CN106227003A - A kind of developer composition and preparation method thereof - Google Patents
A kind of developer composition and preparation method thereof Download PDFInfo
- Publication number
- CN106227003A CN106227003A CN201610861011.8A CN201610861011A CN106227003A CN 106227003 A CN106227003 A CN 106227003A CN 201610861011 A CN201610861011 A CN 201610861011A CN 106227003 A CN106227003 A CN 106227003A
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- Prior art keywords
- water
- developer composition
- organic solvent
- developer solution
- ether
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Classifications
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—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
Abstract
The present invention relates to a kind of developer solution, percentage by weight composition is as follows: organic base: 0.01 60%, nonionic surfactant: 0.01 10%, amphoteric surfactant: 0.01 15%, organic solvent: 1 10%, surplus is water.Present invention application organic alkali developer solution, the good penetrability to photoresist, developing rate is fast, and tenor is ppb rank, thus eliminates the impurity metal ion adverse effect to TFT transistor；Add nonionic surfactant and zwitterionic surfactant etc., not only taken into account defoaming, dispersion stabilization, and overcome the shortcoming that prior art development liquid film slag remains and operating temperature range is narrow；With the addition of water-miscible organic solvent, substantially increase persistency when development uses.This developer solution, while having the developing performance of excellence, also has low foam, has good dispersion stabilization to chromatic photoresist, effectively reduces the formation of film slag, and developing performance is good, without features such as residue, operating temperature range width.
Description
Technical field
The invention belongs to technical field of flat panel display, relate to one and be applied to narrow linewidth integrated circuit and high-resolution thin film
The developer solution of transistor liquid crystal display (TFT-LCD) (TFT-LCD).
Background technology
Along with expansion and the continuous progress of technology of semiconductor IC industry scale, degree of integration is according to Moore's Law
Increasing, live width constantly reduces, and requires day by day to improve to the process technology of Micropicture.Although dry etching than wet etching to micro-
The accuracy of fining-off is high, but its etching period is long, is relatively applicable to shallow table retrofit, thus the wet method photoetch of mature and reliable
Remain the processing technique accounting for main flow.Wet method is lithographically formed the principle of photoetching agent pattern, by irradiating ultraviolet with predetermined pattern
The light (exposure) of line etc., by base resin (photosensitive resin) modification in the photoresist of exposed portion, (alkali of photoresist can
Molten or alkali is soluble), then pass through developer solution and make the resist composition dissolution in exposed portion or unexposed portion thus remove, root
Eurymeric or the corrosion-resisting pattern of minus is formed according to exposing patterns.
At present the most general developer solution has a following deficiency: metal residual, film slag residual, foam residual etc..
Metal residual: in order to avoid Na+、K+Cause liquid crystal pollution Deng the residual of metal ion, thus cause image retention etc. bad
Problem, have the metal-free organo-alkali compound of Scheme Choice (CN201310744140.5) or acid as being main developing agent
(CN201310198744.4)。
Film slag remains: film slag constantly pile up attachment, directly affect development effect, be difficult to obtain accurate after causing development
Wiring pattern (Japanese Unexamined Patent Publication 02-166452 publication).In order to prevent the generation of this residue, form high accuracy corrosion-resisting pattern
Developer solution, developer solution adds appropriate surfactant, largely can alleviate residue phenomenon, be effectively improved aobvious
Show image quality: nonionic surfactant (United States Patent (USP) US7150960, CN201010592729.4), anionic surface are lived
Property agent (No. 2589408 publications of Japanese Patent Publication No.) etc., wherein, nonionic surfactant is due to its excellent moistening, infiltration, breast
Change the features such as dispersion, be widely adopted, but the dissolubility that nonionic surfactant is in aqueous slkali exists certain limit,
During transport and storage, due to the change of temperature, nonionic surfactant is easily generated nebulousurine and lamination, causes development
Liquid stability declines, and impact is normal to be used.There are some researches show that the polar organic matter infinitely dissolved each other with water can improve nonionic table
(additive affects petroleum journal (PETROLEUM PROCESSING) 2005 to nonionic surfactant AEO9 cloud point for the cloud point of face activating agent
The 5th phase of volume 21), therefore proposed to add ionic surface active agent by scheme and nonionic surfactant forms composite surface and lives
Property agent (CN201010604187.8, CN201210184138.2, CN201180011006.3).
Foam remains: foam residual can stop contacting of developer solution and photoresistance, causes unexposed photoresistance to be removed insufficient, shows
Shadow weak effect, thus affect integrity and the fineness (Japanese Unexamined Patent Publication 10-010749 publication) of wiring.In order to suppress foam
The side effect brought, adding defoamer in developer solution is common means, but some defoamer are using along with developer solution
During constantly dissolve and dispersion resist, defoaming effect is difficult to persistently (Japanese Unexamined Patent Publication 10-293964 publication).The side of having
Case proposes to add water soluble organic substance (CN201310198744.4) in developer solution, such as water-soluble alcohol, water solublity alcohol ether
Deng, have the effect of stably dispersing, froth breaking and hydrotropy concurrently, make developer solution have good dispersion stabilization and defoaming
(CN200810046078.1)。
Summary of the invention
It is an object of the invention to solve the deficiencies in the prior art, it is provided that one is applied to narrow linewidth integrated circuit and high score
The developer solution of resolution Thin Film Transistor-LCD (TFT-LCD).
The technical solution adopted for the present invention to solve the technical problems is:
The present invention provides a kind of developer composition, and percentage by weight composition is as follows: organic base: 0.01-60%, nonionic
Surfactant: 0.01-10%, amphoteric surfactant: 0.01-15%, organic solvent: 1-10%, surplus is water.
Preferably, percentage by weight composition is as follows: organic base: 0.03-15%；Nonionic surfactant: 0.02-5%；
Amphoteric surfactant: 0.02%-10%；Organic solvent: 2-5%；Surplus is water.
Ionic surface active agent can be effectively improved cloud point with nonionic surfactant composition complexed surfactant, but
Due to the addition of ionic surfactant, often strengthen frothing capacity, be easily caused foam residual, water-soluble solvent such as alcohol
Or alcohol ether compound has stably dispersing, froth breaking and hydrotropy effect concurrently, developer solution is made to have good dispersion stabilization and froth breaking
Property.And the addition of organic solvent, the developer composition dissolubility to organic polymer salt can be strengthened, substantially increase development
Persistency when liquid uses.
Preferably, organic base is selected from TMAH (Tetramethylammonium hydroxide), TEAH (tetraethyl ammonium hydroxide) and TMAC (tetramethyl
Base ammonium carbonic acid (hydrogen) salt) any one or any two kinds mix；
Preferably, nonionic surfactant is alkylphenol polyoxyethylene and/or alkyl polyoxyethylene ether.
Preferably, amphoteric surfactant is soluble amphoteric surfactant, including carboxylate surfactant, phosphorus
Acid esters type surfactant etc..
Preferably, organic solvent be selected from water-miscible organic solvent, such as water-soluble alcohol: methanol, ethanol, propanol, ethylene glycol, third
Glycol, isopropanol etc.；Alcohol ether compound: propylene glycol monomethyl ether, propylene-glycol ethyl ether, diethylene glycol monomethyl ether, diethylene glycol diformazan
Ether, butyl etc.；Amides compound: DMF, N,N-dimethylacetamide etc.；Acetone, N-first
Any one or two kinds such as base ketopyrrolidine, N-ethyl pyrrolidone, dimethyl sulfoxide.The use of organic solvent can bring more
Good development effect, strengthens the developer composition dissolubility to organic polymer salt, substantially increases when developer solution uses
Persistency.Water-soluble alcohol or alcohol ether compound have stably dispersing, froth breaking and hydrotropy effect concurrently, make developer solution have good dividing
Dissipate stability and defoaming.
Preferably, described water is deionized water, and the total concentration of metal ions no more than 500 in described water receives grams per liter, specifically
Grams per liter is received for no more than 50.With the developer solution that water is dispersion matchmaker, there is hypotoxicity, without flammable, liquid waste processing simplicity and cost
The feature such as cheap.
The developer solution preparation method of the present invention is as follows: under room temperature, by one or more additions of nonionic surfactant
In water, after stirring and dissolving, add one or both mixture of water-miscible organic solvent, add amphoteric surfactant one or
Several, it is sufficiently stirred for, is finally slowly added to the one of which of alkaline matter TMAH or TMAC or TEAH or two kinds of mixture, fills
Divide stirring.
This product is suitable for and is not limited to narrow linewidth ultraviolet positive photoresist, applies also for chemical amplification type negative photoresist etc., special
It it not the photoresist being mainly composed of polyacrylic of resin in photoresist；The photoresist thickness being suitable for is 0.5 μm-5 μm, phase
The development pre-bake temperature answered is 80 DEG C-140 DEG C, and between development temperature is 20-25 DEG C, developing time is between 15s-90s.
The invention has the beneficial effects as follows, present invention application organic alkali developer solution, the good penetrability to photoresist, development speed
Rate is fast, and tenor is ppb rank, thus eliminates the impurity metal ion adverse effect to TFT transistor；Add nonionic
Surfactant and zwitterionic surfactant etc., not only taken into account defoaming, dispersion stabilization, and overcome existing skill
The shortcoming that art development liquid film slag remains and operating temperature range is narrow；With the addition of water-miscible organic solvent, substantially increase development and make
The persistency of used time.This developer solution have excellence developing performance while, also have low foam, chromatic photoresist is had good
Good dispersion stabilization, effectively reduces the formation of film slag, and developing performance is good, without the features such as residue, operating temperature range width, application
In narrow linewidth integrated circuit and high-resolution Thin Film Transistor-LCD (TFT-LCD).
Detailed description of the invention
Below by specific embodiment, technical scheme is described in further detail.
The developer solution component of the present invention is described in detail below in conjunction with specific embodiment.Embodiment of the present invention D1-D6 such as table 1
Shown in.Cancelling and add amphoteric surfactant and organic solvent shown in table 1, surplus is supplemented by water, it is thus achieved that comparative example, such as table 2
Shown in, the advantage of developer solution component of the present invention is illustrated by Experimental comparison.
Table 1, table 2 are respectively ingredient names and the consumption list of developer solution D1-D6 and S1-S6, and wherein, described each component is used
Amount is mass percent.
Embodiment 1, prepares developer solution D1:
Under room temperature, by 1% non-ionic surfactant OP-10 (OPEO), 3% water-miscible organic solvent
DMSO (dimethyl sulfoxide), 0.5% amphoteric surfactant Miranol JEMC (Luo Diya), alkaline matter 2.38%TMAH,
Add in deionized water, stir.Wherein, the total concentration of metal ions in deionized water used is not more than 50
Receive grams per liter.
It is prepared D2-D6 according to method identical with embodiment 1.
Comparative example 1, prepares developer solution S1:
Under room temperature, by 1% non-ionic surfactant OP-10, alkaline matter 2.38%TMAH, add in deionized water,
Stir.Wherein, the total concentration of metal ions no more than 50 in deionized water used receives grams per liter.According to right
The identical method of ratio S1 is prepared S2-S6.
Table 1 developer solution D1-D6 composition and consumption list
Table 2 developer solution S1-S6 composition and consumption list
TMAH: Tetramethylammonium hydroxide (Hangzhou Greenda Chemical Co., Ltd.)
TEAH: tetraethyl ammonium hydroxide (Anqing Jin Shan Chemical Industry Science Co., Ltd)
TMAC: tetramethyl-ammonium carbonic acid (hydrogen) salt (Hangzhou Greenda Chemical Co., Ltd.)
OP-10: OPEO (Guangzhou Rui Yang surfactant company limited)
C16: long EO chain fatty race's polyoxyethylene ether (C10～18, EO=20) (the Hangzhou electrification group limited public affairs of auxiliary agent chemical industry
Department)
602: styrene phenol polyoxyethylene ether (EO=20) (Electro-group compounding chemicals Chemical Industry Co., Ltd. of Hangzhou)
Miranol JEMC: amphoteric surfactant (Luo Diya)
Miranol JC-HA: amphoteric surfactant (Luo Diya)
DMSO: dimethyl sulfoxide (Shanghai Aladdin biochemical technology limited company)
DMAC:N, N-dimethyl acetylamide (Shanghai Aladdin biochemical technology limited company)
DM: diethylene glycol monomethyl ether (lark prestige Science and Technology Ltd.)
The development effect of developer solution, fixing efficiency, development residue and the operation the temperature by the following method present invention provided
Degree scope etc. is evaluated: in gold-tinted room, and the TFT glass substrate forming thin film transistor (TFT) and pixel electrode is being turned round coating just
Type photosensitive composite, 100 DEG C are dried, and form the base material of about 2 μ m-thick positive type light sensitive films, by aforementioned substrates after light shield exposes,
Aforementioned substrates be impregnated in following developer composition about 90 seconds, liquid temperature controls at 23 DEG C ± 1 DEG C all the time, the most again with 200
DEG C baking 1 hour, the photoresist substrate after i.e. can being developed.Carry out observation by light microscope and SEM (scanning electron subsequently
Microscope) observe, measure the development effect of photoresist.
One, development effect: whether observe the pattern edge on substrates after development with 50 power microscopes after being disposed
Smooth:
◎: be expressed as pattern edge clean, smooth without burr；
×: it is expressed as pattern edge clean, out-of-flatness and have burr.
Two, fixing efficiency: develop according to method described in development effect, to put in developer solution after uv-exposure
Starting timing, to developing, complete taking-up terminates timing, and the gained time is developing time, according to following standard to developing time and
Fixing efficiency is evaluated:
Less than ◎: 30 minutes, fixing efficiency was high；
Zero: 30～90 minute, fixing efficiency was general；
×: more than 90 minutes, fixing efficiency was poor.
Three, development residue: whether the figure position after having developed with 250 power microscopes observation aforesaid substrates has a residue:
◎: be expressed as without residue,
×: level of residue is many.
Four, antifoam performance: contain 20mL with 100mL graduated cylinder after above-mentioned developer composition is diluted 20 times, with rectilinear
Vibrating machine sways 10 minutes under appropriate frequency, measures its foam height after standing 10 minutes, and according to following benchmark evaluation:
◎: foam height is less than 0.5cm；
Zero: foam height is between 0.5～2cm；
×: foam height is more than 2cm.
Five, stably dispersing performance: take above-mentioned developer composition 500mL, adds 1 gram of photo-induced etching agent, and stirring and evenly mixing is quiet
Put 1 hour.Then with the filter paper filtering of 5 microns, filter paper is being dried to constant weight at 100 DEG C.Make according to filter paper mass change
Evaluate:
When ◎: filter paper mass change is less than 0.02 gram, dispersion stabilization is good；
Zero: filter paper mass change is 0.02-0.04 gram, dispersion stabilization is general；
×: filter paper mass change is more than 0.04 gram, and dispersion stabilization is poor.
Six, operation temperature: contain above-mentioned developer composition 20mL with test tube, test tube is inserted into mercurial thermometer, will examination
Pipe is placed in water-bath (water bath is clear glass), and horizontal plane needs higher than developer solution liquid level, after gradually heat up heating, wait to show
Read muddy temperature (this reads temperature and is cloud point) when shadow liquid is muddiness, then developer solution is put to room temperature cooling, developer solution
Read this clarifying temp during in clarification, above-mentioned muddy cloud point temperature and clarifying temp are averaged, enters according to meansigma methods size
Row is evaluated:
◎: temperature averages, more than 45 DEG C, represents that operating temperature range is broad；
Zero: temperature averages, at 38-45 DEG C, represents that operating temperature range is moderate；
×: temperature averages, below 38 DEG C, represents that operating temperature range is narrow.
Table 3 developer solution D1-S6 property indices evaluates list
By the result of table 3 it can be seen that the developer solution that the present invention provides can obtain extraordinary developability, and image without
Residue, and above-mentioned properties is superior in comparative example corresponding properties.
The foregoing is only the several preferable possible embodiments of the present invention, all be familiar with technique personage, according to scope
The change made, all ought to be included in this case right.
Claims (10)
1. a developer composition, it is characterised in that the percentage by weight composition of described developer composition is as follows: organic
Alkali: 0.01-60%, nonionic surfactant: 0.01-10%, amphoteric surfactant: 0.01-15%, organic solvent: 1-
10%, surplus is water.
Developer composition the most according to claim 1, it is characterised in that the percentage by weight of described developer composition
Form as follows: organic base: 0.03-15%, nonionic surfactant: 0.02-5%, amphoteric surfactant: 0.02%-
10%, organic solvent: 2-5%, surplus is water.
Developer composition the most according to claim 1, it is characterised in that organic base selected from Tetramethylammonium hydroxide, four
Any one or any two kinds of mixture of ethyl ammonium hydroxide, tetramethyl-ammonium carbonate and tetramethyl-ammonium bicarbonate.
Developer composition the most according to claim 1, it is characterised in that nonionic surfactant is alkyl phenol polyoxy
Vinyl Ether and/or alkyl polyoxyethylene ether.
Developer composition the most according to claim 1, it is characterised in that amphoteric surfactant is soluble amphoteric table
Face activating agent.
Developer composition the most according to claim 1, it is characterised in that organic solvent is selected from water-miscible organic solvent.
Developer composition the most according to claim 6, it is characterised in that water-miscible organic solvent is water-soluble alcohol, alcohol
In ether compound, amides compound, acetone, N-Methyl pyrrolidone, N-ethyl pyrrolidone, dimethyl sulfoxide any one
Plant or two kinds.
Developer composition the most according to claim 7, it is characterised in that water-soluble alcohol is methanol, ethanol, propanol, second
Glycol, propylene glycol or isopropanol；Alcohol ether compound is propylene glycol monomethyl ether, propylene-glycol ethyl ether, diethylene glycol monomethyl ether, diethyl two
Diethylene glycol dimethyl ether or butyl；Amides compound is DMF or N,N-dimethylacetamide.
Developer composition the most according to claim 1, it is characterised in that described water is deionized water, the total gold in water
Belong to ion concentration no more than 500 and receive grams per liter.
10. the preparation method of the developer composition described in a claim 1-9 any one, it is characterised in that under room temperature,
Nonionic surfactant is added to the water, after stirring and dissolving, adds water-miscible organic solvent and amphoteric surfactant, fully
Stirring, is finally slowly added to organic base, is sufficiently stirred for.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106527065A (en) * | 2017-01-25 | 2017-03-22 | 绵阳艾萨斯电子材料有限公司 | Photoresist developing solution |
| 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 |
| CN107678252A (en) * | 2017-09-19 | 2018-02-09 | 合肥惠科金扬科技有限公司 | One kind is used for AMOLED negative photo glue developing solutions |
| CN108732874A (en) * | 2017-04-19 | 2018-11-02 | 蓝思科技（长沙）有限公司 | The cleaning method of uv-curable glue is remained after a kind of nano impression |
| CN109240037A (en) * | 2018-11-07 | 2019-01-18 | 天津市康华健晔医用材料有限公司 | A kind of aobvious fixing bath liquid of environmental protection |
| CN109856910A (en) * | 2017-11-30 | 2019-06-07 | 北京鼎材科技有限公司 | A kind of Photosensitve resin composition and its application |
| CN112859550A (en) * | 2021-01-19 | 2021-05-28 | 宁波南大光电材料有限公司 | Water-phase developing solution for retarding aluminum corrosion and preparation method thereof |
| CN113534623A (en) * | 2021-07-28 | 2021-10-22 | 南通群安电子材料有限公司 | Developer additive composition |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106527065A (en) * | 2017-01-25 | 2017-03-22 | 绵阳艾萨斯电子材料有限公司 | Photoresist developing solution |
| CN108732874A (en) * | 2017-04-19 | 2018-11-02 | 蓝思科技（长沙）有限公司 | The cleaning method of uv-curable glue is remained after a kind of nano impression |
| 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 |
| CN107678252A (en) * | 2017-09-19 | 2018-02-09 | 合肥惠科金扬科技有限公司 | One kind is used for AMOLED negative photo glue developing solutions |
| CN109856910A (en) * | 2017-11-30 | 2019-06-07 | 北京鼎材科技有限公司 | A kind of Photosensitve resin composition and its application |
| CN109856910B (en) * | 2017-11-30 | 2022-08-02 | 北京鼎材科技有限公司 | Photosensitive resin composition and application thereof |
| CN109240037A (en) * | 2018-11-07 | 2019-01-18 | 天津市康华健晔医用材料有限公司 | A kind of aobvious fixing bath liquid of environmental protection |
| CN112859550A (en) * | 2021-01-19 | 2021-05-28 | 宁波南大光电材料有限公司 | Water-phase developing solution for retarding aluminum corrosion and preparation method thereof |
| CN113534623A (en) * | 2021-07-28 | 2021-10-22 | 南通群安电子材料有限公司 | Developer additive composition |
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