CN110658697A - Developing solution composition - Google Patents
Developing solution composition Download PDFInfo
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- CN110658697A CN110658697A CN201910800235.1A CN201910800235A CN110658697A CN 110658697 A CN110658697 A CN 110658697A CN 201910800235 A CN201910800235 A CN 201910800235A CN 110658697 A CN110658697 A CN 110658697A
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- 239000000203 mixture Substances 0.000 title claims abstract description 16
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 11
- 239000012498 ultrapure water Substances 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 22
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 150000007529 inorganic bases Chemical class 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 24
- 239000011550 stock solution Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000004377 microelectronic Methods 0.000 abstract description 2
- 229920002120 photoresistant polymer Polymers 0.000 description 13
- 230000018109 developmental process Effects 0.000 description 11
- 230000000694 effects Effects 0.000 description 8
- 239000000049 pigment Substances 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000007261 regionalization Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000008093 supporting effect Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Classifications
-
- 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
- G03F7/30—Imagewise removal using liquid means
- G03F7/32—Liquid compositions therefor, e.g. developers
- G03F7/322—Aqueous alkaline compositions
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optical Filters (AREA)
Abstract
A developer composition belongs to the field of functional microelectronic materials and comprises the following components in percentage by weight: 0.1 to 25 percent of inorganic alkali, 30 to 98.9 percent of high-purity water, 1 to 45 percent of anionic surfactant with a structure shown in formula I,
wherein R is1＝CnH2n+1；R2H or CnH2n+1(ii) a n is 1 to 50, and M is Na+Or K+Or NH4 +Or Mg2+Or Al3+. The high-concentration developing solution stock solution contains an anionic surfactant with a special structure, and has the characteristics of no residue, high developing pattern precision and the like.
Description
Technical Field
The invention relates to the field of functional microelectronic materials, in particular to a negative photoresist developing solution composition suitable for a liquid crystal display (TFT-LCD) Color filter (Color filter) manufacturing process, wherein a developing solution stock solution is diluted by high-purity water for use.
Background
Liquid crystal displays have been widely used in various display terminals because of their advantages of small size, light weight, low radiation, low power consumption, full color, and the like. Its industrial scale is still in a high-speed growth stage and will be a mainstream product in the display field for a long time now and in the future. The Color filter (Color filter) is a key component of the colorization of the liquid crystal display, and the performance of the Color filter directly affects the contrast, brightness, viewing angle and surface quality of the display.
The basic structure of the color filter consists of a glass substrate, a black matrix, a color layer, a protective layer and an ITO conductive film. The color filter is manufactured by manufacturing red, green and blue three-primary-color organic materials in each pixel on a glass substrate. In the past, printing methods, dyeing methods, Pigment dispersion methods, electronic printing methods, dry film methods, etc. have appeared, but the most popular mass production method at present is a Pigment dispersion method (Pigment Dispersed method) in which a Pigment Dispersed Color Resist (PDCR) is a raw material for forming a Color layer. The preparation process of the color layer of the pigment dispersion method is similar to TFT (array) photoetching process or semiconductor yellow light process, firstly, the pigment dispersion type photoresist is coated on a glass substrate of a formed black matrix, and the three-color pattern of R, G, B is formed by repeating the procedures of soft baking (Pre-bake), exposure alignment (Aligned), development (Developed) and hard baking (Post-bake) for three times.
The photoresist used in the TFT array process and the semiconductor yellow light process is usually a transparent positive photoresist, and the color photoresist used in the color filter process is usually a negative photoresist, and its basic components include pigment, dispersant, additive, binding polymer, crosslinking component, photoinitiator, solvent, etc. After the negative color photoresist is irradiated by ultraviolet light, the light-irradiated part is crosslinked to cause the dissolution rate of an exposed area and a non-exposed area in a developing solution to change, the part which is not irradiated by the light is removed during the development, and the light-irradiated part is remained, thereby forming a required pattern. The main function of the binding polymer in the color photoresist is as a carrier of other components, the binding polymer is soluble in a developing solution and has a supporting property, and a film layer can be formed and a crosslinking reaction can be supported. The color photoresist is mainly carboxylic resin material, and contains a large amount of carboxylic functional groups. Currently, inorganic bases (such as KOH, Na) are commonly used2CO3) And an alkaline developer such as an organic base (e.g., TMAH tetramethylammonium hydroxide).
Patent JP2006220961A relates to a color filter developer composition comprising an inorganic base, a surfactant intermediate, a co-solvent and other additives and water. The product has the advantages of large operation window, no residue in the developing solution, high precision of the developed graph and the like. US2006/0166147 a1 relates to a high concentration color filter developer solution containing an alkaline component, a nonionic surfactant of a specific structure, an organic acid or carboxylate and water. Then, the developer has problems such as incomplete development and residue in the developer. TW201643564A relates to a photoresist developer solution, which contains a nonionic surfactant of a specific structure and an alkaline substance. The developer can prevent surfactant residue, inhibit bubble generation, and improve product fine pattern formation. CN105093862A relates to a surfactant and a developer for negative photoresist of color filter, wherein the developer contains a block polyether nonionic surfactant, is a polyoxyethylene-polyoxypropylene block copolymer, and further contains strong base and purified water. The developing solution can generate serious problems such as bubbles and the like in the developing process, particularly in the sputtering developing process, so that the developing effect is reduced.
Disclosure of Invention
The invention aims to provide a developer composition suitable for a color filter process. The developing solution contains an anionic surfactant with a special structure, the surfactant has an excellent wetting and cleaning effect, and can effectively reduce defects such as residues after development, surface pollution and the like, so that a high-precision developed pattern is obtained.
The technical scheme adopted by the invention for realizing the purpose is as follows:
the composition of the high-concentration developing solution stock solution of the invention is as follows: a) an anionic surfactant with a special structure (shown as a formula I), b) inorganic alkali and c) high-purity water.
The developer composition comprises the following components in percentage by weight: 0.1-25 percent (preferably 0.2-20 percent) of inorganic base, 30-98.9 percent (preferably 40-98 percent) of high-purity water, 1-45 percent (preferably 3-30 percent) of anionic surfactant with a structure shown in formula I,
The inorganic alkali is selected from one or more of potassium hydroxide, sodium hydroxide, lithium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, sodium silicate and the like.
The high-purity water is deionized water with the resistance value of more than 2M omega/cm.
The developing solution is obtained by adding the anionic surfactant with the structure shown in the formula I, inorganic base and high-purity water in sequence, stirring and dissolving, controlling the temperature in the dissolving process to be less than or equal to 30 ℃, and filtering through a filter element of 0.2um after dissolving.
The developer is directly used or diluted by 5-600 times (preferably 50-300 times), and the pH value of the diluted solution is controlled to be 9-14. The developing solution of the invention is not particularly limited in the use process, and can adopt a soaking type or a spraying type.
The invention has the beneficial effects that:
the high-concentration developing solution stock solution contains an anionic surfactant with a special structure, and has the characteristics of no residue, high developing pattern precision and the like.
Drawings
Fig. 1 is a post-development SEM image of example 1.
Fig. 2 is a post-development SEM image of example 2.
Fig. 3 is a post-development SEM image of example 3.
Fig. 4 is a post-development SEM image of example 4.
Fig. 5 is a post-development SEM image of example 5.
Fig. 6 is a SEM image after development of comparative example 1.
Detailed Description
The invention is further illustrated by the following specific examples to further illustrate the advantages of the invention, but the scope of the invention is not limited to the following examples.
Detailed description of the preferred embodiments
The compositions and contents of the high concentration developing solution stock solutions of examples and comparative examples are shown in table 1.
TABLE 1
Second, Effect test
In order to further examine the developing effect of the developing solution, the invention adopts the following technical means: a negative color photoresist with the thickness of 0.2um is coated on a glass substrate with the thickness of 10cm multiplied by 10cm in a spin coating mode, and prebaking is carried out for 80s in an oven at the temperature of 120 ℃. And then, carrying out exposure by using a pattern mask, and developing by using the developing solution diluted by a certain multiple after the exposure is finished. After the development treatment, the resultant was washed with high-purity water, then dried with nitrogen gas, and hard-baked in an oven at 220 ℃. The development effect was confirmed by observation with an optical microscope and an electron microscope. The developing effect after the developer was diluted is shown in table 2 below.
TABLE 2
Note: wt% all refer to mass percent.
As can be seen from Table 2 above, the developer compositions of the present invention can give solutions which are uniformly dissolved in the temperature range of 5 to 35 ℃ as shown in examples 1 to 5. The development effect after dilution shows that the development result without residue and with clear pattern can be obtained. In comparison with example 2, comparative example 1 contains only KOH and does not contain such an anionic surfactant, and there is a phenomenon that the residue and the pattern are not sharp after development.
In summary, the present invention is directed to a developer composition comprising an anionic surfactant having a specific structure, an inorganic alkaline substance and high-purity water. The developing solution is suitable for developing the color photoresist in the TFT-LCD process color filter process. The developing solution has a large operation window, no residue after development, clear patterns and high-precision patterns. The developing effect of the developing solution reaches or even exceeds that of the color filter developing solution imported currently.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (5)
1. The developer composition is characterized by comprising the following components in percentage by weight: 0.1 to 25 percent of inorganic alkali, 30 to 98.9 percent of high-purity water, 1 to 45 percent of anionic surfactant with a structure shown in formula I,
2. The developer composition according to claim 1, wherein the inorganic base is one or more selected from potassium hydroxide, sodium hydroxide, lithium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, and sodium silicate.
3. The developer composition according to claim 1, wherein the high purity water is deionized water having a resistivity of greater than 2M Ω/cm.
4. The developer composition of claim 1, wherein the developer is prepared by sequentially adding the anionic surfactant having the structure of formula I, the inorganic base and the high-purity water, stirring and dissolving, controlling the temperature in the dissolving process to be less than or equal to 30 ℃, and passing through a filter element of 0.2um after dissolving.
5. The developer composition according to claim 1, wherein the developer is diluted 5-600 times and the pH of the diluted solution is controlled to 9-14.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910800235.1A CN110658697A (en) | 2019-08-28 | 2019-08-28 | Developing solution composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910800235.1A CN110658697A (en) | 2019-08-28 | 2019-08-28 | Developing solution composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110658697A true CN110658697A (en) | 2020-01-07 |
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| CN201910800235.1A Pending CN110658697A (en) | 2019-08-28 | 2019-08-28 | Developing solution composition |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111999993A (en) * | 2020-08-27 | 2020-11-27 | 福建天甫电子材料有限公司 | Preparation process of electronic-grade TFT developing solution |
| CN114280900A (en) * | 2021-12-24 | 2022-04-05 | 福建省佑达环保材料有限公司 | A kind of high-efficiency CF developer composition |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04204454A (en) * | 1990-11-30 | 1992-07-24 | Tokyo Ohka Kogyo Co Ltd | Developer composition for resist |
| JP2000155428A (en) * | 1998-11-24 | 2000-06-06 | Sumitomo Bakelite Co Ltd | Developing solution for positive photosensitive resin composition and pattern forming method using same |
| CN1802609A (en) * | 2003-06-13 | 2006-07-12 | 东京应化工业株式会社 | Developer composition for resists and method for formation of resist pattern |
| CN1809791A (en) * | 2003-06-27 | 2006-07-26 | 东京应化工业株式会社 | Developer composition for resists and method for formation of resist pattern |
-
2019
- 2019-08-28 CN CN201910800235.1A patent/CN110658697A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04204454A (en) * | 1990-11-30 | 1992-07-24 | Tokyo Ohka Kogyo Co Ltd | Developer composition for resist |
| JP2000155428A (en) * | 1998-11-24 | 2000-06-06 | Sumitomo Bakelite Co Ltd | Developing solution for positive photosensitive resin composition and pattern forming method using same |
| CN1802609A (en) * | 2003-06-13 | 2006-07-12 | 东京应化工业株式会社 | Developer composition for resists and method for formation of resist pattern |
| CN1809791A (en) * | 2003-06-27 | 2006-07-26 | 东京应化工业株式会社 | Developer composition for resists and method for formation of resist pattern |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111999993A (en) * | 2020-08-27 | 2020-11-27 | 福建天甫电子材料有限公司 | Preparation process of electronic-grade TFT developing solution |
| CN111999993B (en) * | 2020-08-27 | 2023-03-07 | 福建天甫电子材料有限公司 | Preparation process of electronic-grade TFT developing solution |
| CN114280900A (en) * | 2021-12-24 | 2022-04-05 | 福建省佑达环保材料有限公司 | A kind of high-efficiency CF developer composition |
| CN114280900B (en) * | 2021-12-24 | 2025-02-11 | 福建省佑达环保材料有限公司 | A high-efficiency CF developer composition |
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Application publication date: 20200107 |