CA3024242A1 - High concentration developer liquid composition - Google Patents

High concentration developer liquid composition Download PDF

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Publication number
CA3024242A1
CA3024242A1 CA3024242A CA3024242A CA3024242A1 CA 3024242 A1 CA3024242 A1 CA 3024242A1 CA 3024242 A CA3024242 A CA 3024242A CA 3024242 A CA3024242 A CA 3024242A CA 3024242 A1 CA3024242 A1 CA 3024242A1
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Prior art keywords
acid
concentration developer
surfactant
composition according
purity water
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Abandoned
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CA3024242A
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French (fr)
Inventor
Tao Wang
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Individual
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Individual
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    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03FPHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26Processing photosensitive materials; Apparatus therefor
    • G03F7/30Imagewise removal using liquid means
    • G03F7/32Liquid compositions therefor, e.g. developers
    • G03F7/322Aqueous alkaline compositions

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Photosensitive Polymer And Photoresist Processing (AREA)
  • Exposure Of Semiconductors, Excluding Electron Or Ion Beam Exposure (AREA)

Abstract

The invention discloses a high concentration developer liquid stock composition, and the components used and the mass percentage thereof are: 1-45% of a special structure surfactant, 0.1-50% of a dissolution aid, and 0.1-25 of an inorganic base %, high purity water 30-99.9%, the sum of the component content percentage is 100%.
The utility model has the beneficial effects that the high-concentration developer liquid composition contains a special structure surfactant, has the characteristics of no residue, high development pattern precision, and the comprehensive performance reaches or exceeds the existing developer product.

Description

High concentration developer liquid composition Technical field The present invention relates to the field of photoresist developer solutions, and more particularly to a high concentration developer solution stock solution.
Background technique Due to its small size, light weight, low radiation, low power consumption, and full color, liquid crystal displays have been widely applied to various display terminals, and will continue to be the mainstream products in the display field for a long time in the present and future. As a key component of colorization of liquid crystal displays, color filters directly affect the contrast, brightness, viewing angle and even picture quality of the display.
The basic structure of the color filter is composed of a glass substrate, a black matrix, a color layer, a protective layer, and an ITO conductive film. The color filter is produced on the glass substrate, and the red, green, and blue primary color organic materials are produced in each. In one pixel, printing, dyeing, pigment dispersion, electrophoresis, dry film, etc. have appeared in the history of color filter production. However, the current mainstream method is pigment dispersion, in which pigment dispersion type color photoresist is formed. The raw material of the color layer, the color layer preparation process of the pigment dispersion method is to first apply the pigment dispersion type photoresist on the glass substrate of the formed black matrix, and repeat it by soft baking, exposure alignment, development, hard baking, and repetition. This process three times to form three colors of red, green and blue.
Patent US2006/0166147A1 relates to a high concentration color filter developer containing an alkaline component, a special structure of nonionic surfactant, an organic acid or a carboxylate and water, but the developer is present. The development is incomplete, the developer has a residue, and the like, and the patent CN105093862A relates to a surfactant and a developer which can be used for a color filter negative photoresist, the developer containing a block type polyether non-ion Exciting, is a polyoxyethylene-polyoxypropylene block copolymer, the developer also contains a strong base and purified water, which develops serious bubbles during development, especially in the sputtering development process. Such problems, resulting in a reduction in the development effect.
Summary of the invention It is an object of the present invention to provide a high concentration developer solution composition containing a special structure of a nonionic surfactant which has an excellent wet cleaning effect and can effectively reduce residue, surface contamination, etc. after development. , obtaining a high-precision development pattern, which also contains a special dissolution aid, in the process of preparing a higher concentration of the developer liquid solution, keeping the developer liquid solution uniform, without delamination, and the dissolution aid can also Enhance the development effect.
In order to achieve the above object, a high concentration developer solution composition is provided, and the components used and their mass percentages are: 1-45% of a surfactant having a special structure, 0.1-50% of a dissolution aid, and 0.1 by an inorganic base. -25%, high purity water 30-99.9%, and the sum of the component content percentages is 100%.
The components used in the high-concentration developer stock composition and the mass percentage thereof are: 3% of a surfactant having a special structure, 12% of a dissolution aid, 4% of an inorganic base, and 81% of high-purity water.
The components used in the high-concentration developer stock composition and the mass percentage thereof are: a surfactant having a specific structure of 15%, a dissolution aid of 6%, an inorganic base of 10%, and a high-purity water of 69%.
The surfactant of the specific structure is a nonionic surfactant having the following structural formula (I).
, m H
( I ) In the formula (I), m is 0-4, n is 3-30, m and n are integers, and R is hydrogen or methyl. The surfactant structure may contain both hydrogen and methyl groups.
The dissolution aid is an organic amine, an organic acid, a polyol or an alcohol ether solvent; wherein the organic amine is ethanolamine, isopropanolamine, diethanolamine, diglycolamine, triethanolamine, diethylenetriamine, polyethene One or more of polyamines; the organic acid is one or more of acetic acid, propionic acid, caproic acid, caprylic acid, salicylic acid, ascorbic acid, iminodiacetic acid, ethylenediaminetetraacetic acid; One or more of alcohol, propylene glycol, glycerol, butylene glycol; alcohol ether solvent is ethylene glycol butyl ether, diethylene glycol butyl ether, diethylene glycol methyl ether, propylene glycol methyl ether, dipropylene glycol One or several of ethers.
The addition of the dissolution aid can enhance the solubility of the surfactant in the solution, and prepare a uniform stable high concentration developer solution.
The inorganic base is one or more of potassium hydroxide, sodium hydroxide, lithium hydroxide, sodium
2 carbonate, potassium carbonate, sodium hydrogencarbonate, and sodium silicate.
The high purity water is deionized water having a resistance value greater than 18 MS-2/cm.
The high-concentration developer liquid composition of the present invention only needs to add the above composition to the stirring and dissolve, and the phenomenon of strong alkali exotherm is controlled in the dissolution process, the temperature of the whole dissolution process is controlled below 30 degrees, and the dissolution is completed after 0.1. The filter element of p.m can be filtered.
The high concentration developer solution composition of the invention needs to be diluted and used, the dilution factor is 5-600 times, and the pH of the solution after dilution is controlled between 9-14. The high concentration developer solution composition of the invention is in use. There are no special restrictions, and it can be immersed or sprayed.
The utility model has the beneficial effects that the high-concentration developer liquid composition contains a special structure surfactant, has the characteristics of no residue, high development pattern precision, and the comprehensive performance reaches or exceeds the existing developer product.
Detailed descriptions A high concentration developer liquid stock composition, the components used and the mass percentage thereof are: 1-45% of a special structure surfactant, 0.1-50% of a dissolution aid, 0.1-25% of an inorganic base, and 30%
of high purity water. -99.9%, the sum of the component content percentages is 100%.
The components used in the high-concentration developer stock composition and the mass percentage thereof are: 3% of a surfactant having a special structure, 12% of a dissolution aid, 4% of an inorganic base, and 81% of high-purity water.
The components used in the high-concentration developer stock composition and the mass percentage thereof are: a surfactant having a specific structure of 15%, a dissolution aid of 6%, an inorganic base of 10%, and a high-purity water of 69%.
The surfactant of the specific structure is a nonionic surfactant having the following structural formula (I).
m )H
( I ) In the formula (I), m is 0-4, n is 3-30, m and n are integers, and R is hydrogen or methyl. The surfactant structure may contain both hydrogen and methyl groups.
3 The dissolution aid is an organic amine, an organic acid, a polyol or an alcohol ether solvent; wherein the organic amine is ethanolamine, isopropanolamine, dieth anol amine, d igl ycol amine, trieth anolamine, diethylenetriamine, polyethene One or more of polyamines; the organic acid is one or more of acetic acid, propionic acid, caproic acid, caprylic acid, salicylic acid, ascorbic acid, iminodiacetic acid, ethylenediaminetetraacetic acid; One or more of alcohol, propylene glycol, glycerol, butylene glycol; alcohol ether solvent is ethylene glycol butyl ether, diethylene glycol butyl ether, diethylene glycol methyl ether, propylene glycol methyl ether, dipropylene glycol One or several of ethers.
The addition of the dissolution aid can enhance the solubility of the surfactant in the solution, and prepare a uniform stable high concentration developer solution.
The inorganic base is one or more of potassium hydroxide, sodium hydroxide, lithium hydroxide, sodium carbonate, potassium carbonate, sodium hydrogencarbonate, and sodium silicate.
The high purity water is deionized water having a resistance value greater than 18 MS/cm.
There may be various specific combinations of the types and ratios of the components in the high-concentration developer liquid composition of the present invention. The present invention will be further described in detail below by way of specific examples, and the comparison with the comparative examples will be described. Advantages of the invention.
In the high concentration developer solution composition of the present invention, in Example 1, the mass percentage of the nonionic surfactant represented by the formula (I) is 3%;
the solvent auxiliary agent is propylene glycol, and the mass percentage thereof is 12%; The base is potassium hydroxide, the mass percentage thereof is
4%; the high purity water mass percentage is 81%, wherein m is 3, n is 25, and R is hydrogen.
In the high concentration developer solution composition of the present invention, in Example 2, the mass percentage of the nonionic surfactant represented by the formula (I) is 15%;
the solvent auxiliary is caproic acid, and the mass percentage thereof is 6%; The inorganic base is potassium hydroxide in a mass percentage of 10%;
the high purity water is 69% by mass, wherein m is 2, n is 18, and R is hydrogen and methyl.
In the high concentration developer solution composition of the present invention, in Example 3, the mass percentage of the nonionic surfactant represented by the formula (I) is 8%;
the solvent auxiliary is diethylene glycol butyl ether, and the mass percentage thereof 2%; the inorganic base is potassium hydroxide, the mass percentage is 2%; the high purity water mass percentage is 88%, wherein m is 2, n is 12, and R is hydrogen.
In the high concentration developer solution composition of the present invention, in Example 4, the mass percentage of the nonionic surfactant represented by the formula (I) is 5%;
the solvent auxiliary is isopropanolamine, and the mass percentage thereof is 22. %; inorganic base is sodium carbonate and sodium hydrogencarbonate, sodium carbonate is 5% by mass, sodium hydrogencarbonate is 1% by mass; high purity water is 67% by mass, wherein m is 1, n is 20, and R is hydrogen.
In the high concentration developer solution composition of the present invention, in Example 5, the mass percentage of the nonionic surfactant represented by the formula (I) is 25%;
the solvent auxiliary is iminodiacetic acid, and the mass percentage thereof is 1. %; inorganic base is sodium carbonate, the mass percentage is 15%;
high purity water mass percentage is 59%, wherein m is 3, n is 15, and R is methyl.
Hereinafter, the advantages of the high-concentration developer stock composition of the present invention will be specifically described by a test comparison, and a high-concentration developer stock composition of the following composition is used as a comparative example:
In Comparative Example 1, 15% by mass of a nonionic surfactant represented by the formula (I), 10% by mass of potassium hydroxide, and 75% by mass of high-purity water were sequentially added to a stirring solution, and the temperature of the entire dissolution process was controlled. After 30 degrees or less, the solution was completely filtered and filtered with a 0.1 pm filter to prepare a high concentration developer solution composition, wherein m was 2, n was 18, and R was hydrogen and methyl.
In Comparative Example 2, 3% by mass of a nonionic surfactant represented by the formula (I), 10% by mass of potassium hydroxide, and 87% by mass of high-purity water were sequentially added to a stirring solution, and the temperature of the entire dissolution process was controlled. After 30 degrees or less, the solution was completely filtered and filtered with a 0.1 gm filter to prepare a high concentration developer solution composition, wherein m was 2, n was 18, and R was hydrogen and methyl.
In Comparative Example 3, 10% by mass of potassium hydroxide and 90% by mass of high-purity water were sequentially added to stir and dissolve, and the temperature of the whole dissolution process was controlled to be 30 degrees or less. After the dissolution was completed, the filter was filtered with a 0.1 pm filter to prepare a high-concentration developer. Stock solution.
In order to further investigate the development effect of the high-concentration developer liquid composition of the present invention, the following technical means is employed: a negative-color color photoresist of a certain thickness is spin-coated on a 10 cm x 10 cm glass substrate, and is carried out in an oven at 120 C. 80s pre-baked, and then exposed by using a pattern mask. After the exposure is completed, the above-mentioned Example 1, Example 2, Example 3, Example 4, Example 5, Comparative Example 1, and Comparative Example were respectively diluted by a certain multiple. 2. The high-concentration developer stock solution composition of Comparative Example 3 was developed, and after development treatment, it was washed with high-purity water, then dried with nitrogen, and hard baked in an oven at 220 C, and observed by an optical microscope and an electron microscope to confirm development. effect. The properties of the high-concentration developer stock solution of the above-mentioned Example 1, Example 2, Example 3, Example 4, Example 5 and Comparative Example 1, Comparative Example 2, and Comparative Example 3, and the development effect after dilution are as shown in Table 1. Show:
Table 1 Solution properties Developing effect Dilution factor (5-35 C) Residue Graphic edge Example 1 Dissolved uniformity 80 no Innocent Example 2 Dissolved uniformity 200 no Innocent Example 3 Dissolved uniformity 20 no Innocent Example 4 Dissolved uniformity 120 no Innocent Example 5 Dissolved uniformity 60 no Innocent Comparative Layering 200 Have have flaws example 1 Comparative Dissolved uniformity 200 Have have flaws example 2 Comparative Dissolved uniformity 200 Have have flaws example 3 As can be seen from Table 1, the high-concentration developer stock composition of the present invention can obtain a solution having a uniform solubility in the range of 5-35 C as shown in Examples 1-5, and the development effect after dilution indicates that no Residue, clear-cut development results, compared with Example 2, Comparative Example 1 could not obtain a uniformly dissolved solution because it did not contain a dissolution aid, and there was a phenomenon that residue and pattern were unclear after development, Comparative Example 2 The surfactant content is low, and a solution with uniform dissolution can be obtained.
However, after the same multiple dilution, no residue and high-precision clear pattern can be obtained.
Comparative Example 3 contains only potassium hydroxide, and no residue and high precision are obtained. Clear graphics.
In summary, the progress of the present invention is to provide a high concentration developer solution composition containing a special structure of a surfactant, a dissolution aid, an inorganic base and high purity water, which is suitable for use in TFT-LCD process color filter process in the development of color photoresist, large operating window, no residue after development, clear graphics, can get high-precision patterns, its development effect meets or exceeds the current imported color filter developer.
The basic principles, main features and advantages of the present invention have been shown and described above. It should be understood by those skilled in the art that the present invention is not limited by the foregoing embodiments, and that the present invention is only described in the foregoing description and the description of the present invention, without departing from the spirit and scope of the invention. Various changes and modifications are intended to be included within the scope of the invention as claimed.

Claims (3)

Claims
1 A
high concentration developer solution composition characterized in that each component used and its mass percentage are: 1-45% of a surfactant having a special structure, 0.1-50% of a dissolution aid, and 0.1-25 of an inorganic base. %, high purity water 30-99.9%, the sum of the component content percentage is 100%.
2 . The high-concentration developer stock composition according to claim 1 , wherein each component used and its mass percentage are: 3% of a special structure surfactant, 12% of a dissolution aid, Inorganic alkali 4%, high purity water 81%.
3. A high concentration developer solution composition according to claim 1, wherein each component used and its mass percentage are: 15% of a surfactant having a specific structure, 6% of a dissolution aid, Inorganic base 10%, high purity water 69%.
The high-concentration developer stock composition according to any one of claims 1 to 3, wherein the surfactant of the specific structure is a nonionic surface having the following structural formula (I). Active agent, In the formula (I), m is 0-4, n is 3-30, m and n are integers, and R is hydrogen or methyl. The surfactant structure may contain both hydrogen and methyl groups.
The high-concentration developer liquid composition according to any one of claims 1 to 3, wherein the dissolution aid is an organic amine, an organic acid, a polyol or an alcohol ether solvent; The organic amine is one or more of ethanolamine, isopropanolamine, diethanolamine, diglycolamine, triethanolamine, diethylenetriamine, polyethene polyamine; the organic acid is acetic acid, propionic acid, caproic acid, octanoic acid, One or more of salicylic acid, ascorbic acid, iminodiacetic acid, ethylenediaminetetraacetic acid; polyhydric alcohol is one or more of ethylene glycol, propylene glycol, glycerol, butanediol; alcohol ether solvent It is one or more of ethylene glycol butyl ether, diethylene glycol butyl ether, diethylene glycol methyl ether, propylene glycol methyl ether, and dipropylene glycol methyl ether.
The high concentration developer solution composition according to any one of claims 1 to 3, wherein the inorganic base is potassium hydroxide, sodium hydroxide, lithium hydroxide, sodium carbonate or potassium carbonate. One or more of sodium bicarbonate and sodium silicate.
The high-concentration developer stock solution composition according to any one of claims 1 to 3, wherein the high-purity water is deionized water having a resistance value of more than 18 M.OMEGA./cm.
CA3024242A 2018-09-18 2018-11-15 High concentration developer liquid composition Abandoned CA3024242A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN2018110892821 2018-09-18
CN201811089282.1A CN109062015A (en) 2018-09-18 2018-09-18 A kind of high concentration developer solution stoste composition

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CA3024242A1 true CA3024242A1 (en) 2020-03-18

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CA (1) CA3024242A1 (en)
WO (1) WO2020056627A1 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112099321A (en) * 2020-08-27 2020-12-18 江苏中德电子材料科技有限公司 High-concentration CF developing solution and preparation method thereof
CN113253580A (en) * 2021-05-11 2021-08-13 绵阳艾萨斯电子材料有限公司 Negative photoresist developing solution and preparation method and application thereof

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001312073A (en) * 2000-04-28 2001-11-09 Shin Sti Technology Kk Developing solution for negative photoresist
US7482316B2 (en) * 2001-01-04 2009-01-27 Henkel Kommanditgesellschaft Auf Aktien Water-based flushing solution for paints and other coatings
JP2003140357A (en) * 2001-11-05 2003-05-14 Fuji Photo Film Co Ltd Developer composition and method for forming image
JP3970740B2 (en) * 2002-10-03 2007-09-05 奇美實業股▲分▼有限公司 Developer composition
CN1811602B (en) * 2005-01-27 2010-10-06 明德国际仓储贸易(上海)有限公司 Developer solution composition
CN1928724B (en) * 2005-09-05 2010-09-29 比亚迪股份有限公司 Photoresistance developer
CN105093862A (en) * 2015-09-25 2015-11-25 富士胶片电子材料(苏州)有限公司 Surface active agent and developing solution used for color filter negative photoresist
CN107219731A (en) * 2017-05-11 2017-09-29 苏州新滤精环保科技有限公司 A kind of developer composition and preparation method thereof
CN107145044A (en) * 2017-06-17 2017-09-08 广州西陇精细化工技术有限公司 The developer composition that a kind of FPD is used
CN108170010A (en) * 2017-12-29 2018-06-15 苏州碳方新材料科技有限公司 A kind of environmental protection developer solution
CN108227410A (en) * 2018-03-15 2018-06-29 昆山长优电子材料有限公司 Develop adjuvant

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WO2020056627A1 (en) 2020-03-26

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Effective date: 20220517

FZDE Discontinued

Effective date: 20220517