阅读说明：本技术 一种有机硅改性丙烯酸酯类光刻胶及其制备方法 (Organic silicon modified acrylate photoresist and preparation method thereof ) 是由 刘兴江 魏柳荷 吴林志 张文英 于 2019-01-05 设计创作，主要内容包括：本发明涉及一种有机硅改性丙烯酸酯类光刻胶及其制备方法,属于胶黏剂技术领域。以质量百分数计算,由以下组份组成：成膜树脂14.2～23.7份,交联剂4.2～7.5份,光引发剂0.8～1.4份,助剂0.06～0.13份,溶剂67.3～80.7份。本发明的光刻胶,利用有机硅对成膜树脂进行改性,增强了其与基材的粘接性,同时也降低了光刻胶的脆性,制备的光刻胶附着力好、分辨率高,在液晶显示屏的制备过程中有着很好的应用前景。(The invention relates to an organic silicon modified acrylate photoresist and a preparation method thereof, belonging to the technical field of adhesives. The coating consists of the following components in percentage by mass: 14.2-23.7 parts of film-forming resin, 4.2-7.5 parts of cross-linking agent, 0.8-1.4 parts of photoinitiator, 0.06-0.13 part of auxiliary agent and 67.3-80.7 parts of solvent. According to the photoresist disclosed by the invention, the film-forming resin is modified by using the organic silicon, so that the adhesion between the film-forming resin and a base material is enhanced, meanwhile, the brittleness of the photoresist is also reduced, and the prepared photoresist is good in adhesive force, high in resolution and good in application prospect in the preparation process of a liquid crystal display screen.)

1. An organic silicon modified acrylate photoresist and a preparation method thereof are characterized by comprising the following raw materials in parts by weight:

14.2 to 23.7 parts of film-forming resin

4.2-7.5 parts of cross-linking agent

0.8-1.4 parts of photoinitiator

0.06-0.13 part of assistant

67.3-80.7 parts of solvent

The film-forming resin is prepared from an acrylic acid derivative monomer by a solution free radical polymerization method, and specifically has the following structural general formula:(m, n, o, p, q indicate the degree of polymerization);

wherein, the cross-linking agent is acrylic acid derivative monomer with the functionality of more than 2, more than two of the acrylic acid derivative monomers are mixed for use, and the specific structure is as follows:

wherein the photoinitiator is one or two of hexaarylbiimidazole, benzophenone and benzoin dimethyl ether;

wherein the auxiliary agent is one of a fluorine modified leveling agent KMT-1020 and a silicon polyether modified leveling agent ZY-8533;

wherein the solvent is butanone, isopropanol and ethylene glycol monomethyl ether, and one or more of the solvents are mixed for use.

2. The silicone-modified methacrylate photoresist of claim 1, wherein the film-forming resin is a monomerThe preparation method is characterized in that N- (3- (3-methoxy silicon) -propyl) -acrylamide and N- (3- (3-ethoxy silicon) -propyl) -acrylamide are introduced as organosilicon modifier, and one or two of the organosilicon modifier are mixed for use.

3. The organosilicon modified methacrylate photoresist as claimed in claim 2, wherein the film-forming resin is prepared by the following method: (a) adding a solvent (butanone, isopropanol or ethylene glycol monomethyl ether) and a mixed monomer of methacrylic acid, methyl methacrylate and phenyl methacrylate into a reaction kettle provided with a mechanical stirring and condensing reflux pipe, heating to 87 ℃, adding an initiator, and reacting for 40 minutes; (b) adding a solvent (butanone, isopropanol or ethylene glycol monomethyl ether), methacrylic acid, a mixed monomer of methyl methacrylate and phenyl methacrylate and an initiator, and reacting for 3 hours; (c) adding a mixed monomer of a solvent (butanone, isopropanol or ethylene glycol monomethyl ether), N- (3- (3-methoxylsilane) -propyl) -acrylamide and N- (3- (3-ethoxylsilane) -propyl) -acrylamide and an initiator, and continuously reacting for 8 hours; (d) the reaction is stopped and the film-forming resin is obtained after post-treatment.

Technical Field

The invention relates to an organic silicon modified acrylate photoresist and a preparation method thereof, belonging to the technical field of adhesives.

Background

Photoresists, also known as photoresists, are key materials for microfabrication technology in the electronics industry and are mainly used in the fabrication of integrated circuits, semiconductor separators, and flat panel displays in the electronics industry. The photoresist, in short, is excited by a light source to undergo a chemical reaction, which results in a change in molecular structure and thus a change in solubility in a particular solution. The solubility of the photoresist in a particular solution increases under the excitation of a light source, which is referred to as a positive photoresist, and vice versa, as a negative photoresist. At present, the photoresist produced in China mainly meets the requirements of middle and low-end markets, the high-grade photoresist mainly depends on import, and the production technology of the high-grade photoresist is mainly monopolized by Korea and Japan. Methacrylic acid photoresist is a traditional photoresist, and has the defects of low resolution, high brittleness, poor adhesion with a base material and the like. The invention mainly utilizes organic silicon to modify the photoresist, and overcomes the defects of the traditional acrylate photoresist.

Disclosure of Invention

The invention aims to provide an organic silicon modified acrylate photoresist and a preparation method thereof.

The invention relates to an organic silicon modified acrylate photoresist which is prepared from the following raw materials in parts by weight:

14.2 to 23.7 parts of film-forming resin

4.2-7.5 parts of cross-linking agent

0.8-1.4 parts of photoinitiator

0.06-0.13 part of assistant

67.3-80.7 parts of solvent

The film-forming resin of the present invention has the following general structural formula (m, n, o, p, q refer to the degree of polymerization):

the film-forming resin is prepared from acrylic monomers by a solution free radical polymerization method, wherein the monomers are as follows:

the preparation process comprises the following steps: (a) adding a solvent (butanone, isopropanol or ethylene glycol monomethyl ether), a mixed monomer of methacrylic acid, methyl methacrylate and phenyl methacrylate into a reaction kettle provided with a mechanical stirring and condensing reflux pipe, heating to 87 ℃, adding an initiator, and reacting for 40 minutes; (b) adding a solvent (butanone, isopropanol or ethylene glycol monomethyl ether), a mixed monomer of methacrylic acid, methyl methacrylate and phenyl methacrylate and an initiator, and reacting for 3 hours; (c) adding a mixed monomer of a solvent (butanone, isopropanol or ethylene glycol monomethyl ether), N- (3- (3-methoxylsilane) -propyl) -acrylamide and N- (3- (3-ethoxylsilane) -propyl) -acrylamide and an initiator, and continuously reacting for 8 hours; (d) stopping heating, cooling to room temperature, and performing post-treatment to obtain the film-forming resin.

The organosilicon modifier N- (3- (3-methoxylsilane) -propyl) -acrylamide and N- (3- (3-ethoxylsilane) -propyl) -acrylamide are prepared according to the following routes:

the preparation method comprises the following steps: (a) dissolving acrylic acid and 3- (methyl/ethoxy silicon) -propyl-1-amine in dry dichloromethane, and stirring for 10 minutes in an ice water bath; (b) adding Dicyclohexylcarbodiimide (DCC) into a reaction bottle, and reacting for 3 hours at 0 ℃; (c) the ice-water bath was removed, the reaction mixture was allowed to react at room temperature for 1 hour, and then the reaction mixture was poured into ice-water, filtered, and the solvent was distilled off under reduced pressure to give N- (3- (3-methyl/ethoxysilyl) -propyl) -acrylamide.

The cross-linking agent is an acrylic acid derivative monomer with the functionality of more than 2, more than two of the acrylic acid derivative monomers are mixed for use, and the specific structure is as follows:

the photoinitiator is one or two of hexaarylbiimidazole, benzophenone and benzoin dimethyl ether which are mixed for use.

The auxiliary agent is one of a fluorine modified leveling agent KMT-1020 and a silicon polyether modified leveling agent ZY-8533.

The solvent is butanone, isopropanol and ethylene glycol monomethyl ether, and one or more of the solvents are mixed for use.

The weight average polymer molecular weight of the film forming resin prepared by the invention is Mw.45000.

The photoresist of the invention is exposed by a contact exposure method using an SBG-type exposure machine (3000W ultraviolet lamp).

The technological process of the photoresist comprises the following steps: gluing, pre-baking, exposing, developing, hardening, etching and removing the film.

The photoresist has good adhesion with a base material, low brittleness and high resolution.

Detailed description of the preferred embodiment