of Rewinding the third polyurethane adhesive film can obtain a fourth polyamic acid adhesive film with a larger thickness. Since the thicknesses of the first polyamic acid adhesive film and the second polyamic acid adhesive film are relatively small, the time for heating and curing the polyamic acid can be reduced, thereby improving the processing efficiency.

10: The first layered structure

11: The first carrier film

13: The first polyamide coating film

15: The first polyamide film

210: The first unwinding device

230: The first coating device

250: First Oven

270: The first winding device

20: Second Laminated Structure

21: Second carrier film

23: The second polyamide coating film

25: The second polyamide film

310: The second unwinding device

330: Second coating device

350: Second oven

30: Third Laminated Structure

35: The third polyamide film

420: The first bonding roller

430: The third unwinding device

450: The second winding device

40: The fourth polyamide film

510: Fourth unwinding device

530: Second bonding roller

550: The third winding device

100: Polyimide thick film

FIG. 1 is a schematic diagram of the preparation of a first laminated structure provided by an embodiment of the present application.

FIG. 2 is a schematic diagram of rewinding the first laminated structure and the second laminated structure according to an embodiment of the present application.

FIG. 3 is a schematic diagram of rewinding the second and third stacked structures according to an embodiment of the present application.

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the protection scope of the present invention.

It should be noted that, unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the technical field of the present invention. The terms used in the embodiments of the present invention are only for the purpose of describing a particular embodiment, and are not intended to limit the present invention.

Referring to FIG. 1 , in step S1 , a first stacked structure 10 is provided, and the first stacked structure 10 is heated. Wherein, the first laminated structure 10 includes a first carrier film 11 and a first polyamic acid coating film 13 coated and formed on the first carrier film 11 , and the first polyamic acid coating film 13 is coated with Heating to form the first polyamide adhesive film 15 .

Specifically, step S1 includes: transferring the first carrier film 11 from the first unwinding device 210 to the first winding device 270 through the first coating device 230 and the first oven 250 in sequence, wherein the polyamide acid solution is passed through the first winding device 270. The first coating device 230 coats the first carrier film 11 to form the first polyurethane coating film 13 . After being heated and baked in the first oven 250 , part of the solvent in the first polyamic acid coating film 13 is removed to form the first polyamic acid adhesive film 15 . The first winding device 270 is used for winding the first laminated structure 10 after heating and baking.

The polyamic acid solution is formed by mixing and reacting dianhydride monomer, diamine monomer and organic solvent. The dianhydride monomer can be selected from tetrabenzoic dianhydride (PMDA), 4,4'-(hexafluoroisopropene)diphthalic anhydride (6FDA), 1,2,3,4-cyclobutanetetracarboxylic acid At least one of dianhydride (CBDA). The diamine monomer can be selected from 4,4'-diaminodiphenyl ether (ODA), p-phenylenediamine (p-PDA), 3,5-diamino-1,2,4-triazole (DTZ) at least one. The organic solvent is selected from at least one of dimethylacetamide (DMAc), N-methylpyrrolidone (NMP) and N,N-dimethylformamide (DMF).

Referring to FIG. 2 , in step S2 , a second stacked structure 20 is provided, and the second stacked structure 20 is heated. Wherein, the second laminated structure 20 includes a second carrier film 21 and a second polyamide coating film 23 coated and formed on the second carrier film 21. The second polyamide coating film 23 is coated with The second polyamide film 25 is formed by heating.

Specifically, step S2 includes: transferring the second carrier film 21 from the second unwinding device 310 through the second coating device 330 to the second oven 350 for heating, wherein the polyamic acid solution is heated through The second polyamide coating film 23 is formed by coating on the second carrier film 21 by the second coating device 330 . After being heated and baked in the second oven 350 , part of the solvent in the second polyamic acid coating film 23 is removed to form the second polyamic acid adhesive film 25 .

In an optional embodiment, the heating and baking temperatures of the first oven 250 and the second oven 350 are both 110 to 150° C., and the first polyamide film 15 and the second The content of the solvent in the polyamide film 25 is 30-45%.

In an optional embodiment, the first carrier film 11 and the second carrier film 21 are both release films to facilitate peeling of the polyimide film.

Referring to FIG. 2, in step S3, the heated first laminated structure 10 and the second laminated structure 20 are rewound to obtain a third laminated structure 30, wherein the first polyurethane adhesive film 15 and the The second polyamic acid adhesive film 25 is bonded to form a third polyamic acid adhesive film 35 . The third laminated structure 30 includes a third polyamide adhesive film 35 and a first carrier film 11 and a second carrier film 21 located on opposite sides of the third polyamic acid adhesive film 35 .

Specifically, step S3 includes: transferring the heated first laminated structure 10 and the heated second laminated structure 20 to between the two first laminating rollers 420 at the same time, and performing the pressing action of the two first laminating rollers 420 Next, the first polyamic acid adhesive film 15 and the second polyamic acid adhesive film 25 are pressed together to form the third polyamic acid adhesive film 35 . Wherein, the heated first laminated structure 10 is unwound through the third unwinding device 430, and is directly rewound with the second laminated structure 20 heated by the second oven 350. The third laminated structure 30 It is wound on the second winding device 450 .

Referring to FIG. 3 , in step S4 , the two third laminated structures 30 are rewound, wherein the two third polyamide adhesive films 35 are attached to each other to form a fourth polyamic acid adhesive film 40 .

Specifically, step S4 includes: winding the first carrier films 11 of the two third laminated structures 30 respectively, so that the third polyamide adhesive film 35 is exposed; at the same time, rolling the two third laminated structures 30 from the The second and fourth unwinding devices 510 are transferred between the two second laminating rollers 530, and under the pressing action of the two second laminating rollers 530, the exposed two and third polyurethane adhesive films 35 are pressed together to form The fourth polyamide The acid adhesive film 40; after being pressed by the two second laminating rollers 530, the second carrier films 21 of the two third lamination structures 30 are respectively wound by the third winding device 550, so that the fourth polyamide The acid glue film 40 is exposed.

In an optional embodiment, the temperature ranges of the first bonding roller 420 and the second bonding roller 530 are both from room temperature to 100°C.

Referring to FIG. 3 , in step S5 , the fourth polyimide film 40 is heated for imidization to obtain the polyimide thick film 100 . The thickness of the polyimide thick film 100 exceeds 200μm.

In an optional embodiment, the heating temperature for the imidization of the fourth polyamide adhesive film 40 is 250-400°C.

In an optional embodiment, the thicknesses of the first polyamic acid adhesive film 15 and the second polyamic acid adhesive film 25 both account for the thickness of the fourth polyamic acid adhesive film 40 . quarter. In other embodiments, the thickness ratio of the first polyamic acid film 15 and the second polyamic acid film 25 to the fourth polyamic acid film 40 can be set according to actual needs; It is also possible to rewind more than two third polyamic acid adhesive films 35 to obtain a fourth polyamic acid adhesive film 40 with a required thickness.

Further, before heating the fourth polyamic acid adhesive film 40 , the preparation method further includes the following step: stretching the fourth polyamic acid adhesive film 40 .

In the method for preparing the thick polyimide film provided by the present application, the third polyimide film 35 is obtained by rewinding the first polyimide film 15 and the second polyimide film 25, and then the Rewinding the plurality of third polyamic acid adhesive films 35 can obtain a fourth polyamic acid adhesive film 40 having a larger thickness. Since the thicknesses of the first polyamic acid adhesive film 15 and the second polyamic acid adhesive film 25 are relatively small, the time for heating and curing the polyamic acid can be reduced, thereby improving the processing efficiency.

The polyimide film of the present application will be described below with specific examples.

Example 1

The first carrier film 11 is transferred from the first unwinding device 210 to the first winding device 270 through the first coating device 230 and the first oven 250 in sequence, and the first coating device 230 Coat the polyamic acid solution on the first carrier film 11 to form a first polyamic acid coating film 13 with a thickness of 50 μm. The unwinding speed of the first unwinding device 210 and the first winding device 270 The rewinding speed is 6m/min. The heating and baking temperature of the first oven 250 is 110-150° C., the baking time of the first oven 250 is 2.5 minutes, and the solvent content in the first polyamide film 15 is 30-45° C. %. The man-hour required to prepare the 2000m first polyamide film 15 is 5.6h.

The second carrier film 21 is transferred from the second unwinding device 310 through the second coating device 330 to the second oven 350 for heating, and the second coating device 330 coats the polyamic acid solution A second polyamic acid coating film 23 with a thickness of 50 μm is formed on the second carrier film 21 . Then, the heated second laminated structure 20 and the heated first laminated structure 10 unwound from the third unwinding device 430 are simultaneously conveyed between the two first laminating rollers 420 and then conveyed to the first lamination roller 420. Two rewinding devices 450 . The unwinding speed of the second unwinding device 310 , the unwinding speed of the third unwinding device 430 and the winding speed of the second winding device 450 are all 6 m/min. The heating and baking temperature of the second oven 350 is 110 to 150° C., the baking time of the second oven 350 is 2.5 minutes, and the solvent content in the second polyamide film 25 is 30 to 45 minutes. %. The temperature range of the first bonding roller 420 is from room temperature to 100°C. The thickness of the third polyamic acid adhesive film 35 is 100 μm, and the man-hour required for preparing the 2000 m third polyamic acid adhesive film 35 is 5.6 hours.

The first carrier films 11 of the two and third laminated structures 30 are respectively wound to expose the third polyurethane film 35; at the same time, the two and third laminated structures 30 are respectively released from the two fourth unwinding devices 510 Transferred to between the two second laminating rollers 530 . Then, the second carrier film 21 of the second and third laminate structures 30 is wound by the second and third winding devices 550, and the fourth polyamide film 40 is stretched and imidized in sequence and then wound up. On the fourth winding device 620, the polyimide thick film 100 is obtained. The unwinding speed of the fourth unwinding device 510 The winding speed of the fourth winding device 620 is all 5 m/min. The temperature range of the second bonding roller 530 is room temperature to 100°C. The temperature at which the fourth polyamide film 40 is imidized is 250-400° C., and the time is 5 minutes. The thickness of the polyimide thick film 100 is 200 μm, and the man-hour required to prepare a 1000 m thick polyimide film 100 is 3.5 hours.

Example 2

The first carrier film 11 is transferred from the first unwinding device 210 to the first winding device 270 through the first coating device 230 and the first oven 250 in sequence, and the first coating The cloth device 230 coats the polyamic acid solution on the first carrier film 11 to form the first polyamic acid coating film 13 with a thickness of 100 μm. The unwinding speed of the first unwinding device 210 and the winding speed of the first winding device 270 are both 5 m/min. The heating and baking temperature of the first oven 250 is 110 to 150° C., the baking time of the first oven 250 is 3 minutes, and the solvent content in the first polyamide film 15 is 30 to 45%. . The man-hour required to prepare the 2000m first polyamide film 15 is 6.7h.

The second carrier film 21 is transferred from the second unwinding device 310 through the second coating device 330 to the second oven 350 for heating, and the second coating device 330 coats the polyamic acid solution A second polyamide coating film 23 with a thickness of 100 μm is formed on the second carrier film 21 . Then, the heated second laminated structure 20 and the heated first laminated structure 10 unwound from the third unwinding device 430 are simultaneously conveyed between the two first laminating rollers 420 and then conveyed to the first lamination roller 420. Two rewinding devices 450 . The unwinding speed of the second unwinding device 310 , the unwinding speed of the third unwinding device 430 and the winding speed of the second winding device 450 are all 5 m/min. The heating and baking temperature of the second oven 350 is 110 to 150° C., the baking time of the second oven 350 is 3 minutes, and the solvent content in the second polyamide film 25 is 30 to 45%. . The temperature range of the first bonding roller 420 is from room temperature to 100°C. The thickness of the third polyamic acid adhesive film 35 is 200 μm, and the man-hour required for preparing the 2000 m third polyamic acid adhesive film 35 is 6.7 hours.

The first carrier films 11 of the two and third laminated structures 30 are respectively wound to expose the third polyurethane film 35; at the same time, the two and third laminated structures 30 are respectively released from the two fourth unwinding devices 510 Transferred to between the two second laminating rollers 530 . Then, the second carrier film 21 of the second and third laminate structures 30 is wound by the second and third winding devices 550, and the fourth polyamide film 40 is stretched and imidized in sequence and then wound up. On the fourth winding device 620, the polyimide thick film 100 is obtained. The unwinding speed of the fourth unwinding device 510 The winding speed of the fourth winding device 620 is all 4 m/min. The temperature range of the second bonding roller 530 is room temperature to 100°C. The temperature at which the fourth polyamide film 40 is imidized is 250-400° C., and the time is 6 minutes. The thickness of the polyimide thick film 100 is 400 μm, and the man-hour required to prepare a 1000 m thick polyimide film 100 is 4.4 hours.

Example 3

The first carrier film 11 is transferred from the first unwinding device 210 to the first winding device 270 through the first coating device 230 and the first oven 250 in sequence, and the first coating device 230 Coat the polyamic acid solution on the first carrier film 11 to form a first polyamic acid coating film 13 with a thickness of 150 μm. The unwinding speed of the first unwinding device 210 and the winding speed of the first winding device 270 are both 4 m/min. The heating and baking temperature of the first oven 250 is 110 to 150° C., the baking time of the first oven 250 is 3.8 minutes, and the solvent content in the first polyamide film 15 is 30 to 45 minutes. %. The man-hour required to prepare the 2000m first polyamide film 15 is 8.4h.

The second carrier film 21 is transferred from the second unwinding device 310 through the second coating device 330 to the second oven 350 for heating, and the second coating device 330 coats the polyamic acid solution A second polyamide coating film 23 with a thickness of 150 μm is formed on the second carrier film 21 . Then, the heated second laminated structure 20 and the heated first laminated structure 10 unwound from the third unwinding device 430 are simultaneously conveyed between the two first laminating rollers 420 and then conveyed to the first lamination roller 420. Two rewinding devices 450 . The unwinding speed of the second unwinding device 310 , the unwinding speed of the third unwinding device 430 and the winding speed of the second winding device 450 are all 4 m/min. The heating and baking temperature of the second oven 350 is 110 to 150° C., the baking time of the second oven 350 is 3.8 minutes, and the solvent content in the second polyamide film 25 is 30 to 45 minutes. %. The temperature range of the first bonding roller 420 is from room temperature to 100°C. The thickness of the third polyamic acid adhesive film 35 is 300 μm, and the man-hour required for preparing the 2000 m third polyamic acid adhesive film 35 is 8.4 hours.

The first carrier films 11 of the two and third laminated structures 30 are respectively wound to expose the third polyurethane film 35; at the same time, the two and third laminated structures 30 are respectively released from the two fourth unwinding devices 510 Transferred to between the two second laminating rollers 530 . Then, the second carrier film 21 of the second and third laminate structures 30 is wound by the second and third winding devices 550, and the fourth polyamide film 40 is stretched and imidized in sequence and then wound up. On the fourth winding device 620, the polyimide thick film 100 is obtained. The unwinding speed of the fourth unwinding device 510 The winding speed of the fourth winding device 620 is all 3 m/min. The temperature range of the second bonding roller 530 is room temperature to 100°C. The fourth polyamide film 40 is subjected to The amination temperature was 250-400°C, and the time was 8 min. The thickness of the polyimide thick film 100 is 600 μm, and the man-hour required for preparing a 1000 m thick polyimide film 100 is 5.8 hours.

It can be seen from Examples 1-3 that by using the preparation method of the present application, a thick polyimide film 100 with a thickness of 200-600 μm can be prepared, and the winding speed for preparing the polyimide film is 4-6 m/min.

In addition, those skilled in the art can also make other changes within the spirit of the present invention. Of course, these changes made according to the spirit of the present invention should all be included within the scope of the claimed protection of the present invention.

11: The first carrier film

21: Second carrier film

30: Third Laminated Structure

35: The third polyamide film

40: The fourth polyamide film

510: Fourth unwinding device

530: Second bonding roller

550: The third winding device

100: Polyimide thick film

Claims (10)

A method for preparing a thick polyimide film, comprising the steps of: providing a first laminated structure and heating the first laminated structure, wherein the first laminated structure includes a first carrier film and a coating formed on the a first polyamic acid coating film on the first carrier film, the first polyamic acid coating film is heated to form a first polyamic acid adhesive film; a second laminated structure is provided and the second laminated structure is heating, wherein the second laminated structure includes a second carrier film and a second polyamide coating film coated and formed on the second carrier film, and the second polyamide coating film is formed by heating The second polyamide adhesive film; rewinding the heated first laminated structure and the heated second laminated structure to obtain a third laminated structure, wherein the first polyamic acid adhesive film and the second polyamic acid The adhesive films are adhered to form a third polyamic acid adhesive film; the second and third laminated structures are rewound, wherein the two and third polyamic acid adhesive films are adhered to form a fourth polyamic acid adhesive film; The fourth polyimide adhesive film is subjected to imidization to obtain the polyimide thick film. The method for preparing a thick polyimide film according to claim 1, wherein the thicknesses of the first polyimide film and the second polyimide film both account for the thickness of the fourth polyimide film. 1/4 of the thickness of the amino acid film. The method for preparing a thick polyimide film according to claim 1, wherein the thickness of the fourth polyimide adhesive film is 200-600 μm, and the thickness of the first laminated structure and the second laminated structure is The heating temperature is 110~150℃, and the heating time is 2.5~3.8min. The method for preparing a thick polyimide film according to claim 1, wherein before heating the fourth polyimide film, the method further comprises the following steps: pulling the fourth polyimide film stretch. The method for preparing a thick polyimide film according to claim 1, wherein the step of rewinding the second and third laminate structures specifically includes: rewinding the first carrier film of the two and third laminate structures, so that the The third polyamide film is exposed; Unwind the two and third laminated structures and transfer them to between the two second laminating rollers, so that the exposed third polyamic acid adhesive films are laminated together to form a fourth polyamic acid adhesive film. The method for preparing a thick polyimide film according to claim 5, wherein after the third laminated structures are respectively transferred from the two unwinding devices to between the two second laminating rolls, the two third laminated structures are processed The step of rewinding further includes: rewinding the second carrier film of the second and third laminated structures to expose the fourth polyamide adhesive film. The method for preparing a thick polyimide film according to claim 5, wherein the temperature of the second laminating roller ranges from room temperature to 100°C. The method for preparing a thick polyimide film according to claim 1, wherein the heating temperature of the fourth polyimide film is 250-400°C. The method for preparing a thick polyimide film according to claim 1, wherein the step of providing a first laminated structure and heating the first laminated structure specifically includes: placing the first carrier film from the first layer The roll device is sequentially transferred to the first winding device through the first coating device and the first oven, wherein the polyamide acid solution is coated on the first carrier film through the first coating device to form the first polyamide Acid coating. A thick polyimide film is prepared by using the method for preparing a thick polyimide film according to any one of claims 1 to 9, wherein the thickness of the thick polyimide film is 200-600 μm.

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