TW202248365A - Pigment dispersion composition for black matrix, photoresist composition for black matrix, and black photoresist film capable of obtaining a photoresist composition excellent in thin line adhesion - Google Patents

Pigment dispersion composition for black matrix, photoresist composition for black matrix, and black photoresist film capable of obtaining a photoresist composition excellent in thin line adhesion Download PDF

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TW202248365A
TW202248365A TW111108822A TW111108822A TW202248365A TW 202248365 A TW202248365 A TW 202248365A TW 111108822 A TW111108822 A TW 111108822A TW 111108822 A TW111108822 A TW 111108822A TW 202248365 A TW202248365 A TW 202248365A
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black matrix
black
pigment dispersion
mentioned
composition
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辻康人
杉江俊輔
井上拓也
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日商阪田油墨股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/0041—Optical brightening agents, organic pigments
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
    • C08K5/3415—Five-membered rings
    • C08K5/3417—Five-membered rings condensed with carbocyclic rings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/04—Homopolymers or copolymers of esters
    • C08L33/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur, or oxygen atoms in addition to the carboxy oxygen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/56—Treatment of carbon black ; Purification
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • 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
    • G03F7/0045—Photosensitive materials with organic non-macromolecular light-sensitive compounds not otherwise provided for, e.g. dissolution inhibitors
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Materials For Photolithography (AREA)

Abstract

The invention relates to a pigment dispersion composition for a black matrix, which contains: carbon black, a pigment dispersant containing an alkaline group , a pigment dispersing aid containing an acid group, an epoxy resin, an alkali-soluble resin, and a solvent; the carbon black is surface-treated carbon black treated with inorganic aluminum salts. This pigment dispersion composition for a black matrix can obtain a photoresist composition excellent in thin line adhesion.

Description

黑矩陣用顏料分散組成物、黑矩陣用光阻組成物、及黑色光阻膜Pigment dispersion composition for black matrix, photoresist composition for black matrix, and black photoresist film

本發明涉及一種黑矩陣用顏料分散組成物、黑矩陣用光阻組成物、及黑色光阻膜。The invention relates to a pigment dispersion composition for a black matrix, a photoresist composition for a black matrix, and a black photoresist film.

以往，已知有一種光阻組成物，其使用含有碳黑、含有鹼性基的顏料分散劑、含有酸性基的顏料分散助劑、環氧樹脂、多官能硫醇化合物、及溶劑的黑矩陣用顏料分散組成物（專利文獻1）。另外，已知藉由使用其表面經由金屬鹽等被覆（固定）有染料的黑矩陣用碳黑作為黑矩陣用碳黑，能夠提升黑矩陣的隱蔽性。 [先前技術文獻] [專利文獻] Conventionally, there is known a photoresist composition using a black matrix containing carbon black, a pigment dispersant containing a basic group, a pigment dispersing aid containing an acidic group, an epoxy resin, a polyfunctional thiol compound, and a solvent. The composition is dispersed with a pigment (Patent Document 1). Moreover, it is known that the concealment property of a black matrix can be improved by using the carbon black for black matrices whose surface was coated (fixed) with the dye via a metal salt etc. as the carbon black for black matrices. [Prior Art Literature] [Patent Document]

[專利文獻1]日本特開2021-38289號公報 [專利文獻2]國際公開第2013/129554號 [Patent Document 1] Japanese Patent Laid-Open No. 2021-38289 [Patent Document 2] International Publication No. 2013/129554

[發明所欲解決之課題][Problem to be Solved by the Invention]

據專利文獻1記載，使用黑矩陣用顏料分散組成物的光阻組成物的細線密接性優異，但是由於該組成物將多官能硫醇化合物作為必須成分，故存在臭氣等問題。因此，需要一種黑矩陣用顏料分散組成物，其能夠藉由與此種組成物不同的方法，獲得細線密接性優異的光阻組成物。According to Patent Document 1, a photoresist composition using a pigment dispersion composition for a black matrix has excellent fine line adhesion, but since this composition contains a multifunctional thiol compound as an essential component, it has problems such as odor. Therefore, there is a need for a pigment dispersion composition for a black matrix, which can obtain a photoresist composition with excellent thin line adhesion by a method different from the composition.

本發明係鑒於上述情況而完成者，目的在於提供一種黑矩陣用顏料分散組成物，其能夠獲得細線密接性優異的光阻組成物。 [解決課題之技術手段] This invention was made in view of the said situation, and it aims at providing the pigment dispersion composition for black matrices which can obtain the photoresist composition excellent in thin line adhesiveness. [Technical means to solve the problem]

即，本發明涉及一種黑矩陣用顏料分散組成物，其含有：碳黑、含有鹼性基的顏料分散劑、含有酸性基的顏料分散助劑、環氧樹脂、鹼溶性樹脂、及溶劑，上述碳黑為經無機鋁鹽處理的表面處理碳黑。That is, the present invention relates to a pigment dispersion composition for a black matrix, which contains: carbon black, a pigment dispersant containing an alkaline group, a pigment dispersion aid containing an acidic group, an epoxy resin, an alkali-soluble resin, and a solvent. Carbon black is surface treated carbon black treated with inorganic aluminum salt.

另外，本發明涉及一種黑矩陣用光阻組成物，其含有：上述黑矩陣用顏料分散組成物、光聚合性化合物、及光聚合起始劑。Moreover, this invention relates to the photoresist composition for black matrices containing the said pigment dispersion composition for black matrices, a photopolymerizable compound, and a photopolymerization initiator.

進而，本發明涉及一種黑色光阻膜，其是使用黑矩陣用光阻組成物而獲得。 [發明之效果] Furthermore, this invention relates to the black resist film obtained using the resist composition for black matrices. [Effect of Invention]

本發明的黑矩陣用顏料分散組成物含有：碳黑、含有鹼性基的顏料分散劑、含有酸性基的顏料分散助劑、環氧樹脂、鹼溶性樹脂、及溶劑，上述碳黑為經無機鋁鹽處理的表面處理碳黑。尤其是上述表面處理碳黑與未處理碳黑相比，親水性受到適度抑制，能夠抑制鹼性顯影及水洗導致所形成的圖案部溶出、剝離，因此，本發明的黑矩陣用顏料分散組成物的細線密接性優異。The pigment dispersion composition for black matrix of the present invention contains: carbon black, pigment dispersant containing basic group, pigment dispersion aid containing acid group, epoxy resin, alkali-soluble resin, and solvent, and the above-mentioned carbon black is obtained by inorganic Aluminum salt treated surface treated carbon black. In particular, the above-mentioned surface-treated carbon black has moderately suppressed hydrophilicity compared with untreated carbon black, and can suppress the dissolution and peeling of the formed pattern part caused by alkaline development and water washing. Therefore, the pigment dispersion composition for black matrix of the present invention Excellent thin wire adhesion.

本發明的黑矩陣用顏料分散組成物含有：碳黑、含有鹼性基的顏料分散劑、含有酸性基的顏料分散助劑、環氧樹脂、鹼溶性樹脂、及溶劑，上述碳黑為經無機鋁鹽處理的表面處理碳黑。The pigment dispersion composition for black matrix of the present invention contains: carbon black, pigment dispersant containing basic group, pigment dispersion aid containing acid group, epoxy resin, alkali-soluble resin, and solvent, and the above-mentioned carbon black is obtained by inorganic Aluminum salt treated surface treated carbon black.

＜表面處理碳黑＞ 上述表面處理碳黑為碳黑表面經無機鋁鹽處理的表面處理碳黑。 ＜Surface treated carbon black＞ The above-mentioned surface-treated carbon black is a surface-treated carbon black whose surface is treated with an inorganic aluminum salt.

作為上述碳黑，可使用黑矩陣用顏料分散組成物中所使用的公知碳黑，例如可列舉：乙炔黑、槽黑、爐黑（furness black）、科琴黑（Ketjen black）等。作為上述碳黑的具體例，可列舉：三菱化學公司所製造的MA7、MA8、MA11、MA14、＃1000、＃2350等；Orion Engineered Carbons公司所製造的SpecialBlack350、SpecialBlack250、SpecialBlack550、NEROX2500、NEROX3500、NEROX305等；Cabot公司所製造的MOGULL、REGAL400R、TPK1101R、TPK1104R、TPK1227R等；Columbia Carbon公司所製造的RAVEN1200、RAVEN1250、RAVEN1255、RAVEN1190U、RAVEN1170、RAVEN1035、RAVEN1080U、RAVEN1060U、RAVEN1100U等。關於上述碳黑，優選為pH為5以下且具有羧基等酸性基的酸性碳黑，另外，粒徑優選為20～60 nm。作為上述酸性碳黑，例如可列舉：NEROX2500、NEROX3500、TPK1101R、TPK1104R、TPK1227R等。另外，上述粒徑是指藉由顯微鏡觀察所測定或算出的平均一次粒徑，在市售品的情況下，將目錄值作為參考。上述碳黑可單獨使用或組合兩種以上使用。As said carbon black, the well-known carbon black used for the pigment dispersion composition for black matrices can be used, For example, acetylene black, channel black, furnace black (furness black), Ketjen black etc. are mentioned. Specific examples of the above carbon black include: MA7, MA8, MA11, MA14, #1000, #2350 manufactured by Mitsubishi Chemical Corporation; SpecialBlack350, SpecialBlack250, SpecialBlack550, NEROX2500, NEROX3500, NEROX305 manufactured by Orion Engineered Carbons etc.; MOGULL, REGAL400R, TPK1101R, TPK1104R, TPK1227R manufactured by Cabot Corporation; RAVEN1200, RAVEN1250, RAVEN1255, RAVEN1190U, RAVEN1170, RAVEN1035, RAVEN1080U, RAVEN1060U, etc. manufactured by Columbia Carbon Company. The above-mentioned carbon black is preferably an acidic carbon black having a pH of 5 or less and having an acidic group such as a carboxyl group, and the particle diameter is preferably 20 to 60 nm. As said acidic carbon black, NEROX2500, NEROX3500, TPK1101R, TPK1104R, TPK1227R etc. are mentioned, for example. In addition, the said particle diameter means the average primary particle diameter measured or calculated by microscope observation, and in the case of a commercial item, a catalog value is taken as a reference. The above carbon blacks may be used alone or in combination of two or more.

關於上述無機鋁鹽，只要是公知無機鋁鹽即可使用，例如可列舉：硫酸鋁、（聚）氯化鋁、硝酸鋁等。As for the above-mentioned inorganic aluminum salt, any known inorganic aluminum salt can be used, and examples thereof include aluminum sulfate, (poly)aluminum chloride, aluminum nitrate, and the like.

上述表面處理碳黑中，上述無機鋁的使用量相對於上述碳黑100質量份，從細線密接性的觀點而言，優選為0.5質量份以上，更優選為8質量份以上，並且，從黑色度的觀點而言，優選為200質量份以下，更優選為150質量份以下。In the surface-treated carbon black, the amount of the inorganic aluminum to be used is preferably 0.5 parts by mass or more, more preferably 8 parts by mass or more from the viewpoint of fine wire adhesion with respect to 100 parts by mass of the above-mentioned carbon black. From the viewpoint of the degree, it is preferably 200 parts by mass or less, and more preferably 150 parts by mass or less.

上述表面處理碳黑於上述黑矩陣用顏料分散組成物中，從提升形成了黑矩陣膜的情況下的遮光性的觀點而言，優選為3質量%以上，更優選為10質量%以上，並且，從顏料分散的觀點而言，優選為70質量%以下，更優選為50質量%以下。The above-mentioned surface-treated carbon black is preferably 3% by mass or more, more preferably 10% by mass or more, in the above-mentioned pigment dispersion composition for black matrix, from the viewpoint of improving the light-shielding properties when a black matrix film is formed, and , from the viewpoint of pigment dispersion, preferably 70% by mass or less, more preferably 50% by mass or less.

上述表面處理碳黑中的表面處理方法並無特別限定，例如可列舉：一面於混合機或攪拌機中攪拌碳黑（使碳黑流動），一面1）添加上述無機鋁鹽或包含上述無機鋁鹽的水溶液進行攪拌處理的方法；2）利用包含上述無機鋁鹽的水溶液，使用噴霧器等噴霧機進行噴霧處理的方法；以及3）在用於碳黑的造粒步驟中的水中添加上述無機鋁鹽進行處理的方法等。The surface treatment method of the above-mentioned surface-treated carbon black is not particularly limited, for example, while stirring the carbon black in a mixer or a stirrer (making the carbon black flow), while 1) adding the above-mentioned inorganic aluminum salt or containing the above-mentioned inorganic aluminum salt 2) A method of spraying an aqueous solution containing the above-mentioned inorganic aluminum salt with a sprayer such as a sprayer; and 3) Adding the above-mentioned inorganic aluminum salt to water in the granulation step for carbon black method of processing, etc.

＜含有鹼性基的顏料分散劑＞ 上述含有鹼性基的顏料分散劑只要能夠使上述碳黑分散即可，可使用黑矩陣用顏料分散組成物中所使用的公知的含有鹼性基的顏料分散劑，例如可列舉：陰離子性表面活性劑、含有鹼性基的聚酯系顏料分散劑、含有鹼性基的丙烯酸系顏料分散劑、含有鹼性基的胺酯（urethane）系顏料分散劑、含有鹼性基的碳二醯亞胺系顏料分散劑等。作為上述鹼性基，尤其是從分散性優異的觀點而言，優選為一級、二級或三級胺基。上述含有鹼性基的顏料分散劑可單獨使用或組合兩種以上使用。 ＜Pigment dispersants containing basic groups＞ As long as the above-mentioned pigment dispersant containing basic groups can disperse the above-mentioned carbon black, known pigment dispersants containing basic groups used in the pigment dispersion composition for black matrix can be used, for example, anionic surface Active agent, basic group-containing polyester pigment dispersant, basic group-containing acrylic pigment dispersant, basic group-containing urethane pigment dispersant, basic group-containing carbodiamide Amine pigment dispersant, etc. As the above-mentioned basic group, a primary, secondary, or tertiary amino group is preferable especially from the viewpoint of excellent dispersibility. The above-mentioned basic group-containing pigment dispersants may be used alone or in combination of two or more.

從獲得良好的顏料分散性的方面而言，上述含有鹼性基的顏料分散劑優選為高分子型含有鹼性基的顏料分散劑。作為上述高分子型含有鹼性基的顏料分散劑，例如可列舉：含有鹼性基的胺酯系高分子顏料分散劑、含有鹼性基的聚酯系高分子顏料分散劑、含有鹼性基的丙烯酸系高分子顏料分散劑等。該等之中，優選為含有鹼性基的胺酯系高分子顏料分散劑、含有鹼性基的丙烯酸系高分子顏料分散劑。上述含有鹼性基的胺酯系高分子顏料分散劑更優選為具有選自由聚酯鏈、聚醚鏈、及聚碳酸酯鏈所組成的群中的至少一種的含有鹼性基的胺酯系高分子顏料分散劑。From the viewpoint of obtaining good pigment dispersibility, the above-mentioned basic group-containing pigment dispersant is preferably a polymer type basic group-containing pigment dispersant. Examples of the above-mentioned polymer type pigment dispersants containing basic groups include: basic group-containing urethane polymer pigment dispersants, basic group-containing polyester polymer pigment dispersants, basic group-containing Acrylic polymer pigment dispersant, etc. Among them, a basic group-containing urethane polymer pigment dispersant and a basic group-containing acrylic polymer pigment dispersant are preferable. The above-mentioned basic group-containing urethane-based polymer pigment dispersant is more preferably a basic group-containing urethane-based pigment dispersant having at least one selected from the group consisting of polyester chains, polyether chains, and polycarbonate chains. Polymer pigment dispersant.

上述含有鹼性基的顏料分散劑相對於上述表面處理碳黑100質量份，優選為1～100質量份，更優選為2～50質量份。The said basic group containing pigment dispersant is preferably 1-100 mass parts with respect to 100 mass parts of said surface-treated carbon blacks, More preferably, it is 2-50 mass parts.

＜含有酸性基的顏料分散助劑＞ 上述含有酸性基的顏料分散助劑是為了進一步改善顏料的分散性而使用，例如可列舉：於內醯胺黑（lactam black）、苝系化合物、二酮吡咯并吡咯（diketo-pyrrolo-pyrrole）系化合物、偶氮萘酚系化合物、二㗁𠯤系化合物、喹吖酮系化合物、酞青系化合物及其金屬錯合物、蒽醌、萘、吖啶酮、或三𠯤等色素中導入羧基、磺酸基等酸性基而成的化合物（具有酸性基的色素衍生物）；或者利用有機胺等中和該等而成的化合物。作為上述具有酸性基的色素衍生物，從碳黑分散性良好的觀點而言，優選為具有磺酸基的酞青系（具有酞青骨架的）色素衍生物。上述含有酸性基的顏料分散助劑可單獨使用或組合兩種以上使用。 ＜Pigment Dispersion Aids Containing Acidic Group＞ The above-mentioned pigment dispersing aids containing acid groups are used to further improve the dispersibility of pigments, for example, lactam black (lactam black), perylene compounds, diketo-pyrrolo-pyrrole (diketo-pyrrolo-pyrrole) Carboxyl groups are introduced into pigments such as azonaphthol-based compounds, azonaphthol-based compounds, quinacridone-based compounds, phthalocyanine-based compounds and their metal complexes, anthraquinones, naphthalene, acridone, or tri-methanol-based pigments , sulfonic acid groups and other acidic groups (pigment derivatives having acidic groups); or compounds neutralized with organic amines and the like. As the above-mentioned dye derivative having an acidic group, a phthalocyanine-based (having a phthalocyanine skeleton) dye derivative having a sulfonic acid group is preferable from the viewpoint of good carbon black dispersibility. The above-mentioned acidic group-containing pigment dispersion aids may be used alone or in combination of two or more.

上述含有酸性基的顏料分散助劑相對於上述表面處理碳黑100質量份，優選為0.1～20質量份，更優選為1～10質量份。The amount of the above-mentioned acidic group-containing pigment dispersion aid is preferably 0.1 to 20 parts by mass, more preferably 1 to 10 parts by mass, based on 100 parts by mass of the above-mentioned surface-treated carbon black.

＜環氧樹脂＞ 上述環氧樹脂為具有兩個以上環氧基的多官能環氧樹脂。作為上述環氧樹脂，例如可列舉：雙酚A型環氧樹脂、雙酚F型環氧樹脂、雙酚S型環氧樹脂、聯苯酚型環氧樹脂、脂環式環氧樹脂、脂肪族鏈狀環氧樹脂、環氧丙酯型環氧樹脂、酚化合物（苯酚、甲酚、烷基酚、鄰苯二酚、雙酚F、雙酚A、雙酚S等）與醛類化合物（甲醛、柳醛等）的縮合物的環氧丙醚化物、二官能酚的環氧丙醚化物、二官能醇的環氧丙醚化物、三官能以上的多酚的環氧丙醚化物、以及該等的氫化物或鹵化物等。上述環氧樹脂可為具有脂環或芳香環的多官能環氧樹脂，也可為具有作為脂環的二環戊二烯骨架的多官能環氧樹脂，其中，從提升細線密接性的觀點而言，優選為具有芳香環的多官能環氧樹脂。作為上述環氧樹脂的具體例，可列舉：Epolight 40E、Epolight 100E、Epolight 200E、Epolight 400E、Epolight 70P、Epolight 200P、Epolight 400P、Epolight 1500NP、Epolight 80MF、Epolight 4000、Epolight 3002（以上，共榮公司化學公司製造）；Denacol EX-212L、Denacol EX-214L、Denacol EX-216L、Denacol EX-850L、Denacol EX-321L（以上，Nagase ChemteX公司製造）；GAN、GOT、NC3000、NC6000、EPPN502H（以上，日本化藥公司製造）；Epikote 828、Epikote 1002、Epikote 1750、Epikote 1007、YX8100-BH30、E1256、E4250、E4275（以上，Japan Epoxy Resins公司製造）；EPICLON EXA-9583、EPICLON N695、HP7200、HP4032（以上，大日本油墨化學工業公司製造）；VG3101（三井化學公司製造）；TEPIC S、TEPIC G、TEPIC P（以上，日產化學工業公司製造）；Epotohto YH-434L（東都化成公司製造）等。另外，從反應性等方面而言優選的是上述環氧樹脂不具有二氫茚結構或聯苯結構。 ＜Epoxy resin＞ The above-mentioned epoxy resin is a polyfunctional epoxy resin having two or more epoxy groups. Examples of the above-mentioned epoxy resins include bisphenol A epoxy resins, bisphenol F epoxy resins, bisphenol S epoxy resins, biphenol epoxy resins, alicyclic epoxy resins, aliphatic epoxy resins, and bisphenol epoxy resins. Chain epoxy resin, glycidyl epoxy resin, phenolic compounds (phenol, cresol, alkylphenol, catechol, bisphenol F, bisphenol A, bisphenol S, etc.) and aldehyde compounds ( Glycidyl ether compounds of condensates such as formaldehyde, salicaldehyde, etc.), glycidyl ether compounds of difunctional phenols, glycidyl ether compounds of difunctional alcohols, glycidyl ether compounds of trifunctional or higher polyphenols, and These hydrides or halides, etc. The above-mentioned epoxy resin may be a polyfunctional epoxy resin having an alicyclic or aromatic ring, or may be a polyfunctional epoxy resin having a dicyclopentadiene skeleton as an alicyclic ring. In other words, a polyfunctional epoxy resin having an aromatic ring is preferable. Specific examples of the above-mentioned epoxy resins include: Epolight 40E, Epolight 100E, Epolight 200E, Epolight 400E, Epolight 70P, Epolight 200P, Epolight 400P, Epolight 1500NP, Epolight 80MF, Epolight 4000, Epolight 3002 (above, Kyoyoung Co., Ltd. Chemical company); Denacol EX-212L, Denacol EX-214L, Denacol EX-216L, Denacol EX-850L, Denacol EX-321L (above, manufactured by Nagase ChemteX Corporation); GAN, GOT, NC3000, NC6000, EPPN502H (above, Nippon Kayaku Corporation); Epikote 828, Epikote 1002, Epikote 1750, Epikote 1007, YX8100-BH30, E1256, E4250, E4275 (the above, manufactured by Japan Epoxy Resins Corporation); EPICLON EXA-9583, EPICLON N695, HP7200, HP4032 ( The above are manufactured by Dainippon Ink Chemical Industry Co., Ltd.); VG3101 (manufactured by Mitsui Chemicals Co., Ltd.); TEPIC S, TEPIC G, and TEPIC P (the above are manufactured by Nissan Chemical Industry Co., Ltd.); Epotohto YH-434L (manufactured by Tohto Kasei Co., Ltd.), etc. In addition, it is preferable that the above-mentioned epoxy resin does not have an indane structure or a biphenyl structure from the viewpoint of reactivity and the like.

作為上述環氧樹脂，例如可列舉下述式1～7所示的具有芳香環的多官能環氧樹脂為優選。As said epoxy resin, the polyfunctional epoxy resin which has an aromatic ring represented by following formula 1-7 is mentioned, for example, Preferably it is.

Figure 02_image001
(m為0～20)
Figure 02_image001
(m is 0~20)

Figure 02_image003
Figure 02_image003

Figure 02_image005
(n為1～20)
Figure 02_image005
(n is 1~20)

Figure 02_image007
(R 1~6各自獨立為碳數為1~6的飽和烴基，n為1~20)
Figure 02_image007
(R 1~6 are each independently a saturated hydrocarbon group with a carbon number of 1~6, and n is 1~20)

Figure 02_image009
(n為1~20)
Figure 02_image009
(n is 1~20)

Figure 02_image011
(R 1~2各自獨立為氫或碳數為1~6的飽和烴基，n為1~20)
Figure 02_image011
(R 1~2 are each independently hydrogen or a saturated hydrocarbon group with 1~6 carbons, n is 1~20)

Figure 02_image013
(n為1~20)
Figure 02_image013
(n is 1~20)

上述環氧樹脂相對於上述黑矩陣用顏料分散組成物或後述黑矩陣用光阻組成物中所包含的碳黑100質量份，從作為黑矩陣的阻抗值的觀點而言，優選為1質量份以上，更優選為2質量份以上，進而優選為5質量份以上，並且，從基於顏料濃度的黑色度的觀點而言，優選為30質量份以下，更優選為20質量份以下，進而優選為15質量份以下。The above-mentioned epoxy resin is preferably 1 part by mass from the viewpoint of the impedance value of the black matrix with respect to 100 parts by mass of carbon black contained in the above-mentioned pigment dispersion composition for black matrix or the photoresist composition for black matrix described later. Above, more preferably 2 parts by mass or more, still more preferably 5 parts by mass or more, and from the viewpoint of the blackness based on the pigment concentration, preferably 30 parts by mass or less, more preferably 20 parts by mass or less, still more preferably 15 parts by mass or less.

＜鹼溶性樹脂＞ 上述鹼溶性樹脂只要是能夠溶解於鹼性顯影液中的鹼溶性樹脂則並無特別限制，優選為含有羧基、磺酸基、膦酸基（-P(=O)(OH 2)）等陰離子性基中的一種或兩種以上的樹脂。上述鹼溶性樹脂可單獨使用或組合兩種以上使用。 <Alkali-soluble resin> The above-mentioned alkali-soluble resin is not particularly limited as long as it is an alkali-soluble resin that can be dissolved in an alkaline developer, and preferably contains a carboxyl group, a sulfonic acid group, a phosphonic acid group (-P(=O)(OH 2 )) One or two or more resins in such anionic groups. The above-mentioned alkali-soluble resins may be used alone or in combination of two or more.

從鹼性顯影性的觀點而言，上述鹼溶性樹脂的酸值優選為10 mgKOH/g以上300 mgKOH/g以下，更優選為20 mgKOH/g以上200 mgKOH/g以下。From the viewpoint of alkali developability, the acid value of the alkali-soluble resin is preferably 10 mgKOH/g to 300 mgKOH/g, more preferably 20 mgKOH/g to 200 mgKOH/g.

從光阻膜的形成性的觀點而言，上述鹼溶性樹脂的重量平均分子量優選為5,000以上，更優選為10,000以上。從提高於鹼性顯影液中的溶解性的觀點而言，上述鹼溶性樹脂的重量平均分子量優選為100,000以下，更優選為50,000以下。The weight average molecular weight of the above-mentioned alkali-soluble resin is preferably 5,000 or more, more preferably 10,000 or more, from the viewpoint of the formability of a photoresist film. The weight average molecular weight of the alkali-soluble resin is preferably 100,000 or less, more preferably 50,000 or less, from the viewpoint of improving solubility in an alkaline developing solution.

上述重量平均分子量可利用凝膠滲透層析（GPC）法進行測定。作為一例，GPC裝置使用Water2690（Waters公司製造），管柱使用PLgel 5 μm MIXED-D（Polymer Laboratories公司製造），使用四氫呋喃作為展開溶劑，在管柱溫度25℃、流速1毫升/分鐘、RI檢測器、試樣注入濃度10毫克/毫升、注入量100微升的條件下進行層析術，從而能夠以聚苯乙烯換算的重量平均分子量的形式求出。The said weight average molecular weight can be measured by the gel permeation chromatography (GPC) method. As an example, the GPC device uses Water2690 (manufactured by Waters), the column uses PLgel 5 μm MIXED-D (manufactured by Polymer Laboratories), and tetrahydrofuran is used as the developing solvent. Chromatography was performed under the conditions of a sample injection concentration of 10 mg/ml and an injection volume of 100 microliters, and it was possible to obtain the polystyrene-equivalent weight average molecular weight.

作為上述鹼溶性樹脂，例如可列舉：鹼溶性聚醯亞胺樹脂、鹼溶性聚醯亞胺前驅物、鹼溶性聚苯并

Figure 111108822-001
唑樹脂、鹼溶性聚苯并
Figure 111108822-001
唑前驅物、鹼溶性卡多樹脂、鹼溶性環氧(甲基)丙烯酸酯樹脂、鹼溶性聚矽氧烷樹脂、鹼溶性酚醛清漆樹脂、鹼溶性(甲基)丙烯酸樹脂、鹼溶性聚胺酯樹脂、鹼溶性聚酯樹脂等。該等之中，從塗膜耐熱性的觀點而言，優選為鹼溶性卡多樹脂、鹼溶性環氧(甲基)丙烯酸酯樹脂。Examples of the alkali-soluble resin include: alkali-soluble polyimide resins, alkali-soluble polyimide precursors, alkali-soluble polybenzoic acid
Figure 111108822-001
Azole resin, alkali-soluble polybenzo
Figure 111108822-001
Azole precursors, alkali-soluble cardo resins, alkali-soluble epoxy (meth)acrylate resins, alkali-soluble polysiloxane resins, alkali-soluble novolak resins, alkali-soluble (meth)acrylic resins, alkali-soluble polyurethane resins, Alkali-soluble polyester resin, etc. Among them, alkali-soluble cardo resins and alkali-soluble epoxy (meth)acrylate resins are preferable from the viewpoint of coating film heat resistance.

上述鹼溶性卡多樹脂是指具有卡多骨架的鹼溶性樹脂，卡多骨架是指2個芳香族基藉由單鍵連接在作為構成環狀結構的環碳原子的四級碳原子上而成的骨架。作為鹼溶性卡多樹脂的具體例，例如可列舉：ADEKA ARKLS WR-301（ADEKA製造）；OGSOL CR-TR1、CR-TR2、CR-TR3、CR-TR4、CR-TR5、CR-TR6（以上，Osaka Gas Chemicals製造）。The above-mentioned alkali-soluble cardo resin refers to an alkali-soluble resin having a cardo skeleton, and the cardo skeleton refers to the formation of two aromatic groups connected by a single bond to a quaternary carbon atom as a ring carbon atom constituting a ring structure. skeleton. Specific examples of the alkali-soluble cardo resin include: ADEKA ARKLS WR-301 (manufactured by ADEKA); OGSOL CR-TR1, CR-TR2, CR-TR3, CR-TR4, CR-TR5, CR-TR6 (above , manufactured by Osaka Gas Chemicals).

上述鹼溶性環氧(甲基)丙烯酸酯樹脂是指「以如下方法所獲得之酸改質環氧樹脂中，不具有上述卡多骨架的相當於上述鹼溶性樹脂的樹脂」：藉由使乙烯性不飽和單羧酸所具有的羧基開環加成至環氧樹脂所具有的環氧基來導入乙烯性不飽和基，進而藉由使多元羧酸（或其酐）加成至由於環氧基的開環而產生的羥基的至少一部分來導入羧基獲得酸改質環氧樹脂。上述鹼溶性環氧(甲基)丙烯酸酯樹脂中，作為成為母體原料的環氧樹脂，例如可列舉：雙酚A型環氧樹脂、雙酚F型環氧樹脂、具有聯苯結構的環氧樹脂、苯酚酚醛清漆型環氧樹脂、甲酚酚醛清漆型環氧樹脂為優選。作為用於使環氧樹脂改質的乙烯性不飽和單羧酸，例如可列舉丙烯酸、甲基丙烯酸為優選。作為多元羧酸（或其酐），例如可列舉馬來酸酐、琥珀酸酐、四氫鄰苯二甲酸酐為優選。該等之中，從提升細線密接性的觀點而言，優選為具有聯苯骨架的鹼溶性環氧(甲基)丙烯酸酯樹脂。作為上述鹼溶性環氧(甲基)丙烯酸酯樹脂的具體例，例如可列舉：ZAR-1494H、ZAR-2001H、ZFR-1491H、ZCR-1797H、ZCR-1569H、ZCR-1798H（以上，日本化藥製造）。另外，作為優選的具體例，可列舉具有下述結構式中任一者所表示的部分結構的鹼溶性環氧(甲基)丙烯酸酯樹脂。The above-mentioned alkali-soluble epoxy (meth)acrylate resin refers to "a resin corresponding to the above-mentioned alkali-soluble resin that does not have the above-mentioned cardo skeleton among acid-modified epoxy resins obtained by the following method": The carboxyl group possessed by the unsaturated monocarboxylic acid is ring-opened and added to the epoxy group possessed by the epoxy resin to introduce an ethylenically unsaturated group, and then by adding the polycarboxylic acid (or its anhydride) to the epoxy group due to the epoxy resin At least a part of the hydroxyl group generated by the ring opening of the group is introduced into the carboxyl group to obtain an acid-modified epoxy resin. Among the above-mentioned alkali-soluble epoxy (meth)acrylate resins, examples of epoxy resins used as matrix materials include bisphenol A type epoxy resins, bisphenol F type epoxy resins, and epoxy resins having a biphenyl structure. Resins, phenol novolak type epoxy resins, and cresol novolak type epoxy resins are preferable. As ethylenically unsaturated monocarboxylic acid for modifying an epoxy resin, acrylic acid and methacrylic acid are preferable, for example. As polyhydric carboxylic acid (or its anhydride), for example, maleic anhydride, succinic anhydride, tetrahydrophthalic anhydride are preferable. Among these, the alkali-soluble epoxy (meth)acrylate resin which has a biphenyl skeleton is preferable from a viewpoint of improving fine wire adhesiveness. Specific examples of the alkali-soluble epoxy (meth)acrylate resins include, for example: ZAR-1494H, ZAR-2001H, ZFR-1491H, ZCR-1797H, ZCR-1569H, ZCR-1798H (the above, Nippon Kayaku manufacture). Moreover, the alkali-soluble epoxy (meth)acrylate resin which has the partial structure represented by any one of following structural formulas is mentioned as a preferable specific example.

Figure 02_image015
Figure 02_image015

上述鹼溶性樹脂相對於上述表面處理碳黑100質量份優選為1～70質量份，更優選為5～30質量份。The said alkali-soluble resin is preferably 1-70 mass parts with respect to 100 mass parts of said surface-treated carbon blacks, More preferably, it is 5-30 mass parts.

＜溶劑＞ 上述溶劑可使用黑矩陣用顏料分散組成物中所使用的公知溶劑。從能夠使顏料穩定地分散並且能夠使上述含有鹼性基的顏料分散劑或上述鹼溶性樹脂充分溶解的觀點而言，上述溶劑優選為酯系溶劑、醚系溶劑、醚酯系溶劑、酮系溶劑、芳香族烴系溶劑、含氮系溶劑等。上述溶劑可單獨使用或組合兩種以上使用。 <Solvent> As said solvent, the well-known solvent used for the pigment dispersion composition for black matrices can be used. From the viewpoint of stably dispersing the pigment and sufficiently dissolving the above-mentioned pigment dispersant containing a basic group or the above-mentioned alkali-soluble resin, the above-mentioned solvent is preferably an ester-based solvent, an ether-based solvent, an ether-ester-based solvent, or a ketone-based solvent. Solvents, aromatic hydrocarbon solvents, nitrogen-containing solvents, etc. These solvents may be used alone or in combination of two or more.

作為上述酯系溶劑，可列舉：2-羥基丙酸甲酯、2-羥基丙酸乙酯、2-羥基-2-甲基丙酸乙酯、丙酸3-甲基-3-甲氧基丁酯，3-甲氧基丙酸甲酯、3-甲氧基丙酸乙酯、3-乙氧基丙酸甲酯、3-乙氧基丙酸乙酯、乙氧基乙酸乙酯、羥基乙酸酯、甲酸正戊酯等。作為上述醚系溶劑，例如可列舉：乙二醇單甲醚、乙二醇單乙醚、乙二醇單異丙醚、乙二醇單丁醚、二乙二醇單甲醚、二乙二醇單乙醚、丙二醇單甲醚、丙二醇單乙醚、丙二醇單丁醚、二乙二醇二乙醚、二乙二醇二甲醚、二乙二醇甲基乙基醚等。作為上述醚酯系溶劑，例如可列舉：乙二醇單甲醚乙酸酯、乙二醇單乙醚乙酸酯、乙二醇單丁醚乙酸酯、丙二醇單甲醚乙酸酯、丙二醇單乙醚乙酸酯等。作為上述酮系溶劑，例如可列舉：甲基異丁基酮、環己酮、2-庚酮、δ-丁內酯等。作為上述芳香族烴系溶劑，例如可列舉：甲苯、二甲苯、烷基萘等。作為上述含氮系溶劑，例如可列舉：N-甲基吡咯啶酮，N,N-二甲基甲醯胺、N,N-二甲基乙醯胺等。Examples of the above-mentioned ester-based solvents include methyl 2-hydroxypropionate, ethyl 2-hydroxypropionate, ethyl 2-hydroxy-2-methylpropionate, 3-methyl-3-methoxypropionate Butyl ester, methyl 3-methoxypropionate, ethyl 3-methoxypropionate, methyl 3-ethoxypropionate, ethyl 3-ethoxypropionate, ethyl ethoxyacetate, Glycolic acid ester, n-pentyl formate, etc. Examples of the aforementioned ether-based solvents include ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monoisopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol Monoethyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monobutyl ether, diethylene glycol diethyl ether, diethylene glycol dimethyl ether, diethylene glycol methyl ethyl ether, etc. Examples of the above-mentioned ether ester solvents include ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether acetate, ethylene glycol monobutyl ether acetate, propylene glycol monomethyl ether acetate, propylene glycol monomethyl ether acetate, and propylene glycol monomethyl ether acetate. Ether acetate etc. As said ketone solvent, methyl isobutyl ketone, cyclohexanone, 2-heptanone, δ-butyrolactone, etc. are mentioned, for example. As said aromatic hydrocarbon type solvent, toluene, xylene, alkylnaphthalene etc. are mentioned, for example. As said nitrogen-containing solvent, N-methylpyrrolidone, N,N- dimethylformamide, N,N- dimethylacetamide etc. are mentioned, for example.

上述溶劑於上述黑矩陣用顏料分散組成物中的比率從步驟性的觀點而言，優選為40質量%以上，更優選為50質量%以上，並且，從分散穩定性的觀點而言，優選為90質量%以下，更優選為80質量%以下。The ratio of the above-mentioned solvent in the above-mentioned pigment dispersion composition for black matrix is preferably 40% by mass or more, more preferably 50% by mass or more from the viewpoint of processability, and preferably 50% by mass or more from the viewpoint of dispersion stability. 90% by mass or less, more preferably 80% by mass or less.

上述黑矩陣用顏料分散組成物中，也可進而視需要添加調平劑、上述環氧樹脂及上述鹼溶性樹脂以外的樹脂、抗氧化劑、消泡劑等添加劑。其中，從臭氣性的觀點而言，優選為不含硫醇化合物（例如，分子量為1000以下的硫醇化合物）。Additives such as a leveling agent, the above-mentioned epoxy resin and resins other than the above-mentioned alkali-soluble resin, antioxidant, and antifoaming agent may be further added to the above-mentioned pigment dispersion composition for a black matrix. Among them, it is preferable not to contain a thiol compound (for example, a thiol compound having a molecular weight of 1000 or less) from the viewpoint of odor properties.

上述黑矩陣用顏料分散組成物中，上述碳黑、上述含有鹼性基的顏料分散劑、上述含有酸性基的顏料分散助劑、上述環氧樹脂、上述鹼溶性樹脂、及上述溶劑的總比率優選為75質量%以上，更優選為85質量%以上，進而優選為95質量%以上。In the above-mentioned pigment dispersion composition for black matrix, the total ratio of the above-mentioned carbon black, the above-mentioned basic group-containing pigment dispersant, the above-mentioned acidic group-containing pigment dispersion aid, the above-mentioned epoxy resin, the above-mentioned alkali-soluble resin, and the above-mentioned solvent Preferably it is 75 mass % or more, More preferably, it is 85 mass % or more, More preferably, it is 95 mass % or more.

關於上述黑矩陣用顏料分散組成物，使用輥磨機、捏合機、高速攪拌機、珠磨機、球磨機、砂磨機、超音波分散機、高壓分散裝置等對上述各成分進行分散處理而製備即可。The above-mentioned pigment dispersion composition for black matrix is prepared by dispersing the above-mentioned components using a roll mill, a kneader, a high-speed mixer, a bead mill, a ball mill, a sand mill, an ultrasonic disperser, a high-pressure dispersing device, etc. Can.

＜黑矩陣用光阻組成物＞ 本發明的黑矩陣用光阻組成物包含上述黑矩陣用顏料分散組成物、光聚合性化合物、及光聚合起始劑。另外，上述表面處理碳黑於上述黑矩陣用光阻組成物的固體成分中的比率優選為30質量%以上80質量%以下。 ＜Photoresist composition for black matrix＞ The photoresist composition for black matrices of this invention contains the said pigment dispersion composition for black matrices, a photopolymerizable compound, and a photopolymerization initiator. Moreover, it is preferable that the ratio of the said surface-treated carbon black in the solid content of the said photoresist composition for black matrices is 30 mass % or more and 80 mass % or less.

＜光聚合性化合物＞ 上述光聚合性化合物可使用黑矩陣用光阻組成物中所使用的公知光聚合性化合物，例如可列舉：具有光聚合性不飽和鍵的單體、低聚物等。上述光聚合性化合物可單獨使用或組合兩種以上使用。 ＜Photopolymerizable compound＞ As the photopolymerizable compound, a known photopolymerizable compound used in a photoresist composition for a black matrix can be used, and examples thereof include monomers and oligomers having a photopolymerizable unsaturated bond. The said photopolymerizable compound can be used individually or in combination of 2 or more types.

作為具有1個光聚合性不飽和鍵的單體，例如可列舉：甲基丙烯酸甲酯、甲基丙烯酸丁酯、甲基丙烯酸2-乙基己酯、丙烯酸甲酯、丙烯酸丁酯、丙烯酸-2-乙基己酯等甲基丙烯酸烷基酯或丙烯酸烷基酯；甲基丙烯酸苄酯、丙烯酸苄酯等甲基丙烯酸芳烷基酯或丙烯酸芳烷基酯；甲基丙烯酸丁氧基乙酯、丙烯酸丁氧基乙酯等甲基丙烯酸烷氧基烷基酯或丙烯酸烷氧基烷基酯；甲基丙烯酸N,N-二甲胺基乙酯、丙烯酸N,N-二甲胺基乙酯等甲基丙烯酸胺基烷基酯或丙烯酸胺基烷基酯；二乙二醇單乙醚、三乙二醇單丁醚、二丙二醇單甲醚等聚烷二醇單烷基醚的甲基丙烯酸酯或丙烯酸酯；六乙二醇單苯醚等聚烷二醇單芳基醚的甲基丙烯酸酯或丙烯酸酯；甲基丙烯酸異莰酯或丙烯酸異莰酯；丙三醇甲基丙烯酸酯或丙三醇丙烯酸酯；甲基丙烯酸2-羥基乙酯或丙烯酸2-羥基乙酯等。As a monomer having one photopolymerizable unsaturated bond, for example, methyl methacrylate, butyl methacrylate, 2-ethylhexyl methacrylate, methyl acrylate, butyl acrylate, acrylic acid- Alkyl methacrylate or acrylate such as 2-ethylhexyl ester; aralkyl methacrylate or aralkyl acrylate such as benzyl methacrylate or benzyl acrylate; butoxyethyl methacrylate Alkoxyalkyl methacrylate or alkoxyalkyl acrylate such as butoxyethyl acrylate; N,N-dimethylaminoethyl methacrylate, N,N-dimethylaminoethyl acrylate Aminoalkyl methacrylate or aminoalkyl acrylate such as ethyl ester; form of polyalkylene glycol monoalkyl ether such as diethylene glycol monoethyl ether, triethylene glycol monobutyl ether, dipropylene glycol monomethyl ether, etc. Acrylates or acrylates; methacrylates or acrylates of polyalkylene glycol monoaryl ethers such as hexaethylene glycol monophenyl ether; isobornyl methacrylate or isobornyl acrylate; glycerol methacrylate ester or glycerol acrylate; 2-hydroxyethyl methacrylate or 2-hydroxyethyl acrylate, etc.

作為具有2個以上光聚合性不飽和鍵的單體，例如可列舉：雙酚A二甲基丙烯酸酯、1,4-丁二醇二甲基丙烯酸酯、1,3-丁二醇二甲基丙烯酸酯、二乙二醇二甲基丙烯酸酯、丙三醇二甲基丙烯酸酯、新戊二醇二甲基丙烯酸酯、聚乙二醇二甲基丙烯酸酯、聚丙二醇二甲基丙烯酸酯、四乙二醇二甲基丙烯酸酯、三羥甲基丙烷三甲基丙烯酸酯、新戊四醇三甲基丙烯酸酯、新戊四醇四甲基丙烯酸酯、二新戊四醇四甲基丙烯酸酯、二新戊四醇六甲基丙烯酸酯、二新戊四醇五甲基丙烯酸酯、雙酚A二丙烯酸酯、1,4-丁二醇二丙烯酸酯、1,3-丁二醇二丙烯酸酯、二乙二醇二丙烯酸酯、丙三醇二丙烯酸酯、新戊二醇二丙烯酸酯、聚乙二醇二丙烯酸酯、聚丙二醇二丙烯酸酯、四乙二醇二丙烯酸酯、三羥甲基丙烷三丙烯酸酯、新戊四醇三丙烯酸酯、新戊四醇四丙烯酸酯、二新戊四醇四丙烯酸酯、二新戊四醇六丙烯酸酯、二新戊四醇五丙烯酸酯等。Examples of monomers having two or more photopolymerizable unsaturated bonds include bisphenol A dimethacrylate, 1,4-butanediol dimethacrylate, 1,3-butanediol dimethyl Acrylate, Diethylene Glycol Dimethacrylate, Glycerol Dimethacrylate, Neopentyl Glycol Dimethacrylate, Polyethylene Glycol Dimethacrylate, Polypropylene Glycol Dimethacrylate , tetraethylene glycol dimethacrylate, trimethylolpropane trimethacrylate, neopentylthritol trimethacrylate, neopentylthritol tetramethacrylate, dipenteoerythritol tetramethyl Acrylates, diperythritol hexamethacrylate, diperythritol pentamethacrylate, bisphenol A diacrylate, 1,4-butanediol diacrylate, 1,3-butanediol Diacrylate, Diethylene Glycol Diacrylate, Glycerol Diacrylate, Neopentyl Glycol Diacrylate, Polyethylene Glycol Diacrylate, Polypropylene Glycol Diacrylate, Tetraethylene Glycol Diacrylate, Tri Methylolpropane Triacrylate, Neopentylthritol Triacrylate, Neopentylthritol Tetraacrylate, Di-Neopentylthritol Tetraacrylate, Di-Neopentylthritol Hexaacrylate, Di-Neopentylthritol Pentaacrylate Wait.

作為具有光聚合性不飽和鍵的低聚物，例如可列舉：使上述單體適當聚合所獲得的低聚物。As an oligomer which has a photopolymerizable unsaturated bond, the oligomer obtained by suitably polymerizing the said monomer is mentioned, for example.

上述光聚合性化合物於上述黑矩陣用光阻組成物的固體成分中優選為2～20質量%，更優選為4～15質量%。It is preferable that the said photopolymerizable compound is 2-20 mass % in the solid content of the said photoresist composition for black matrices, and it is more preferable that it is 4-15 mass %.

上述光聚合起始劑可使用黑矩陣用光阻組成物中所使用的公知光聚合起始劑，例如可列舉：二苯甲酮、N,N'-四乙基-4,4'-二胺基二苯甲酮、4-甲氧基-4'-二甲基胺基二苯甲酮、二苯基乙二酮、2,2-二乙氧基苯乙酮、安息香、安息香甲醚、安息香異丁醚、二苯二乙酮二甲基縮酮、α-羥基異丁基苯酮、9-氧硫𠮿

Figure 111108822-002
、2-氯9-氧硫𠮿
Figure 111108822-002
、1-羥基環己基苯基酮、第三丁基蒽醌、1-氯蒽醌、2,3-二氯蒽醌、3-氯-2-甲基蒽醌、2-乙基蒽醌、1,4-萘醌、1,2-苯并蒽醌（1,2-benzanthraquinone）、1,4-二甲基蒽醌、2-苯基蒽醌、三𠯤系光聚合起始劑、肟酯系光聚合起始劑等。上述光聚合起始劑可單獨使用或組合兩種以上使用。As the above-mentioned photopolymerization initiator, known photopolymerization initiators used in photoresist compositions for black matrices can be used, for example, benzophenone, N,N'-tetraethyl-4,4'-di Aminobenzophenone, 4-methoxy-4'-dimethylaminobenzophenone, diphenylethanedione, 2,2-diethoxyacetophenone, benzoin, benzoin methyl ether , Benzoin isobutyl ether, Diphenyldiphenone dimethyl ketal, α-Hydroxyisobutyl benzophenone, 9-Oxysulfur 𠮿
Figure 111108822-002
, 2-Chloro9-oxosulfur 𠮿
Figure 111108822-002
, 1-hydroxycyclohexyl phenyl ketone, tertiary butylanthraquinone, 1-chloroanthraquinone, 2,3-dichloroanthraquinone, 3-chloro-2-methylanthraquinone, 2-ethylanthraquinone, 1,4-Naphthoquinone, 1,2-Benzanthraquinone (1,2-Benzanthraquinone), 1,4-Dimethylanthraquinone, 2-Phenylanthraquinone, Trioxane photopolymerization initiator, Oxime Ester-based photopolymerization initiators, etc. The said photoinitiator can be used individually or in combination of 2 or more types.

上述光聚合起始劑於上述黑矩陣用光阻組成物的固體成分中優選為0.1～15質量%，更優選為1～10質量%。It is preferable that the said photoinitiator is 0.1-15 mass % in the solid content of the said photoresist composition for black matrices, and it is more preferable that it is 1-10 mass %.

從基於鹼性顯影液的顯影性的觀點而言，上述黑矩陣用光阻組成物也可進而添加上述鹼溶性樹脂。另外，上述鹼溶性樹脂總量於上述黑矩陣用光阻組成物的固體成分中優選為10質量%以上50質量%以下。另外，從提升塗裝性的觀點而言，上述黑矩陣用光阻組成物也可進而添加上述溶劑。上述溶劑總量於上述黑矩陣用光阻組成物中的比率優選為50質量%以上，更優選為70質量%以上。The above-mentioned photoresist composition for black matrices may further add the above-mentioned alkali-soluble resin from the viewpoint of developability by an alkaline developing solution. Moreover, it is preferable that the said alkali-soluble resin total amount is 10 mass % or more and 50 mass % or less in the solid content of the said photoresist composition for black matrices. Moreover, the said photoresist composition for black matrices may further add the said solvent from a viewpoint of improving coatability. The ratio of the total amount of the solvent to the photoresist composition for a black matrix is preferably 50% by mass or more, more preferably 70% by mass or more.

上述黑矩陣用光阻組成物中，也可進而視需要添加調平劑、抗氧化劑、消泡劑等添加劑。Additives such as a leveling agent, an antioxidant, and a defoamer may further be added to the above-mentioned photoresist composition for a black matrix.

關於上述黑矩陣用光阻組成物，使用攪拌裝置等對上述黑矩陣用顏料分散組成物、光聚合性化合物、及光聚合起始劑等各成分進行攪拌混合而製備即可。 [實施例] The photoresist composition for a black matrix may be prepared by stirring and mixing the components such as the pigment dispersion composition for a black matrix, the photopolymerizable compound, and the photopolymerization initiator using a stirring device or the like. [Example]

以下藉由實施例等對本發明進行說明，但本發明並非僅限定於該等。Hereinafter, although an Example etc. demonstrate this invention, this invention is not limited to these.

＜製備例A～E＞ ＜表面處理碳黑的準備＞ 將表1中所示的各種原料以成為表1中所示的摻合組成（質量份）的方式進行混合後，於室溫攪拌12小時。其後，進行抽氣過濾，之後，利用純化水反復洗淨，進行乾燥而獲得表面處理碳黑A～E。 ＜Preparation Examples A～E＞ ＜Preparation of carbon black for surface treatment＞ After mixing the various raw materials shown in Table 1 so as to have the blend composition (parts by mass) shown in Table 1, it was stirred at room temperature for 12 hours. Thereafter, suction filtration was performed, followed by repeated washing with purified water and drying to obtain surface-treated carbon blacks A to E.

[表1] 表面處理碳黑 A B C D E 材料 （質量份） TPK1104R 200 200 200 200 200 SS12000S - 6 6 6 6 ALFINE 83 20 200 20 - - 液體硫酸鋁 - - - 200 - 純化水 780 600 780 600 800 [Table 1] surface treatment carbon black A B C D. E. Material (parts by mass) TPK1104R 200 200 200 200 200 SS12000S - 6 6 6 6 ALFINE 83 20 200 20 - - Liquid Aluminum Sulfate - - - 200 - purified water 780 600 780 600 800

表1中，TPK1104R表示酸性碳黑（吸油量：38 ml/100 g，pH約3.0，Cabot公司製造）； SS12000S表示具有磺酸基的酞青系色素衍生物（Lubrizol公司製造）； ALFINE 83表示聚氯化鋁水溶液（按氧化鋁換算為23%，大明化學工業公司製造）； 液體硫酸鋁表示硫酸鋁水溶液（按氧化鋁換算為8%，大明化學工業公司製造）。 In Table 1, TPK1104R represents acid carbon black (oil absorption: 38 ml/100 g, pH about 3.0, manufactured by Cabot); SS12000S means a phthalocyanine pigment derivative with a sulfonic acid group (manufactured by Lubrizol); ALFINE 83 means polyaluminum chloride aqueous solution (23% based on alumina conversion, manufactured by Daming Chemical Industry Company); Liquid aluminum sulfate refers to an aqueous solution of aluminum sulfate (8% in terms of alumina conversion, manufactured by Daemyung Chemical Industry Co., Ltd.).

＜實施例1-1～4-1、比較例1-1～2-1＞ ＜黑矩陣用顏料分散組成物的製備＞ 將表2中所示的各種原料以成為表2中所示的摻合組成（質量%）的方式進行混合後，利用珠磨機進行碾磨，製備各製備例及比較製備例的黑矩陣用顏料分散組成物。 <Examples 1-1 to 4-1, Comparative Examples 1-1 to 2-1> ＜Preparation of pigment dispersion composition for black matrix＞ After mixing the various raw materials shown in Table 2 to become the blending composition (mass %) shown in Table 2, they were ground with a bead mill to prepare black matrices for each preparation example and comparative preparation example. Pigment dispersion composition.

[表2]    實施例1-1 實施例2-1 實施例3-1 實施例4-1 比較例1-1 比較例2-1 碳黑 表面處理碳黑A 25.0 - - - - - 表面處理碳黑B - 25.0 - - - - 表面處理碳黑C - - 25.0 - - - 表面處理碳黑D - - - 25.0 - - 表面處理碳黑E - - - - 25.0 - TPK1104R - - - - - 25.0 含有鹼性基的顏料分散劑 DB167（固體成分52%） 4.8 4.8 4.8 4.8 4.8 4.8 含有酸性基的顏料分散助劑 SS12000S 0.8 0.8 0.8 0.8 0.8 0.8 環氧樹脂 VG3101L 2.5 2.5 2.5 2.5 2.5 2.5 鹼溶性樹脂 ZCR-1569H（固體成分69%） 3.6 3.6 3.6 3.6 3.6 3.6 有機溶劑 PGMEA 63.3 63.3 63.3 63.3 63.3 63.3 總計 100.0 100.0 100.0 100.0 100.0 100.0 [Table 2] Example 1-1 Example 2-1 Example 3-1 Example 4-1 Comparative example 1-1 Comparative example 2-1 carbon black Surface Treatment Carbon Black A 25.0 - - - - - Surface Treatment Carbon Black B - 25.0 - - - - Surface treatment carbon black C - - 25.0 - - - Surface Treatment Carbon Black D - - - 25.0 - - Surface Treatment Carbon Black E - - - - 25.0 - TPK1104R - - - - - 25.0 Pigment dispersants with basic groups DB167 (solid content 52%) 4.8 4.8 4.8 4.8 4.8 4.8 Pigment Dispersion Aids Containing Acidic Groups SS12000S 0.8 0.8 0.8 0.8 0.8 0.8 epoxy resin VG3101L 2.5 2.5 2.5 2.5 2.5 2.5 Alkali soluble resin ZCR-1569H (solid content 69%) 3.6 3.6 3.6 3.6 3.6 3.6 Organic solvents PGMEA 63.3 63.3 63.3 63.3 63.3 63.3 total 100.0 100.0 100.0 100.0 100.0 100.0

表2中，DB167表示具有聚酯鏈的含有胺基的聚胺酯系高分子分散劑（BYK-Chemie公司製造，固體成分52質量%）； SS12000S表示具有磺酸基的酞青系色素衍生物（Lubrizol公司製造）； VG3101L表示環氧樹脂（固體成分100%，Printec公司製造）； ZCR-1569H表示具有聯苯骨架的鹼溶性環氧(甲基)丙烯酸酯樹脂（固體成分69%，日本化藥公司製造）； PGMEA表示丙二醇單甲醚乙酸酯。 In Table 2, DB167 represents an amine-containing polyurethane-based polymer dispersant having a polyester chain (manufactured by BYK-Chemie, solid content 52% by mass); SS12000S means a phthalocyanine pigment derivative with a sulfonic acid group (manufactured by Lubrizol); VG3101L means epoxy resin (100% solid content, manufactured by Printec); ZCR-1569H represents an alkali-soluble epoxy (meth)acrylate resin with a biphenyl skeleton (solid content 69%, manufactured by Nippon Kayaku); PGMEA stands for propylene glycol monomethyl ether acetate.

＜實施例1-2～4-2、比較例1-2～2-2＞ ＜黑矩陣用光阻組成物的製備＞ 將表3中所示的各種原料以成為表3中所示的摻合組成（質量%）的方式，使用高速攪拌機進行混合後，利用孔徑0.5 μm的過濾器進行過濾，製備各實施例及比較例的黑矩陣用光阻組成物。 <Examples 1-2 to 4-2, Comparative Examples 1-2 to 2-2> ＜Preparation of photoresist composition for black matrix＞ Various raw materials shown in Table 3 were mixed using a high-speed mixer so that the blend composition (mass %) shown in Table 3 was obtained, and then filtered through a filter with a pore size of 0.5 μm to prepare each example and comparison Example of a photoresist composition for a black matrix.

＜黑色光阻膜的細線密接性的評價＞ 利用旋轉塗布機將實施例及比較例中所製造的各黑矩陣用光阻組成物以成為膜厚1 μm的方式塗布在玻璃基板（EAGLE XG）上，於100℃預烤3分鐘。接著，對於1 μm至20 μm的線寬，使用具有1 μm間隔的線圖的光罩，使用高壓水銀燈，以UV累計光量100 mJ/cm 2曝光。其後，於23℃、0.05%氫氧化鉀水溶液中，以1 kgf/cm 2的噴淋顯影（shower development）壓力，從顯影圖案開始出現的時間（顯影點）起開始顯影，於成為顯影點的2倍的時間時結束顯影，進行1 kgf/cm 2壓力的噴霧水洗。對玻璃基板上殘存的最小線圖的尺寸（μm）進行評價。將結果示於表3。 <Evaluation of thin-line adhesion of black resist film> Each resist composition for black matrix produced in Examples and Comparative Examples was coated on a glass substrate (EAGLE XG) with a film thickness of 1 μm using a spin coater On, pre-bake at 100°C for 3 minutes. Next, for a line width of 1 μm to 20 μm, using a mask having a line pattern at 1 μm intervals, exposure was performed at a UV cumulative light intensity of 100 mJ/cm 2 using a high-pressure mercury lamp. Thereafter, at 23°C, in 0.05% potassium hydroxide aqueous solution, with a shower development pressure of 1 kgf/cm 2 , the development starts from the time when the development pattern starts to appear (development point), and becomes the development point The development is finished at twice the time, and spray water washing with a pressure of 1 kgf/cm 2 is carried out. The size (μm) of the smallest line pattern remaining on the glass substrate was evaluated. The results are shown in Table 3.

[表3]    實施例1-2 實施例2-2 實施例3-2 實施例4-2 比較例1-2 比較例2-2 顏料分散組成物 實施例1-1 51 - - - - - 實施例2-1 - 51 - - - - 實施例3-1 - - 51 - - - 實施例4-1 - - - 51 - - 比較例1-1 - - - - 51 - 比較例2-1 - - - - - 51 光聚合起始劑 OXE02 1 1 1 1 1 1 光聚合性化合物 DPHA 2 2 2 2 2 2 鹼溶性樹脂 WR-301（固體成分44%） 4 4 4 4 4 4 有機溶劑 PGMEA 42 42 42 42 42 42 總計 100 100 100 100 100 100 評價結果 密接性（μm） 7 7 7 7 13 14 [table 3] Example 1-2 Example 2-2 Example 3-2 Example 4-2 Comparative example 1-2 Comparative example 2-2 Pigment Dispersion Composition Example 1-1 51 - - - - - Example 2-1 - 51 - - - - Example 3-1 - - 51 - - - Example 4-1 - - - 51 - - Comparative example 1-1 - - - - 51 - Comparative example 2-1 - - - - - 51 Photopolymerization initiator OXE02 1 1 1 1 1 1 photopolymerizable compound DPHA 2 2 2 2 2 2 Alkali soluble resin WR-301 (solid content 44%) 4 4 4 4 4 4 Organic solvents PGMEA 42 42 42 42 42 42 total 100 100 100 100 100 100 Evaluation results Adhesiveness (μm) 7 7 7 7 13 14

表3中，DPHA表示二新戊四醇六丙烯酸酯； OXE02表示肟酯系光聚合起始劑（BASF JAPAN公司製造）； WR-301表示鹼溶性卡多樹脂（固體成分44%，ADEKA公司製造）； PGMEA表示丙二醇單甲醚乙酸酯。 In Table 3, DPHA represents diperythritol hexaacrylate; OXE02 represents an oxime ester photopolymerization initiator (manufactured by BASF JAPAN); WR-301 represents alkali-soluble cardo resin (solid content 44%, manufactured by ADEKA); PGMEA stands for propylene glycol monomethyl ether acetate.

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Claims (8)

一種黑矩陣用顏料分散組成物，其含有：碳黑、含有鹼性基的顏料分散劑、含有酸性基的顏料分散助劑、環氧樹脂、鹼溶性樹脂、及溶劑， 上述碳黑為經無機鋁鹽處理的表面處理碳黑。 A pigment dispersion composition for a black matrix, which contains: carbon black, a pigment dispersant containing an alkaline group, a pigment dispersion aid containing an acidic group, an epoxy resin, an alkali-soluble resin, and a solvent, The above-mentioned carbon black is a surface-treated carbon black treated with an inorganic aluminum salt. 如請求項1之黑矩陣用顏料分散組成物，其中，上述無機鋁鹽為選自由氯化鋁及硫酸鋁所組成的群中的一種以上。The pigment dispersion composition for black matrix according to Claim 1, wherein the above-mentioned inorganic aluminum salt is at least one selected from the group consisting of aluminum chloride and aluminum sulfate. 如請求項1或2之黑矩陣用顏料分散組成物，其中，上述碳黑為酸性碳黑。The pigment dispersion composition for black matrix according to claim 1 or 2, wherein the carbon black is acidic carbon black. 如請求項1或2之黑矩陣用顏料分散組成物，其中，上述環氧樹脂為具有芳香環的多官能環氧樹脂。The pigment dispersion composition for black matrix according to claim 1 or 2, wherein the above-mentioned epoxy resin is a polyfunctional epoxy resin having an aromatic ring. 如請求項1或2之黑矩陣用顏料分散組成物，其中，上述鹼溶性樹脂為具有聯苯骨架的鹼溶性環氧(甲基)丙烯酸酯樹脂。The pigment dispersion composition for a black matrix according to claim 1 or 2, wherein the above-mentioned alkali-soluble resin is an alkali-soluble epoxy (meth)acrylate resin having a biphenyl skeleton. 如請求項1或2之黑矩陣用顏料分散組成物，其中，上述含有酸性基的顏料分散助劑具有酞青骨架。The pigment dispersion composition for black matrix according to claim 1 or 2, wherein the above-mentioned acidic group-containing pigment dispersion aid has a phthalocyanine skeleton. 一種黑矩陣用光阻組成物，其含有：請求項1至6中任一項之黑矩陣用顏料分散組成物、光聚合性化合物、及光聚合起始劑。A photoresist composition for a black matrix, which contains: the pigment dispersion composition for a black matrix according to any one of claims 1 to 6, a photopolymerizable compound, and a photopolymerization initiator. 一種黑色光阻膜，其係使用請求項7之黑矩陣用光阻組成物而獲得。A black photoresist film obtained by using the photoresist composition for a black matrix of claim 7.
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