CN111592759A - Modified polyamic acid material and application thereof - Google Patents
Modified polyamic acid material and application thereof Download PDFInfo
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- CN111592759A CN111592759A CN202010405917.5A CN202010405917A CN111592759A CN 111592759 A CN111592759 A CN 111592759A CN 202010405917 A CN202010405917 A CN 202010405917A CN 111592759 A CN111592759 A CN 111592759A
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- flexible substrate
- polyamic acid
- glass substrate
- polyimide flexible
- ultraviolet
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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
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/005—Stabilisers against oxidation, heat, light, ozone
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/80—Manufacture or treatment specially adapted for the organic devices covered by this subclass using temporary substrates
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
- H10K77/10—Substrates, e.g. flexible substrates
- H10K77/111—Flexible substrates
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The application discloses a modified polyamic acid material and application thereof. The invention provides a modified polyamic acid material and application thereof, wherein an ultraviolet absorbent is added into a polyimide flexible substrate, the ultraviolet absorbent generates inert gas after absorbing ultraviolet light, the pressure generated by the inert gas can reduce the adhesive force between the polyimide flexible substrate and a glass substrate, so that the polyimide flexible substrate and the glass substrate are automatically separated, the damage to the polyimide flexible substrate in the process of laser stripping or mechanical stripping can be improved, the separation yield of the flexible substrate and the glass substrate is improved, meanwhile, the ultraviolet absorbent is low in price, and the production cost is also reduced.
Description
Technical Field
The application relates to the technical field of display panels, in particular to a modified polyamic acid material and application thereof.
Background
Compared with the traditional display panel taking glass as a substrate, the flexible display panel taking the flexible film material as the substrate can realize various display forms such as inward and outward folding, multifolding and even curling. Therefore, flexible displays are becoming popular in the current display field and are also a major development direction.
Polyimide (PI), especially transparent PI, is the preferred material for flexible substrates in flexible display panels due to its excellent combination of optical and heat resistance properties.
In the prior art, in order to separate a PI flexible substrate from a glass substrate, the following 2 methods are commonly used: (1) and (3) mechanical stripping process: the mechanical separation of the PI flexible substrate and the glass substrate is realized by introducing a debonding layer between the PI flexible substrate and the rigid glass substrate and setting the adhesive force between the debonding layer and the glass substrate to be larger than the adhesive force between the debonding layer and the PI flexible substrate; (2) the laser stripping process comprises the following steps: laser is irradiated from one side of the glass substrate far away from the PI flexible substrate, and PI on the upper surface of the glass substrate is carbonized through high temperature generated by high-energy laser, so that the bonding force between the PI and the glass substrate is reduced, and the separation of the PI flexible substrate and the glass substrate is realized.
The mechanical stripping process has the defects that the material of the debonding layer is immature and expensive, the laser stripping process has the defects that the laser stripping equipment is expensive, the production cost is increased, and the PI flexible substrate has the defects of holes, even fragments and the like in the laser stripping process, so that the yield of the product is low.
Therefore, there is a need to develop a new method for manufacturing a display panel to overcome the drawbacks of the prior art.
Disclosure of Invention
An object of the present invention is to provide a method for manufacturing a display panel, which can solve the problem of low yield of products in the prior art due to separation of a PI flexible substrate and a glass substrate.
In order to achieve the above object, the present invention provides a modified polyamic acid material, which includes a polyamic acid and an ultraviolet absorber, wherein the ultraviolet absorber includes an ultraviolet absorbing group.
Wherein the polyamic acid is synthesized by low-temperature multiple copolymerization of fluorine-containing dianhydride and alicyclic diamine-containing monomer.
Further, in other embodiments, wherein the modified polyamic acid material further comprises a polar aprotic solvent; in the modified polyamic acid material, the mass fraction of the polyamic acid is 10-20 wt.%, the mass fraction of the ultraviolet absorber is 2-5 wt.%, and the mass fraction of the polar aprotic solvent is 75-88 wt.%.
Further, in other embodiments, wherein the polar aprotic solvent is at least one of N-methylpyrrolidone (NMP), Dimethylformamide (DMF) and Dimethylacetamide (DMAC).
Further, in other embodiments, wherein the uv absorber comprises a benzophenone-based mixture, the uv absorbing group comprises an unsaturated double bond group.
In order to achieve the above object, the present invention further provides a method for manufacturing a display panel, including the steps of: providing a glass substrate and the modified polyamic acid material according to the invention, wherein the modified polyamic acid material is in a liquid state; coating the modified polyamic acid material on the glass substrate; carrying out thermal imidization on the modified polyamic acid material to form a solid polyimide flexible substrate; sequentially preparing functional film layers on the polyimide flexible substrate; and reducing the adhesive force between the polyimide flexible substrate and the glass substrate by irradiating ultraviolet light from the side of the glass substrate far away from the polyimide flexible substrate, so that the polyimide flexible substrate and the glass substrate are automatically separated.
Further, in other embodiments, the step of sequentially preparing each functional film layer on the polyimide flexible substrate comprises: preparing a water-oxygen barrier layer on the polyimide flexible substrate; preparing a thin film transistor layer on the water and oxygen barrier layer; preparing an organic light-emitting layer on the thin film transistor layer; and preparing an encapsulation layer on the organic light-emitting layer.
Further, in other embodiments, the film forming temperature of the water-oxygen barrier layer is lower than 300 ℃, the water-oxygen barrier layer is a stacked structure of silicon nitride and silicon oxide, and the thickness of the silicon nitride is much smaller than that of the silicon oxide.
Further, in other embodiments, before the step of irradiating by ultraviolet light, the ultraviolet absorber is uniformly distributed on the surface of the polyimide flexible substrate close to the glass substrate. Because the density of the ultraviolet absorbent is less than that of the polyimide flexible substrate, the ultraviolet absorbent can be uniformly distributed on the surface of the polyimide flexible substrate close to the glass substrate.
Further, in other embodiments, wherein the ultraviolet absorber has a light transmittance in the visible light range of more than 90%, the ultraviolet absorber has a particle size of less than 100 nm.
Further, in other embodiments, wherein the thermal imidization temperature ranges from 300 ℃ to 400 ℃, the uv absorber has excellent thermal stability at 350 ℃ and above the process temperature, so that the transmittance of the uv absorber can be kept constant during the preparation process before the step of irradiating with uv light.
Further, in other embodiments, wherein the modified polyamic acid material is thermally imidized to form a solid polyimide flexible substrate, the degree of cure is greater than 99.9%.
Further, in other embodiments, the thickness of the polyimide flexible substrate is 5-20 um.
Further, in other embodiments, wherein the adhesion of the polyimide flexible substrate and the glass substrate is greater than 10.0N/cm prior to the step of irradiating with ultraviolet light2。
Further, in other embodiments, wherein after the step of irradiating by ultraviolet light, the adhesion of the polyimide flexible substrate and the glass substrate is less than 0.3N/cm2。
Further, in other embodiments, wherein the wavelength of the ultraviolet light irradiation is 254-400nm, the irradiation energy is 4000mJ/cm2。
Further, in other embodiments, after the step of irradiating by ultraviolet light, the ultraviolet absorber generates an inert gas after absorbing the ultraviolet light, and the inert gas generates a pressure capable of reducing the adhesive force between the polyimide flexible substrate and the glass substrate, so that the polyimide flexible substrate and the glass substrate are automatically separated.
Further, in other embodiments, wherein the inert gas comprises ammonia.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a modified polyamic acid material and application thereof, wherein an ultraviolet absorbent is added into a polyimide flexible substrate, the ultraviolet absorbent generates inert gas after absorbing ultraviolet light, the pressure generated by the inert gas can reduce the adhesive force between the polyimide flexible substrate and a glass substrate, so that the polyimide flexible substrate and the glass substrate are automatically separated, the damage to the polyimide flexible substrate in the process of laser stripping or mechanical stripping can be improved, the separation yield of the flexible substrate and the glass substrate is improved, meanwhile, the ultraviolet absorbent is low in price, and the production cost is also reduced.
Drawings
The technical solution and other advantages of the present application will become apparent from the detailed description of the embodiments of the present application with reference to the accompanying drawings.
Fig. 1 is a flowchart of a method for manufacturing a display panel according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a step 4 of a method for manufacturing a display panel according to an embodiment of the present invention;
fig. 3 is a schematic structural diagram of step 5 of the method for manufacturing a display panel according to the embodiment of the present invention.
Description of the drawings:
a glass substrate-110;
polyimide flexible substrate-120; water oxygen barrier-130;
a thin film transistor layer-140; an organic light-emitting layer-150;
an encapsulation layer-160; ultraviolet absorber-121.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The embodiment of the invention provides a modified polyamic acid material, which comprises polyamic acid, a polar aprotic solvent and an ultraviolet absorber.
In the modified polyamic acid material, the mass fraction of the polyamic acid is 10-20 wt.%, the mass fraction of the ultraviolet absorber is 2-5 wt.%, and the mass fraction of the polar aprotic solvent is 75-88 wt.%.
Wherein the polyamic acid is synthesized by low-temperature multiple copolymerization of fluorine-containing dianhydride and alicyclic diamine-containing monomer.
The ultraviolet absorbent contains ultraviolet absorption groups, the ultraviolet absorbent comprises benzophenone mixtures, and the ultraviolet absorption groups comprise unsaturated double bond groups.
Wherein the polar aprotic solvent is at least one of N-methylpyrrolidone (NMP), Dimethylformamide (DMF), and Dimethylacetamide (DMAC).
Referring to fig. 1, fig. 1 is a flowchart illustrating a method for manufacturing a display panel according to an embodiment of the present invention, where the method includes steps 1-5.
Step 1: the invention provides a glass substrate and the modified polyamic acid material according to the embodiment of the invention, wherein the modified polyamic acid material is in a liquid state.
The modified polyamic acid material contains an ultraviolet absorber, and the ultraviolet absorber contains an ultraviolet absorbing group.
Step 2: and coating the modified polyamic acid material on the glass substrate.
And step 3: carrying out thermal imidization on the modified polyamic acid material to form a solid polyimide flexible substrate; the degree of cure to form a solid polyimide flexible substrate is greater than 99.9%.
Wherein the thickness of the polyimide flexible substrate is 5-20 um.
The ultraviolet absorbent is uniformly distributed on the surface of the polyimide flexible substrate close to the glass substrate. Because the density of the ultraviolet absorbent is less than that of the polyimide flexible substrate, the ultraviolet absorbent can be uniformly distributed on the surface of the polyimide flexible substrate close to the glass substrate.
Wherein the light transmittance of the ultraviolet absorbent in a visible light region exceeds 90%, and the particle size of the ultraviolet absorbent is less than 100 nm.
The thermal imidization temperature range is 300-400 ℃, and the ultraviolet absorbent has excellent thermal stability at 350 ℃ and above the process temperature, so that the light transmittance of the ultraviolet absorbent can be kept constant after the ultraviolet absorbent forms a solid polyimide flexible substrate.
And 4, step 4: sequentially preparing functional film layers on the polyimide flexible substrate; referring to fig. 2, fig. 2 is a schematic structural diagram of a manufacturing method of a display panel according to step 4.
The method for sequentially preparing the functional film layers on the polyimide flexible substrate comprises the following steps: preparing a water oxygen barrier layer 130 on the polyimide flexible substrate 120; preparing a thin film transistor layer 140 on the water and oxygen barrier layer 130; preparing an organic light emitting layer 150 on the thin film transistor layer 140; an encapsulation layer 160 is prepared on the organic light emitting layer 150.
The display panel includes a glass substrate 110, a polyimide flexible substrate 120, an ultraviolet absorber 121, a water and oxygen barrier layer 130, a thin film transistor layer 140, an organic emission layer 150, and an encapsulation layer 160.
The film forming temperature of the water-oxygen barrier layer 130 is lower than 300 ℃, the process highest temperature of the thin-film transistor layer 140 is 350 ℃, the water-oxygen barrier layer 130 is a laminated structure of silicon nitride and silicon oxide, and the thickness of the silicon nitride is far smaller than that of the silicon oxide.
The ultraviolet absorbent has excellent thermal stability at 350 ℃ and above the processing temperature, so that the light transmittance of the ultraviolet absorbent can be kept constant in the preparation process of preparing each functional film layer.
In the step 3 and the step 4, the bonding force of the polyimide flexible substrate and the glass substrate is more than 10.0N/cm2。
And 5: and reducing the adhesive force between the polyimide flexible substrate and the glass substrate by irradiating ultraviolet light from the side of the glass substrate far away from the polyimide flexible substrate, so that the polyimide flexible substrate and the glass substrate are automatically separated. Referring to fig. 3, fig. 3 is a schematic structural diagram of step 5 in the method for manufacturing a display panel according to the embodiment of the present invention.
Wherein the wavelength of the ultraviolet irradiation is 254-400nm, and the irradiation energy is 4000mJ/cm2。
After the step of irradiating by ultraviolet light, the ultraviolet absorbent distributed on the surface of the polyimide flexible substrate close to the glass substrate absorbs the ultraviolet light, the ultraviolet absorption group in the ultraviolet absorbent generates inert gas after absorbing the ultraviolet light, the pressure generated by the inert gas can reduce the adhesive force between the polyimide flexible substrate and the glass substrate, and the adhesive force between the polyimide flexible substrate and the glass substrate is less than 0.3N/cm2And automatically separating the polyimide flexible substrate and the glass substrate.
The polyimide flexible substrate and the glass substrate are automatically separated, so that damage to the polyimide flexible substrate in a laser stripping or mechanical stripping process can be improved, the separation yield of the flexible substrate and the glass substrate is improved, and meanwhile, the ultraviolet absorbent is low in price and the production cost is also reduced.
Wherein the inert gas comprises ammonia.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a modified polyamic acid material and application thereof, wherein an ultraviolet absorbent is added into a polyimide flexible substrate, the ultraviolet absorbent generates inert gas after absorbing ultraviolet light, the pressure generated by the inert gas can reduce the adhesive force between the polyimide flexible substrate and a glass substrate, so that the polyimide flexible substrate and the glass substrate are automatically separated, the damage to the polyimide flexible substrate in the process of laser stripping or mechanical stripping can be improved, the separation yield of the flexible substrate and the glass substrate is improved, meanwhile, the ultraviolet absorbent is low in price, and the production cost is also reduced.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The modified polyamic acid material and the application thereof provided in the embodiments of the present application are described in detail above, and the principle and the implementation manner of the present application are described herein by applying specific examples, and the description of the above embodiments is only used to help understanding the technical solution and the core concept of the present application; those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the present disclosure as defined by the appended claims.
Claims (10)
1. A modified polyamic acid material, comprising: the ultraviolet absorber comprises polyamic acid and an ultraviolet absorber, wherein the ultraviolet absorber contains an ultraviolet absorbing group.
2. The modified polyamic acid material according to claim 1, wherein: polar aprotic solvents are also included; in the modified polyamic acid material, the mass fraction of the polyamic acid is 10-20 wt.%, and the mass fraction of the ultraviolet absorber is 2-5 wt.%.
3. The modified polyamic acid material according to claim 2, wherein: the polar aprotic solvent is at least one of N-methylpyrrolidone, dimethylformamide and dimethylacetamide.
4. The modified polyamic acid material according to claim 1, wherein: the ultraviolet absorbent comprises benzophenone mixture, and the ultraviolet absorption group comprises unsaturated double bond group.
5. A preparation method of a display panel is characterized by comprising the following steps:
providing a glass substrate and the modified polyamic acid material according to any one of claims 1 to 4, wherein the modified polyamic acid material is in a liquid state;
coating the modified polyamic acid material on the glass substrate;
carrying out thermal imidization on the modified polyamic acid material to form a solid polyimide flexible substrate;
sequentially preparing functional film layers on the polyimide flexible substrate;
and reducing the adhesive force between the polyimide flexible substrate and the glass substrate by irradiating ultraviolet light from the side of the glass substrate far away from the polyimide flexible substrate, so that the polyimide flexible substrate and the glass substrate are automatically separated.
6. The method of claim 5, wherein: before the step of irradiating by ultraviolet light, the ultraviolet absorbent is uniformly distributed on the surface of the polyimide flexible substrate close to the glass substrate.
7. The method of claim 5, wherein a light transmittance of the ultraviolet absorber in a visible light region exceeds 90%, and the ultraviolet absorber has a particle size of less than 100 nm.
8. The method of claim 5, wherein the adhesion of the polyimide flexible substrate to the glass substrate is greater than 10.0N/cm prior to the step of irradiating with ultraviolet light2。
9. The method of claim 5, wherein the step of preparing the composition comprisesThe adhesion force of the polyimide flexible substrate and the glass substrate is less than 0.3N/cm after the step of irradiating by ultraviolet light2。
10. The method according to claim 5, wherein after the step of irradiating with the ultraviolet light, the ultraviolet absorber generates an inert gas after absorbing the ultraviolet light, and the inert gas generates a pressure capable of reducing a bonding force of the polyimide flexible substrate and the glass substrate to automatically separate the polyimide flexible substrate and the glass substrate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010405917.5A CN111592759A (en) | 2020-05-14 | 2020-05-14 | Modified polyamic acid material and application thereof |
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| CN202010405917.5A CN111592759A (en) | 2020-05-14 | 2020-05-14 | Modified polyamic acid material and application thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636898A (en) * | 2012-03-14 | 2012-08-15 | 京东方科技集团股份有限公司 | Manufacturing method of flexible display devices |
| JP2015174379A (en) * | 2014-03-17 | 2015-10-05 | ユニチカ株式会社 | laminate |
| CN107356998A (en) * | 2016-05-10 | 2017-11-17 | 住友化学株式会社 | Optical film and the flexible apparatus using the optical film |
| CN108431136A (en) * | 2015-12-28 | 2018-08-21 | 宇部兴产株式会社 | The polyimide precursor composition used in polyimide material, its manufacturing method and its manufacture |
| CN109216589A (en) * | 2018-09-19 | 2019-01-15 | 深圳市化讯半导体材料有限公司 | A kind of preparation method and application of flexible device |
-
2020
- 2020-05-14 CN CN202010405917.5A patent/CN111592759A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636898A (en) * | 2012-03-14 | 2012-08-15 | 京东方科技集团股份有限公司 | Manufacturing method of flexible display devices |
| JP2015174379A (en) * | 2014-03-17 | 2015-10-05 | ユニチカ株式会社 | laminate |
| CN108431136A (en) * | 2015-12-28 | 2018-08-21 | 宇部兴产株式会社 | The polyimide precursor composition used in polyimide material, its manufacturing method and its manufacture |
| CN107356998A (en) * | 2016-05-10 | 2017-11-17 | 住友化学株式会社 | Optical film and the flexible apparatus using the optical film |
| CN109216589A (en) * | 2018-09-19 | 2019-01-15 | 深圳市化讯半导体材料有限公司 | A kind of preparation method and application of flexible device |
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Application publication date: 20200828 |