CN115109289B - Polyimide film with strong physical adhesion with glass substrate and preparation method thereof - Google Patents
Polyimide film with strong physical adhesion with glass substrate and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of polymer film material manufacturing, and particularly relates to a polyimide film with strong physical adhesion to a glass substrate and a preparation method thereof. Firstly, preparing a polyamic acid precursor solution with controllable molecular weight by adjusting solid content and cyclization degree; then, processing the surface of the glass substrate, and keeping certain cleanliness; finally, the aggregation structure of the film is controlled by adjusting the temperature program, the pressure and the like in the film forming process. Due to the change of molecular weight and aggregation state structure, molecular chain arrangement is more regular, relaxation time is slower, and the probability of forming hydrogen bonds is higher, so that the obtained polyimide film has stronger physical adhesion with glass.
Description
Technical Field
The invention belongs to the technical field of polymer film material manufacturing, and particularly relates to a polyimide film with strong physical adhesion with a glass substrate and a preparation method thereof.
Background
In recent years, the photoelectric display industry is continuously developing towards flexible devices. Polyimide materials are preferred materials for flexible electro-optic display substrates due to their excellent thermal stability, mechanical properties, and insulating properties. However, in the whole process of manufacturing electronic devices, the polyimide film serving as the substrate needs to be bonded with the base glass all the time, and if interlayer peeling occurs between the polyimide film and the base glass, the problems of cracking, warping, curling and the like of the polyimide film are easily caused, so that the subsequent manufacturing process is directly influenced, and inevitable loss is brought. Therefore, it is one of the important points of research to improve the adhesion property of the polyimide film to the glass substrate.
In the prior art, for example, by introducing chemical groups into the molecular structure of polyimide and chemically treating the surface of the glass substrate, the chemical adhesion between the two is increased. However, the chemical structure of the polyimide film is changed by improving the adhesion degree by a chemical method, and the inherent mechanical property and thermal property of the film are easily damaged. Furthermore, chemical bonding can also cause problems with later peeling, leading to difficulty in peeling or damage to the polyimide film during peeling.
Disclosure of Invention
In view of the above problems in the prior art, the present invention provides a polyimide film having strong physical adhesion to a glass substrate and a method for preparing the same. The invention improves the physical adhesive property of the polyimide film and the glass substrate on the premise of ensuring the inherent property of the polyimide film, does not damage the polyimide film during stripping, and is beneficial to optimizing the manufacturing process of the flexible display device. Furthermore, the invention controls the molecular weight of the polyamic acid precursor solution by processing and modifying the polyamic acid precursor solution, and controls the aggregation structure of the film by adjusting the temperature program and the pressure in the film forming process, thereby obviously improving the physical adhesion between the polyimide film and the glass.
The preparation method of the polyimide film provided by the invention comprises the following steps:
(1) Adding a diamine monomer and an anhydride monomer to a first portion of the aprotic polar solvent, wherein the molar ratio of diamine monomer to anhydride monomer is in the range of 1:1.05-1:1.2, reacting for 6-10 hours at low temperature (-5 to 60 ℃) to obtain a first part of polyamic acid solution;
(2) Diluting the first part of the polyamic acid solution by using a second part of the aprotic polar solvent according to a certain proportion, and adjusting the solid content and the apparent viscosity of the solution for the second time to obtain a mixed solvent type polyamic acid solution within a certain viscosity range;
(3) Filtering the mixed solvent type polyamic acid solution by a filter, reducing the content of particle impurities in the solution, and cleaning the surface of a glass substrate used in a subsequent film forming process to ensure the cleanliness of the film coating process and avoid the influence caused by the particle impurities;
(4) Coating the filtered mixed solvent type polyimide-polyamide acid solution obtained in the step (3) on a clean glass substrate through a slit, drying at a low temperature (40-70 ℃) for 10-50 min under vacuum (30-100 Pa), and finally completing high-temperature cyclization through different temperature programs under the protection of inert gases such as nitrogen and the like to obtain a polyimide film with strong physical adhesion with glass;
the first part of diamine monomer and the anhydride monomer in the step (1) are respectively one or more of the following structures, and the diamine monomer has the following structure:
the anhydride monomer has the following structure:
the first part of the aprotic polar solvent of step (1) comprises: one of N, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone; the solid content is 12-18 wt%.
The second part of the aprotic polar solvent in the step (2) comprises: one of N, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide and N-methylpyrrolidone; the solid content is 5-10wt%, and the apparent viscosity is 2000-8000 cp.
The first part of the aprotic polar solvent in the step (1) and the second part of the aprotic polar solvent in the step (2) are required to be kept different, and the adhesive force between the film and the glass is increased by adjusting the volatilization temperature of the solvents to be different.
The impurities of the solution particles to be filtered in the step (3) mainly come from the solvent and the impurity particles in the equipment. The filter is a polytetrafluoroethylene capsule filter, and two grades with the grain diameter of 5.0um and 0.45um are connected in series to control the number of particles with the grain diameter >1um in the solution to be less than 50/mL. Prevent to influence the inside homogeneity of film, bring the film defect, also prevent to leave more gaps because of impurity exists between film and the glass, reduce the adhesive force.
The pressure, temperature and time of vacuum drying in the step (4) are preferably selected from the following fixed matching, such as: 30Pa,70 deg.C, 10min;40Pa,60 deg.C, 15min;110Pa,40 ℃ for 20min.
The high-temperature cyclization procedure in the step (4) adopts a stage temperature rise mode under a nitrogen atmosphere, and the cyclization temperature is as follows: the temperature is 180 to 450 ℃, and the time is 200 to 250 min.
Has the advantages that: compared with the prior art, the invention provides a preparation method of a polyimide film with stronger physical adhesion with a glass substrate, which comprises the steps of firstly preparing a polyamic acid precursor solution with controllable molecular weight by adjusting the solid content and cyclization degree of monomer slurry; then cleaning the surface of the glass substrate; finally, the aggregation structure of the film is controlled by adjusting the temperature program, the pressure and the like in the film forming process. Due to the change of molecular weight and aggregation state structure, molecular chain arrangement is more regular, relaxation time is slower, and the probability of forming hydrogen bonds is higher, so that the obtained polyimide film has stronger physical adhesion with glass. The method does not adopt a chemical crosslinking means to change the structures of the polyimide film and the surface of the glass substrate, so the inherent performance of the polyimide film can be maintained, the physical adhesion has reversibility, and the film is not easy to damage when the polyimide film is stripped.
Drawings
FIG. 1 is a chart showing the infrared spectrum of a sample;
FIG. 2 is a graph showing a contrast in orientation of a sample;
fig. 3 shows the XRD pattern of the sample.
Detailed Description
The invention is further illustrated by the following specific examples, which are illustrative and intended to illustrate the problem and explain the invention, but not limiting.
Example 1
(1) At room temperature, 0.038mol (7.5974 g) of 4,4' -diaminodiphenyl ether (ODA) monomer is added into 100ml of N, N-dimethylacetamide solvent and stirred until the monomer is completely dissolved, 0.041mol (8.9379 g) of 1,2,4, 5-pyromellitic dianhydride (PMDA) is added, and stirring is continued for 12 hours to obtain a first part of polyamic acid solution with solid content of 15 wt%;
(2) Weighing 50 g of the first part of the polyamic acid solution, adding 25g of N-methyl pyrrolidone solvent, and stirring for 30-60 min at room temperature until a uniform mixed solvent type polyamic acid solution with the solid content of 10wt% is obtained.
(3) Filtering mixed solvent type polyamic acid solution through a filter to reduce the content of particle impurities in the solution, cleaning a glass substrate used in a subsequent film forming process through ethanol spray washing, and performing N-phase cleaning 2 And (5) drying.
(4) And (4) coating the filtered mixed solvent type polyamic acid solution obtained in the step (3) on a clean glass substrate through a slit to form a wet film with the thickness of 150 mu m, and drying for 15min at a low temperature (60 ℃) through vacuum (40 Pa).
(5) And under the protection of nitrogen, carrying out high-temperature cyclization at the temperature of 100 ℃,30min, 150 ℃,10min, 180 ℃,30min, 250 ℃,30min, 300 ℃ and 30min to obtain the polyimide film with strong physical adhesion with glass, wherein the thickness of the polyimide film is 15 mu m.
Example 2
(1) At room temperature, 0.038mol (7.5974 g) of 4,4' -diaminodiphenyl ether (ODA) monomer is added into 100ml of N, N-dimethylacetamide solvent and stirred until the monomer is completely dissolved, 0.041mol (8.9379 g) of 1,2,4, 5-pyromellitic dianhydride (PMDA) is added, and stirring is continued for 12 hours to obtain a first part of polyamic acid solution with solid content of 15 wt%;
(2) Weighing 50 g of the first part of the polyamic acid solution, adding 43.75 g of N-methyl pyrrolidone solvent, and stirring for 30-60 min at room temperature until a uniform mixed solvent type polyamic acid solution with the solid content of 8wt% is obtained.
(3) Filtering the mixed solvent type polyamic acid solution through a filter to reduce the content of particle impurities in the solution, cleaning a glass substrate used in a subsequent film forming process through ethanol spray washing, and performing N-layer cleaning 2 And (5) drying.
(4) And (4) coating the filtered mixed solvent type polyamic acid solution obtained in the step (3) on a clean glass substrate through a slit to form a wet film with the thickness of 150 mu m, and drying for 15min at a low temperature (60 ℃) through vacuum (40 Pa).
(5) And under the protection of nitrogen, carrying out high-temperature cyclization at the temperature programs of 100 ℃,30min, 150 ℃,10min, 180 ℃,30min, 250 ℃,30min, 300 ℃ and 30min to obtain the polyimide film with strong physical adhesion with glass, wherein the thickness of the polyimide film is 15 mu m.
Example 3
(1) At room temperature, 0.034mol (3.7199 g) of p-Phenylenediamine (PDA) monomer is added into 100ml of N-methylpyrrolidone solvent, stirred until the monomer is completely dissolved, then 0.035mol (10.2983 g) of 3, 4-biphenyltetracarboxylic dianhydride (BPDA) is added, and stirring is continued for 12 hours to obtain a first part of polyamic acid solution with the solid content of 12 wt%;
(2) Weighing 50 g of the first part of the polyamic acid solution, adding 25g of N, N-dimethylacetamide solvent, and stirring for 30-60 min at room temperature until obtaining uniform mixed solvent type polyamic acid solution with solid content of 8wt%.
(3) Filtering the mixed solvent type polyamic acid solution through a filter, reducing the content of particle impurities in the solution, and cleaning a glass substrate used in a subsequent film forming process through ethanol spray washing.
(4) And (4) coating the filtered mixed solvent type polyamic acid solution obtained in the step (3) on a clean glass substrate through a slit to form a wet film with the thickness of 180 mu m, and drying for 15min at a low temperature (60 ℃) through vacuum (40 Pa).
(5) And under the protection of nitrogen, carrying out high-temperature cyclization by using a temperature program of 100 ℃,30min, 150 ℃,10min, 180 ℃,30min, 250 ℃,30min, 400 ℃,10min, 450 ℃ and 30min to obtain the polyimide film with strong physical adhesion with glass, wherein the thickness of the polyimide film is 15 mu m.
Example 4
(1) At room temperature, 0.034mol (3.7199 g) of p-Phenylenediamine (PDA) monomer is added into 100ml of N-methylpyrrolidone solvent, stirred until the monomer is completely dissolved, then 0.035mol (10.2983 g) of 3, 4-biphenyltetracarboxylic dianhydride (BPDA) is added, and stirring is continued for 12 hours to obtain a first part of polyamic acid solution with the solid content of 12 wt%;
(2) Weighing 50 g of the first part of the polyamic acid solution, adding 25g of N, N-dimethylacetamide solvent, and stirring for 30-60 min at room temperature until a uniform mixed solvent type polyamic acid solution with a solid content of 8wt% is obtained.
(3) Filtering the mixed solvent type polyamic acid solution through a filter, reducing the content of particle impurities in the solution, and cleaning a glass substrate used in a subsequent film forming process through ethanol spray washing.
(4) And (4) coating the filtered mixed solvent type polyamic acid solution obtained in the step (3) on a clean glass substrate through a slit to form a wet film with the thickness of 180 mu m, and drying for 20min at a low temperature (40 ℃) through vacuum (110 Pa).
(5) And under the protection of nitrogen, carrying out high-temperature cyclization at the temperature programs of 100 ℃,30min, 150 ℃,10min, 180 ℃,30min, 250 ℃,30min, 400 ℃,20min, 450 ℃ and 25min to obtain the polyimide film with strong physical adhesion to glass, wherein the thickness of the polyimide film is 15 mu m.
Comparative examples 1 and 2
Comparative example 1 differs from example 1 in that the same aprotic polar solvent as in step (1) is used in step (2); comparative example 2 is also different from example 2 in that the same aprotic polar solvent as in step (1) is used in step (2). The specific implementation of comparative examples 1 and 2 is as follows.
(1) At room temperature, 0.038mol (7.5974 g) of 4,4' -diaminodiphenyl ether (ODA) monomer is added into 100ml of N, N-dimethylacetamide solvent and stirred until the monomer is completely dissolved, 0.041mol (8.9379 g) of 1,2,4, 5-pyromellitic dianhydride (PMDA) is added, and stirring is continued for 12 hours to obtain a first part of polyamic acid solution with solid content of 15 wt%;
(2) The first part of polyamic acid solution was weighed in two parts of 50 g, and then 25g (comparative example 1) and 43.75 g (comparative example 2) of N, N-dimethylacetamide solvent were added, respectively, and stirred at room temperature for 30-60 min until two uniform mixed solvent type polyamic acid solutions were obtained, the sample solutions of comparative example 1 and comparative example 2 having solid contents of 10wt% and 8wt%, respectively.
(3) Filtering the mixed solvent type polyamic acid solution through a filter to reduce the content of particle impurities in the solution, cleaning a glass substrate used in a subsequent film forming process through ethanol spray washing, and performing N-layer cleaning 2 And (5) drying.
(4) And (4) coating the filtered mixed solvent type polyamic acid solution obtained in the step (3) on a clean glass substrate through a slit to form a wet film with the thickness of 150 mu m, and drying for 15min at a low temperature (60 ℃) under vacuum (40 Pa).
(5) And under the protection of nitrogen, carrying out high-temperature cyclization by using temperature programs of 100 ℃,30min, 150 ℃,10min, 180 ℃,30min, 250 ℃,30min, 300 ℃ and 30min to obtain the polyimide films of the comparative sample 1 and the comparative sample 2, wherein the thickness of the polyimide films is 15 mu m.
Comparative examples 3 and 4
Comparative example 3 differs from example 3 in that the same aprotic polar solvent as in step (1) is used in step (2); comparative example 4 is different from example 4 in that the same aprotic polar solvent as in step (1) is used in step (2). The specific implementation procedures of comparative example 3 and comparative example 4 are as follows.
(1) At room temperature, 0.034mol (3.7199 g) of p-Phenylenediamine (PDA) monomer is added into 100ml of N-methylpyrrolidone solvent, stirred until the monomer is completely dissolved, then 0.035mol (10.2983 g) of 3, 4-biphenyltetracarboxylic dianhydride (BPDA) is added, and the stirring is continued for 12 hours to obtain a first part of polyamic acid solution with the solid content of 12 wt%;
(2) Weighing 50 g of the first part of the polyamic acid solution, adding 25g of N-methyl pyrrolidone solvent, and stirring for 30-60 min at room temperature until a uniform mixed solvent type polyamic acid solution with the solid content of 8wt% is obtained.
(3) Filtering the mixed solvent type polyamic acid solution through a filter, reducing the content of particle impurities in the solution, and cleaning a glass substrate used in a subsequent film forming process through ethanol spray washing.
(4) And (4) coating the filtered mixed solvent type polyamic acid solution obtained in the step (3) on a clean glass substrate through a slit to form a wet film with the thickness of 180 mu m, dividing the wet film into two parts, wherein one part is dried for 15min at a low temperature (60 ℃) in vacuum (40 Pa) (comparative example 3), and the other part is dried for 20min at a low temperature (40 ℃) in vacuum (110 Pa) (comparative example 4).
(5) And under the protection of nitrogen, carrying out high-temperature cyclization on two membrane materials by a temperature program of 100 ℃,30min, 150 ℃,10min, 180 ℃,30min, 250 ℃,30min, 400 ℃,10min, 450 ℃ and 30min to obtain the polyimide film samples of the comparative examples 3 and 4, wherein the thickness of the polyimide film samples is 15 mu m.
In order to determine the magnitude of the adhesive force between the polyimide film and the glass substrate, the peel strength of the material, which is the force required to peel a tape having a certain width from the surface of a specific adherend, is measured, and is one of the most important indexes of the tape. The polyimide film was cut into a sample having a width of 25 mm and a length of 200 mm together with the glass substrate according to the standard of the market application, and the test was carried out using a peeling angle of 180 DEG and a peeling speed of 50/100/200 mm/min, respectively, and the results are shown in Table 1.
Table 1 peel strength test results
FIG. 1 schematically provides the infrared spectra at 0, 90, 180 polarization for the film of example 2.
FIG. 2 shows the degree of orientation of the samples of example 1, example 2, comparative example 1, and comparative example 2. The dichroic ratio (R) can be used to characterize the in-plane orientation of the molecule, which is calculated by the formula R = (A0 ° + a180 °)/a90 =DEG, wherein A represents a characteristic absorption peak 1348 cm of C-N-C -1 The absorbance of (2).
The result shows that the degree of motion of the molecular chain in the curing process can be adjusted by adjusting the solvent ratio and the volatilization process, and when the molecular chains are arranged more closely, the orientation degree is higher, so that the generated internal stress is larger, and the peeling strength between the film and the glass is improved.
FIG. 3 shows XRD patterns of example 3, example 4, comparative example 3, and comparative example 4 according to the Bragg formula: 2dsin θ = n λ, and the crystallinity of the samples of example 3, example 4, comparative example 3, and comparative example 4 was 31%, 33%, 22%, and 24%, respectively, as calculated by integrating diffraction peaks. The higher the crystallinity, the higher the regularity of molecular chain arrangement, and thus, adjusting the temperature, pressure and time of the solvent volatilization process can make the molecular chain move more violently and generate more stress in the curing process, thereby improving the peeling strength.
The above embodiments are exemplary only, and are intended to illustrate the technical concept and features of the present invention so that those skilled in the art can understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. A preparation method of a polyimide film with strong physical adhesion with a glass substrate is characterized in that: the method comprises the following steps:
(1) Adding a diamine monomer and an anhydride monomer into a first part of aprotic polar solvent, wherein the molar ratio of the diamine monomer to the anhydride monomer is 1.05-1.2, and reacting at-5 to 60 ℃ for 6-10 hours to obtain a first part of polyamic acid solution;
(2) Diluting the first part of polyamic acid solution with a second part of aprotic polar solvent until the solid content is 5-10wt% and the apparent viscosity is 2000-8000 cp; the second portion of aprotic polar solvent is a different kind of solvent than the first portion of aprotic polar solvent to ensure different volatility characteristics;
(3) Filtering the mixed solvent type polyamic acid solution through a filter to reduce the content of particle impurities in the solution;
(4) Uniformly coating the solution obtained in the step (3) on the surface of a clean glass substrate, and drying for 10-50 min in a vacuum low-temperature environment with the pressure of 30-100Pa and the temperature of 40-70 ℃; under the protection of inert gas, performing cyclization reaction for 200-250 min at 180-450 ℃ to obtain the polyimide film with strong physical adhesion with the glass substrate;
the solid content of the first part of the polyamic acid solution is 12-18 wt%;
in the step (1), the first part of aprotic polar solvent is selected from one of N, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone; the second part of the aprotic polar solvent in the step (2) is one selected from N, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
2. The method for producing a polyimide film according to claim 1, wherein: in the step (1), the first part of diamine monomer and the anhydride monomer are respectively one or more of the following structures, and the diamine monomer has the following structure:
the anhydride monomer has the following structure:
3. the method for producing a polyimide film according to claim 1, wherein: in the step (3), the filter is a polytetrafluoroethylene capsule filter, and two grades with the particle size of 5.0um and 0.45um are connected in series to control the number of particles with the particle size of more than 1um in the solution to be less than 50/mL.
4. The method for producing a polyimide film according to claim 1, wherein: in the step (4), the pressure, temperature and time of the drying operation are selected from one of the following fixed collocation: 30Pa,70 deg.C, 10min;40Pa,60 deg.C, 15min;110Pa,40 ℃ for 20min.
5. The method for producing a polyimide film according to claim 1, wherein: in the step (4), the temperature is 100 ℃ for 30min; 150. 10min at the temperature; 180. 30min at the temperature; 250. 30min at the temperature; 300. the temperature rise and cyclization reaction were carried out at 30min temperature program.
6. The method for producing a polyimide film according to claim 1, wherein: in the step (4), the temperature program of 100 ℃,30min, 150 ℃,10min, 180 ℃,30min, 250 ℃,30min, 400 ℃,10min, 450 ℃ and 30min is adopted for carrying out heating and cyclization reaction.
7. A polyimide film having strong physical adhesion to a glass substrate, characterized in that: prepared by the method of any one of claims 1 to 6.
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