CN106633134A - Film forming method of polyimide film - Google Patents
Film forming method of polyimide film Download PDFInfo
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- CN106633134A CN106633134A CN201611140576.3A CN201611140576A CN106633134A CN 106633134 A CN106633134 A CN 106633134A CN 201611140576 A CN201611140576 A CN 201611140576A CN 106633134 A CN106633134 A CN 106633134A
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- dried
- acid solution
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- polyamic acid
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
Abstract
The invention provides a film forming method of a polyimide film. The film forming method comprises the following steps: (1) defoaming a polyamide acid solution in vacuum, painting the polyamide acid solution on a support material through a solution tape-casting method, and placing the support material in a far infrared drying box; and (2) removing the solvent from the polyamide acid solution and carrying out imidization by adopting a programmed gradually increased temperature method; wherein the temperature increasing program is carried out as follows: drying for 1-3 hours at a temperature of 75-85 DEG C, drying for 0.5-2 hours at a temperature of 145-155 DEG C, drying for 0.5-2 hours at a temperature of 195-205 DEG C, and drying for 0.5 to 2 hours at a temperature of 275 to 285 DEG C. During the solution tape-casting preparation process of the polyimide film, the polyamide acid solution is heated by far infrared rays to remove the solvent quickly, at the same time, the rate of imidization is also accelerated, and the degree of imidization is improved. Compared with a conventional polyimide film forming method, the provided film forming method has the advantages of convenient operation, short film forming period, and high efficiency.
Description
Technical field
The present invention relates to a kind of film build method of organic polymer film, and in particular to a kind of film forming of Kapton
Method.
Background technology
Polyimides is the high-molecular organic material containing imide ring in molecule structure, is to use temperature highest
One family macromolecule material, with the combination property that high mechanical strength, high temperature resistant, chemically stable, creep resistant etc. are very excellent, in boat
The aspect such as sky, space flight, electric, machinery, microelectronics, chemical industry is widely used.
Kapton (PIF) is a kind of new high temperature resistant organic polymer thin film.It has high-modulus, low receipts
Contracting, high intensity, low water absorption, hydrolysis, radiation hardness, nontoxic, excellent insulating properties and resistance to thermo oxidative stability.Because it is current
In the world one of most expensive thin-film material is so be referred to as " gold film ".It is the key insulating materials of electric apparatus,
It is the key material of micro-electronic manufacturing and encapsulation.
Kapton is obtained using two-step method mostly, i.e., by aromatic diamine compound and dianhydride compound by contracting
It is poly- that polyimide precursor-polyamic acid solution is synthesized, then heat is carried out using the tape casting in drying box or on casting machine
Imidization makes polyamic acid cyclodehydration obtain Kapton.Film is prepared in drying box typically using glass as base
Plate, using progressively intensification or gradient increased temperature, the film-forming process time is longer, and power consumption is high, and the shortening time then easily makes for heating schedule
Into there is dissolvent residual, the problems such as imidization is incomplete, its commercial application is limited.
The Chinese invention patent document of the A of Publication No. CN 105175725 discloses a kind of preparation of Kapton
Method and Kapton and purposes, the method is coated on polyamic acid resin solution on glass plate or stainless surface
Peel off, obtain the polyamic acid resin glued membrane of self-supporting；Described self-supporting polyamic acid resin glued membrane surrounding is fixed on metal
On the framework of mould, using temperature-programmed mode, high temperature imidization is completed；Then polyimides is obtained through annealing
Film.Whole process needs at least 9 hours.
The content of the invention
The technical problem to be solved is to overcome above-mentioned the deficiencies in the prior art, there is provided a kind of technological process letter
Single, energy-efficient, film formation time is short, and homogeneous heating, the more excellent Kapton film build method of product property.
A kind of film build method of Kapton, comprises the following steps：
(1) by polyamic acid solution vacuum defoamation, by solution casting method on backing material film, be subsequently placed in remote red
In outer drying box；
(2) polyamic acid solution desolvation and the imidization, heating schedule is made to be using the method for program gradient increased temperature：In
1～3h is dried at 80 ± 5 DEG C, 0.5～2h is dried at 150 ± 5 DEG C, 0.5～2h is dried at 200 ± 5 DEG C, done at 280 ± 5 DEG C
Dry 0.5～2h.
The present invention makes polyamic acid solution while fast eliminating solvent using the method for Heated by Far-Infrared Radiation, plus
Fast imidization speed, improves imidization degree.
Preferably, the heating schedule is：1～2h is dried at 80 ± 5 DEG C, 0.5～1h is dried at 150 ± 5 DEG C,
0.5～1h is dried at 200 ± 5 DEG C, 0.5～1h is dried at 280 ± 5 DEG C.Polyamic acid solution contains a large amount of solvents, needs drying
Remove in dry process, in addition, moisture can be produced in imidization, heat up too fast, 150～200 DEG C of retention times are inadequate, meeting
The solvent or moisture for causing internal layer has little time effusion, causes film to produce bubble or absorb water and turns white.
Preferably, the heating schedule is：1h is dried at 80 ± 5 DEG C, dry 0.5～1h at 150 ± 5 DEG C, 200
0.5h is dried at ± 5 DEG C, at 280 ± 5 DEG C 0.5h is dried.
Preferably, each temperature-rise period is spaced 10min.
Atmosphere in far infrared drying oven is air, inert gas or vacuum.
Preferably, the backing material is glass or steel plate.
Preferably, the preparation method of the polyamic acid solution includes：Aromatic diamine compound is dissolved in into non-matter
In sub- polar solvent, nitrogen protection is passed through, temperature control is gradually added into batches equimolar aromatic dianhydride at 0～25 DEG C
Compound, reacts under agitation 8～20h, obtains the polyamic acid solution of homogeneous transparent.
Preferably, the solid content of the polyamic acid solution is 5～20%.
Compared with prior art, the invention has the advantages that：
(1) using the method for Heated by Far-Infrared Radiation, polyamic acid solution is made while fast eliminating solvent, accelerate sub-
Amination speed, improves imidization degree.
(2) compared with the film build method of conventional polyimide film, the technological operation that the present invention is provided is convenient, membrane preparation cycle
It is short, efficiency high.
(3) using the method for Heated by Far-Infrared Radiation, the technique that can prepare flat transparent Kapton is explored
Condition.
Description of the drawings
Fig. 1 is the infrared comparison diagram of comparative example of the present invention 1 and gained sample in embodiment 4；
Fig. 2 is the infrared comparison diagram of gained sample in embodiment 1～4；
Fig. 3 is the thermal weight loss comparison chart of gained sample and blank sample in embodiment 1, comparative example.
Specific embodiment
With reference to embodiment, the present invention will be further described, preferred embodiment described herein be merely to illustrate and
The present invention is explained, is not intended to limit the present invention.
The preparation of polyamic acid solution：
4,4'- diaminodiphenyl ethers and DMA are added in there-necked flask, high pure nitrogen is passed through, is opened
Mechanical agitation is opened, after diamines solid is completely dissolved, equimolar 3,3'4,4'- bibenzene tetracarboxylics is dividedly in some parts in reaction bulb
12h is stirred under dianhydride, room temperature, the polyamic acid solution of homogeneous transparent is obtained, logarithmic viscosity number is 1.20dL/g.
Embodiment 1
It is 10% that above-mentioned gained polyamic acid solution DMA is diluted into solid content, vacuum defoamation,
By solution casting method on the glass plate of dried and clean film, in being then placed into far infrared drying oven, using program gradient
The method of intensification makes polyamic acid solution desolvation and imidization, and heating schedule is 2h, 1h at 150 DEG C at 80 DEG C, at 200 DEG C
1h, 1h at 280 DEG C, each temperature-rise period interval 10min, the atmosphere in far infrared drying oven is air.Gained polyimides is thin
Film (numbering is PAA-1) is characterized through infrared spectrum and thermogravimetic analysis (TGA), and characterization result is as shown in Figures 1 to 3.
Embodiment 2
It is 10% that above-mentioned gained polyamic acid solution DMA is diluted into solid content, vacuum defoamation,
By solution casting method on the glass plate of dried and clean film, in being then placed into far infrared drying oven, using program gradient
The method of intensification makes polyamic acid solution desolvation and imidization, and heating schedule is 2h, 1h at 150 DEG C at 80 DEG C, at 200 DEG C
1h, 0.5h at 280 DEG C, each temperature-rise period interval 10min, the atmosphere in far infrared drying oven is air.Gained polyimides
Film (numbering is PAA-2) is characterized through infrared spectrum and thermogravimetic analysis (TGA), and characterization result is as shown in Fig. 1～2.
Embodiment 3
It is 10% that above-mentioned gained polyamic acid solution DMA is diluted into solid content, vacuum defoamation,
By solution casting method on the glass plate of dried and clean film, in being then placed into far infrared drying oven, using program gradient
The method of intensification makes polyamic acid solution desolvation and imidization, and heating schedule is 1h, 1h at 150 DEG C at 80 DEG C, at 200 DEG C
0.5h, 0.5h at 280 DEG C, each temperature-rise period interval 10min, the atmosphere in far infrared drying oven is air.Gained polyamides is sub-
Amine film (numbering is PAA-3) is characterized through infrared spectrum and thermogravimetic analysis (TGA), and characterization result is as shown in Fig. 1～2.
Embodiment 4
It is 10% that above-mentioned gained polyamic acid solution DMA is diluted into solid content, vacuum defoamation,
By solution casting method on the glass plate of dried and clean film, in being then placed into far infrared drying oven, using program gradient
The method of intensification makes polyamic acid solution desolvation and imidization, and heating schedule is 1h, 0.5h at 150 DEG C at 80 DEG C, 200 DEG C
Lower 0.5h, 0.5h at 280 DEG C, each temperature-rise period interval 10min, the atmosphere in far infrared drying oven is air.Gained polyamides
Imines film (numbering is PAA-4) is characterized through infrared spectrum and thermogravimetic analysis (TGA), and characterization result is as shown in Fig. 1～2.As a result show
Show, the present embodiment only needs process 3h, and just energy imidization is complete.
Comparative example 1
It is 10% that above-mentioned gained polyamic acid solution DMA is diluted into solid content, vacuum defoamation,
By solution casting method on the glass plate of dried and clean film, in being then placed into common drying box, using program gradient liter
The method of temperature makes polyamic acid solution desolvation and imidization, and heating schedule is 2h, 1h at 150 DEG C at 80 DEG C, at 200 DEG C
1h, 1h at 280 DEG C, each temperature-rise period interval 10min, the atmosphere in common drying box is air.Gained Kapton
(numbering is PAA-5) characterizes through infrared spectrum and thermogravimetic analysis (TGA), and characterization result is as shown in Figure 1, Figure 3.
In Fig. 3, the blank heating schedules that differ only in comparative example 1 of PAA- are that the polyamides that 2h is obtained is dried at 80 DEG C
Imines film.
Comparative example 2
It is 10% that above-mentioned gained polyamic acid solution DMA is diluted into solid content, vacuum defoamation,
By solution casting method on the glass plate of dried and clean film, in being then placed into common drying box, using program gradient liter
The method of temperature makes polyamic acid solution desolvation and imidization, and heating schedule is 1h, 0.5h at 150 DEG C at 80 DEG C, at 200 DEG C
0.5h, 0.5h at 280 DEG C, each temperature-rise period interval 10min, the atmosphere in common drying box is air.Gained polyimides
The visible corrugation of substantially turning white of film (numbering is PAA-6), reason is that the water generated in imidization cannot be removed smoothly.
Comparative example 3
It is 10% that above-mentioned gained polyamic acid solution DMA is diluted into solid content, vacuum defoamation,
By solution casting method on the glass plate of dried and clean film, in being then placed into far infrared drying oven, using being rapidly heated
Method make polyamic acid solution desolvation and imidization, heating schedule is 2h at 80 DEG C, 0.8h at 280 DEG C, temperature-rise period
Interval 10min, the atmosphere in far infrared drying oven is air.Gained Kapton (numbering is PAA-7) is visible substantially big
Amount bubble.
Comparative example 4
It is 10% that above-mentioned gained polyamic acid solution DMA is diluted into solid content, vacuum defoamation,
By solution casting method on the glass plate of dried and clean film, in being then placed into far infrared drying oven, using program gradient
The method of intensification makes polyamic acid solution desolvation and imidization, and heating schedule is 0.5h, 0.3h at 280 DEG C at 150 DEG C, is risen
Atmosphere of the warm interprocedual in 10min, far infrared drying oven is air.Gained Kapton (numbering is PAA-8) is visible
Substantially turn white corrugation, reason is that the water generated in imidization cannot be removed smoothly.
Heating schedule in the various embodiments described above and comparative example is summarized in following table：
| Sequence number | Numbering | 80℃ | 150℃ | 200℃ | 280℃ | Total timea | Atmosphere | Baking oven | Experimental phenomena |
| Embodiment 1 | PAA-1 | 2h | 1h | 1h | 1h | 5.5h | Air | It is infrared | Flat transparent |
| Embodiment 2 | PAA-2 | 2h | 1h | 1h | 0.5h | 5h | Air | It is infrared | Flat transparent |
| Embodiment 3 | PAA-3 | 1h | 1h | 0.5h | 0.5h | 3.5h | Air | It is infrared | Flat transparent |
| Embodiment 4 | PAA-4 | 1h | 0.5h | 0.5h | 0.5h | 3h | Air | It is infrared | Flat transparent |
| Comparative example 1 | PAA-5 | 2h | 1h | 1h | 1h | 5.5h | Air | Commonly | Flat transparent |
| Comparative example 2 | PAA-6 | 1h | 0.5h | 0.5h | 0.5h | 3h | Air | Commonly | Turn white corrugation |
| Comparative example 3 | PAA-7 | 2h | 0 | 0 | 0.8h | 3h | Air | It is infrared | A large amount of bubbles |
| Comparative example 4 | PAA-8 | 0 | 0.5h | 0 | 0.3h | 1h | Air | It is infrared | Turn white corrugation |
aEach temperature-rise period interval 10min in table.
Compared with comparative example 2 by embodiment 4, it can be seen that during using same heating schedule, using a conventional oven
Being dried the Kapton for obtaining can turn white corrugation, and the polyimides for obtaining is dried using far infrared drying oven
Film then flat transparent.Compared with comparative example 3 by embodiment 4, it can be seen that reprogramming heating process, 100～200
DEG C retention time is too short, and Kapton can produce a large amount of bubbles.
Hot property in the various embodiments described above and comparative example is as shown in the table：
| Sequence number | Numbering | Thermal weight loss Td5%(℃) |
| Comparative example 1 | PAA-5 | 545 |
| Embodiment 1 | PAA-1 | 555 |
| Embodiment 2 | PAA-2 | 553 |
| Embodiment 3 | PAA-3 | 554 |
| Embodiment 4 | PAA-4 | 550 |
As can be seen from the above table, the Kapton for obtaining is dried using far infrared drying oven with drying time
Shortening, 5% thermal weight loss temperature can reduce slightly, but all thin higher than the polyimides for obtaining is dried using a conventional oven
Film, this be heated due to far-infrared element after can far infrared of the radiation wave band more than 2～15 microns, it can be by polyamide
Acid solution is more effective and uniformly absorbs, and solution in heat energy, with a conventional oven can be directly translated into after absorption and be relied on by thermal evaporation
The drying effect for reaching is compared, and while can obtaining flash drying effect using far infrared drying oven, gained film solvent is residual
Stay less, cyclodehydration is more abundant, so heat endurance also can have been lifted.
Claims (7)
1. a kind of film build method of Kapton, it is characterised in that comprise the following steps：
(1) by polyamic acid solution vacuum defoamation, by solution casting method on backing material film, be subsequently placed in far infrared do
In dry case；
(2) polyamic acid solution desolvation and the imidization, heating schedule is made to be using the method for program gradient increased temperature：In 80 ±
1～3h is dried at 5 DEG C, 0.5～2h is dried at 150 ± 5 DEG C, 0.5～2h is dried at 200 ± 5 DEG C, be dried at 280 ± 5 DEG C
0.5～2h.
2. the film build method of Kapton according to claim 1, it is characterised in that the heating schedule is：In
1～2h is dried at 80 ± 5 DEG C, 0.5～1h is dried at 150 ± 5 DEG C, 0.5～1h is dried at 200 ± 5 DEG C, done at 280 ± 5 DEG C
Dry 0.5～1h.
3. the film build method of Kapton according to claim 1, it is characterised in that the heating schedule is：In
1h is dried at 80 ± 5 DEG C, 0.5～1h is dried at 150 ± 5 DEG C, 0.5h is dried at 200 ± 5 DEG C, be dried at 280 ± 5 DEG C
0.5h。
4. the film build method of Kapton according to claim 1, it is characterised in that each temperature-rise period interval
10min。
5. the film build method of Kapton according to claim 1, it is characterised in that the gas in far infrared drying oven
Atmosphere is air, inert gas or vacuum.
6. the film build method of Kapton according to claim 1, it is characterised in that the polyamic acid solution
Solid content is 5～20%.
7. the film build method of Kapton according to claim 1, it is characterised in that the backing material is glass
Or steel plate.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109366826A (en) * | 2018-10-26 | 2019-02-22 | 镇江龙成绝缘材料有限公司 | A kind of polyimide film curtain coating method production technology |
| CN109627438A (en) * | 2018-11-05 | 2019-04-16 | 广东丹邦科技有限公司 | The preparation method of polyamic acid solution and the preparation method of transparent polyimide film |
| CN110618482A (en) * | 2019-09-19 | 2019-12-27 | 中国科学院重庆绿色智能技术研究院 | Preparation method of polyimide film diffraction lens with high thickness uniformity |
| CN112409595A (en) * | 2020-11-26 | 2021-02-26 | 广东工业大学 | Polyimide film and preparation method thereof |
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| CN109366826A (en) * | 2018-10-26 | 2019-02-22 | 镇江龙成绝缘材料有限公司 | A kind of polyimide film curtain coating method production technology |
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Application publication date: 20170510 |