CN108976793B - Transparent polyimide film capable of warning microcracks and preparation method thereof - Google Patents
Transparent polyimide film capable of warning microcracks and preparation method thereof Download PDFInfo
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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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/045—Fullerenes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/01—Hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/02—Halogenated hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/02—Halogenated hydrocarbons
- C08K5/03—Halogenated hydrocarbons aromatic, e.g. C6H5-CH2-Cl
Abstract
The invention discloses a transparent polyimide film for early warning microcracks and a preparation method thereof, wherein the transparent polyimide film comprises the following substances in parts by weight: 200-500 parts of polyimide, 3-8 parts of fullerene and 3-8 parts of microcrack discoloring agent. The transparent polyimide film for early warning the microcracks adopts the technical scheme of compounding the fullerene and the microcrack discoloring agent, so that the material is sensitive to lines with small microcracks, shows observable changes by naked eyes, is easy to identify, has clear and visible color changes within a range of a few millimeters around the cracks, can effectively monitor the safety condition of the composite materials used in airplanes and automobiles, and further avoids sudden accidents.
Description
Technical Field
The invention belongs to the technical field of polyimide film preparation, and particularly relates to a transparent polyimide film capable of early warning microcracks and a preparation method thereof.
Background
Minor damage to critical components of aircraft, automobiles, etc. can result in serious consequences. At present, the method of human eye observation and scanning instrument scanning is mainly adopted for tiny fission of components, human eyes can observe large cracks but cannot effectively observe the tiny fission, equipment scanning needs a large amount of time, and parts with complex components are difficult to scan.
The structural damage of the material usually begins from some tiny cracks and deformation, the distortion deformation of the natural materials such as shells of colored crustaceans can cause the color change, because the shells contain microcrack discoloring substances, if the polyimide film material is added with artificial microcrack discoloring substances in the preparation process, the polyimide film material is prepared into a 'microcrack Early-Warning transparent polyimide film', the hidden damage can be warned for the cracks and the perceived defects which are in micron order and difficult to detect, and the damage Sensitivity and Early Warning (Early Warning) and other fields are used for monitoring the safety condition of the composite materials used in airplanes and automobiles, thereby avoiding the occurrence of sudden accidents. The technology is not found to have a breakthrough at present, and is a technology which urgently needs to be developed and applied.
Disclosure of Invention
The invention aims to provide a transparent polyimide film capable of warning microcracks and a preparation method thereof.
A transparent polyimide film capable of warning microcracks comprises the following materials in parts by weight: 200-500 parts of polyimide, 3-8 parts of fullerene and 3-8 parts of microcrack discoloring agent.
The microcrack discoloring agent is 3-methyl cholanthracene, 7, 12-dimethyl benzanthracene and fluoranthene-d 10.
The microcrack color-changing agent is a compound having the following molecular formula:
wherein X is methyl, ethyl, halogen or phenyl, and Y is butyl, halogen or phenyl.
The polyimide is prepared from diamine and dianhydride by a two-step solution polycondensation method.
The diamine is 2, 2-bis [4- (4-aminophenoxy) phenyl ] propane, α, omega-bis (methylamino) polydimethylsiloxane, 2' -bis (trifluoromethyl) benzidine, 2, 4-diaminofluorobenzene, 2- (trifluoromethyl) -1, 4-phenylenediamine, 4-trifluoromethyl-1, 2-phenylenediamine or 4, 5-difluorobenzene-1, 2-diamine.
The dianhydride is 3, 3 ', 4, 4 ' -biphenyl tetracarboxylic dianhydride, 4, 4 ' -oxydiphthalic anhydride, pyromellitic dianhydride, bisphenol A dianhydride or hexafluoroisopropylidene diphthalic dianhydride.
The preparation method of the transparent polyimide film with the function of early warning the microcracks comprises the following steps:
(1) at room temperature, adding diamine and dianhydride into a reaction kettle, adding m-cresol under the protection of nitrogen, uniformly stirring, adding isoquinoline, heating to 170-200 ℃, reacting for 10-14 hours, cooling, and then pouring the reaction liquid into ethanol for precipitation to prepare polyimide resin;
(2) putting fullerene in an organic solvent, carrying out high-temperature treatment by a high-shear disperser, and then dispersing in advance, wherein the treatment temperature is 200-800 ℃;
(3) adding the synthesized polyimide resin and the treated fullerene into a reaction kettle, and stirring at the stirring speed of 800-1200rpm for 1-2h to prepare a membrane liquid;
(4) adding a microcrack discoloring agent into the membrane liquid, and continuously stirring at the stirring speed of 300-500rpm for 2-5h to prepare a discoloring membrane liquid;
(5) pressing the color-changing film into a defoaming kettle, removing bubbles in the color-changing film liquid under a vacuum condition, and casting the defoamed color-changing film liquid into a casting machine to form a polyimide film with uniform thickness;
(6) putting the polyimide film into an imidization furnace for imidization, and processing the polyimide film by a winding machine and a splitting machine to prepare a finished product.
The organic solvent is dimethyl acetamide, dimethyl sulfoxide, N-dimethyl acetamide, N-dimethyl formamide, dimethyl sulfoxide or N-methyl pyrrolidone.
The invention has the beneficial effects that: the transparent polyimide film for early warning the microcracks adopts the technical scheme of compounding the fullerene and the microcrack discoloring agent, so that the material is sensitive to lines with small microcracks, shows observable changes by naked eyes, is easy to identify, has clear and visible color changes within a range of a few millimeters around the cracks, can effectively monitor the safety condition of the composite materials used in airplanes and automobiles, and further avoids sudden accidents.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
A transparent polyimide film capable of warning microcracks comprises the following materials in parts by weight: 350g of polyimide, 5g of fullerene and 5g of 3-methylcholanthrene.
The transparent polyimide film with the microcrack early warning function is prepared according to the following steps:
(1) at room temperature, 1180g of 2, 2-bis [4- (4-aminophenoxy) phenyl ] propane and 990g of 4, 4' -oxydiphthalic anhydride are added into a reaction kettle, 15000g of m-cresol is added under the protection of nitrogen, after uniform stirring, 500g of isoquinoline is added, the temperature is increased to 190 ℃, the reaction is carried out for 12 hours, and after cooling, the reaction solution is poured into ethanol for precipitation to prepare polyimide resin;
(2) putting 5g of fullerene in 500g N-methyl pyrrolidone, and pre-dispersing the fullerene after high-temperature treatment by a high-shear disperser at the treatment temperature of 500 ℃;
(3) adding 350g of prepared polyimide resin into the fullerene dispersion liquid prepared in the step (2), and stirring the mixture by a reaction kettle at the stirring speed of 1000rpm for 1.5h to prepare membrane liquid;
(4) adding 5g of 3-methylcholanthrene into the membrane liquid, and continuously stirring at the stirring speed of 400rpm for 3 hours to prepare a color-changing membrane liquid;
(5) pressing the color-changing film into a defoaming kettle, removing bubbles in the color-changing film liquid under a vacuum condition, and casting the defoamed color-changing film liquid into a casting machine to form a polyimide film with uniform thickness;
(6) putting the polyimide film into an imidization furnace for imidization, and processing the polyimide film by a winding machine and a splitting machine to prepare a finished product.
Example 2
A transparent polyimide film capable of warning microcracks comprises the following materials in parts by weight: 200g of polyimide, 3g of fullerene, and 3g of 7, 12-dimethylbenzanthracene.
The preparation method of the transparent polyimide film with the function of early warning the microcracks comprises the following steps:
(1) at room temperature, adding 1108g of 2, 2' -bis (trifluoromethyl) benzidine and 880g of pyromellitic dianhydride into a reaction kettle, adding 13000g of m-cresol under the protection of nitrogen, stirring uniformly, adding 400g of isoquinoline, heating to 170 ℃, reacting for 10 hours, cooling, and then pouring the reaction solution into ethanol for precipitation to prepare polyimide resin;
(2) putting 3g of fullerene in 300g N-methyl pyrrolidone, and pre-dispersing the fullerene after high-temperature treatment by a high-shear disperser at the treatment temperature of 300 ℃;
(3) adding 200g of prepared polyimide resin into the fullerene dispersion liquid prepared in the step (2), and stirring the mixture by a reaction kettle at the stirring speed of 800rpm for 1h to prepare a membrane liquid;
(4) adding 3g of 7, 12-dimethylbenzanthracene into the membrane liquid, and continuously stirring at the stirring speed of 400rpm for 3 hours to prepare a color-changing membrane liquid;
(5) pressing the color-changing film into a defoaming kettle, removing bubbles in the color-changing film liquid under a vacuum condition, and casting the defoamed color-changing film liquid into a casting machine to form a polyimide film with uniform thickness;
(6) putting the polyimide film into an imidization furnace for imidization, and processing the polyimide film by a winding machine and a splitting machine to prepare a finished product.
Example 3
A transparent polyimide film capable of warning microcracks comprises the following materials in parts by weight: 500g of polyimide, 8g of fullerene and fluoranthene-d 108 g.
The preparation method of the transparent polyimide film with the function of early warning the microcracks comprises the following steps:
(1) at room temperature, adding 1320g of α, omega-bis (methylamino) polydimethylsiloxane and 1010g of bisphenol A type dianhydride into a reaction kettle, adding 15000g of m-cresol under the protection of nitrogen, stirring uniformly, adding 500g of isoquinoline, heating to 200 ℃, reacting for 14 hours, cooling, and then pouring the reaction liquid into ethanol for precipitation to prepare polyimide resin;
(2) putting 8g of fullerene in 500g of N-methyl pyrrolidone, and pre-dispersing the fullerene after high-temperature treatment by a high-shear disperser at 800 ℃;
(3) adding the synthesized polyimide resin and the treated fullerene into a reaction kettle, stirring at the stirring speed of 1200rpm for 2 hours, and preparing a membrane liquid;
(4) adding fluoranthene-d 108g into the membrane liquid, continuing stirring at the stirring speed of 500rpm for 5 hours to prepare a color-changing membrane liquid;
(5) pressing the color-changing film into a defoaming kettle, removing bubbles in the color-changing film liquid under a vacuum condition, and casting the defoamed color-changing film liquid into a casting machine to form a polyimide film with uniform thickness;
(6) putting the polyimide film into an imidization furnace for imidization, and processing the polyimide film by a winding machine and a splitting machine to prepare a finished product.
Example 4
A transparent polyimide film capable of warning microcracks comprises the following materials in parts by weight: 350g of polyimide, 5g of fullerene, and 5g of 2- (chloromethyl) -4- (2-chloropentyl) -1-pentylbenzene.
The transparent polyimide film with the microcrack early warning function is prepared according to the following steps:
(1) at room temperature, 1180g of 2, 2-bis [4- (4-aminophenoxy) phenyl ] propane and 990g of 4, 4' -oxydiphthalic anhydride are added into a reaction kettle, 15000g of m-cresol is added under the protection of nitrogen, after uniform stirring, 500g of isoquinoline is added, the temperature is increased to 190 ℃, the reaction is carried out for 12 hours, and after cooling, the reaction solution is poured into ethanol for precipitation to prepare polyimide resin;
(2) putting 5g of fullerene in 500g N-methyl pyrrolidone, and pre-dispersing the fullerene after high-temperature treatment by a high-shear disperser at the treatment temperature of 500 ℃;
(3) adding 350g of prepared polyimide resin into the fullerene dispersion liquid prepared in the step (2), and stirring the mixture by a reaction kettle at the stirring speed of 1000rpm for 1.5h to prepare membrane liquid;
(4) adding 5g of 2- (chloromethyl) -4- (2-chloropentyl) -1-pentylbenzene into the membrane liquid, and continuously stirring at the stirring speed of 400rpm for 3 hours to prepare a color-changing membrane liquid;
(5) pressing the color-changing film into a defoaming kettle, removing bubbles in the color-changing film liquid under a vacuum condition, and casting the defoamed color-changing film liquid into a casting machine to form a polyimide film with uniform thickness;
(6) putting the polyimide film into an imidization furnace for imidization, and processing the polyimide film by a winding machine and a splitting machine to prepare a finished product.
Example 5
A transparent polyimide film capable of warning microcracks comprises the following materials in parts by weight: 350g of polyimide, 5g of fullerene and 5g of 2-phenyl-1-pentyl-4-pentylbenzene.
The transparent polyimide film with the microcrack early warning function is prepared according to the following steps:
(1) at room temperature, 1180g of 2, 2-bis [4- (4-aminophenoxy) phenyl ] propane and 990g of 4, 4' -oxydiphthalic anhydride are added into a reaction kettle, 15000g of m-cresol is added under the protection of nitrogen, after uniform stirring, 500g of isoquinoline is added, the temperature is increased to 190 ℃, the reaction is carried out for 12 hours, and after cooling, the reaction solution is poured into ethanol for precipitation to prepare polyimide resin;
(2) putting 5g of fullerene in 500g N-methyl pyrrolidone, and pre-dispersing the fullerene after high-temperature treatment by a high-shear disperser at the treatment temperature of 500 ℃;
(3) adding 350g of prepared polyimide resin into the fullerene dispersion liquid prepared in the step (2), and stirring the mixture by a reaction kettle at the stirring speed of 1000rpm for 1.5h to prepare membrane liquid;
(4) adding 5g of 2-phenyl-1-pentyl-4-pentylbenzene into the membrane liquid, and continuously stirring at the stirring speed of 400rpm for 3 hours to prepare a color-changing membrane liquid;
(5) pressing the color-changing film into a defoaming kettle, removing bubbles in the color-changing film liquid under a vacuum condition, and casting the defoamed color-changing film liquid into a casting machine to form a polyimide film with uniform thickness;
(6) putting the polyimide film into an imidization furnace for imidization, and processing the polyimide film by a winding machine and a splitting machine to prepare a finished product.
Example 6
A transparent polyimide film capable of warning microcracks comprises the following materials in parts by weight: 350g of polyimide, 5g of fullerene, and 5g of (2-cyclohexyl) benzene.
The transparent polyimide film with the microcrack early warning function is prepared according to the following steps:
(1) at room temperature, 1180g of 2, 2-bis [4- (4-aminophenoxy) phenyl ] propane and 990g of 4, 4' -oxydiphthalic anhydride are added into a reaction kettle, 15000g of m-cresol is added under the protection of nitrogen, after uniform stirring, 500g of isoquinoline is added, the temperature is increased to 190 ℃, the reaction is carried out for 12 hours, and after cooling, the reaction solution is poured into ethanol for precipitation to prepare polyimide resin;
(2) putting 5g of fullerene in 500g N-methyl pyrrolidone, and pre-dispersing the fullerene after high-temperature treatment by a high-shear disperser at the treatment temperature of 500 ℃;
(3) adding 350g of prepared polyimide resin into the fullerene dispersion liquid prepared in the step (2), and stirring the mixture by a reaction kettle at the stirring speed of 1000rpm for 1.5h to prepare membrane liquid;
(4) adding 5g of (2-cyclohexyl) benzene into the membrane liquid, and continuously stirring at the stirring speed of 400rpm for 3 hours to prepare a color-changing membrane liquid;
(5) pressing the color-changing film into a defoaming kettle, removing bubbles in the color-changing film liquid under a vacuum condition, and casting the defoamed color-changing film liquid into a casting machine to form a polyimide film with uniform thickness;
(6) putting the polyimide film into an imidization furnace for imidization, and processing the polyimide film by a winding machine and a splitting machine to prepare a finished product.
Example 7
A transparent polyimide film capable of warning microcracks comprises the following materials in parts by weight: 350g of polyimide, 5g of fullerene, 5g of 3-methylcholanthrene and 3g of tortoise shell extract.
The extraction method of the tortoise shell extract comprises the following steps: grinding the shell of the scarab beetle, sieving with a 60-mesh sieve, adding 8 weight parts of 75% ethanol aqueous solution, reflux-extracting for 3 times, mixing filtrates, decolorizing with active carbon, and evaporating to dryness.
The transparent polyimide film with the microcrack early warning function is prepared according to the following steps:
(1) at room temperature, 1180g of 2, 2-bis [4- (4-aminophenoxy) phenyl ] propane and 990g of 4, 4' -oxydiphthalic anhydride are added into a reaction kettle, 15000g of m-cresol is added under the protection of nitrogen, after uniform stirring, 500g of isoquinoline is added, the temperature is increased to 190 ℃, the reaction is carried out for 12 hours, and after cooling, the reaction solution is poured into ethanol for precipitation to prepare polyimide resin;
(2) putting 5g of fullerene in 500g N-methyl pyrrolidone, and pre-dispersing the fullerene after high-temperature treatment by a high-shear disperser at the treatment temperature of 500 ℃;
(3) adding 350g of prepared polyimide resin into the fullerene dispersion liquid prepared in the step (2), and stirring the mixture by a reaction kettle at the stirring speed of 1000rpm for 1.5h to prepare membrane liquid;
(4) adding 5g of 3-methylcholanthrene and 3g of tortoise shell extract into the membrane liquid, and continuously stirring at the stirring speed of 400rpm for 3 hours to prepare a color-changing membrane liquid;
(5) pressing the color-changing film into a defoaming kettle, removing bubbles in the color-changing film liquid under a vacuum condition, and casting the defoamed color-changing film liquid into a casting machine to form a polyimide film with uniform thickness;
(6) putting the polyimide film into an imidization furnace for imidization, and processing the polyimide film by a winding machine and a splitting machine to prepare a finished product.
Comparative example 1
A transparent polyimide film capable of warning microcracks comprises the following materials in parts by weight: 350g of polyimide and 5g of fullerene.
The transparent polyimide film with the microcrack early warning function is prepared according to the following steps:
(1) at room temperature, 1180g of 2, 2-bis [4- (4-aminophenoxy) phenyl ] propane and 990g of 4, 4' -oxydiphthalic anhydride are added into a reaction kettle, 15000g of m-cresol is added under the protection of nitrogen, after uniform stirring, 500g of isoquinoline is added, the temperature is increased to 190 ℃, the reaction is carried out for 12 hours, and after cooling, the reaction solution is poured into ethanol for precipitation to prepare polyimide resin;
(2) putting 5g of fullerene in 500g N-methyl pyrrolidone, and pre-dispersing the fullerene after high-temperature treatment by a high-shear disperser at the treatment temperature of 500 ℃;
(3) adding 350g of prepared polyimide resin into the fullerene dispersion liquid prepared in the step (2), and stirring the mixture by a reaction kettle at the stirring speed of 1000rpm for 1.5h to prepare membrane liquid;
(4) pressing the membrane liquid into a defoaming kettle, removing bubbles in the membrane liquid under a vacuum condition, and casting the defoamed membrane liquid into a casting machine to form a polyimide membrane with uniform thickness;
(6) putting the polyimide film into an imidization furnace for imidization, and processing the polyimide film by a winding machine and a splitting machine to prepare a finished product.
Experimental example:
taking the polyimide films prepared in the examples 1 to 7 and the comparative example 1, scratching a micro scratch with the length of 1cm and the width of 0.2mm by using a sharp knife, observing whether the color change exists around the scratch of the polyimide film, calculating the width of a color band, and obtaining the experimental result shown in the table 1:
TABLE 1
Note: represents P <0.05 compared to the example 1 group.
As can be seen from table 1, the microcrack discoloring agent was not added in comparative example 1, no color band was generated, the colored bands of examples 1 to 4 were generated, the colored bands of examples 5 to 7 were generated, and the width of the color band was significantly higher than that of example 1.
Claims (6)
1. The transparent polyimide film capable of warning microcracks is characterized by comprising the following substances in parts by weight: 500 parts of polyimide 200-one, 3-8 parts of fullerene and 3-8 parts of microcrack discoloring agent; the microcrack discoloring agent is 3-methylcholanthrene, 7, 12-dimethylbenzanthracene, fluoranthene-d 10, 2- (chloromethyl) -4- (2-chloropentyl) -1-pentylbenzene, 2-phenyl-1-pentyl-4-pentylbenzene or (2-cyclohexyl) benzene.
2. The transparent polyimide film with the function of pre-warning microcracks according to claim 1, wherein the polyimide is prepared from diamine and dianhydride by a two-step solution polycondensation method.
3. The microcrack-forewarning transparent polyimide film according to claim 1, wherein the diamine is 2, 2-bis [4- (4-aminophenoxy) phenyl ] propane, α, ω -bis (methylamino) polydimethylsiloxane, 2' -bis (trifluoromethyl) benzidine, 2, 4-diaminofluorobenzene, 2- (trifluoromethyl) -1, 4-phenylenediamine, 4-trifluoromethyl-1, 2-phenylenediamine or 4, 5-difluorobenzene-1, 2-diamine.
4. The transparent polyimide film for warning microcracks according to claim 1, wherein the dianhydride is 3, 3 ', 4, 4 ' -biphenyltetracarboxylic dianhydride, 4, 4 ' -oxydiphthalic anhydride, pyromellitic dianhydride, bisphenol a dianhydride, or hexafluoroisopropylidene diphthalic dianhydride.
5. The preparation method of the transparent polyimide film with the function of early warning microcracks in claim 1 is characterized by comprising the following steps:
(1) at room temperature, adding diamine and dianhydride into a reaction kettle, adding m-cresol under the protection of nitrogen, uniformly stirring, adding isoquinoline, heating to 170-200 ℃, reacting for 10-14 hours, cooling, and then pouring the reaction liquid into ethanol for precipitation to prepare polyimide resin;
(2) putting fullerene in an organic solvent, carrying out high-temperature treatment by a high-shear disperser, and then dispersing in advance, wherein the treatment temperature is 200-800 ℃;
(3) adding the synthesized polyimide resin and the treated fullerene into a reaction kettle, and stirring at the stirring speed of 800-1200rpm for 1-2h to prepare a membrane liquid;
(4) adding a microcrack discoloring agent into the membrane liquid, and continuously stirring at the stirring speed of 300-500rpm for 2-5h to prepare a discoloring membrane liquid;
(5) pressing the color-changing film into a defoaming kettle, removing bubbles in the color-changing film liquid under a vacuum condition, and casting the defoamed color-changing film liquid into a casting machine to form a polyimide film with uniform thickness;
(6) putting the polyimide film into an imidization furnace for imidization, and processing the polyimide film by a winding machine and a splitting machine to prepare a finished product.
6. The method for preparing the transparent polyimide film with the function of warning microcracks according to claim 5, wherein the organic solvent is N, N-dimethylacetamide, N-dimethylformamide, dimethyl sulfoxide or N-methylpyrrolidone.
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| PCT/CN2018/107196 WO2020029392A1 (en) | 2018-08-07 | 2018-09-25 | Transparent polyimide film with slight crack early-warning function and preparation method therefor |
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