WO2019024547A1 - 正性光刻胶组合物、过孔的形成方法、显示基板及显示装置 - Google Patents

正性光刻胶组合物、过孔的形成方法、显示基板及显示装置 Download PDF

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Publication number
WO2019024547A1
WO2019024547A1 PCT/CN2018/084484 CN2018084484W WO2019024547A1 WO 2019024547 A1 WO2019024547 A1 WO 2019024547A1 CN 2018084484 W CN2018084484 W CN 2018084484W WO 2019024547 A1 WO2019024547 A1 WO 2019024547A1
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Prior art keywords
photoresist composition
group
positive photoresist
compound
layer
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Ceased
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PCT/CN2018/084484
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English (en)
French (fr)
Inventor
李伟
苏同上
李广耀
胡迎宾
马睿
邵继峰
张扬
张建业
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BOE Technology Group Co Ltd
Hefei Xinsheng Optoelectronics Technology Co Ltd
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BOE Technology Group Co Ltd
Hefei Xinsheng Optoelectronics Technology Co Ltd
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Priority to US16/300,474 priority Critical patent/US11526077B2/en
Publication of WO2019024547A1 publication Critical patent/WO2019024547A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/004—Photosensitive materials
    • G03F7/039—Macromolecular compounds which are photodegradable, e.g. positive electron resists
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/004—Photosensitive materials
    • G03F7/022—Quinonediazides
    • G03F7/0226—Quinonediazides characterised by the non-macromolecular additives
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/136—Liquid crystal cells structurally associated with a semi-conducting layer or substrate, e.g. cells forming part of an integrated circuit
    • G02F1/1362—Active matrix addressed cells
    • G02F1/136227—Through-hole connection of the pixel electrode to the active element through an insulation layer
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/004—Photosensitive materials
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/004—Photosensitive materials
    • G03F7/027—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds
    • G03F7/028—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds with photosensitivity-increasing substances, e.g. photoinitiators
    • G03F7/031—Organic compounds not covered by group G03F7/029
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/004—Photosensitive materials
    • G03F7/039—Macromolecular compounds which are photodegradable, e.g. positive electron resists
    • G03F7/0392—Macromolecular compounds which are photodegradable, e.g. positive electron resists the macromolecular compound being present in a chemically amplified positive photoresist composition
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/004—Photosensitive materials
    • G03F7/085—Photosensitive compositions characterised by adhesion-promoting non-macromolecular additives
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/16—Coating processes; Apparatus therefor
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/20—Exposure; Apparatus therefor
    • G03F7/2002—Exposure; Apparatus therefor with visible light or UV light, through an original having an opaque pattern on a transparent support, e.g. film printing, projection printing; by reflection of visible or UV light from an original such as a printed image
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26—Processing photosensitive materials; Apparatus therefor
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26—Processing photosensitive materials; Apparatus therefor
    • G03F7/40—Treatment after imagewise removal, e.g. baking
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D86/00—Integrated devices formed in or on insulating or conducting substrates, e.g. formed in silicon-on-insulator [SOI] substrates or on stainless steel or glass substrates
    • H10D86/01—Manufacture or treatment
    • H10D86/021—Manufacture or treatment of multiple TFTs
    • H10D86/0212—Manufacture or treatment of multiple TFTs comprising manufacture, treatment or coating of substrates
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D86/00—Integrated devices formed in or on insulating or conducting substrates, e.g. formed in silicon-on-insulator [SOI] substrates or on stainless steel or glass substrates
    • H10D86/01—Manufacture or treatment
    • H10D86/021—Manufacture or treatment of multiple TFTs
    • H10D86/0231—Manufacture or treatment of multiple TFTs using masks, e.g. half-tone masks
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D86/00—Integrated devices formed in or on insulating or conducting substrates, e.g. formed in silicon-on-insulator [SOI] substrates or on stainless steel or glass substrates
    • H10D86/40—Integrated devices formed in or on insulating or conducting substrates, e.g. formed in silicon-on-insulator [SOI] substrates or on stainless steel or glass substrates characterised by multiple TFTs
    • H10D86/451—Integrated devices formed in or on insulating or conducting substrates, e.g. formed in silicon-on-insulator [SOI] substrates or on stainless steel or glass substrates characterised by multiple TFTs characterised by the compositions or shapes of the interlayer dielectrics
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D86/00—Integrated devices formed in or on insulating or conducting substrates, e.g. formed in silicon-on-insulator [SOI] substrates or on stainless steel or glass substrates
    • H10D86/40—Integrated devices formed in or on insulating or conducting substrates, e.g. formed in silicon-on-insulator [SOI] substrates or on stainless steel or glass substrates characterised by multiple TFTs
    • H10D86/60—Integrated devices formed in or on insulating or conducting substrates, e.g. formed in silicon-on-insulator [SOI] substrates or on stainless steel or glass substrates characterised by multiple TFTs wherein the TFTs are in active matrices
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P50/00—Etching of wafers, substrates or parts of devices
    • H10P50/20—Dry etching; Plasma etching; Reactive-ion etching
    • H10P50/28—Dry etching; Plasma etching; Reactive-ion etching of insulating materials
    • H10P50/286—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of organic materials
    • H10P50/287—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of organic materials by chemical means
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P50/00—Etching of wafers, substrates or parts of devices
    • H10P50/73—Etching of wafers, substrates or parts of devices using masks for insulating materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P76/00—Manufacture or treatment of masks on semiconductor bodies, e.g. by lithography or photolithography
    • H10P76/20—Manufacture or treatment of masks on semiconductor bodies, e.g. by lithography or photolithography of masks comprising organic materials
    • H10P76/204—Manufacture or treatment of masks on semiconductor bodies, e.g. by lithography or photolithography of masks comprising organic materials of organic photoresist masks
    • H10P76/2041—Photolithographic processes

Definitions

  • the present invention relates to the field of display technologies, and in particular, to a positive photoresist composition, a via forming method using the positive photoresist composition, a display substrate including the via formed by the via forming method, and a display substrate The display device of the foregoing display substrate.
  • Lithography is an indispensable process in the fabrication of thin film transistor arrays, which plays a role in pattern transfer. Applying a photoresist on the clean film to be etched, and obtaining a designed reticle pattern (ie, a photoresist pattern) by soft baking, exposure, development, post-baking, etc., and then exposing the photoresist pattern The film region is etched to form a target pattern conforming to the photoresist pattern, and the remaining photoresist pattern is stripped to expose the target pattern for subsequent processing.
  • a designed reticle pattern ie, a photoresist pattern
  • the implementation of the lithography process is inseparable from the photoresist.
  • the main component of the photoresist is a kind of photosensitive group-containing polymer. Under ultraviolet light, a series of chemical changes occur in the photosensitive group of the exposed portion, resulting in development of the photosensitive portion and the unexposed portion of the photoresist. The solubility in the liquid produces a significant difference, resulting in a specific pattern after development.
  • Thin film transistor array manufacturing process usually involves several lithography processes, including metal film process, inorganic insulating layer (such as silicon oxide SiO x , silicon nitride SiN x ) process, active layer process, ITO (Indium Tin Oxide, Indium tin oxide) layer process, etc.
  • metal film process inorganic insulating layer (such as silicon oxide SiO x , silicon nitride SiN x ) process, active layer process, ITO (Indium Tin Oxide, Indium tin oxide) layer process, etc.
  • inorganic passivation layer PVX
  • an organic film layer to protect the underlying film layer and provide a planarized substrate. effect.
  • the organic film layer has an organic film hole exposing the underlying PVX layer, and a via (ie, Via) process is performed in the organic film hole, specifically including a photolithography, etching, and stripping process to form a Via hole on the PVX layer.
  • a via ie, Via
  • the organic film layer is usually composed of a non-polar organic material, and the main component polymer in the photoresist is also a non-polar organic material (such as a phenol-formaldehyde polymer), so the polarities of the two are similar and are formed.
  • the photoresist is directly coated on an organic film having a similar polarity, and the adhesion between the photoresist and the organic film layer is large, and the photoresist is not completely peeled off after the Via hole etching.
  • the problem is that photoresist residue occurs, which affects the subsequent process of the Oxide backplane and reduces production yield.
  • the present disclosure provides a positive photoresist composition, a via forming method using the positive photoresist composition, and a via formed by the foregoing via forming method.
  • the display substrate and the display device comprising the display substrate, wherein the positive photoresist composition comprises a photoisomerization compound, and the structure is converted into an ion structure with an increased degree of molecular polarity after being irradiated by ultraviolet light, which is reduced.
  • the adhesion between the positive photoresist and the organic film layer facilitates peeling after formation of the via hole and improves the production yield of the product.
  • the present disclosure provides a positive photoresist composition
  • a positive photoresist composition comprising a host rubber and a photosensitizer, wherein the photoresist composition further comprises a photoisomerization compound, the photoisomerization compound being subjected to After ultraviolet light irradiation, the structure is transformed into an ion structure with an increased degree of molecular polarity.
  • the photoisomerizable compound includes at least one of a spiropyran compound, a spirooxazine compound, an aziridine compound, and a bipyridine compound.
  • the spiropyran compound has the structure of the following formula (I):
  • R 1 group is an alkyl chain, an ether chain, or a phenyl group
  • R 2 is a carboxyl group or a hydroxyl group.
  • the aforementioned alkyl chain is selected from the group consisting of butyl, pentyl and hexyl; and/or the aforementioned ether chain is (CH 2 CH 2 O) m CH 3 wherein m is an integer and 1 ⁇ m ⁇ 5.
  • the spiropyran compound has the structure of the following formula (I'):
  • the spiropyran compound has the structure of the following formula (II):
  • n is an integer and 4 ⁇ n ⁇ 10; and R is a carboxyl group or a hydroxyl group.
  • the spirooxazine compound has the structure of the following formula (III):
  • R 1 is CH 2 CH 2 OH; and the R 2 group is a carboxyl group or a hydroxyl group.
  • the aziridine compound has the structure of the following formula (IV):
  • R is C 2 H 4 OH.
  • the bipyridine compound has the structure of the following formula (V):
  • R 1 is hydrogen, any of a methyl, ethyl, propyl, butyl ether chain
  • R 2 is carboxymethyl, carboxyethyl, carboxypropyl any one of
  • R 3 is Any one of hydrogen, a methyl group, an ethyl group, a propyl group, a butyl group, and an ether chain
  • R 4 is any one of a carboxymethyl group, a carboxyethyl group, and a carboxypropyl group.
  • the positive photoresist composition further comprises a solvent and an additive.
  • the main adhesive material accounts for 5% to 30% of the total weight of the positive photoresist composition;
  • the photosensitizer accounts for the positive lithography 2% to 5% by weight of the total weight of the gel composition;
  • the photoisomerization compound is 0.1% to 2% by weight of the total weight of the positive photoresist composition;
  • the additive accounts for the positive photoresist combination 0.1% to 1% by weight of the total weight; and the solvent accounts for 62% to 92.8% of the total weight of the positive photoresist composition.
  • the host rubber is a phenolic resin; and/or the photosensitizer is a diazonaphthoquinone type photosensitizer; and/or the solvent is N-methylpyrrolidone, dimethyl sulfoxide, propylene glycol Any of monomethyl ether acetate, ethoxyethyl acetate, and dimethoxyacetaldehyde.
  • the present disclosure provides a method of forming a via, the method comprising:
  • the photoresist layer being formed of the positive photoresist composition of the present disclosure, and the organic film layer and the positive photoresist The composition is similar in polarity before being exposed to light;
  • the photoresist layer and the exposed passivation layer are processed by a patterning process to form via holes penetrating the passivation layer, and covering the organic film layer and the blunt exposed by the organic film layer a photoresist retention portion on the layer;
  • the photoresist remaining portion is removed by a stripper.
  • the ultraviolet light is irradiated in a wavelength range of 330 to 380 nm, and the light intensity is 1 to 10 mW/cm 2 .
  • the present disclosure provides another method of forming vias, the method comprising:
  • An organic film layer and a photoresist layer are sequentially formed on the substrate, the photoresist layer is formed by the positive photoresist composition of the present disclosure, and the organic film layer and the positive photoresist composition are exposed to light Similar in polarity;
  • the photoresist remaining portion is removed by a stripper.
  • the ultraviolet light is irradiated in a wavelength range of 330 to 380 nm, and the light intensity is 1 to 10 mW/cm 2 .
  • the polarity of the organic film layer and the positive photoresist composition before being irradiated is similar.
  • the polymer as a main component in the organic film layer is a non-polar or weakly polar organic resin.
  • the polymer as a main component in the organic film layer is a non-polar or weakly polar organic resin.
  • the main chain is a non-polar organic carbon chain
  • the side chain is a weakly polar organic ester
  • the polymer as a main component in the positive photoresist composition is also non-polar or weak.
  • Organic resins such as phenolic resins, have a non-polar organic carbon chain in the main chain and a weakly polar ether chain in the side chain, so the polarity is similar.
  • the present disclosure provides a display substrate, the vias on the display substrate being formed using the via formation method of the present disclosure.
  • the present disclosure provides a display device including the display substrate of the present disclosure.
  • the display device of the present disclosure includes an LCD display, an LCD TV, an OLED display, an OLED TV, a mobile phone, a tablet, a digital photo frame, and a navigator.
  • the present disclosure proposes a novel positive photoresist composition
  • a novel positive photoresist composition comprising a photoisomerized compound which is converted into an increased degree of molecular polarity after being irradiated by ultraviolet light.
  • the ionic structure reduces the adhesion between the positive photoresist and the organic film layer, facilitates the peeling after the via formation, improves the production yield of the TFT back sheet on which the via is formed, and further improves the basis The display quality of the LCD device and the OLED device of the TFT backplane.
  • Figure 1 is a graph showing the change of ultraviolet absorption spectrum of a solution of N-hydroxyethyl-6-hydroxyspiropyran tetrahydrofuran prepared in Example 1 of the present invention under different illumination times.
  • Fig. 2 is a graph showing changes in contact angle of water droplets on the surface of an N-hydroxyethyl-6-hydroxyspiropyran/phenolic resin film prepared in Example 1 of the present invention under ultraviolet light.
  • Fig. 3 is a graph showing the change of ultraviolet absorption spectrum of a tetrahydrofuran solution of spiropyran (f) prepared in Example 2 of the present invention under different illumination times.
  • Fig. 4 is a graph showing changes in contact angle of the surface of a spiropyran (f)/phenolic resin film prepared by the water droplets in Example 2 of the present invention under ultraviolet light.
  • Figure 5 is a graph showing the change of ultraviolet absorption spectrum of a solution of N-hydroxyethyl-5'-carboxy-5,7-dimethoxyspirobenzoxazine in tetrahydrofuran prepared in Example 3 of the present invention under different illumination times.
  • Figure 6 is a graph showing the contact angle of the surface of N-hydroxyethyl-5'-carboxy-5,7-dimethoxyspirobenzoxazine/phenolic resin film prepared by water droplets in Example 3 of the present invention under ultraviolet light. .
  • FIG. 7 is a schematic flow chart of a method for forming a via hole according to the present disclosure.
  • the terms “first”, “second” and similar terms used in the specification and claims of the invention are not intended to indicate any order, quantity or importance, and are merely used to distinguish different components.
  • the word “comprising” or “comprises” or the like means that the element or item preceding the word is intended to encompass the element or the item recited after the word and its equivalent, and does not exclude other element or item.
  • the term “upper/upper”, or the like, of the orientation or positional relationship is based on the orientation or positional relationship shown in the drawings, and is merely for the convenience of explaining the simplified description of the technical solution of the present invention, and does not indicate or imply the indicated device. Or the components must have a particular orientation, are constructed and operated in a particular orientation, and thus are not to be construed as limiting the invention.
  • a positive photoresist composition comprising a host rubber, a photosensitizer, and a photoisomerization compound, wherein the photoisomerization compound is subjected to After ultraviolet light irradiation, the structure is transformed into an ion structure with an increased degree of molecular polarity.
  • the photoisomerization compound is a photoinducing agent whose structural characteristic group is a closed-loop structure before being exposed to ultraviolet light. After being irradiated by ultraviolet light of a certain wavelength, the closed-loop structure changes. With the change of polarity, the double ion form which is converted into open-loop charge separation changes the electron arrangement, forming an ionic compound-like structure (ie, ion structure) with uneven charge distribution, that is, the polarity increases after being illuminated. The molecular structure exhibits polarity (or weak polarity).
  • the wavelength of the ultraviolet light can be flexibly adjusted according to the specific structure of the photoinducing agent photo-isomerizing compound, which is not limited in the present disclosure.
  • the above-mentioned photoresist composition is positive, that is, it is not dissolved in the developer before exposure, and after exposure to ultraviolet light, a part of the chemical property of the light is changed, and it can be dissolved in the developer to be removed.
  • the positive photoresist composition is exposed and developed through a corresponding mask to form an unilluminated photoresist retention portion. And dissolved in the removal area of the developer after being exposed to light.
  • a corresponding etching process is performed on the film layer under the photoresist removal region to form via holes. After the via is formed, ultraviolet irradiation of the remaining portion of the photoresist can increase the polarity of the photo-isomerized compound and reduce the adhesion of the residual photoresist to the underlying organic film layer, thereby facilitating the residual photoresist. Stripping.
  • the present disclosure proposes a novel positive photoresist composition
  • a novel positive photoresist composition comprising a photoisomerized compound which is converted into an increased degree of molecular polarity after being irradiated by ultraviolet light.
  • the ionic structure reduces the adhesion between the positive photoresist and the organic film layer, facilitates the peeling after the via formation, and improves the production of the TFT (Thin Film Transistor) back sheet on which the via is formed.
  • the yield is improved, and the display quality of an LCD (Liquid Crystal Display) device and an OLED (Organic Light-Emitting Display) device based on the TFT backplane is further improved.
  • the positive photoresist composition of the present disclosure comprises a host gel.
  • the main adhesive material is a photosensitive resin or a photoresist resin. After the light is irradiated, the photochemical reaction can be quickly performed in the exposed region, so that the physical properties, particularly the solubility, of the material are significantly changed.
  • Any photosensitive resin that can be used as a positive photoresist composition can be used as the main body of the present disclosure.
  • the host rubber provides adhesion and chemical resistance of the photoresist.
  • a phenol resin can be mentioned as the main rubber.
  • the phenolic resin can be obtained by reacting a phenol compound with an aldehyde compound or a ketone compound in the presence of an acidic catalyst.
  • the positive photoresist composition of the present disclosure contains a photosensitizer in addition to the host rubber.
  • a photosensitizer sometimes referred to as a sensitizer, sensitizer or sensitizer, is a photoactive compound.
  • any photosensitizer suitable for a positive photoresist composition can be used.
  • a diazonaphthoquinone type photosensitizer such as 2,3,4,4'-tetrahydroxybenzophenone-2, 1,4-diazonaphthoquinone sulfonate, 2, 3, may be mentioned.
  • Diazonaphthoquinone can be obtained by reacting a diazonaphthoquinone sulfonyl halide compound with a phenol compound in the presence of a weak base.
  • the photoisomerizable compound of the present disclosure includes at least one of a spiropyran compound, a spirooxazine compound, an aziridine compound, and a bipyridine compound.
  • a spiropyran compound especially having a photoisomerized spiro ring structure
  • the (spiro) ring can be opened by ultraviolet light to form a trans-ionic structure.
  • the spiropyran compound may have the structure of the following formula (I):
  • R 1 is selected from the group consisting of an alkyl chain, an ether chain, a phenyl group, and the like; and R 2 is a carboxyl group or a hydroxyl group.
  • the aforementioned alkyl chain is selected from the group consisting of butyl, pentyl and hexyl; and/or the aforementioned ether chain is (CH 2 CH 2 O) m CH 3 wherein m is an integer and 1 ⁇ m ⁇ 5.
  • the developer is usually an alkaline aqueous solution of TMAH (Tetra Methyl Ammonium Hydroxide, tetramethylammonium hydroxide)
  • TMAH Tetra Methyl Ammonium Hydroxide, tetramethylammonium hydroxide
  • the mass fraction of TMAH is 2% to 3%, in order to ensure that the positive photoresist is exposed to light after exposure.
  • the R 2 group may be a -COOH or -OH group which is soluble in an alkaline liquid.
  • the spiropyran compound may also have the structure of the following formula (I'):
  • the spiropyran compounds of the formulae (I) and (I') can be prepared by refluxing hydrazine with dihydroxybenzaldehyde or hydroxycarboxybenzaldehyde in the presence of triethylamine in absolute ethanol.
  • the spiropyran compound can be synthesized as follows:
  • N-hydroxyethyl-2,3,3-trimethylsulfonium iodide salt is obtained by 2,3,3-trimethylsulfonium iodide salt.
  • N-hydroxyethyl-2,3,3-trimethylsulfonium iodide is reacted with 2,5-dihydroxybenzaldehyde in the presence of a basic catalyst to obtain N-hydroxyethyl-6-hydroxyspiro Pyran.
  • the reaction of 2,3,3-trimethylhydrazine with iodoethanol is usually carried out in a solvent such as acetonitrile, and it is advantageous that the reaction is carried out under reflux.
  • N-hydroxyethyl-2,3,3-trimethylsulfonium iodide with 2,5-dihydroxybenzaldehyde is usually carried out also in a solvent such as ethanol, advantageously at 40-90 ° C. get on.
  • a solvent such as ethanol
  • the base catalyst used in the reaction it may be an organic base such as triethylamine, trimethylamine or the like.
  • the compound of the formula (I) wherein R 1 has other definitions can also be produced by appropriately changing the starting materials in the above preparation route.
  • R 1 is an alkyl chain or a phenyl group
  • the corresponding iodoalkane or iodobenzene IR 1 may be used, wherein R 1 is an alkyl chain such as butyl, pentyl or hexyl, Or phenyl.
  • R 2 is a hydroxyl group
  • hydroxycarboxybenzaldehyde can be used instead of dihydroxybenzaldehyde.
  • the spiropyran compound according to the present disclosure may also have the structure of the following formula (II):
  • the spiropyran group at both ends of the compound of formula (II) can be isomerized under ultraviolet light irradiation, and ring-opening forms a polar trans-ionic structure.
  • n in the formula (II) is an integer of 4 to 10 to ensure the compatibility of the spiropyran compound as an inducer in the above positive photoresist composition, and to ensure the photoresist layer before being irradiated and
  • the organic film layer has a certain adhesion to avoid degumming before the light, which affects the subsequent film etching.
  • the R group may be a -COOH or -OH group to ensure that the illuminated portion is removed in the developing unit after ultraviolet light.
  • the spiropyran compound of the formula (II) can be obtained by using a dicarboxy PEG (Polyethylene Glycol) and a hydroxyethyl spiropyran in the presence of a basic catalyst such as DMAP (4-Dimethylaminopyridine, 4-dimethylaminopyridine).
  • a basic catalyst such as DMAP (4-Dimethylaminopyridine, 4-dimethylaminopyridine).
  • the spiropyran compound undergoes isomerization of molecular structure under ultraviolet light, in which the spirocarbon-oxygen bond is heterolyzed, and the ring opening forms a trans-ion structure of charge separation.
  • the isomerization process under ultraviolet light can be expressed as follows:
  • the spirocarbon-oxygen bond is split, and the ring-opening forms a trans-ion structure of charge separation, and the neutral SP structure (ie, the spiro structure) is converted into
  • the more polar MC structure ie, the open-loop structure of the cyanine
  • the structural change caused by this illumination can be demonstrated by the ultraviolet absorption spectrum before and after illumination of the spiropyran solution.
  • the spirooxazine compound of the present disclosure may have the structure of the following formula (III):
  • the R 1 group is CH 2 CH 2 OH; the R 2 group may be a -COOH or -OH group to ensure that the illuminated portion is removed in the developing unit after ultraviolet light.
  • the spirooxazine compound of the formula (III) can be produced by refluxing hydrazine with nitrosophenol in anhydrous ethanol. Taking N-hydroxyethyl-5'-carboxy-5,7-dimethoxyspirobenzoxazine as an example, the synthesis of the spirooxazine compound can be expressed as follows:
  • N-hydroxyethyl-2,3,3-trimethyl-5'-carboxyindole iodide salt is reacted with 2-nitroso-3,5-dimethoxyphenol in the presence of a basic catalyst.
  • N-hydroxyethyl-5'-carboxy-5,7-dimethoxyspirobenzoxazine is reacted with 2-nitroso-3,5-dimethoxyphenol in the presence of a basic catalyst.
  • the reaction of 2,3,3-trimethyl-5'-carboxyindole with iodoethanol is usually carried out in a solvent such as acetonitrile, and it is advantageous to carry out the reaction under reflux.
  • the reaction of N-hydroxyethyl-2,3,3-trimethyl-5'-carboxy oxime iodide with 2-nitroso-3,5-dimethoxyphenol is usually carried out also in a solvent such as ethanol.
  • the reaction is carried out at 40-90 °C.
  • the base catalyst used in the reaction it may be an organic base such as triethylamine, trimethylamine or the like.
  • the spirocarbon-oxygen bond in the compound of the formula (III) is heterolyzed, and the ring-opening forms a trans-ionic structure of charge separation, and the molecular polarity increases.
  • the aziridine compound of the present disclosure may have the structure of the following formula (IV):
  • R group is C 2 H 4 OH to ensure that the illuminated portion is removed in the developing unit after ultraviolet light.
  • the isomerization process of the aziridine compound of formula (IV) under ultraviolet light (labeled h ⁇ in the figure) can be expressed as follows (labeled as h ⁇ ):
  • the carbon-carbon bond breaks open-loop, and the ring-opening forms a trans-ion structure of charge separation, and the molecular polarity increases.
  • the bipyridyl compound of the present disclosure may have the structure of the following formula (V):
  • R 1 is hydrogen, any of a methyl, ethyl, propyl, butyl ether chain
  • R 2 is carboxymethyl, carboxyethyl, carboxypropyl any one of
  • R 3 is Any one of hydrogen, a methyl group, an ethyl group, a propyl group, a butyl group, and an ether chain
  • R 4 is any one of a carboxymethyl group, a carboxyethyl group, and a carboxypropyl group.
  • the carbon-carbon bond is broken, and the ring-opening forms a trans-ionic structure of charge separation, and the molecular polarity increases.
  • the positive photoresist composition of the present disclosure may further comprise a solvent and an additive.
  • the additives herein are other additives than the photosensitizer and the photoinducing agent described above.
  • the additive may include a surfactant for improving colloidal coating characteristics, preventing radiation coating unevenness (Mura) of the colloid, and a sensitizing agent for improving exposure sensitivity.
  • the solvent places the photoresist in a liquid state and allows the photoresist to be applied to the surface of the wafer by a spin to form a thin layer.
  • the positive resist composition of the present disclosure is not particularly limited in the selection of the solvent, and any solvent suitable for the positive photoresist composition can be used.
  • the solvent mention may be made of N-methyl-2-pyrrolidone (NMP), dimethyl sulfoxide (DMSO), propylene glycol monomethyl ether acetate, and ethoxyethyl acetate. As well as dimethoxyacetaldehyde, any of these solvents can be used.
  • the distribution ratio of each group in the positive photoresist composition of the present disclosure is preferably as follows: the main rubber material accounts for 5% to 30% of the total weight of the positive photoresist composition; The agent accounts for 2% to 5% of the total weight of the positive photoresist composition; the photoisomer compound accounts for 0.1% to 2% of the total weight of the positive photoresist composition; the additive accounts for the total positive photoresist composition
  • the solvent is from 0.1% to 1% by weight and the balance of the solvent, i.e., the solvent, is from 62% to 92.8% by weight based on the total weight of the positive photoresist composition.
  • the stripping liquid corresponding to the positive photoresist of the present disclosure may comprise: a base of 10%-30% by mass, which may be MEA (Monoethanolamine), KOH, NaOH, etc.; mass fraction 50%-70%
  • MEA Methoxyethanolamine
  • KOH KOH
  • NaOH NaOH
  • the ether may be, for example, Butyldigol (BDG). Specific components may be used in the prior art, which is not limited in the present disclosure.
  • a method of forming a via hole comprising:
  • a passivation layer 102 and an organic film layer 103 are sequentially formed on the substrate 101, and the organic film layer 103 has an exposed passivation.
  • the area of the layer ie, the organic film via 104;
  • a photoresist layer 105 covering the organic film layer 103 and the passivation layer 102 is formed by, for example, a coating process, and the photoresist layer 105 is formed of the positive photoresist composition of the present disclosure.
  • the organic film layer 103 and the positive photoresist composition of the present disclosure are similar in polarity before being irradiated, that is, the photoresist layer 105 has strong adhesion on the non-polar or weakly-polar organic film layer 103.
  • the photoresist layer 105 and the exposed passivation layer 102 are processed by a patterning process to form vias 106 penetrating the passivation layer 102, and overlying the organic film. a layer 103 and a photoresist retention portion 105a on the passivation layer 102 exposed by the organic film layer 103;
  • the photoresist retaining portion 105a is irradiated with ultraviolet light to convert the structure of the photo-isomerized compound in the positive resist composition into an ion structure having an increased degree of molecular polarity, that is, reducing the photoresist remaining portion 105a and Adhesion between the contacting organic film layers 103;
  • the photoresist remaining portion is removed by the stripping liquid.
  • the organic film layer 103 is usually composed of a photoresist material, and is directly exposed and developed through a mask plate to form a corresponding organic film. Hole 104, so there is no problem of photoresist residue.
  • the above-described patterning process refers to a process of applying a single reticle through exposure, development, and etching of a photoresist to form a specific pattern.
  • the photoresist layer 105 and the exposed passivation layer 102 are processed by a patterning process to form vias 106 penetrating the passivation layer 102, and a passivation layer 102 covering the organic film layer 103 and exposed by the organic film layer 103.
  • the specific process of the photoresist retaining portion 105a may be: exposing and developing the coated photoresist layer 105 using a reticle to form a photoresist retaining portion 105a and a photoresist removing region; wherein, the photoresist The removal region corresponds to the region of the passivation layer 102 where via holes are to be formed, and the passivation layer 102 exposed by the photoresist removal region is etched by plasma dry etching to form vias 106 penetrating the passivation layer.
  • an ultraviolet light irradiation unit is added to perform illumination treatment on the entire substrate, the wavelength range may be 330 to 380 nm, and the light intensity may be 1 to 10 mW/cm 2 , and then performed.
  • the conventional photoresist is peeled off to obtain a target pattern, that is, a substrate on which passivation layer via holes are formed.
  • the present disclosure also provides another method of forming vias for an organic film layer composed of a non-photoresist material that needs to be etched to form a via pattern.
  • An organic film layer and a photoresist layer are sequentially formed on the substrate, the photoresist layer is formed of the positive photoresist composition of the present disclosure, and the organic film layer and the positive photoresist composition of the present disclosure are illuminated
  • the former polarity is similar;
  • the photoresist remaining portion is removed by a stripper.
  • the method for forming another via hole provided by the above third aspect is also to add an ultraviolet light irradiation unit to irradiate the entire substrate before the stripping of the remaining photoresist remaining portion, and the wavelength range may be 330 ⁇ .
  • the light intensity may be 1 to 10 mW/cm 2 , and then conventional photoresist stripping is performed to obtain a target pattern, that is, a substrate on which an organic film via is formed.
  • a display substrate formed with a via hole forming method of the present disclosure.
  • the display substrate may specifically be an array substrate.
  • a display device comprising the above display substrate.
  • the display device may specifically be a product or component having any display function, such as an LCD display, an LCD TV, an OLED display, an OLED TV, a digital photo frame, a mobile phone, a tablet computer, a digital photo frame, a navigator, and the like.
  • N-hydroxyethyl-2,3,3-trimethylsulfonium iodide (b) The obtained N-hydroxyethyl-2,3,3-trimethylsulfonium iodide salt (1.31 g, 4 mmol) and 1 mL of triethylamine were dissolved in 20 ml of ethanol, and added to a three-necked flask. Gas for 30min.
  • 2,5-Dihydroxybenzaldehyde (0.68 g, 5 mmol) was weighed and dissolved in 5 ml of ethanol, and slowly added to the reaction solution at 45 ° C with a syringe, and the addition was completed in 15 minutes.
  • the temperature was raised to 70 ° C, and the reaction was kept for 0.5 h; the temperature was raised to 80 ° C to maintain the reaction for 2.5 h; and the temperature was further raised to 90 ° C to continue the reaction for 2.5 h.
  • the reaction was stopped, cooled, and the reaction mixture was dark red.
  • Fig. 1 It can be seen from Fig. 1 that the system before irradiation (lighting 0s) has no absorption in the visible light region (400-700nm), and an absorption peak is added at 590nm after ultraviolet light irradiation, which increases with the increase of irradiation time, and the absorption peak belongs to the flowering cyanine.
  • the absorption peak of the open-loop structure indicates that the illumination causes the occurrence of open loop.
  • the ionic structure formed by the open loop results in an increase in polarity, that is, an increase in hydrophilicity. In aqueous or other highly polar dispersants, an increase in hydrophilicity will reduce the interfacial tension of the dispersant on its surface. This can be verified by the fact that the wetting angle is significantly reduced after UV radiation.
  • the contact angle change of the surface water of the N-hydroxyethyl-6-hydroxyspiropyran/phenolic resin film is shown in Fig. 2.
  • the contact angle of the water droplets was observed as a function of the irradiation time. It can be seen from Fig. 2 that under the UV light intensity of 10 mW/cm 2 , the contact angle decreases from the initial 86° to 75° in one minute, which indicates that the N-hydroxyethyl-6-hydroxy spiropyran compound is exposed to ultraviolet light. The interfacial tension is lowered and the hydrophilicity is increased, that is, the polarity is increased. Ultraviolet-visible absorption spectroscopy proved that the reason for the increase in polarity was that the spiropyran was broken by the UV bond and the CO bond of the spiro structure was broken to form a trans-ion open-loop structure.
  • the system before irradiation has no absorption in the visible light region (400-700nm), and an absorption peak is added at 590nm after ultraviolet light irradiation, and increases with the irradiation time.
  • the absorption peak of the open-loop structure indicates that the illumination causes the occurrence of open loop.
  • the ionic structure formed by the open loop results in an increase in polarity, that is, an increase in hydrophilicity. In aqueous or other highly polar dispersants, an increase in hydrophilicity will reduce the interfacial tension of the dispersant on its surface. This can be verified by the fact that the wetting angle is significantly reduced after UV radiation.
  • the contact angle change of the surface water of the spiropyran (f)/phenolic resin film is shown in Fig. 4.
  • the obtained solution was coated on a glass substrate, air-dried into a film, and water droplets were dropped thereon, and then irradiated with UV light having a wavelength of 365 nm at an irradiation intensity of 10 mW/cm 2 to observe a change in the contact angle of the water droplets with the irradiation time. It can be seen from Fig. 4 that under the UV light intensity of 10 mW/cm 2 , the contact angle decreases from the initial 89° to 74° in one minute, which indicates that the interfacial tension of the spiropyran (f) is reduced by ultraviolet light, and hydrophilicity Increase, that is, increase in polarity.
  • the reason why the ultraviolet-visible absorption spectrum proves to cause the polarity to become large is that the spiropyran (f) is broken by the CO bond of the spiro ring structure after ultraviolet light irradiation to form a trans-ion open-loop structure.
  • the resulting N-hydroxyethyl-2,3,3-trimethyl-5-carboxyindole iodide salt (1.3 g, 4 mmol) and 1 mL of triethylamine were dissolved in 20 ml of ethanol and added to a three-necked bottle. Nitrogen gas was exhausted for 30 min.
  • the system before irradiation has no absorption in the visible light region (400-700nm), and a broad absorption peak is added at 400-550nm after ultraviolet light.
  • the absorption peak belongs to the open-loop trans-ion of oxazine.
  • the absorption peak of the structure indicates that the illumination caused the occurrence of open loop.
  • the ionic structure formed by the open loop results in an increase in polarity, that is, an increase in hydrophilicity.
  • the contact angle change of the surface water of the N-hydroxyethyl-5'-carboxy-5,7-dimethoxyspirobenzoxazine/phenolic resin film is shown in Fig. 6.

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Abstract

本发明提供一种正性光刻胶组合物，其包含主体胶材和光敏剂，其中所述光刻胶组合物还包含光致异构化合物，该光致异构化合物受到紫外光照射后结构转变为分子极性程度增加的离子结构。该分子极性程度增加的离子结构的形成降低了该正性光刻胶与有机膜层间的附着力，有利于过孔形成后的剥离，提高产品的生产良率。此外，本发明还提供使用所述正性光刻胶组合物的过孔形成方法、包含通过前述过孔形成方法形成的过孔的显示基板及包含前述显示基板的显示装置。

Description

正性光刻胶组合物、过孔的形成方法、显示基板及显示装置
相关申请的交叉引用
本申请要求于2017年08月02日递交的中国专利申请第201710651692.X号的优先权，在此全文引用上述中国专利申请公开的内容以作为本申请的一部分。
技术领域
本发明涉及显示技术领域，尤其涉及一种正性光刻胶组合物、使用该正性光刻胶组合物的过孔形成方法、包含通过前述过孔形成方法形成的过孔的显示基板及包含前述显示基板的显示装置。
背景技术
光刻工艺是薄膜晶体管阵列制造过程中必不可少的一道制程，起到图案转移的作用。在待刻蚀的洁净薄膜上涂覆光刻胶，通过软烘、曝光、显影、后烘等工序，获得设计好的掩模版图案(即光刻胶图案)，之后对光刻胶图案露出的薄膜区域进行刻蚀，形成与光刻胶图案一致的目标图案，再剥离残留的光刻胶图案，以露出该目标图案进行后续的制程。
光刻制程的实施离不开光刻胶。光刻胶的主体成分是一类含光敏性基团的聚合物，在紫外光照条件下，受光照部分的光敏基团发生一系列化学变化，导致光刻胶感光部分和未受光照部分在显影液中的溶解性产生明显差异，从而在显影后形成特定的图案。
薄膜晶体管阵列制造过程中通常要经过数道光刻制程，包括金属膜层制程、无机绝缘层(如氧化硅SiO x、氮化硅SiN x)制程、有源层制程、ITO(Indium Tin Oxide，氧化铟锡)层制程等。目前在氧化物型阵列基板(即Oxide背板)制作工艺中，无机钝化层(Passivation Layer，PVX) 上通常涂覆有一层有机膜层，起保护下方膜层并提供一个平坦化衬底的作用。有机膜层上具有露出下方PVX层的有机膜孔，在有机膜孔内进行过孔(即Via孔)工艺，具体包括有光刻、刻蚀、剥离工艺，从而在PVX层上形成Via孔。
然而，有机膜层通常由非极性的有机材料构成，光刻胶中的主体成分聚合物也为非极性的有机材料(如苯酚-甲醛聚合物)，因此二者极性相似，在形成Via孔的过程中，光刻胶直接涂敷在极性与其相似的有机膜上，光刻胶与有机膜层之间的附着力较大，易发生Via孔刻蚀后光刻胶剥离不彻底的问题，即发生光刻胶残留，影响Oxide背板的后续制程，降低生产良率。
发明内容
鉴于此，为解决现有技术的问题，本公开提供一种正性光刻胶组合物、使用该正性光刻胶组合物的过孔形成方法、包含通过前述过孔形成方法形成的过孔的显示基板及包含前述显示基板的显示装置，该正性光刻胶组合物中包含有光致异构化合物，该化合物受到紫外光照射后结构转变为分子极性程度增加的离子结构，降低了该正性光刻胶与有机膜层间的附着力，有利于过孔形成后的剥离，提高产品的生产良率。
为达到上述目的，本公开采用如下技术方案：
第一方面，本公开提供了一种正性光刻胶组合物，其包含主体胶材和光敏剂，其中所述光刻胶组合物还包含光致异构化合物，该光致异构化合物受到紫外光照射后结构转变为分子极性程度增加的离子结构。
优选地，所述光致异构化合物包括螺吡喃化合物、螺噁嗪类化合物、氮丙啶化合物、联吡啶化合物中的至少一种。
作为一种可选的方式，所述螺吡喃化合物具有下式(I)结构：
Figure PCTCN2018084484-appb-000001
其中，R 1基团为烷基链、醚链、苯基；R 2为羧基或羟基。优选地，前述烷基链选自丁基、戊基和己基；和/或，前述醚链为(CH 2CH 2O) mCH 3，其中m为整数，且1≤m≤5。
作为另一种可选的方式，所述螺吡喃化合物具有下式(I’)结构：
Figure PCTCN2018084484-appb-000002
作为再一种可选的方式，所述螺吡喃化合物具有下式(II)结构：
Figure PCTCN2018084484-appb-000003
其中，n为整数，且4≤n≤10；和R为羧基或羟基。
优选地，所述螺噁嗪化合物具有下式(III)结构：
Figure PCTCN2018084484-appb-000004
其中，R 1为CH 2CH 2OH；和R 2基团为羧基或羟基。
优选地，所述氮丙啶化合物具有下式(IV)结构：
Figure PCTCN2018084484-appb-000005
其中，R为C 2H 4OH。
优选地，所述联吡啶化合物具有下式(V)结构：
Figure PCTCN2018084484-appb-000006
其中，R 1为氢、甲基、乙基、丙基、丁基、醚链中的任一种；R 2为羧甲基、羧乙基、羧丙基中的任一种；R 3为氢、甲基、乙基、丙基、丁基、醚链中的任一种；和R 4为羧甲基、羧乙基、羧丙基中的任一种。
优选地，所述正性光刻胶组合物还包含溶剂和添加剂。
优选地，在所述正性光刻胶组合物中，所述主体胶材占所述正性光刻胶组合物总重量的5％～30％；所述光敏剂占所述正性光刻胶组合物总重量的2％～5％；所述光致异构化合物占所述正性光刻胶组合物总重量的0.1％～2％；所述添加剂占所述正性光刻胶组合物总重量的0.1％～1％；以 及所述溶剂占所述正性光刻胶组合物总重量的62％～92.8％。
优选地，所述主体胶材为酚醛树脂；和/或，所述光敏剂为重氮萘醌型光敏剂；和/或，所述溶剂为N-甲基吡咯烷酮、二甲基亚砜、丙二醇单甲醚乙酸酯、乙酸乙氧乙酯、二甲氧基乙醛中的任一种。
第二方面，本公开提供了一种过孔的形成方法，该方法包括：
在基板上依次形成钝化层和有机膜层，该有机膜层上具有露出所述钝化层的区域；
形成覆盖所述有机膜层和所述钝化层的光刻胶层，该光刻胶层由本公开的正性光刻胶组合物形成，且所述有机膜层与所述正性光刻胶组合物受光照前的极性相似；
采用构图工艺对所述光刻胶层和露出的所述钝化层进行处理，形成贯穿钝化层的过孔，和覆盖在所述有机膜层以及被所述有机膜层露出的所述钝化层上的光刻胶保留部分；
对所述光刻胶保留部分进行紫外光照射，以使所述正性光刻胶组合物中的光致异构化合物的结构转变为分子极性程度增加的离子结构；以及
通过剥离液去除所述光刻胶保留部分。
优选地，所述紫外光照射的波长范围为330～380nm，光照强度为1～10mW/CM 2。
第三方面，本公开提供了另一种过孔的形成方法，该方法包括：
在基板上依次形成有机膜层和光刻胶层，该光刻胶层由本公开的正性光刻胶组合物形成，且所述有机膜层与所述正性光刻胶组合物受光照前的极性相似；
采用构图工艺对所述光刻胶层和所述有机膜层进行处理，形成贯穿所述有机膜层的过孔和覆盖在所述有机膜层除所述过孔所在区域之外的光刻胶保留部分；
对所述光刻胶保留部分进行紫外光照射，以使所述正性光刻胶组合物中的光致异构化合物的结构转变为分子极性程度增加的离子结构；以及
通过剥离液去除所述光刻胶保留部分。
优选地，所述紫外光照射的波长范围为330～380nm，光照强度为1～10mW/CM 2。
在本公开中，有机膜层与正性光刻胶组合物受光照前的极性相似这指的是：有机膜层中作为主体成分的聚合物为非极性或弱极性的有机树脂，如聚甲基丙烯酸甲酯，主链为非极性有机碳链，侧链为弱极性有机酯类；正性光刻胶组合物中作为主体成分的聚合物也为非极性或弱极性的有机树脂，如酚醛树脂，主链为非极性有机碳链，侧链为弱极性醚链，因此极性相似。
第四方面，本公开提供了一种显示基板，该显示基板上的过孔采用本公开的过孔形成方法形成。
第五方面，本公开提供了一种显示装置，其包括本公开的显示基板。
优选地，本公开的显示装置包括LCD显示器、LCD电视、OLED显示器、OLED电视、手机、平板电脑、数码相框和导航仪。
基于此，本公开提出一种新型正性光刻胶组合物，该正性光刻胶组合物中包含有光致异构化合物，该化合物受到紫外光照射后结构转变为分子极性程度增加的离子结构，降低了该正性光刻胶与有机膜层间的附着力，有利于过孔形成后的剥离，提高了形成有该过孔的TFT背板的生产良率，并进一步提高了基于该TFT背板的LCD装置和OLED装置的显示质量。
附图说明
图1为本发明实施例1中制备的N-羟乙基-6-羟基螺吡喃的四氢呋喃 溶液在不同光照时间下的紫外吸收光谱变化图。
图2为紫外光照下水滴在本发明实施例1中制备的N-羟乙基-6-羟基螺吡喃/酚醛树脂薄膜表面上的接触角变化图。
图3为本发明实施例2中制备的螺吡喃(f)的四氢呋喃溶液在不同光照时间下的紫外吸收光谱变化图。
图4为紫外光照下水滴在本发明实施例2中制备的螺吡喃(f)/酚醛树脂薄膜表面的接触角变化图。
图5为本发明实施例3中制备的N-羟乙基-5'-羧基-5,7-二甲氧基螺苯并噁嗪的四氢呋喃溶液在不同光照时间下的紫外吸收光谱变化图。
图6为紫外光照下水滴在本发明实施例3中制备的N-羟乙基-5'-羧基-5,7-二甲氧基螺苯并噁嗪/酚醛树脂薄膜表面的接触角变化图。
图7为本公开提供的一种过孔的形成方法流程示意图。
附图标记：
101-基板；102-钝化层；103-有机膜层；104-有机膜过孔；105-光刻胶层；105a-光刻胶保留部分；106-贯穿钝化层的过孔。
具体实施方式
需要指出的是，除非另有定义，本公开中所使用的所有术语(包括技术和科学术语)具有与本发明所属领域的普通技术人员共同理解的相同含义。还应当理解，诸如在通常字典里定义的那些术语应当被解释为具有与它们在相关技术的上下文中的含义相一致的含义，而不应用理想化或极度形式化的意义来解释，除非这里明确地这样定义。
例如，本发明专利申请说明书以及权利要求书中所使用的术语“第一”、“第二”以及类似的词语并不表示任何顺序、数量或者重要性，仅是用来区分不同的组成部分。“包括”或者“包含”等类似的词语意指出现该词前面的元件或者物件涵盖出现在该词后面列举的元件或者物 件及其等同，而不排除其他元件或者物件。“上/上方”、等指示的方位或位置关系的术语为基于附图所示的方位或位置关系，仅是为了便于说明本发明的技术方案的简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。
根据本公开的第一方面，提供了一种正性光刻胶组合物，该正性光刻胶组合物包含主体胶材、光敏剂以及光致异构化合物，其中该光致异构化合物受到紫外光照射后结构转变为分子极性程度增加的离子结构。
需要说明的是，上述光致异构化合物作为一种光诱导剂，其结构上的特征基团在受到紫外光照前为闭环态结构，受到一定波长的紫外线照射后，其闭环态结构发生变化并伴随极性变化，转变为开环的电荷分离的双离子形式，电子排布发生变化，形成电荷分布不均的类似于离子化合物的结构(即离子结构)，即受光照后极性增加，其分子结构呈现出极性(或弱极性)。
这里，紫外光的波长可根据光诱导剂光致异构化合物的具体结构灵活调整，本公开对此不作限定。
上述光刻胶组合物为正性，即曝光前不溶解于显影液，经紫外线曝光后，受光照的部分化学性质发生转变，能够溶解于显影液从而被去除。
这样一来，在利用上述正性光刻胶组合物进行光刻制程时，通过相应的掩模版对该正性光刻胶组合物进行曝光、显影处理，形成未受光照的光刻胶保留部分和受光照后溶解于显影液的去除区域。对光刻胶去除区域下方的膜层进行相应的刻蚀工艺，以形成过孔。而在过孔形成后，对光刻胶保留部分进行紫外线照射，可使光致异构化合物极性增加，降低残留的光刻胶与下方有机膜层的附着力，从而有利于残留光刻胶的剥离。
基于此，本公开提出一种新型正性光刻胶组合物，该正性光刻胶组合物中包含有光致异构化合物，该化合物受到紫外光照射后结构转变为 分子极性程度增加的离子结构，降低了该正性光刻胶与有机膜层间的附着力，有利于过孔形成后的剥离，提高了形成有该过孔的TFT(Thin Film Transistor，薄膜晶体管)背板的生产良率，并进一步提高了基于该TFT背板的LCD(Liquid Crystal Display，液晶显示)装置和OLED(Organic Light-Emitting Display，有机发光显示)装置的显示质量。
本公开的正性光刻胶组合物包含主体胶材。该主体胶材即为感光树脂或光刻胶树脂，该树脂经光照后，在曝光区能很快地发生光化学反应，使得这种材料的物理性能，特别是溶解性等发生明显变化。任何能用作正性光刻胶组合物的感光树脂都可用作本公开的主体胶材。该主体胶材提供光刻胶的粘附性、化学抗蚀性。典型地，作为主体胶材，可提及酚醛树脂。酚醛树脂可通过酚化合物与醛化合物或酮化合物在酸性催化剂的存在下的反应制得。
本公开的正性光刻胶组合物除了包含主体胶材外还包含光敏剂。光敏剂有时亦称作感光剂、增感剂或敏化剂，是一种光敏化合物。对于本公开而言，任何适合正性光刻胶组合物的光敏剂都可使用。作为典型实例，可提及重氮萘醌型光敏剂，比如2,3,4,4’-四羟基二苯甲酮-2,1,4-重氮萘醌磺酸酯，2,3,4-三羟基二苯甲酮-2,1,4-重氮萘醌磺酸酯，2,3,4-三羟基二苯甲酮-2,1,5-重氮萘醌磺酸酯，2,3,4,4'-四羟基二苯甲酮-2,1,5-重氮萘醌磺酸酯。重氮萘醌可通过重氮萘醌磺酰卤化合物与酚化合物在弱碱的存在下的反应制得。
优选地，本公开的光致异构化合物包括螺吡喃类化合物、螺噁嗪类化合物、氮丙啶类化合物、联吡啶类化合物中的至少一种。上述化合物中均具有光致异构性环结构(尤其是具有光致异构性螺环结构)，该(螺)环受紫外光照后可发生开环，形成反式离子结构。
下面对上述各种化合物的优选化合物作详细说明。
螺吡喃化合物
螺吡喃化合物可以具有下式(I)结构：
Figure PCTCN2018084484-appb-000007
其中R 1为选自烷基链、醚链、苯基等；和R 2为羧基或羟基。优选地，前述烷基链选自丁基、戊基和己基；和/或，前述醚链为(CH 2CH 2O) mCH 3，其中m为整数，且1≤m≤5。
这里，由于显影液通常为呈碱性的TMAH(Tetra Methyl Ammonium Hydroxide，四甲基氢氧化铵)水溶液，TMAH的质量分数2％-3％，为了保证上述正性光刻胶在曝光后受光照部分在显影单元被显影液去除，R 2基团可以为在碱性液中易溶的-COOH或-OH基团。
螺吡喃化合物还可以具有下式(I’)结构：
Figure PCTCN2018084484-appb-000008
(I’)式(I)和(I’)的螺吡喃化合物可以通过吲哚与二羟基苯甲醛或羟基羧基苯甲醛在三乙胺存在下在无水乙醇中回流制备而成。
以式(I’)的N-羟乙基-6-羟基螺吡喃为例，该螺吡喃化合物可通过如下方式合成：
Figure PCTCN2018084484-appb-000009
首先，使2,3,3-三甲基吲哚与碘代乙醇反应，得到N-羟乙基-2,3,3-三甲基吲哚碘盐。然后，使N-羟乙基-2,3,3-三甲基吲哚碘盐与2,5-二羟基苯甲醛在碱性催化剂存在下反应，得到N-羟乙基-6-羟基螺吡喃。2,3,3-三甲基吲哚与碘代乙醇的反应通常在溶剂如乙腈中进行，有利的是该反应在回 流下进行。N-羟乙基-2,3,3-三甲基吲哚碘盐与2,5-二羟基苯甲醛的反应通常也在溶剂如乙醇中进行，有利的是该反应在40-90℃下进行。作为该反应中使用的碱催化剂，它可以是有机碱，如三乙胺、三甲胺等。
如果要制备R 1为醚链(CH 2CH 2O) mCH 3的式(I)化合物，则可将上述反应过程中的碘代乙醇改为I(CH 2CH 2O) mCH 3即可。
R 1具有其它定义的式(I)化合物也可通过适当改变上述制备路线中原料来制备。例如，为了制备R 1为烷基链或苯基的式(I)化合物，可以使用相应的碘代烷或碘代苯IR 1，其中R 1为烷基链如丁基、戊基或己基，或者苯基。至于R 2为羟基的式(I)化合物，则可使用羟基羧基苯甲醛来代替二羟基苯甲醛。
根据本公开的螺吡喃化合物还可以具有下式(II)结构：
Figure PCTCN2018084484-appb-000010
式(II)化合物两端的螺吡喃基团在紫外光照射下可发生异构化，开环形成极性反式离子结构。式(II)中的n为4-10的整数，以保证作为诱导剂的该螺吡喃化合物在上述正性光刻胶组合物中的相容性，并保证受光照前光刻胶层和有机膜层间具有一定的粘附力，以避免在光照前出现脱胶现象，影响后续的膜层刻蚀。R基团可以为-COOH或-OH基团，以保证紫外光照后受光照部分在显影单元被去除。
式(II)的螺吡喃化合物可通过二羧基PEG(Polyethylene Glycol，聚乙二醇)与羟乙基螺吡喃在碱性催化剂如DMAP(4-Dimethylaminopyridine，4-二甲氨基吡啶)存在下反应制得，其反应可表示如下：
Figure PCTCN2018084484-appb-000011
螺吡喃化合物在紫外光照下会发生分子结构的异构化，其中螺碳-氧键发生异裂，开环形成电荷分离的反式离子结构。以式(I)的螺吡喃化合物为例，其在紫外光照下的异构化过程可表示如下：
Figure PCTCN2018084484-appb-000012
其中，螺吡喃类化合物在紫外(Ultraviolet，UV)光照情况下，螺碳-氧键发生异裂，开环形成电荷分离的反式离子结构，其中性SP结构(即螺环结构)转变为极性更强的MC结构(即花菁开环结构)，使得光照后其亲水性增加，即极性增加。该光照导致的结构变化可通过螺吡喃溶液的光照前后的紫外吸收光谱来证明。
螺噁嗪化合物
本公开的螺噁嗪化合物可以具有下式(III)结构：
Figure PCTCN2018084484-appb-000013
Figure PCTCN2018084484-appb-000014
其中，R 1基团为CH 2CH 2OH；R 2基团可以为-COOH或-OH基团，以保证紫外光照后受光照部分在显影单元被去除。
式(III)的螺噁嗪化合物可以通过吲哚与亚硝基苯酚在无水乙醇中回流反应制备而成。以N-羟乙基-5'-羧基-5,7-二甲氧基螺苯并噁嗪为例，该螺噁嗪化合物的合成可表示如下：
Figure PCTCN2018084484-appb-000015
首先，使2,3,3-三甲基-5’-羧基吲哚与碘代乙醇反应，得到N-羟乙基-2,3,3-三甲基-5’-羧基吲哚碘盐。然后，使N-羟乙基-2,3,3-三甲基-5’-羧基吲哚碘盐与2-亚硝基-3,5-二甲氧基苯酚在碱性催化剂存在下反应，得到N-羟乙基-5'-羧基-5,7-二甲氧基螺苯并噁嗪。2,3,3-三甲基-5’-羧基吲哚与碘代乙醇的反应通常在溶剂如乙腈中进行，有利的是该反应在回流下进行。N-羟乙基-2,3,3-三甲基-5’-羧基吲哚碘盐与2-亚硝基-3,5-二甲氧基苯酚的反应通常也在溶剂如乙醇中进行，有利的是该反应在40-90℃下进行。作为该反应中使用的碱催化剂，它可以是有机碱，如三乙胺、三甲胺等。
至于其中R 2为-OH的式(III)化合物的制备，可以与N-羟乙基-5'-羧基-5,7-二甲氧基螺苯并噁嗪相似的方式制备，不同之处在于：将2,3,3-三甲基-5’-羧基吲哚原料替换为2,3,3-三甲基-5’-羟基吲哚。
式(III)的螺噁嗪化合物在一定紫外光照下的异构化过程可表示如下(图中标记为hν)：
Figure PCTCN2018084484-appb-000016
其中，式(III)化合物中的螺碳-氧键发生异裂，开环形成电荷分离的反式 离子结构，分子极性增加。
氮丙啶化合物
本公开的氮丙啶化合物可具有下式(IV)结构：
Figure PCTCN2018084484-appb-000017
其中，R基团为C 2H 4OH，以保证紫外光照后受光照部分在显影单元被去除。
式(IV)的氮丙啶化合物在紫外光照(图中标记为hν)下的异构化过程可表示如下(图中标记为hν)：
Figure PCTCN2018084484-appb-000018
其中，碳-碳键断裂开环，开环形成电荷分离的反式离子结构，分子极性增加。
联吡啶化合物
本公开的联吡啶化合物可以具有下式(V)结构：
Figure PCTCN2018084484-appb-000019
其中，R 1为氢、甲基、乙基、丙基、丁基、醚链中的任一种；R 2为羧甲基、羧乙基、羧丙基中的任一种；R 3为氢、甲基、乙基、丙基、丁基、醚链中的任一种；和R 4为羧甲基、羧乙基、羧丙基中的任一种。
式(V)的联吡啶化合物在紫外光照(图中标记为hν)及加热处理(图 中标记为Heat)下的异构化过程可表示如下：
Figure PCTCN2018084484-appb-000020
其中，碳-碳键发生断裂，开环形成电荷分离的反式离子结构，分子极性增加。
在一个优选方案中，本公开的正性光刻胶组合物还可包含溶剂和添加剂。显然，这里的添加剂为不同于光敏剂和上文所述光诱导剂的其它添加剂。添加剂的实例可以包括界面活性剂，用于改善胶体涂布特性，防止胶体出现放射线状涂布不均(Mura)；增感剂，用于提高曝光感度。
溶剂使光刻胶处于液态，并且使光刻胶能够通过旋转的方法涂在晶圆表面形成一个薄层。本公开正性光刻胶组合物对于溶剂的选择没有特别的限制，任何适于正性光刻胶组合物的溶剂都可以使用。作为溶剂的实例，可提及N-甲基吡咯烷酮(N-methyl-2-pyrrolidone，NMP)、二甲基亚砜(Dimethyl sulfoxide，DMSO)、丙二醇单甲醚乙酸酯、乙酸乙氧乙酯以及二甲氧基乙醛，可以使用这些溶剂中的任一种。
在本公开的一个优选实施方案中，本公开的正性光刻胶组合物中的各组分配比优选如下：主体胶材占正性光刻胶组合物总重量的5％～30％；光敏剂占正性光刻胶组合物总重量的2％～5％；光致异构化合物占正性光刻胶组合物总重量的0.1％～2％；添加剂占正性光刻胶组合物总重量的0.1％～1％以及余量的溶剂，即溶剂占正性光刻胶组合物总重量的62％～92.8％。
与本公开的正性光刻胶相对应的剥离液可以包含：质量分数10％-30％的碱类，可以是MEA(Monoethanolamine，乙醇胺)、KOH、NaOH等；质量分数50％-70％的醚类，可以是二乙二醇单丁醚(Butyldigol，BDG)。具体组分可沿用现有技术，本公开对此不作限定。
根据本公开的第二方面，提供了一种过孔的形成方法，该形成方法包括：
如图5(a)所示，在基板101上依次形成钝化层102和有机膜层103(该有机膜层103具有非极性或弱极性)，该有机膜层103上具有露出钝化层的区域(即有机膜过孔104)；
如图5(b)所示，采用例如涂布工艺，形成覆盖有机膜层103和钝化层102的光刻胶层105，该光刻胶层105由本公开的正性光刻胶组合物形成，且有机膜层103与本公开的正性光刻胶组合物受光照前的极性相似，即光刻胶层105在非极性或弱极性的有机膜层103上的附着力较强，
如图5(c)和图5(d)所示，采用构图工艺对光刻胶层105和露出的钝化层102进行处理，形成贯穿钝化层102的过孔106，和覆盖在有机膜层103以及被有机膜层103露出的钝化层102上的光刻胶保留部分105a；
对光刻胶保留部分105a进行紫外光照射，以使正性光刻胶组合物中的光致异构化合物的结构转变为分子极性程度增加的离子结构，即降低光刻胶保留部分105a与相接触的有机膜层103之间的粘附力；以及
如图5(e)所示，通过剥离液去除光刻胶保留部分。
需要说明的是，在本公开第二方面提供的上述过孔形成方法中，有机膜层103通常由光刻胶材料构成，通过掩模版直接对其进行曝光、显影即可形成相应的有机膜过孔104，故不存在光刻胶残留的问题。
上述的构图工艺是指应用一次掩模版，通过光刻胶曝光、显影、刻蚀以形成特定图案的工艺。上述采用构图工艺对光刻胶层105和露出的钝化层102进行处理，形成贯穿钝化层102的过孔106，和覆盖在有机膜层103以及被有机膜层103露出的钝化层102上的光刻胶保留部分105a的具体过程可以为：采用掩模版对涂布的光刻胶层105进行曝光、显影，形成光刻胶保留部分105a和光刻胶去除区域；其中，光刻胶去除区域对应于钝化层102上待形成过孔的区域，采用等离子干法刻蚀对光刻胶去除区域露出的钝化层102进行刻蚀，形成贯穿钝化层的过孔106。
在对残留的光刻胶保留部分105a进行剥离前，增加一个紫外光照射单元，对整面基板进行光照处理，波长范围可以为330～380nm，光照强度可以为1～10mW/CM 2，之后进行常规的光刻胶剥离，得到目标图案，即形成有钝化层过孔的基板。
对于由非光刻胶材料构成的、需要经过刻蚀形成过孔图案的有机膜层，本公开还提供了另一种过孔的形成方法。
因此，根据本公开的第三方面，提供了另一种过孔的形成方法，该形成方法包括：
在基板上依次形成有机膜层和光刻胶层，该光刻胶层由本公开的正性光刻胶组合物形成，且所述有机膜层与本公开的正性光刻胶组合物受光照前的极性相似；
采用构图工艺对所述光刻胶层和所述有机膜层进行处理，形成贯穿所述有机膜层的过孔和覆盖在所述有机膜层除所述过孔所在区域之外的光刻胶保留部分；
对所述光刻胶保留部分进行紫外光照射，以使本公开的正性光刻胶组合物中的光致异构化合物的结构转变为分子极性程度增加的离子结构；以及
通过剥离液去除光刻胶保留部分。
上述第三方面提供的另一种过孔的形成方法同样是在对残留的光刻胶保留部分进行剥离前，增加一个紫外光照射单元，对整面基板进行光照处理，波长范围可以为330～380nm，光照强度可以为1～10mW/CM 2，之后进行常规的光刻胶剥离，得到目标图案，即形成有有机膜过孔的基板。
具体形成步骤可参见上述第二方面中的过孔形成方法中的相应描述，此处不再赘述。
根据本公开的第四方面，提供了一种显示基板，该显示基板上的过 孔采用本公开的过孔的形成方法形成。该显示基板具体可以为阵列基板。
根据本公开的第五方面，提供了一种显示装置，包括上述的显示基板。上述显示装置具体可以是LCD显示器、LCD电视、OLED显示器、OLED电视、数码相框、手机、平板电脑、数码相框、导航仪等具有任何显示功能的产品或者部件。
实施例
以下将结合实施例对本发明作进一步说明，但不应将其理解为对本发明保护范围的限制。
实施例1：式(I’)N-羟乙基-6-羟基螺吡喃(c)的制备
Figure PCTCN2018084484-appb-000021
称取碘代乙醇(1.36g，8mmol)溶于10ml乙腈中，通氮气排气30min。称取2,3,3-三甲基吲哚(a)(1.274g，8mmol)溶于5ml乙腈中，由滴液漏斗逐滴加入到反应液中，约1h滴完。继续回流反应36h。反应结束，冷却，旋除乙腈，用正己烷洗涤数次，再用乙醚洗涤数次，得到N-羟乙基-2,3,3-三甲基吲哚碘盐(b)。称取制得的N-羟乙基-2,3,3-三甲基吲哚碘盐(1.31g，4mmol)与1mL三乙胺溶于20ml乙醇中，加入到三口瓶中，通氮气排气30min。称取2,5-二羟基苯甲醛(0.68g，5mmol)溶于5ml乙醇中，在45℃下用注射器将其缓慢加入到反应液中，于15min加完。升温至70℃，保持反应0.5h；升温至80℃保持反应2.5h；再升温至90℃继续反应2.5h。停止反应，冷却，反应液呈暗红色，旋除乙醇，得深红色粘稠状物，溶于60ml CH 2Cl 2中，用水洗涤数次洗去过量水杨醛。收集CH 2Cl 2相，旋干，得深红色固状物，用正己烷重结晶，得到目标产 物N-羟乙基-6-羟基螺吡喃(c)。
1H NMR:δ1.12(s,3H,-CH 3),1.27(s,3H,-CH 3),3.27-4.06(m,4H,-NCH 2CH 2O-),5.68(d,1H,-CH＝),6.68(d,1H,＝CH-),6.47-7.12(m,7H,Ar-H),5.13(d,2H,Ar-OH)。
化合物(c)的四氢呋喃溶液(浓度0.01mg/mL)在室温下用365nm波长、10mW/cm 2光强紫外光照射前后的紫外可见吸收光谱变化见图1。
由图1可见，光照前(光照0s)体系在可见光区域(400-700nm)无吸收，在紫外光照后在590nm处新增一个吸收峰，并随照射时间增加而增加，该吸收峰属于花菁开环结构的吸收峰，说明了光照导致了开环的发生。开环形成的离子结构导致极性增加，即亲水性增加。在水相或者其它强极性分散剂中，亲水性的增加将会降低分散剂在其表面的界面张力。这可通过其润湿角在紫外辐射后明显变小来验证。
N-羟乙基-6-羟基螺吡喃/酚醛树脂薄膜表面水的接触角变化如图2所示。该试验操作如下：将N-羟乙基-6-羟基螺吡喃和酚醛树脂(Mn＝10000g/mol)溶解在四氢呋喃中，使得其中N-羟乙基-6-羟基螺吡喃的浓度为5mg/mL，酚醛树脂的浓度为200mg/mL,将所得溶液涂布在玻璃基板上，风干成膜后，滴上水滴，然后用波长为365nm的UV光以10mW/cm 2的光照强度照射，观察水滴的接触角随照射时间的变化。由图2可见，在10mW/cm 2的UV光照强度下，一分钟内接触角从最初的86°降低到75°，这说明N-羟乙基-6-羟基螺吡喃化合物受紫外光照后界面张力降低，亲水性增加，即极性增加。紫外-可见吸收光谱证明导致极性变大的原因是：螺吡喃经紫外光照后螺环结构C-O键断裂，形成反式离子开环结构。
实施例2：式(II)螺吡喃(f)的制备
Figure PCTCN2018084484-appb-000022
室温条件下将1g二羧基PEG(n＝4)(e)和2g R为羟基的羟乙基螺吡喃(d)溶解在20mL干燥的四氢呋喃中，搅拌分散均匀，加入10mg催化剂DMAP；另配溶解有1.5g二环己基碳二亚胺(Dicyclohexylcarbodiimide,DCC)的四氢呋喃溶液5mL,30min内滴加入上述反应体系中，室温搅拌继续反应48h；过滤，将滤液浓缩至5mL，然后将滤液滴入40mL环己烷中沉淀，去除上层清液，加入5mL四氢呋喃溶解，再次滴入40mL环己烷中沉淀，如此再次重复，沉淀干燥，得到其中R为羟基的目标产物(f)。
1H NMR:δ1.12(s,6H,-CH 3),1.27(s,6H,-CH 3),3.27-4.06(m,24H,-NCH 2CH 2OOCCH 2CH 2OCH 2CH 2OCH 2CH 2OCH 2CH 2OOCCH 2CH 2N-),5.68(d,2H,-CH＝),6.68(d,2H,＝CH-),6.47-7.12(m,14H,Ar-H),5.13(d,2H,Ar-OH)。
螺吡喃(c)的四氢呋喃溶液(浓度0.01mg/mL)在室温下用365nm波长、10mW/cm 2光强紫外光照射前后的紫外可见吸收光谱变化见图3。
由图3可见，光照前(光照0s)体系在可见光区域(400-700nm)无吸收，在紫外光照后在590nm处新增一个吸收峰，并随照射时间增加而增加，该吸收峰属于花菁开环结构的吸收峰，说明了光照导致了开环的发生。开环形成的离子结构导致极性增加，即亲水性增加。在水相或者其它强极性分散剂中，亲水性的增加将会降低分散剂在其表面的界面张力。这可通过其润湿角在紫外辐射后明显变小来验证。
螺吡喃(f)/酚醛树脂薄膜表面水的接触角变化如图4所示。该试验 操作如下：将螺吡喃(f)和酚醛树脂(Mn＝10000g/mol)溶解在四氢呋喃中，使得其中螺吡喃(f)的浓度为10mg/mL，酚醛树脂的浓度为200mg/mL,将所得溶液涂布在玻璃基板上，风干成膜后，滴上水滴，然后用波长为365nm的UV光以10mW/cm 2的光照强度照射，观察水滴的接触角随照射时间的变化。由图4可见，在10mW/cm 2的UV光照强度下，一分钟内接触角从最初的89°降低到74°，这说明螺吡喃(f)受紫外光照后界面张力降低，亲水性增加，即极性增加。紫外-可见吸收光谱证明导致极性变大的原因是：螺吡喃(f)经紫外光照后螺环结构C-O键断裂，形成反式离子开环结构。
实施例3：N-羟乙基-5'-羧基-5,7-二甲氧基螺苯并噁嗪(i)的制备
Figure PCTCN2018084484-appb-000023
称取碘代乙醇(1.36g，8mmol)溶于10ml乙腈中，通氮气排气30min。称取2,3,3-三甲基-5’-羧基吲哚(g)(1.3g，8mmol)溶于5ml乙腈中，由滴液漏斗逐滴加入到反应液中，约1h滴完。继续回流反应36h。反应结束，冷却，旋除乙腈，用正己烷洗涤数次，再用乙醚洗涤数次，得到N-羟乙基-2,3,3-三甲基-5’-羧基吲哚碘盐(h)。将生成的N-羟乙基-2,3,3-三甲基-5-羧基吲哚碘盐(1.3g，4mmol)与1mL三乙胺溶于20ml乙醇中，加入到三口瓶中，通氮气排气30min。称取2-亚硝基-3,5-二甲氧基苯酚(0.9g，5mmol)溶于5ml乙醇中，在45℃下用注射器将其缓慢加入到位于三口瓶中的反应液中，于15min加完。升温至70℃，保持反应0.5h；升温至80℃保持反应2.5h；再升温至90℃继续反应2.5h。停止反应，冷却，反应液呈暗红色，旋除乙醇，得深红色粘稠状物，溶于60ml CH 2Cl 2中，用水洗涤数次洗去过量水杨醛。收集CH 2Cl 2相，旋干，得深 红色固状物，用正己烷重结晶，得到目标产物N-羟乙基-5'-羧基-5,7-二甲氧基螺苯并噁嗪(i)。
1H NMR:δ1.12(s,3H,-CH 3),1.27(s,3H,-CH 3),2.0(s,6H,-OCH 3),3.27-4.06(m,4H,-NCH 2CH 2O-),5.68(d,1H,-CH＝),6.68(d,1H,＝CH-),6.8-8.0(m,5H,Ar-H),5.13(d,2H,Ar-OH).。
化合物(i)的四氢呋喃溶液(浓度0.01mg/mL)在室温下用365nm波长、10mW/cm 2光强紫外光照射前后的紫外可见吸收光谱变化见图5。
由图5可见，光照前(光照0s)体系在可见光区域(400-700nm)无吸收，在紫外光照后在400-550nm处新增一个宽吸收峰，该吸收峰属于噁嗪开环反式离子结构的吸收峰，说明了光照导致了开环的发生。开环形成的离子结构导致极性增加，即亲水性增加。
N-羟乙基-5'-羧基-5,7-二甲氧基螺苯并噁嗪/酚醛树脂薄膜表面水的接触角变化如图6所示。该试验操作如下：将N-羟乙基-5'-羧基-5,7-二甲氧基螺苯并噁嗪(i)和酚醛树脂(Mn＝10000g/mol)溶解在四氢呋喃中，使得其中N-羟乙基-5'-羧基-5,7-二甲氧基螺苯并噁嗪(i)的浓度为5mg/mL，酚醛树脂的浓度为200mg/mL,将所得溶液涂布在玻璃基板上，风干成膜后，滴上水滴，然后用波长为365nm的UV光以10mW/cm 2的光照强度照射，观察水滴的接触角随照射时间的变化。
由图6可见，在10mW/cm 2的UV光照强度下，一分钟内接触角从最初的85°降低到70°，说明该化合物(i)受紫外光照后界面张力降低，亲水性增加，即极性增加。紫外-可见吸收光谱证明导致极性变大的原因是：螺噁嗪经紫外光照后螺环结构C-O键断裂，形成反式离子开环结构。
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应以所述权利要求的保护范围为准。

Claims (14)

  1. 一种正性光刻胶组合物，其包含主体胶材和光敏剂，其中所述光刻胶组合物还包含光致异构化合物，该光致异构化合物受到紫外光照射后结构转变为分子极性程度增加的离子结构。
  2. 根据权利要求1所述的正性光刻胶组合物，其中所述光致异构化合物为选自螺吡喃化合物、螺噁嗪化合物、氮丙啶化合物、联吡啶化合物中的至少一种。
  3. 根据权利要求2所述的正性光刻胶组合物，其中所述螺吡喃化合物具有下式(I)或式(II)结构：
    Figure PCTCN2018084484-appb-100001
    其中R 1为选自烷基链、醚链、苯基；和R 2为羧基或羟基；
    Figure PCTCN2018084484-appb-100002
    其中，n为整数，且4≤n≤10；和R为羧基或羟基；
    所述螺噁嗪化合物具有下式(III)结构：
    Figure PCTCN2018084484-appb-100003
    其中，R 1为CH 2CH 2OH；和R 2为羧基或羟基；
    所述氮丙啶化合物具有下式(IV)结构：
    Figure PCTCN2018084484-appb-100004
    其中，R基团为C 2H 4OH；以及
    所述联吡啶化合物具有下式(V)结构：
    Figure PCTCN2018084484-appb-100005
    其中，R 1基团为氢、甲基、乙基、丙基、丁基、醚链中的任一种；R 2基团为羧甲基、羧乙基、羧丙基中的任一种；R 3为氢、甲基、乙基、丙基、丁基、醚链中的任一种；和R 4为羧甲基、羧乙基、羧丙基中的任一种。
  4. 根据权利要求3所述的正性光刻胶组合物，其中对式(I)中R 1定义的烷基链选自丁基、戊基和己基；和/或，对式(I)中R 1定义的醚链为(CH 2CH 2O) mCH 3，其中m为整数，且1≤m≤5。
  5. 根据权利要求1所述的正性光刻胶组合物，其中所述螺吡喃化合物具有下式(I’)结构：
    Figure PCTCN2018084484-appb-100006
  6. 根据权利要求1-5中任一项所述的正性光刻胶组合物，其中所述正性光刻胶组合物还包含溶剂和添加剂。
  7. 根据权利要求1-6中任一项所述的正性光刻胶组合物，其中，
    所述主体胶材占所述正性光刻胶组合物总重量的5％～30％；
    所述光敏剂占所述正性光刻胶组合物总重量的2％～5％；
    所述光致异构化合物占所述正性光刻胶组合物总重量的0.1％～2％；
    所述添加剂占所述正性光刻胶组合物总重量的0.1％～1％；以及
    所述溶剂占所述正性光刻胶组合物总重量的62％～92.8％。
  8. 根据权利要求1-7中任一项所述的正性光刻胶组合物，其中
    所述主体胶材为酚醛树脂；
    和/或，
    所述光敏剂为重氮萘醌型光敏剂；
    和/或，
    所述溶剂为N-甲基吡咯烷酮、二甲基亚砜、丙二醇单甲醚乙酸酯、乙酸乙氧乙酯、二甲氧基乙醛中的任一种。
  9. 一种过孔的形成方法，该方法包括：
    在基板上依次形成钝化层和有机膜层，该有机膜层上具有露出所述钝化层的区域；
    形成覆盖所述有机膜层和所述钝化层的光刻胶层，该光刻胶层由权利要求1至8任一项所述的正性光刻胶组合物形成，且所述有机膜层与所述正性光刻胶组合物受光照前的极性相似；
    采用构图工艺对所述光刻胶层和露出的所述钝化层进行处理，形成贯穿钝化层的过孔，和覆盖在所述有机膜层以及被所述有机膜层露出的所述钝化层上的光刻胶保留部分；
    对所述光刻胶保留部分进行紫外光照射，以使所述正性光刻胶组合物中的光致异构化合物的结构转变为分子极性程度增加的离子结构；以及
    通过剥离液去除所述光刻胶保留部分。
  10. 一种过孔的形成方法，该方法包括：
    在基板上依次形成有机膜层和光刻胶层，该光刻胶层由权利要求1至8任一项所述的正性光刻胶组合物形成，且所述有机膜层与所述正性光刻胶组合物受光照前的极性相似；
    采用构图工艺对所述光刻胶层和所述有机膜层进行处理，形成贯穿所述有机膜层的过孔和覆盖在所述有机膜层除所述过孔所在区域之外的光刻胶保留部分；
    对所述光刻胶保留部分进行紫外光照射，以使所述正性光刻胶组合物中的光致异构化合物的结构转变为分子极性程度增加的离子结构；以及
    通过剥离液去除所述光刻胶保留部分。
  11. 根据权利要求9或10所述的过孔的形成方法，其中
    所述紫外光照射的波长范围为330～380nm，光照强度为1～10mW/CM 2。
  12. 一种显示基板，其中所述显示基板上的过孔通过如权利要求9-11中任一项所述的过孔的形成方法形成。
  13. 一种显示装置，其包括如权利要求12所示的显示基板。
  14. 根据权利要求13所述的显示装置，其包括LCD显示器、LCD电视、OLED显示器、OLED电视、手机、平板电脑、数码相框和导航仪。
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