WO2020232986A1 - 一种pi基板及其制备方法 - Google Patents

一种pi基板及其制备方法 Download PDF

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WO2020232986A1
WO2020232986A1 PCT/CN2019/115991 CN2019115991W WO2020232986A1 WO 2020232986 A1 WO2020232986 A1 WO 2020232986A1 CN 2019115991 W CN2019115991 W CN 2019115991W WO 2020232986 A1 WO2020232986 A1 WO 2020232986A1
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film layer
substrate
compound
film
glass substrate
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French (fr)
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汪亚民
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Wuhan China Star Optoelectronics Semiconductor Display Technology Co Ltd
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Wuhan China Star Optoelectronics Semiconductor Display Technology Co Ltd
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Priority to US16/615,376 priority Critical patent/US11453751B2/en
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3405—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of organic materials
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/32—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with synthetic or natural resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1039—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors comprising halogen-containing substituents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
    • C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D179/00—Coating compositions based on 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 C09D161/00 - C09D177/00
    • C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • 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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/90—Other aspects of coatings
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/15—Deposition methods from the vapour phase
    • C03C2218/152—Deposition methods from the vapour phase by cvd
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1003—Preparatory processes
    • C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
    • C08G73/101—Preparatory processes from tetracarboxylic acids or derivatives and diamines containing chain terminating or branching agents
    • C08G73/1014—Preparatory processes from tetracarboxylic acids or derivatives and diamines containing chain terminating or branching agents in the form of (mono)anhydrid
    • 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

Definitions

  • the present invention relates to the technical field of flat display panels, and in particular, it relates to a PI substrate used and a preparation method thereof.
  • PI polyimide
  • the flexible substrate used is one of the core problems that it is difficult to overcome. This is because if you want to make optoelectronic devices with specific functions flexible, light and thin, the PI materials used must have comprehensive good performance, and good performance also requires various performance tests to be known. Therefore, It is necessary to debug various properties of the PI film made of the PI material.
  • the industry encountered a prominent problem that the polyimide film after film formation is difficult to manually peel off.
  • the PI material commonly used in the industry the polyamic acid formed in the intermediate step of the film formation process, is easy to form a strong ester structure with the hydroxyl group on the hydrophilic glass substrate during the high temperature curing process. In this way, it is difficult to manually remove the film after film formation, and the film removal operation is very complicated.
  • One aspect of the present invention is to provide a PI substrate, which adopts a novel laminated PI layer structure arrangement, so that in the subsequent PI film test process, only the upper PI film layer needs to be peeled off to perform the sampling film performance test , And the remaining PI film layer of the lowest layer is still set on the substrate, and subsequent production can be continued. In this way, the synchronization of the two is of decisive significance in the mass production of panels, saving a lot of mass production the cost of.
  • a PI substrate includes a glass substrate, wherein a first PI film layer is arranged on the glass substrate, and a second PI film layer is arranged on the first PI film layer.
  • the first PI film layer is made of a first PI material
  • the second PI film layer is made of a second PI material. The arrangement of the second PI film layer on the first PI film layer enables it to be completely peeled off from the first PI film layer by manual peeling.
  • the peeled second PI film layer can be used for subsequent PI film performance testing, while the glass substrate with the first PI film layer can be used for subsequent product production.
  • Each can be carried out in parallel without any mutual interference.
  • the remaining glass substrate can only be scrapped.
  • an additional second The PI film is tested for sampling performance.
  • the remaining first PI film is still set on the glass substrate to form a complete PI substrate, and subsequent production can be continued without causing any waste. This is in the panel mass production
  • the above is of decisive significance and saves a lot of cost for mass panel production.
  • the operation of peeling and sampling the PI film layer from the glass substrate is also very cumbersome.
  • the substrate needs to be immersed in deionized water for 3 to 5 days.
  • the peeling of the upper PI film layer relative to the lower PI film layer can be achieved directly by manual operation, and the operation is very simple; and, the surface of the sampled PI film layer after peeling off The flatness is good, and the problem of natural curvature of the surface of the sampling PI film layer in the prior art will not occur.
  • a third PI film layer is further provided on the second PI film layer, and the third PI film layer is made of a third PI material.
  • the first PI material used in the first PI film layer and the second PI material used in the second PI film layer are the same PI material.
  • the first PI material used in the first PI film layer and the second PI material used in the second PI film layer are different PI materials.
  • the first PI material used in the first PI film layer and the molecular structure general formula used in the polyimide compound (defined as general formula I for subsequent reference) )as follows:
  • the raw materials used for the preparation of the polyimide compound of the general formula I include 2,4-ditrifluoromethyl dianhydride (for ease of description, it is referred to as compound A ), 2,4-ditrifluoromethyl-p-aniline (compound B) and phthalic anhydride (compound C).
  • the molar ratio between the compound A and the compound B is 1:3.
  • Another embodiment of the present invention provides a method for preparing the precursor polyamic acid solution of the polyimide composite according to the present invention, including the following steps:
  • the evacuated solution is allowed to stand at room temperature for 2 to 4 hours to obtain the precursor polyamic acid solution of the PI material polyimide composite.
  • the specific PI material used in the first PI material and/or the second PI material is not limited to the PI material represented by the above-mentioned molecular structure formula, which may be known in the industry.
  • the various PI materials used to form the PI film layer, the PI materials having the molecular structure of the general formula I disclosed above are only examples of PI materials used in the PI substrate involved in the present invention.
  • Another aspect of the present invention is to provide a method for preparing the PI substrate of the present invention, which includes the following steps:
  • the precursor polyamic acid solution that provides the first PI material is coated on the glass substrate, and the first H-VCD treatment is performed to remove 50-80% of the solvent, and then the first constant temperature A recipe to form the first PI film layer by cross-linking and curing on the glass substrate;
  • the polyamic acid solution which is the precursor of the first PI material, is coated on the glass substrate in a slit coater.
  • the first H-VCD treatment is to remove the precursor polyamic acid solution of the first PI material coated on the glass substrate at 110-130°C. 65-75% solvent.
  • the highest constant temperature temperature 430 ⁇ 500°C; heating rate: 4 ⁇ 8°C/min; heating times: 1 ⁇ 5 times; cooling rate: 4 ⁇ 8°C/min.
  • the precursor polyamic acid solution of the second PI material is coated on the first PI film layer in a slit coater manner.
  • the second H-VCD treatment is to remove the precursor polyamic acid solution of the second PI material coated on the glass substrate at 110-130°C. 65-75% solvent.
  • the highest constant temperature temperature 430 ⁇ 500°C; heating rate: 4 ⁇ 8°C/min, heating times: 1 to 5 times, cooling rate: 4 ⁇ 8°C/min.
  • the present invention relates to a PI substrate and a preparation method thereof, wherein the glass substrate in the PI substrate is provided with a PI film structure with a double-layer laminated structure, so that after the upper PI film is peeled off, the lower PI film is combined
  • the substrate can also be used for subsequent product production, and unlike the single-layer PI film substrate in the prior art, after the PI film is peeled off, the substrate can only be scrapped.
  • the peeled upper PI film layer is used to test the film performance of the PI film layer, while the lower PI film layer can continue subsequent production on the glass substrate, and the two are carried out simultaneously.
  • FIG. 1 is a schematic structural diagram of a PI substrate provided in an embodiment of the present invention
  • FIG. 2 is a schematic diagram of a constant temperature process provided in an embodiment of the present invention.
  • Fig. 3 is a schematic diagram of a process of a constant temperature process provided in another embodiment of the present invention.
  • FIG. 4 is a schematic diagram of a constant temperature manufacturing process provided in another embodiment of the present invention.
  • Fig. 5 is a schematic diagram of a process of a constant temperature process provided in another embodiment of the present invention.
  • an embodiment of the present invention provides a PI substrate, including a glass substrate.
  • a first PI film layer 12 is provided on the glass substrate 10, and a second PI film layer 14 is provided on the first PI film layer 12.
  • the glass substrate 10 is preferably made of silica glass
  • the first PI film layer 12 is made of a first PI material
  • the second PI film layer 14 is made of a second PI material.
  • the second PI film layer 14 on the first PI film layer 12 can be completely peeled off from the first PI film layer 12 in a manual peeling manner.
  • the second PI film layer 14 after peeling can be used for subsequent PI film performance testing, while the glass substrate 10 with the first PI film layer 12 can be used for subsequent product production.
  • Each can be carried out in parallel without any mutual interference.
  • the remaining glass substrate can only be scrapped.
  • an additional second PI film is provided. 14 Perform the film sampling performance test.
  • the remaining first PI film 12 is still set on the glass substrate 10 and constitutes a complete PI substrate.
  • the subsequent production can be continued without causing any waste. This is in the panel Mass production is of decisive significance, saving a lot of costs for mass production of panels.
  • the operation of peeling the PI film on the glass substrate to sample is also very cumbersome. It usually needs to be immersed in deionized water for 3 to 5 days before it can be realized. Manual sampling operation.
  • the peeling of the upper PI film layer relative to the lower PI film layer can be achieved directly by manual operation, and the operation is very simple; and, the surface of the sampled PI film layer under peeling The flatness is good, and the problem of natural bending of the existing sampling film will not occur.
  • the number of PI film layers provided on the glass substrate 10 is not limited to two layers, and it can be a multi-layered structure as required, for example, 3 layers, 4 layers, 5 layers and so on, the specifics can be determined as needed and are not limited.
  • first PI material used in the first PI film layer 12 and the second PI material used in the second PI film layer 14 may be the same PI material or different PI materials. It depends on the needs and is not limited.
  • the present invention also discloses a PI material and a preparation method thereof, wherein the general molecular structure of the polyimide compound in the PI material (defined as general formula I for subsequent reference) as follows:
  • the polyimide composite of the present invention involves the introduction of benzene ring-containing 2,4-trifluoromethyl dianhydride and blocked conventional dianhydride, and fluorine-containing p-phenylenediamine to obtain a
  • the fluorine polyamic acid solution is applied to the glass substrate to form the PI film.
  • the PI film can be manually peeled off, which is used in the subsequent film characteristics test, especially the tensile performance test , Bending performance test, CTE test and other performance tests that have higher requirements for the regularity and uniformity of the tested material samples, providing good test samples.
  • polyimide composite material involved in the present invention can be widely used in OLED factories, semiconductor factories, etc., and has broad application prospects and market prospects.
  • the preparation of the polyimide composite includes two stages: the first stage is the preparation stage of its precursor polyamic acid solution, and the second stage is the film forming stage.
  • the raw materials used for the preparation of the precursor polyamic acid solution in the first stage include 2,4-ditrifluoromethyl dianhydride (for ease of description, referred to as compound A), 2,4-ditrifluoro Methyl p-aniline (compound B) and phthalic anhydride (compound C).
  • the first stage includes the following steps:
  • the general structural formula of the precursor polyamic acid of the polyimide composite obtained in the present invention is as follows:
  • the second stage includes the following steps:
  • the precursor polyamic acid solution from which bubbles have been removed is coated on a glass substrate using a slit coater, and 70% of the solvent is removed by H-VCD, and then a flexible film is used.
  • the post-baking machine performs a constant temperature (recipe) process to make it cross-link and solidify to form a PI film layer.
  • the molecular structure of the polyimide compound in the PI material in the film layer is the general formula I.
  • the constant temperature process used therein involves the following parameters: the highest constant temperature temperature: 430-500°C; the heating rate: 4-8°C/min; the number of heating times: 1 to 5 times.
  • the highest constant temperature temperature 430-500°C
  • the heating rate 4-8°C/min
  • the number of heating times 1 to 5 times.
  • Figures 2 to 5 respectively illustrate the process diagrams of 4 different constant temperature processes.
  • Another embodiment of the present invention provides a method for preparing the PI substrate related to the present invention, including the following steps:
  • the parameters involved in the first constant temperature process and the second constant temperature process involved are preferably the constant temperature process parameters disclosed in the present invention, but they can also be other constant temperature process parameters known in the industry, which can be specifically based on the selected PI material The specific selection is not limited.
  • the present invention relates to a PI substrate for testing, which adopts a double-layer PI film structure arranged on the substrate, so that after the upper PI film is peeled off, the lower PI film can be combined with the substrate to perform subsequent product production.
  • the substrate can only be scrapped after the PI film is peeled off.
  • the peeled upper PI film layer is used for sampling performance testing of the PI film layer, and the two can be performed simultaneously, which is of great significance in panel mass production and saves a lot of cost for mass production.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
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  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)

Abstract

本发明提供了一种PI基板，包括玻璃基板，其中所述玻璃基板上设置有第一PI膜层，所述第一PI膜层上设置有第二PI膜层。其中所述第一PI膜层采用第一PI材料构成，所述第二PI膜层采用第二PI材料构成。其中所述第二PI膜层于所述第一PI膜层上的设置方式使得其能够以手动剥离的方式从所述第一PI膜层上完整剥离。本发明提供了一种PI基板，其采用新型的叠层PI层结构设置，使得其在后续的PI膜层测试过程中，只需剥离上层的PI膜层进行取样膜层的性能测试，而保留的最下层的PI膜层依然设置在基板上，还能继续进行后续的生产，如此，两者的同步进行，这在面板量产上具有举足轻重的意义，为大批量生产节约了大量的成本。

Description

一种PI基板及其制备方法 技术领域
本发明涉及平面显示面板技术领域，尤其是，其中涉及使用的PI基板及其制备方法。
背景技术
已知，目前OLED面板、太阳能电池板等越来越多的新型光电器件正在朝着柔性、轻薄的方向发展。而其中涉及的所述光电器件的柔性与否，在很大程度上是取决于其所使用的衬底材料。
对此，业界开发出了一种聚酰亚胺(PI)材料，其所具有的柔性、轻薄的性能在一定程度上满足了业界对于柔性衬底材料的要求。但是由于不同性能的光电器件对于其采用的PI材料会有不同的性能要求，这也使得业界持续不断的对PI材料进行研发。
以OLED领域中的光电器件为例，其采用的柔性衬底即为其难以攻克的核心难题之一。这是因为，若想使得特定功能的光电器件具有柔性、轻薄的性能，必须要求其所使用的PI材料具有综合的良好性能，而良好的性能也需要各种性能测试才能获知，因此，也就需要对采用的PI材料构成的PI膜层进行各种性能的调试。
而在性能测试中，业界遇到了一个突出的问题就是成膜后的聚酰亚胺膜难以进行手动剥离。这是因为，业界通常采用的PI材料，在其成膜过程的中间步骤中形成的聚酰胺酸，在高温固化的过程中容易与亲水的玻璃基板上的羟基形成较强的酯基结构，如此，使得其在成膜之后很难完成手动揭下，取膜操作十分复杂。
进一步的，即使能够完成对成膜后的PI膜层的取样以及后续的性能测试，该取样后的成膜用的玻璃基板，业界只会对其进行报废处理，这也是一种浪费，并在一定程度上导致测试成本上升。
因此，确有必要来开发一种新型的测试用PI基板，来克服现有 技术中的缺陷。
技术问题
本发明的一个方面是提供一种PI基板，其采用新型的叠层PI层结构设置，使得其在后续的PI膜层测试过程中，只需剥离上层的PI膜层进行取样膜层的性能测试，而保留的最下层的PI膜层依然设置在基板上，还能继续进行后续的生产，如此，两者的同步进行，这在面板量产上具有举足轻重的意义，为大批量生产节约了大量的成本。
技术解决方案
本发明采用的技术方案如下：
一种PI基板，包括玻璃基板，其中所述玻璃基板上设置有第一PI膜层，所述第一PI膜层上设置有第二PI膜层。其中所述第一PI膜层采用第一PI材料构成，所述第二PI膜层采用第二PI材料构成。其中所述第二PI膜层于所述第一PI膜层上的设置方式使得其能够以手动剥离的方式从所述第一PI膜层上完整剥离。
进一步的，其中剥离后的所述第二PI膜层可以用于后续的PI膜层性能测试，而存有所述第一PI膜层的所述玻璃基板则可进行后续的产品生产，两者能够各自并行进行，并不会产生任何的相互干扰。相对于现有技术中的单层PI膜层基板，其玻璃基板上的PI膜层被取样剥离后，剩下的所述玻璃基板只能进行报废处理的方式而言，本案设置额外的第二PI膜层进行取样性能测试，剩下的第一PI膜层依旧设置于玻璃基板上并构成一个完整的PI基板，还能继续进行后续的生产，而不会造成任何浪费，这在面板量产上具有举足轻重的意义，为大批量的面板生产节约了大量的成本。
而且，现有技术中涉及的单层PI膜层基板，其上设置的PI膜层从玻璃基板上剥离取样的操作也是十分繁琐，通常需要先将基板放在去离子水中浸泡3～5天后，才能实现其上的PI膜层的手动剥离取样操作。而本发明涉及的这种双PI膜层结构，上层PI膜层相对于下层PI膜层的剥离完全可以直接通过手动操作即可实现，操作十分简便； 且，剥离下的取样PI膜层的表面平整性好，不会出现现有技术中的取样PI膜层出现的表面自然弯曲的问题。
进一步的，在不同实施方式中，其中所述第二PI膜层上还设置有第三PI膜层，其中所述第三PI膜层采用第三PI材料构成。
进一步的，在不同实施方式中，其中所述第一PI膜层采用的第一PI材料与所述第二PI膜层采用的第二PI材料为相同的PI材料。
进一步的，在不同实施方式中，其中所述第一PI膜层采用的第一PI材料与所述第二PI膜层采用的第二PI材料为不同的PI材料。
进一步的，在不同实施方式中，其中所述第一PI膜层采用的第一PI材料，其中的聚酰亚胺复合物采用的分子结构通式(将其定义为通式Ⅰ，便于后续引用)如下：
Figure PCTCN2019115991-appb-000001
进一步的，在不同实施方式中，其中采用所述通式Ⅰ的所述聚酰亚胺复合物采用的制备原料包括2,4－二三氟甲基二酸酐(为便于描述，记为化合物A)、2,4－二三氟甲基对苯胺(化合物B)以及邻苯二甲酸酐(化合物C)。
进一步的，在不同实施方式中，其中所述化合物A和化合物B之间的摩尔比为1:3。
进一步的，在不同实施方式中，其中所述化合物C与所述化合物A/化合物B两者混合物之间的摩尔比为C:A/B＝1：(1～4)。
进一步的，本发明的又一实施方式提供了一种制备本发明涉及的所述聚酰亚胺复合物的前驱体聚酰胺酸溶液的制备方法，包括以下步骤：
将原料中的化合物A：2,4－二三氟甲基二酸酐、化合物B：2,4－二三氟甲基对苯胺加入到N,N－二甲基己酰胺与N－甲基吡咯烷酮的混合物中，然后开始搅拌；
将原料中的化合物C：邻苯二甲酸酐加入到上述搅拌中的混合物中，在20～40度下揽拌24～96h，使其充分溶解；
在真空环境下进行抽滤，将通过抽滤得到的溶液用真空泵抽气0.8～1.5h，除去溶液中的气泡；
将抽气过后的溶液在室温下静置2～4h，进而得到所述PI材料聚酰亚胺复合物的前驱体聚酰胺酸溶液。
进一步的，在不同实施方式中，其中所述第一PI材料和/或所述第二PI材料采用的具体PI材料并不限于上述分子结构通式所表示的PI材料，其可以是业界已知的各种用于形成PI膜层的PI材料，以上揭示的具有所述通式Ⅰ分子结构的PI材料只是对本发明涉及的PI基板中涉及使用的PI材料做举例性说明。
进一步的，本发明的又一方面是提供一种本发明涉及的所述PI基板的制备方法，包括以下步骤：
提供一玻璃基板；
提供所述第一PI材料的前驱体聚酰胺酸溶液涂布于所述玻璃基板上，对其进行第一H-VCD处理以除去其中的50～80％的溶剂，然后对其进行第一恒温制程(recipe)，使其在所述玻璃基板上交联固化形成所述第一PI膜层；
在所述第一PI膜层上涂布所述第二PI材料的前驱体聚酰胺酸溶液，对其进行第二H-VCD处理以除去其中的50～80％的溶剂，然后对其进行第二恒温制程，使其在所述第一PI膜层上交联固化形成所述第二PI膜层。
进一步的，在不同实施方式中，其中所述第一PI材料的前驱体 聚酰胺酸溶液是以平涂(slit coater)的方式涂布在所述玻璃基板上。
进一步的，在不同实施方式中，其中所述第一H-VCD处理为在110～130℃下除去涂布在所述玻璃基板上的所述第一PI材料的前驱体聚酰胺酸溶液中的65～75％的溶剂。
进一步的，在不同实施方式中，其中所述第一恒温制程中，其最高恒温温度:430～500℃；升温速率：4～8℃/min；升温次数：1～5次；降温速率：4～8℃/min。
进一步的，在不同实施方式中，其中所述第二PI材料的前驱体聚酰胺酸溶液是以平涂(slit coater)的方式涂布在所述第一PI膜层上。
进一步的，在不同实施方式中，其中所述第二H-VCD处理为在110～130℃下除去涂布在所述玻璃基板上的所述第二PI材料的前驱体聚酰胺酸溶液中的65～75％的溶剂。
进一步的，在不同实施方式中，其中所述第二恒温制程中，其最高恒温温度:430～500℃；升温速率：4～8℃/min，升温次数：1～5次，降温速率：4～8℃/min。
有益效果
本发明涉及的一种PI基板及其制备方法，其中所述PI基板中的玻璃基板上采用双层叠层结构的PI膜层结构设置，使得上层的PI膜层在剥离后，下层PI膜层结合所述基板还能进行后续的产品生产，而不会如现有技术中的单层PI膜层基板，在PI膜层剥离后，所述基板只能进行报废处理。
且，所述剥离的上层PI膜层用于进行PI膜层的膜层性能测试，而下层PI膜层在玻璃基板上可继续进行后续的生产，两者同步进行，这在面板量产上具有举足轻重的意义，为大批量生产节约了大量的成本。
附图说明
为了更清楚地说明本发明实施例中的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明的一个实施方式中提供的一种PI基板的结构示意图；
图2为本发明的一个实施方式中提供的一种恒温制程的过程示意图；
图3为本发明的又一个实施方式中提供的一种恒温制程的过程示意图；
图4为本发明的又一个实施方式中提供的一种恒温制程的过程示意图；
图5为本发明的又一个实施方式中提供的一种恒温制程的过程示意图。
本发明的实施方式
以下将结合附图和实施例，对本发明涉及的一种PI基板及其制备方法的技术方案作进一步的详细描述。
请参阅图1所示，本发明的一个实施方式提供了一种PI基板，包括玻璃基板。
其中所述玻璃基板10上设置有第一PI膜层12，所述第一PI膜层12上设置有第二PI膜层14。其中所述玻璃基板10优选采用硅玻璃，所述第一PI膜层12采用第一PI材料构成，所述第二PI膜层14采用第二PI材料构成。其中所述第二PI膜层14于所述第一PI膜层12上能够以手动剥离的方式从所述第一PI膜层12上完整剥离。
其中剥离后的所述第二PI膜层14能够用于后续的PI膜层性能测试，而存有所述第一PI膜层12的所述玻璃基板10则可进行后续 的产品生产，两者能够各自并行进行，并不会产生任何的相互干扰。相对于现有技术中的单层PI膜层基板，其在其PI膜层取样剥离后，剩下的所述玻璃基板只能进行报废处理的方式而言，本案设置额外的第二PI膜层14进行膜层取样性能测试，剩下的第一PI膜层12依旧设置于玻璃基板10上并构成一个完整的PI基板，还能继续进行后续的生产，而不会造成任何浪费，这在面板量产上具有举足轻重的意义，为大批量的面板生产节约了大量的成本。
而且，现有技术中涉及的单层PI膜层基板，其上设置的PI膜层从玻璃基板上剥离取样的操作也是十分繁琐，其通常需要先在去离子水中浸泡3～5天后，才能实现手动取样操作。而本发明涉及的这种双PI膜层结构，上层PI膜层相对于下层PI膜层的剥离完全可以直接通过手动操作即可实现，操作十分简便；且，剥离下的取样PI膜层的表面平整性好，不会出现现有取样膜层出现的自然弯曲的问题。
进一步的，在不同实施方式中，其中所述玻璃基板10上设置的PI膜层的数量，并不限于是两层，其可以是根据需要的多叠层结构，例如，3层、4层、5层等等，具体可随需要而定，并无限定。
进一步的，其中所述第一PI膜层12采用的第一PI材料与所述第二PI膜层14采用的第二PI材料可以是相同的PI材料，也可以是不同的PI材料，具体可随需要而定，并无限定。
进一步的，本发明还揭示了一种PI材料及其制备方法，其中所述PI材料中的聚酰亚胺复合物采用的分子结构通式(将其定义为通式Ⅰ，以便于后续引用)如下：
Figure PCTCN2019115991-appb-000002
本发明涉及的所述聚酰亚胺复合物，其通过引入苯环的2,4－三 氟甲基的二酐以及封端的常规二酐，与含氟对苯二胺，进而得到一种含氟的聚酰胺酸溶液，将其应用到玻璃基板上进行PI膜层的成膜，成膜后的PI膜层能够进行手动剥离，从而为后续的膜特性测试中，尤其是，拉伸性能测试、弯曲性能测试、CTE测试等对测试的材料样品的规整性、均一性有较高要求的性能测试，提供了良好的测试样品。
进一步的，本发明涉及的这种聚酰亚胺复合物材料可以广泛应用于OLED工厂、半导体工厂等等，具有广泛的应用前景以及市场前景。
进一步的，为避免不必要的重复，以下将结合本发明涉及的所述聚酰亚胺复合物的制备方法，对本发明涉及的所述聚酰亚胺复合物做进一步的细节说明。其中所述聚酰亚胺复合物的制备包括两个阶段：第一阶段为其前驱体聚酰胺酸溶液的制备阶段，第二阶段则为成膜阶段。
其中所述第一阶段中的所述前驱体聚酰胺酸溶液采用的制备原料包括2,4－二三氟甲基二酸酐(为便于描述，记为化合物A)、2,4－二三氟甲基对苯胺(化合物B)以及邻苯二甲酸酐(化合物C)。
其中所述化合物A、化合物B以及化合物C采用的结构通式分别如下：
Figure PCTCN2019115991-appb-000003
其中所述第一阶段包括以下步骤：
称取制备原料中的化合物A(0.1～10mmol)和化合物B(0.1～10mmol)，其中所述化合物A和化合物B的摩尔比为A:B＝1： (1～3)，加入到放有N,N－二甲基己酰胺与N－甲基吡咯烷酮的混合物(DMAC/NMP＝v/v＝0.2～2)的双口烧瓶中，然后将所述双口烧瓶转移至机械揽拌器，并开启揽拌；
称取化合物C(0.1～5mmol)，其中所述化合物C与所述化合物A和化合物混合物的摩尔比为C:A/B＝1：(1～4)，将所述化合物C逐勺加至上述双口烧瓶中，整个混合溶液在室温下揽拌24～96h，使其充分溶解；
撤去机械揽拌器，在真空环境下对所述混合溶液进行抽滤，再将上述通过抽滤得到的所述混合溶液用真空泵抽气0.8～1.2h，除去溶液中的气泡；将抽气过后的溶液在室温(20～40度)下静置2～4h，使溶液中的气泡进一步减少，直到中无肉眼可见的气泡，至此，所述第一阶段完成。其中得到的本发明涉及的所述聚酰亚胺复合物的前驱体前驱体聚酰胺酸的结构通式如下：
Figure PCTCN2019115991-appb-000004
其中所述第二阶段包括以下步骤：
将除去气泡的所述前驱体聚酰胺酸溶液使用平涂(slit coater)的方式将其涂覆在一玻璃基板上，经过H-VCD除去其中的70％的溶剂部分，再将其使用柔性膜后烘机进行恒温(recipe)制程，使其交联固化，进而形成PI膜层，其中膜层中的PI材料中的聚酰亚胺复合物的分子结构通式即为所述通式Ⅰ。
进一步的，其中涉及使用的恒温制程，其采用的参数为：最高恒温温度:430～500℃；升温速率：4～8℃/min；升温次数：1～5次。具体的，请参阅图2～5所示，其分别图示了4种不同的恒温制程的过程图示。
进一步的，本发明的又一个实施方式提供了一种本发明涉及的所述PI基板的制备方法，包括以下步骤：
提供一玻璃基板；
提供第一PI材料的前驱体聚酰胺酸溶液并以平涂(slit coater)的方式将其涂覆在所述玻璃基板上，对其进行第一H-VCD处理除去其中的70％的溶剂，再将其使用柔性膜后烘机进行第一恒温(recipe)制程，使其交联固化形成第一层PI膜层，将此层PI膜作为第一层测试的基底；
然后再在所述第一层PI膜层上第二次以slit coater的方式将同样的所述PI材料的前驱体聚酰胺酸溶液涂覆于其上，经过第二H-VCD除去其中的70％的溶剂，再将其使用柔性膜后烘机进行第二恒温制程，使其交联固化形成第二层PI膜层。如此，完成本发明涉及的所述双层PI膜层的PI基板结构。
其中涉及的所述第一恒温制程和第二恒温制程中涉及使用的参数优选是上述本发明揭示的恒温制程参数，但也可以是其他业界已知的恒温制程参数，具体可根据选用的PI材料来具体选用，并无限定。
本发明涉及的一种测试用PI基板，其采用基板上设置双层PI膜层结构，使得其上层的PI膜层在剥离后，下层PI膜层结合所述基板还能进行后续的产品生产，而不会如现有技术中的单层PI膜层基板，在PI膜层剥离后，所述基板只能进行报废处理。且，所述剥离的上层PI膜层是用于进行PI膜层的取样性能测试，两者可同步进行，这在面板量产上具有举足轻重的意义，为大批量生产节约了大量的成本。
本发明的技术范围不仅仅局限于上述说明中的内容，本领域技术人员可以在不脱离本发明技术思想的前提下，对上述实施例进行多种变形和修改，而这些变形和修改均应当属于本发明的范围内。

Claims (10)

  1. 一种PI基板，包括玻璃基板，其中所述玻璃基板上设置有第一PI膜层，所述第一PI膜层上设置有第二PI膜层；
    其中所述第一PI膜层采用第一PI材料构成，所述第二PI膜层采用第二PI材料构成；
    其中所述第二PI膜层于所述第一PI膜层上的设置方式使得其能够以手动剥离的方式从所述第一PI膜层上完整剥离。
  2. 根据权利要求1所述的PI基板，其中所述第二PI膜层上还设置有第三PI膜层，其中所述第三PI膜层采用第三PI材料构成。
  3. 根据权利要求1所述的PI基板，其中所述第一PI膜层采用的第一PI材料与所述第二PI膜层采用的第二PI材料为相同的PI材料。
  4. 根据权利要求1所述的PI基板，其中所述第一PI膜层采用的第一PI材料，其中的聚酰亚胺复合物采用的分子结构通式如下：
    Figure PCTCN2019115991-appb-100001
  5. 根据权利要求4所述的PI基板，其中所述聚酰亚胺复合物采用的制备原料包括化合物A：2,4－二三氟甲基二酸酐、化合物B：2,4－二三氟甲基对苯胺以及化合物C：邻苯二甲酸酐。
  6. 根据权利要求5所述的PI基板，其中所述化合物A和化合物B之间的摩尔比为1:3。
  7. 根据权利要求5所述的PI基板，其中所述化合物C与所述化合物A/化合物B两者混合物之间的摩尔比为C:A/B＝1：(1～4)。
  8. 一种制备根据权利要求1所述的PI基板的制备方法，包括以 下步骤：
    提供一玻璃基板；
    提供所述第一PI材料的前驱体聚酰胺酸溶液涂布于所述玻璃基板上，对其进行第一H-VCD处理以除去其中的50～80％的溶剂，然后对其进行第一恒温制程(recipe)，使其在所述玻璃基板上交联固化形成所述第一PI膜层；
    在所述第一PI膜层上涂布所述第二PI材料的前驱体聚酰胺酸溶液，对其进行第二H-VCD处理以除去其中的50～80％的溶剂，然后对其进行第二恒温制程，使其在所述第一PI膜层上交联固化形成所述第二PI膜层。
  9. 根据权利要求8所述的PI基板制备方法，其中所述第一H-VCD处理为在110～130℃下除去涂布在所述玻璃基板上的所述第一PI材料的前驱体聚酰胺酸溶液中的65～75％的溶剂。
  10. 根据权利要求8所述的PI基板制备方法，其中所述第一恒温制程和/或第二恒温制程中，其最高恒温温度:430～500℃；升温速率：4～8℃/min；升温次数：1～5次；降温速率：4～8℃/min。
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