CN104781204A - Glass substrate cleaning method - Google Patents
Glass substrate cleaning method Download PDFInfo
- Publication number
- CN104781204A CN104781204A CN201380059747.8A CN201380059747A CN104781204A CN 104781204 A CN104781204 A CN 104781204A CN 201380059747 A CN201380059747 A CN 201380059747A CN 104781204 A CN104781204 A CN 104781204A
- Authority
- CN
- China
- Prior art keywords
- glass substrate
- scavenging solution
- cleaning
- water system
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000011521 glass Substances 0.000 title claims abstract description 125
- 239000000758 substrate Substances 0.000 title claims abstract description 103
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000004140 cleaning Methods 0.000 title abstract description 133
- 239000002245 particle Substances 0.000 claims abstract description 41
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 20
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 150000007524 organic acids Chemical class 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 74
- 230000002000 scavenging effect Effects 0.000 claims description 55
- 239000002253 acid Substances 0.000 claims description 48
- -1 phospho Chemical class 0.000 claims description 46
- 239000003513 alkali Substances 0.000 claims description 43
- 238000010926 purge Methods 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 28
- 238000000227 grinding Methods 0.000 claims description 22
- 239000013543 active substance Substances 0.000 claims description 13
- 125000003118 aryl group Chemical group 0.000 claims description 13
- 239000003352 sequestering agent Substances 0.000 claims description 13
- 229920005646 polycarboxylate Polymers 0.000 claims description 11
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000005368 silicate glass Substances 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
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- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 abstract description 33
- 229920005989 resin Polymers 0.000 abstract description 31
- 239000011347 resin Substances 0.000 abstract description 31
- 239000003795 chemical substances by application Substances 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 3
- 238000005498 polishing Methods 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 67
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- 230000000052 comparative effect Effects 0.000 description 16
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- 150000001875 compounds Chemical class 0.000 description 13
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 13
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- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 9
- 230000004304 visual acuity Effects 0.000 description 9
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- 238000009736 wetting Methods 0.000 description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 125000002723 alicyclic group Chemical group 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N alpha-methacrylic acid Natural products CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
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- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
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- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
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- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 125000004103 aminoalkyl group Chemical group 0.000 description 2
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- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
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- 239000003153 chemical reaction reagent Substances 0.000 description 2
- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- PCHPORCSPXIHLZ-UHFFFAOYSA-N diphenhydramine hydrochloride Chemical compound [Cl-].C=1C=CC=CC=1C(OCC[NH+](C)C)C1=CC=CC=C1 PCHPORCSPXIHLZ-UHFFFAOYSA-N 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
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- SGUVLZREKBPKCE-UHFFFAOYSA-N 1,5-diazabicyclo[4.3.0]-non-5-ene Chemical compound C1CCN=C2CCCN21 SGUVLZREKBPKCE-UHFFFAOYSA-N 0.000 description 1
- RAXXELZNTBOGNW-UHFFFAOYSA-N 1H-imidazole Chemical class C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 1
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- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
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- VWSLLSXLURJCDF-UHFFFAOYSA-N 2-methyl-4,5-dihydro-1h-imidazole Chemical class CC1=NCCN1 VWSLLSXLURJCDF-UHFFFAOYSA-N 0.000 description 1
- AIDLAEPHWROGFI-UHFFFAOYSA-N 2-methylbenzene-1,3-dicarboxylic acid Chemical compound CC1=C(C(O)=O)C=CC=C1C(O)=O AIDLAEPHWROGFI-UHFFFAOYSA-N 0.000 description 1
- 150000008085 4,5-dihydro-1H-imidazoles Chemical class 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical group OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
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- 241001330002 Bambuseae Species 0.000 description 1
- COSXJWRRYPYAIG-UHFFFAOYSA-N C=C.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NCCN Chemical compound C=C.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NCCN COSXJWRRYPYAIG-UHFFFAOYSA-N 0.000 description 1
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- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/044—Hydroxides or bases
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0075—Cleaning of glass
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2082—Polycarboxylic acids-salts thereof
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/34—Organic compounds containing sulfur
- C11D3/3418—Toluene -, xylene -, cumene -, benzene - or naphthalene sulfonates or sulfates
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/36—Organic compounds containing phosphorus
- C11D3/362—Phosphates or phosphites
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- C11D2111/18—
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- C11D2111/20—
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- C11D2111/44—
Abstract
A method for cleaning a glass substrate after polishing, wherein a decrease in adhesion performance of a resin BM film formed on the cleaned glass substrate surface is suppressed and peeling of the resin BM film is prevented. A glass substrate cleaning method, characterized in that a glass substrate polished using a polishing agent containing cerium oxide particles is washed using an acidic aqueous cleaning liquid containing an organic acid and then washed using an alkaline aqueous cleaning liquid containing a base.
Description
Technical field
The purging method that glass substrate after the abrasive that the present invention relates to for containing cerium oxide particles to utilization grinds cleans, particularly for the purging method of the glass substrate of scavenging solution crystal device use etc.
Background technology
As the glass substrate that the FPD (Flat Panel Display: flat-panel monitor) of liquid crystal indicator (LCD) etc. uses, such as by carrying out the abrasive tool of the glass substrate rotation and revolution that are configured as tabular by melten glass grinding the small concavo-convex and ripple removing surface, thus formed meet Flatness required by FPD glass substrate there is the lamellar of specific thickness (such as 0.4 ~ 1.1mm).
In the grinding of such glass substrate, use containing the abrasive (slurry) of cerium oxide particles as abrasive particle, after grinding, implement abrasive (abrasive particle etc.) the cleaning removing (such as with reference to patent documentation 1) utilizing scavenging solution to be adhered to by glass baseplate surface.
Then, remaining for such abrasive using cerium oxide particles as abrasive particle, such as, when use comprises the scavenging solution of the alkalescence of inorganic or organic alkali composition and tensio-active agent, cleaning is insufficient, fully cannot remove the abrasive particle residue that particle diameter is submicron order.
Prior art document
Patent documentation
Patent documentation 1: Japanese Patent Laid-Open 2009-215093 publication
Summary of the invention
Invent technical problem to be solved
As the way to solve the problem in above-mentioned alkali cleaning, present inventors have proposed the method by using the scavenging solution including the such organic acid acidity of machine phosphonic acid to carry out dissolved oxygen cerium etc., the method (with reference to No. 2011-115353, Japanese patent application) of the residue of the abrasive particle on removing glass substrate.
But, when the substrate be made up of alumina silicate glass of LCD use etc. is cleaned with the scavenging solution of above-mentioned acidity, acted on by lixiviate (leaching, leaching), the Al composition of the Al ion on the surface (top layer) of glass substrate etc. is deviate from, and result forms the high layer (hereinafter referred to as rich OH hydrophilic layer) of the excessive wetting ability of OH base on the surface of glass substrate.
Therefore, glass substrate after cleaning uses the resin combination containing the such black pigment of carbon black formed in the operation of black matrix" (BM:black matrix) of colour filter, there is developing solution and immerse from the interface of the rich OH hydrophilic layer of glass baseplate surface and the black matrix film of resene and the problem that causes film to peel off.
The present invention is the invention completed to solve the problem, its objective is the purging method that glass substrate is provided, the method does not damage the flatness of glass substrate, the grinding abrasive particle of its remained on surface and attachment can be disperseed and removes, and the adaptation of the resene black matrix film (hereinafter also referred to resin B M film) suppressing glass baseplate surface after cleaning to be formed reduces, and prevents the stripping of resin B M film.
The technical scheme that technical solution problem adopts
The feature of the purging method of glass substrate of the present invention is, glass substrate after the abrasive utilized containing cerium oxide particles is ground, clean with the water system scavenging solution containing organic acid acidity, then clean with the water system scavenging solution of the alkalescence containing alkali.
In the purging method of glass substrate of the present invention, the water system scavenging solution of above-mentioned acidity is better at below pH5.In addition, the water system scavenging solution of above-mentioned acidity is better the water system scavenging solution containing (A) organic phospho acid, (B) polycarboxylate, (C) aromatic sulphonic acid and (D) amine-oxirane affixture.In addition, in the water system scavenging solution of above-mentioned acidity, each composition of above-mentioned (A) ~ (D) containing the proportional total amount 100 quality % relative to (A) ~ (D) better respectively: (A) organic phospho acid is 0.01 ~ 50 quality %, (B) polycarboxylate is 0.01 ~ 10 quality %, (C) aromatic sulphonic acid is 0.01 ~ 50 quality %, and (D) amine-oxirane affixture is 0.02 ~ 10 quality %.Further, the water system scavenging solution of above-mentioned alkalescence is better the water system scavenging solution of more than pH10.In addition, the water system scavenging solution of above-mentioned alkalescence is better the water system scavenging solution containing alkali, sequestrant and tensio-active agent.Also have, in the water system scavenging solution of above-mentioned alkalescence, the quality of above-mentioned alkali and above-mentioned sequestrant and above-mentioned tensio-active agent contains ratio (alkali): (sequestrant): (tensio-active agent) is better (1 ~ 10): (1 ~ 10): (1 ~ 10).
In addition, above-mentioned glass substrate is better the glass substrate be made up of alumina silicate glass.In addition, above-mentioned alumina silicate glass is better the aluminium borosilicate glass in fact not containing alkali metal component.Further, above-mentioned glass substrate is better the glass substrate of the liquid crystal indicator forming resene black matrix film thereon.
The effect of invention
According to purging method of the present invention, for the glass substrate after grinding with the abrasive containing cerium oxide particles, can clean efficiently under the prerequisite of flatness not damaging surface, by removing such as the abrasive particle of the cerium oxide particles of remained on surface and attachment etc., and the adaptation of the resin B M film suppressing glass baseplate surface after cleaning to be formed reduces, and prevents the stripping of resin B M film.
Namely, in purging method of the present invention, first the water system scavenging solution containing organic acid acidity is utilized to clean with the glass substrate after above-mentioned abrasive grinding, after the abrasive particle of the left on surfaces of glass substrate and the cerium oxide particles of attachment etc. is removed efficiently, the rich OH hydrophilic layer of the glass baseplate surface utilizing the water system scavenging solution removing containing the alkalescence of alkali to produce because of above-mentioned acid cleaning.The rich OH hydrophilic layer of such removing glass baseplate surface as a result, when forming resin B M film on the glass substrate, developing solution can be suppressed to immerse from the interface of glass substrate and BM resin combination film, improve the adaptation of resin B M film, prevent film from peeling off.
Accompanying drawing explanation
Fig. 1 is the figure of an embodiment of the purging method representing glass substrate of the present invention.
Fig. 2 represents the residual resolving power of resin B M film of the glass baseplate surface obtained in embodiments of the invention etc. and the existence of Al element and the Si element figure than (Al/Si than).
Fig. 3 is the figure of the rheological parameters' change with time of the contact angle on the surface representing the glass substrate obtained in embodiments of the invention etc.
Embodiment
Below, the purging method cleaned for the glass substrate used the FPD as LCD etc. is for example is to illustrate the present invention.The present invention is not limited to this embodiment, as long as technological thought according to the invention, then other embodiment also belongs to category of the present invention.
The feature of the purging method of glass substrate of the present invention is, glass substrate after the abrasive utilized containing cerium oxide particles is ground, clean with the water system scavenging solution (hereinafter also referred to acidic cleaning solution) containing organic acid acidity, then clean with the water system scavenging solution (hereinafter also referred to alkaline cleaning fluid) of the alkalescence containing alkali.In addition, below also by utilizing the cleaning of acidic cleaning solution to be called acid cleaning, be called that alkali cleans by utilizing the cleaning of alkaline cleaning fluid.
In addition, in purging method of the present invention, drying can be carried out between acid cleaning and alkali cleaning.Also can carry out drying after alkali cleaning.As drying means, the method etc. of the air after the method and jet compression of spraying warm braw can be exemplified.
< glass substrate >
In the present invention, the glass substrate as cleaning object thing is the glass substrate of the such FPD of LCD, after grinding, carries out the cleaning of the residue of the abrasive for removing surface etc. with the abrasive containing cerium oxide particles.The glass forming this glass substrate is better have to comprise SiO
2and Al
2o
3and B
2o
3and the alumina silicate glass of the composition of the oxide compound of alkaline-earth metal, be more preferably the aluminium borosilicate glass of the so-called alkali-free of alkali-free metal ingredient in fact in glass composition.In addition, alkali-free metal ingredient refers to that the content of the basic metal acidulants in glass composition is at below 1 quality % in fact.
In grinding before cleaning, for the surface of such glass substrate by such as using grinding pad, utilize and comprise cerium oxide particles and grind as the abrasive (slurry) of abrasive particle.The median size of the abrasive particle scope of such as 0.8 ~ 1.0 μm more fortunately.
The water system scavenging solution > of < acidity
In the present invention, the glass substrate after grinding for utilizing above-mentioned abrasive, carries out cleaning (below this matting being called sour matting) with the scavenging solution containing organic acid acidity.The pH of acidic cleaning solution is better less than 6, is more preferably less than 5, and spy is less than 3.5 well.In addition, the pH of acidic cleaning solution is better more than 1, is more preferably more than 1.5, and spy is more than 2 well.As the organic acid contained in acidic cleaning solution, the such as organic carboxyl acid such as xitix, citric acid and organic phospho acid etc. can be exemplified, but be not limited thereto.At these organic acids of interpolation simultaneously, mineral acid (such as sulfuric acid, phosphoric acid, nitric acid, hydrofluoric acid, hydrochloric acid etc.) can be added.In addition, in order to suppress the variation of pH, while adding above-mentioned mineral acid, the salt of these acid can also be added.
From the removability of the remained on surface of glass substrate after grinding and the cerium oxide of attachment and the viewpoint of aggegation preventing the abrasive particle residue cleaned waste liquid, as acidic cleaning solution, better use the scavenging solution comprising (A) organic phospho acid, (B) polycarboxylate, (C) aromatic sulphonic acid and (D) amine-oxirane affixture.
In this acidic cleaning solution, organic phospho acid as (A) composition plays the effect of the sequestrant of cerium oxide, plays and promotes the dispersion of the surface attachment of glass substrate and the residual abrasive particle be made up of cerium oxide etc. and it peeled off and the effect removed from glass baseplate surface.
Here, organic phospho acid refers to have with formula-P (=O) (OH)
2the phosphonate group represented is combined in the organic compound of the structure on carbon atom.The quantity of the phosphonate group of every 1 molecule organic phospho acid is better more than 2, is more preferably 2 ~ 8, particularly preferably 2 ~ 4.
As organic phospho acid, be better have the structure that hydrogen atom that the carbon can with substituent hydro carbons combines be instead of by phosphonate group compound or have ammonia or amine nitrogen-atoms the hydrogen atom that combines by with-CH
2-P (=O) (OH)
2the compound of the structure that the methylene phosphonic acid base represented instead of.
In the organic phospho acid of above-mentioned front a kind of structure, as substituent hydro carbons can be had, it is better the aliphatic hydrocarbon of aliphatic hydrocarbon or hydroxyl.In these aliphatic hydrocarbons etc., its carbon number is better 1 ~ 6, and hydroxyl value is better less than 2.As the organic phospho acid with this structure, such as methyl di 2 ethylhexyl phosphonic acid and 1-hydroxyl ethane-1,1-di 2 ethylhexyl phosphonic acid etc. specifically can be exemplified.
As also comprise the structure with following methylene phosphonic acid base organic phospho acid the present invention in organic phospho acid, the compound of the structure that the hydrogen atom that the carbon particularly preferably with the aliphatic hydrocarbon of hydroxyl combines be instead of by phosphonate group, specifically, preferably 1-hydroxyl ethane-1,1-di 2 ethylhexyl phosphonic acid.
As the organic phospho acid of above-mentioned rear a kind of structure, it is better the compound of the structure that the hydrogen atom that combines of the nitrogen-atoms with ammonia or fatty amine all be instead of by methylene phosphonic acid base.But a part for the hydrogen atom that amine nitrogen-atoms combines can be replaced by organic groups such as alkyl.As fatty amine, be better Alkylenediamine or the polyalkylene polyamine as its polymkeric substance.The carbon number of Alkylenediamine is better 2 ~ 4.The number of the hydrogen atom (hydrogen atom by methylene phosphonic acid base replaces) that the nitrogen-atoms of these amines combines is better 2 ~ 8, is more preferably 2 ~ 4.
As the organic phospho acid with this structure, specifically can exemplify amino three (methylene phosphonic acids), ethylene diamine four (methylene phosphonic acid), hexamethylene-diamine four (methylene phosphonic acid), trimethylene diamine four (methylene phosphonic acid), diethylene triamine penta(methylene phosphonic acid), Triethylenetetramine (TETA) six (methylene phosphonic acid), three (2-amino-ethyl) amine six (methylene phosphonic acid), trans-1, 2-cyclohexane diamine four (methylene phosphonic acid), glycol ether diamines four (methylene phosphonic acid), and tetren seven (methylene phosphonic acid) etc.
As the polycarboxylate of (B) composition and the aromatic sulphonic acid as (C) composition, improve use above-mentioned (A) organic phospho acid and the grinding abrasive particle that produces dispersiveness, while removability, also play the effect of adhering to again preventing abrasive particle.As the polycarboxylate of (B) composition, the salt etc. of poly-(methyl) acrylate, (methyl) acid-co-maleic acid can be exemplified.
Here, (methyl) acrylic acid statement represents vinylformic acid and methacrylic acid.The weight-average molecular weight (hereinafter referred to as Mw) of polycarboxylic acid, from the viewpoint of abrasive particle adhere to again prevent and low bubble, be better the scope of 2000 ~ 50000.In addition, Mw is the value measured by gel permeation chromatography (hereinafter referred to as GPC).
In polycarboxylate, the counter ion forming salt are not particularly limited, better basic metal (sodium and potassium) salt, ammonium salt, primary amine (such as methylamine, the alkylamine of ethamine and butylamine etc.) salt, secondary amine (such as dimethylamine, the dialkylamine of diethylamine and dibutylamine etc., and the dioxane hydramine of diethanolamine etc.) salt, tertiary amine (such as Trimethylamine 99, the trialkylamine of triethylamine and Tributylamine etc., three alkanolamines of trolamine etc., the N-alkyl dioxane hydramine of N methyldiethanol amine etc., and 1, 8-diazabicyclo [5.4.0]-7-undecylene, 1, 5-diazabicyclo [4.3.0]-5-nonene, 1, 4-diazabicyclo [2.2.2] octane, 1H imidazoles, 2-methyl isophthalic acid H-imidazoles, 2-ethyl-1H-imidazoles, 4, 5-dihydro-1H imidazoles, 2-methyl-4, 5-dihydro-1H imidazoles, 1, 4, 5, 6-tetrahvdro-nvrimidine, 1, the tertiary amine of the nitrogen-containing hetero ring-type of 6 (4)-dihydro-pyrimidins etc.) salt, or quaternary ammonium salt (tetraalkylammonium salt etc.).From the viewpoint of preventing adhering to again of particle, be better basic metal (sodium and potassium) salt, ammonium salt, primary amine salt, secondary amine salt, tertiary ammonium salt or quaternary ammonium salt among them, particularly preferably basic metal (sodium and potassium) salt or ammonium salt.
As the aromatic sulphonic acid of (C) composition, the alkyl benzene sulphonate (ABS) of the alkyl with carbon number 8 ~ 14, sulfonated petro-leum, toluenesulphonic acids, xylene monosulfonic acid (another name: acid dimethyl) and cumene etc. can be exemplified.Particularly preferably use m-xylene-4-sulfonic acid (another name: 2,4-acid dimethyl).
As the amine-oxirane affixture of (D) composition, play and promote that above-mentioned (A) organic phospho acid soaks into the effect at the interface to abrasive particle and glass substrate.As amine-oxirane affixture, it is better the known compound of the nonionic class tensio-active agent as oxirane add-on type.As oxirane, better oxyethane (hereinafter also referred to EO) or propylene oxide (hereinafter also referred to PO), can be the compound of the structure only the side's addition in them obtained, also can be the compound of the structure their both sides' additions obtained.In the compound EO and PO both sides addition obtained, the unit (i.e. oxyethylene group) of EO and the unit (i.e. oxypropylene group) of PO can block-wise exist, and also can exist by random shape.The former is addition EO and PO and obtaining successively respectively on amine, and the mixture of the latter addition EO and PO on amine obtains.PO-EO affixture is any one and the affixture that obtains that use in these addition methods.
As can the amine of addition oxirane, be better that the number of the hydrogen atom that nitrogen-atoms combines is 2 ~ 8, amino number is the amine of 1 ~ 4.In addition, the carbon number of amine is better less than 16, is more preferably less than 10.As such amine, such as aliphatic monoamine or polyamines, alicyclic monoamine or polyamines, aromatic monoamine or polyamines can be exemplified.More specifically, be better alkyl monoamine, Alkylenediamine and as its polymkeric substance polyalkylene polyamine, there is more than 1 alicyclic ring on the alicyclic monoamine of the amino that combines and aminoalkyl group and polyamine, there is more than 1 aromatic nucleus on the aromatic monoamine and polyamine etc. of the amino that combines and aminoalkyl group.
As the amine-oxirane affixture of (D) composition, the PO-EO affixture of to be better it be at least partially Alkylenediamine.As Alkylenediamine, be better the Alkylenediamine of carbon number 2 ~ 4, particularly preferably ethylene diamine.As the PO-EO affixture of ethylene diamine, addition PO and EO on 4 hydrogen atoms such as combining on the nitrogen-atoms of ethylene diamine can be exemplified and the compound obtained.In addition, as (D) amine-oxirane affixture, be better while the PO-EO affixture using above-mentioned ethylene diamine, also use the PO affixture of aromatic amine.As the PO affixture of aromatic amine, the PO affixture of such as m-xylene diamine can be exemplified.As (D) amine-oxirane affixture, when using the PO affixture of the PO-EO affixture of ethylene diamine and aromatic amine at the same time, improve the cleaning of scavenging solution and the stability of removing ability further.
(A) each composition of ~ (D) containing the proportional total amount relative to (A) ~ (D) better respectively: (A) organic phospho acid is 0.01 ~ 50 quality %, (B) polycarboxylate is 0.01 ~ 10 quality %, (C) aromatic sulphonic acid is 0.01 ~ 50 quality %, and (D) amine-oxirane affixture is 0.02 ~ 10 quality %.In addition, the ratio of the total of (B) polycarboxylate and (C) aromatic sulphonic acid is better 0.03 ~ 60 quality %.As (D) amine-oxirane affixture, when using the PO affixture of the PO-EO affixture of Alkylenediamine and aromatic amine simultaneously, be better the PO-EO affixture of Alkylenediamine be 0.01 ~ 5 quality %, the PO affixture of aromatic amine is 0.01 ~ 5 quality %, and its ratio added up to is 0.02 ~ 10 above-mentioned quality %.
The preferred acidic cleaning solution used in the present invention is by the water system scavenging solution of each component dissolves of above-mentioned (A) ~ (D) in water.As water, deionized water, ultrapure water, charge ion water, hydrogeneous water (Japanese: Shui Sushui) and ozone water etc. can be used.In addition, glassware for drinking water has the function of the mobility controlling scavenging solution, so its content suitably can set according to the target cleaning characteristics of cleaning speed etc.Usually, by the aqueous solution (hereinafter referred to as acidic cleaner stoste) comprising each composition of above-mentioned (A) ~ (D) with higher concentration dilute with water and make acidic cleaning solution before use, then the cleaning of glass substrate is used it for.Contain in the acidic cleaner stoste of each composition of (A) ~ (D) with above-mentioned scope, water containing proportional can be 55 ~ 98 quality %.In addition, in this acidic cleaner stoste, except each composition of above-mentioned (A) ~ (D), can by dispersion agent, water-miscible organic solvent, antioxidant, rust-preventive agent, pH adjusting agent, buffer reagent, defoamer, sanitas, help the additive of water solvent etc. to be blended in water.
When such acidic cleaner stoste is used for cleaning, be better that dilute with water uses to make containing after proportional (concentration) reaches 0.5 ~ 2.5 quality % of acidic cleaner stoste.By using after such dilute with water, the abrasive particle be made up of cerium oxide etc. that is residual and attachment can be removed well when not destroying glass baseplate surface.
< acid matting >
In acid cleaning of the present invention, use the diluent (acidic cleaning solution) after by above-mentioned acidic cleaner stoste dilute with water, the surface of the glass substrate after grinding is cleaned.Better clean with single chip mode (Japanese: Mei Leaf mode).As long as make scavenging solution directly contact with the surface of glass substrate and carry out the method for cleaning, purging method is not particularly limited.Can adopt and clean cleaning, cleaning showers (spraywashing), dipping (dipping) cleaning etc.The temperature of scavenging solution is not particularly limited, can uses at room temperature (15 DEG C) ~ 95 DEG C.When more than 95 DEG C, water may seethe with excitement, and on cleaning operation, inconvenience, thus not preferred.Acid scavenging period is better 1.5 seconds ~ 1 hour, is more preferably 1.5 seconds ~ 1 minute, particularly preferably 1.5 seconds ~ 15 seconds.
In acid matting, such as shown in Figure 1, can adopt while to utilizing the acidic cleaning solution 5 that the upper and lower surface injection self-cleaning nozzle 4 of the glass substrate 3 of carrying sprays in purge chamber 2 continuously in the horizontal direction such as the mechanism of conveying roller 1 grade, carry out cleaning the method for (wiping) with the rotating brush 6 being configured in side, two sides.
Here, as the rotating brush 6 of cleaning, the brush of the cylindrical shape of the external diameter 70 ~ 100mm that multiple PVA (polyvinyl alcohol) sponge (foam) can be used to make etc.In addition, by these brushes with rotational axis vertical in glass substrate 3 by the mode of cleaning surface and leading section and glass substrate 3 contacted by cleaning surface or mode across the interval being less than 2mm is configured.The speed of rotation of rotating brush 6 is better 100 ~ 500rpm.
As acidic cleaning solution 5, better use the scavenging solution obtained after above-mentioned acidic cleaner stoste is diluted with water to required concentration, the flow (emitted dose) of the scavenging solution after dilution is better 15 ~ 40 liters/min.In addition, the scouring time is better more than 1.5 seconds.The scouring time is more preferably less than 15 seconds.
The water system scavenging solution > of < alkalescence
In the present invention, for the glass substrate after utilizing acidic cleaning solution to clean in above-mentioned sour matting, alkaline cleaning fluid (namely, containing the water system scavenging solution of the alkalescence of alkali) is then used to carry out cleaning (below this matting being called alkali matting).The pH of alkaline cleaning fluid is better more than 8, is more preferably more than 10, and spy is more than 12 well.In addition, the pH of alkaline cleaning fluid is better less than 14.In addition, except containing except alkali in this alkaline cleaning fluid, also sequestrant and tensio-active agent can be contained.Spy uses sequestrant and tensio-active agent simultaneously.
As alkali contained in alkaline cleaning fluid, the alkali metal compound of alkali metal hydroxide and alkaline carbonate etc., amine and ammonium hydroxide etc. can be exemplified.As alkali, it is better the alkali metal hydroxide such as potassium hydroxide and sodium hydroxide.As sequestrant, can exemplified by ethylene ethylenediamine tetraacetic acid (EDTA) quasi-chelate compound, gluconic acids sequestrant, secondary nitrogen level nitrilotriacetic quasi-chelate compound, iminodisuccinic acid quasi-chelate compound etc.Spy is well ethylene diaminetetraacetic acid quasi-chelate compound.As tensio-active agent, it is better nonionic surface active agent.As nonionic surface active agent, the nonionic surface active agent of the ester class such as nonionic surface active agent, glycerol fatty acid ester of the polyoxyalkylenes such as nonionic surface active agent, the polyoxyethylene sorbitan carboxylic ester ether-ether class of the amine as (D) composition-polyoxyalkylenes such as oxirane affixture, the polyoxyethylene groups lauryl ether ethers of above-mentioned acidic cleaner can be exemplified.
The alkaline cleaning fluid used in the present invention is the water system scavenging solution being dissolved in the water by above-mentioned alkali etc. and obtaining.As water, deionized water, ultrapure water, charge ion water, hydrogeneous water (Japanese: Shui Sushui) and ozone water etc. can be used.In addition, glassware for drinking water has the function of the mobility controlling scavenging solution, so its content suitably can set according to the target cleaning characteristics of cleaning speed etc.Usually, the aqueous solution (hereinafter referred to as alkaline cleaner stoste) comprising above-mentioned alkali etc. with higher concentration is carried out diluting to make alkaline cleaning fluid with water before use, then uses it for cleaning.In alkaline cleaner stoste, water be set to 55 ~ 98 quality % containing proportional.In addition, in this alkaline cleaner stoste, except each composition of above-mentioned alkali, sequestrant and tensio-active agent, can by dispersion agent, water-miscible organic solvent, antioxidant, rust-preventive agent, pH adjusting agent, buffer reagent, defoamer, sanitas, help the additive of water solvent etc. to be blended in water.
Proportional as containing of the above-mentioned each composition in alkaline cleaner stoste, alkali, sequestrant and nonionic surface active agent are better be 1 ~ 10 quality %, and remainder is water.
In alkali matting, be better that the alkaline cleaner stoste dilute with water containing each composition with above-mentioned scope is reached 1 ~ 5 quality % to make contain proportional (concentration) of stoste, thus make alkaline cleaning fluid, and use this alkaline cleaning fluid.By using after such dilute with water, under the prerequisite unduly destroying glass baseplate surface, only except the rich OH hydrophilic layer at the Surface Creation of glass substrate in disacidify matting, the glass baseplate surface that can form the high resin B M film of adaptation can be obtained.
< alkali matting >
In alkali matting, for the glass substrate after utilizing acidic cleaning solution to clean in sour matting, the alkaline cleaning fluid obtained by above-mentioned alkaline cleaner stoste dilute with water is utilized to clean.Better clean with single chip mode.As long as make alkaline cleaning fluid directly contact with the surface of glass substrate and carry out the method for cleaning, purging method is not particularly limited.Same with the cleaning of above-mentioned employing acidic cleaning solution, can adopt and clean cleaning, cleaning showers (spraywashing), dipping (dipping) cleaning etc.In addition, the temperature of alkaline cleaning fluid is also same with above-mentioned acidic cleaning solution, is not particularly limited, and can use at room temperature (15 DEG C) ~ 95 DEG C.When more than 95 DEG C, water may seethe with excitement, and on cleaning operation, inconvenience, thus not preferred.Alkali scavenging period is better 1.5 seconds ~ 1 hour, is more preferably 1.5 seconds ~ 1 minute, particularly preferably 1.5 seconds ~ 15 seconds.
In alkali matting, the sour matting also with above-mentioned is same, and the washing unit shown in Fig. 1 can be used to clean.As shown in Figure 1, can adopt to acid cleaning terminate after glass substrate utilize the mechanism of conveying roller 1 grade to transport in purge chamber 2 continuously in the horizontal direction further, in the downstream side of sour matting to the upper and lower surface of glass substrate 3 while spray self-cleaning nozzle 4 spray alkaline cleaning fluid 7, clean the method on the two sides of glass substrate with the rotating brush 6 being configured in side, two sides.In addition, as scavenging solution 7, better use the alkaline cleaning fluid obtained after above-mentioned alkaline cleaner stoste is diluted with water to required concentration, the flow (emitted dose) of alkaline cleaning fluid is better 15 ~ 40 liters/min.In addition, the scouring time is better more than 1.5 seconds.The scouring time is more preferably less than 15 seconds.
In purging method of the present invention, for the glass substrate after grinding with the abrasive containing cerium oxide particles, first utilize in sour matting and clean containing organic acid acidic cleaning solution, after removing the abrasive particle of the cerium oxide particles of its remained on surface and attachment etc. efficiently, clean with the alkaline cleaning fluid containing alkali in alkali matting, thus remove the rich OH hydrophilic layer on the surface of the glass substrate produced in above-mentioned acid cleaning.Consequently in the formation process of resin B M film, developing solution can be suppressed to immerse from the interface of glass baseplate surface and BM resin combination film, improve the adaptation of resin B M film.Thus, the adaptation that can obtain resin B M film is good and film peels off the glass substrate obtaining preventing.
Embodiment
Below, embodiments of the invention are specifically described, but the present invention is not limited to these embodiments.In following example, when without special instruction, " % " represents quality %, and " part " represents mass parts.
Embodiment 1,2, comparative example 1, comparative example 2
Use the washing unit shown in Fig. 1, according to shown below, effects on surface implements cleaning through the glass substrate of grinding.
As glass substrate, use the LCD glass substrate (Asahi Glass Co., Ltd's system, the trade(brand)name that are made up of alumina silicate glass; AN100), to the surface of this glass substrate, use grinding pad, and use the abrasive slurry (Showa Denko K. K's (Showa Electricity work (strain)) system, the trade(brand)name that comprise the cerium oxide particles of particle diameter 0.8 ~ 1.0 μm; SHOROX A10) grind.
In embodiment 1 and 2, when composition being denoted as 100 parts, by containing organic phospho acid 9.0 parts, polycarboxylate 1.0 parts, aromatic sulphonic acid 10.0 parts and amine-oxirane 1.0 parts, all the other be water acidic cleaner stoste ((パ ー カ ー コ ー ポ レ ー シ ョ Application society of PACKARD) system, trade(brand)name; PK-LCG491A) dilute with water reaches 0.5% to make the concentration of stoste (comprising water), while the acidic cleaning solution (pH2.3 ~ 2.8) obtained was sprayed with the surface of the flow of 25L (hereinafter referred to as scavenging solution flow) to the glass substrate after grinding in 1 minute, while clean with the brush of the PVA rotated, after carrying out acid cleaning, carry out alkali cleaning.Alkali cleaning is implemented by following method: by alkaline cleaner stoste (PACKARD's system, trade(brand)name; PK-LCG211) dilute with water reaches 1.5% to make the concentration of stoste (comprising water), while the alkaline cleaning fluid obtained (pH11 ~ 12) to be ejected in 1 minute the surface of the glass substrate after acid cleaning with the flow of 25L, implement to clean.In addition, the temperature of each scavenging solution during acid cleaning and alkali clean is 25 DEG C in embodiment 1, is 35 DEG C in embodiment 2.In addition, the mean value of the scouring time in sour matting and alkali matting is respectively 2.94 seconds.On glass substrate after the cleaning of embodiment 1,2, remaining to abrasive particle unconfirmed.
In comparative example 1, the surface for the glass substrate after grinding only implements alkali cleaning.Alkali cleaning is implemented by following method: by alkaline cleaner stoste (PACKARD's system, trade(brand)name; PK-LCG211) dilute with water reaches 1.5% to make the concentration of stoste, the alkaline cleaning fluid of obtain 25 DEG C is ejected in 1 minute the surface of glass substrate with the flow of 25L, while carry out cleaning, cleaning with the brush of the PVA rotated.The mean value of scouring time is 2.94 seconds.Glass substrate after the cleaning of comparative example 1 has confirmed the remaining of abrasive particle.
In comparative example 2, acid cleaning is only implemented to the surface of the glass substrate after grinding.Acid cleaning is implemented by the following method: the stoste of the above-mentioned PK-LCG491A as acidic cleaner stoste is diluted to 0.5%, while the acidic cleaning solution of 25 DEG C that obtain was sprayed with the flow of 25L in 1 minute, carry out cleaning, cleaning with the brush of the PVA rotated.The mean value of scouring time is 3.92 seconds.Remaining to abrasive particle unconfirmed on glass substrate after the cleaning of comparative example 2.
For the surface of glass substrate after cleaning thus, the adaptation of resin B M film by the following method evaluation illustrated.In addition, the Al concentration (Al/Si ratio) of glass baseplate surface and the mensuration of contact angle has been carried out.
The evaluation > of the adaptation of < resin B M film
First, according to each composition illustrated below following composition fusion, carry out Homogeneous phase mixing, prepare the photosensitivity BM formation resin combination that solid component concentration is 15%.
[composition of BM formation resin combination]
Adhesive resin (Nippon Kayaku K. K (Japanese chemical drug society) system, trade(brand)name; ZCR1569H) 28.4 parts
Optical active matter (Photoepolymerizationinitiater initiater)
(Ciba Specialty Chemicals (チ バ ス ペ シ ャ Le テ ィ ケ ミ カ Le society) system, trade(brand)name; IRGACURE OXE02) 6.1 parts
Colloidal silica particles (Misao Kusano (Nissan Chemical society) system, trade(brand)name; PMAST) 20.3 parts
Carbon black 32.5 parts
Tensio-active agent (Bi Ke chemistry Amada Co., Ltd. (PVC ッ Network ケ ミ ー ジ ャ パ Application society) system, trade(brand)name; BYK306) 0.3 part
Linking agent (Nippon Kayaku K. K's system, trade(brand)name; UX5002D) 6.1 parts
(Nippon Kayaku K. K's system, trade(brand)name; NC3000H) 3.0 parts
Silane coupling agent (KCC of SHIN-ETSU HANTOTAI system, trade(brand)name; KBM403) 3.0 parts
Phosphate cpd (2:1 (mass ratio) mixture of phosphoric acid and mono phosphoric acid ester methacryloxyethyl ester, di(2-ethylhexyl)phosphate metacryloxy ethyl ester) 0.3 part
Then, the surface of glass substrate after cleaning, uses spin coating device (three large bamboo hat with a conical crown and broad brim Co., Ltd. (ミ カ サ society) system, device name; MS-A100), after 200rpm, 10 seconds coating (spin coating) above-mentioned BM formation resin combinations, hot-plate (Ya Suwang Co., Ltd. (ア ズ ワ Application society) system, device name is used; HI-1000), heat drying 60 seconds at 90 DEG C, forms film.Then, exposure apparatus (development of large Japanese section, device name is used; MA-1200), carry out exposing (illumination: 30mW/cm across photomask
2, exposure: 30mJ/cm
2, exposure GAP:50 μm) after, use developing apparatus (Ai Ketesi Co., Ltd. (ア Network テ ス society) system, device name; ADE-3000S), 0.045%KOH aqueous development 15 seconds are used.Then, by carrying out pure water cleaning, the surface of glass substrate forms the pattern of resin B M film.
Photomask has 4 kinds of pattern forms of the following L1 ~ L4 illustrated, and changes with every 1 μm for the various types of live width that makes, and makes the pattern amounting to 110 kinds.
L1 ... pattern spacing is 100 μm, has 25 linear pattern (live width can change in the scope of 1 ~ 25 μm) in 1 block (2835 μm × 2000 μm)
L2 ... pattern spacing is 50 μm, has 30 linear pattern (live width can change in the scope of 1 ~ 30 μm) in 1 block (2952.6 μm × 2000 μm)
L3 ... pattern spacing is 200 μm, has 25 linear pattern (live width can change in the scope of 1 ~ 25 μm) in 1 block (2682.5 μm × 2000 μm)
L4 ... pattern spacing is 200 μm, has the linear pattern (live width can change in the scope of 1 ~ 25 μm) that 25 short in 1 block (2682.5 μm × 2000 μm)
Utilize laser microscope (Keyemce Co., Ltd. (キ ー エ Application ス society) system, device name; VK-9510) glass substrate after development is observed, for 4 kinds of pattern forms of L1 ~ L4, the live width of the mask that the pattern investigating resin B M film on the glass substrate respectively remains.In addition, calculate live width maximum time line width values (hereinafter referred to as residual resolving power maximum value) and minimum time line width values (hereinafter referred to as residual resolution min) and mean value (hereinafter referred to as residual resolving power mean value).By these results shown in the figure of table 1 and Fig. 2.Residual resolving power is the live width (Line width of the maskwhich remains after developing) of mask residual after development.
In addition, each value of residual resolving power maximum value, residual resolution min and residual resolving power mean value is less, represents that the adaptation of the resin B M film that the glass substrate after cleaning is formed is higher.
The mensuration > of < surface A l concentration (Al/Si ratio)
Use x-ray photoelectron optical spectroscopy to measure Al concentration and the Si concentration of the glass baseplate surface after cleaning, calculate the ratio (Al/Si ratio) of Al concentration and Si concentration.In the mensuration of ESCA (Electron Spectroscopy forChemical Analysis: chemical analysis electron spectroscopy for chemical analysis), use the ESCA5500 that Alba Ke-Fei Co., Ltd. (ア Le バ ッ Network Off ァ イ society) is made, use the peak of Si (2p) and Al (2p), measure under the condition of logical energy 117.4eV, energy rank 0.5eV/step, exit angle (angle that specimen surface and detector are formed) 15 °.The analysis of spectrum uses analysis software MultiPak Ver.8.2.The result of gained is shown in Table 1.
In addition, surface A l concentration and Al/Si are than one of the index of wettability (wetting ability) that can be used as substrate surface.That is, surface A l concentration and Al/Si are than higher, mean that the leaching of the Al composition of glass baseplate surface (top layer) is fewer, represent that the wetting ability (wettability) that the rich OH hydrophilic layer because of glass baseplate surface causes is low.
[table 1]
Known according to table 1, after the glass baseplate surface acidic cleaning solution after grinding being cleaned to (acid cleaning), in the embodiment 1 of carrying out cleaning (alkali cleaning) with alkaline cleaning fluid and embodiment 2, the residual resolving power maximum value of resin B M film, residual resolution min and residual resolving power mean value with only carry out compared with the sour comparative example cleaned little, with only carry out the comparative example 1 of alkali cleaning for same degree, the adaptation of resin B M film and glass baseplate surface is good.
In addition, the temperature of scavenging solution in acid cleaning and alkali cleaning is set to the embodiment 2 of 35 DEG C to clean the embodiment 1 of cleaning with alkali with the scavenging solution acid of use 25 DEG C and compare known, the difference of residual resolving power maximum value and residual resolution min diminishes, by improving the temperature of scavenging solution, the deviation of the adaptation of resin B M film reduces.
Also have, in known embodiment 1 and embodiment 2, Al/Si is than height compared with comparative example 2, be same degree with comparative example 1, clean with alkaline cleaning fluid again after cleaning with acidic cleaning solution, the wetting ability (wettability) of glass baseplate surface with do not carry out acid clean and the comparative example 1 that only carries out alkali cleaning is to same extent lower, the glass baseplate surface that the adaptation of resin B M film is good can be obtained.
The mensuration > of < contact angle
The surface of the glass substrate after just cleaning drips the water droplet of the pure water of about 1 μ L, uses contact angle meter (FACE Co., Ltd. system, device name; CA-X), the contact angle relative to water is measured.In addition, self-stip, after 7 days, 14 days, 21 days and 28 days, measures the surface of glass substrate and the contact angle of water as described above.By measurement result shown in the figure of table 2 and Fig. 3.
In addition, one of index of the wettability (wetting ability) of substrate surface is also can be used as relative to the contact angle of water.The contact angle of glass baseplate surface and water is larger, then represent that wetting ability (wettability) is lower.
[table 2]
According to the known following content of table 2.That is, about the contact angle after just cleaning, embodiment 1 and almost do not have difference between comparative example 1 and comparative example 2, but about by the contact angle of exposure of substrates after more than 1 week, embodiment 1 is low compared with comparative example 1, but high significantly compared with comparative example 2.It can thus be appreciated that, by carrying out alkali cleaning after cleaning with the scavenging solution of acidity, with only carry out compared with the comparative example 2 that cleans of acid, by large for the contact angle that glass substrate exposes the embodiment 1 after more than 1 week, wetting ability (wettability) declines, and can obtain the glass baseplate surface that the adaptation of resin B M film is good.
Industry utilizes possibility
According to purging method of the present invention, can clean efficiently under the prerequisite of flatness not damaging surface for the glass substrate after grinding with the abrasive containing cerium oxide, the abrasive particle of remained on surface and attachment is removed, and the adaptation of the resin B M film suppressing glass baseplate surface after cleaning to be formed reduces, and prevents the stripping of resin B M film.Therefore, purging method of the present invention can be effectively applied to the cleaning of the glass substrate that the such FPD of LCD uses.
In addition, the announcement of all the elements as specification sheets of the present invention of the specification sheets of No. 2012-256714, the Japanese patent application that on November 22nd, 2012 files an application, claims, accompanying drawing and summary is quoted here.
Nomenclature
1 ... conveying roller, 2 ... purge chamber, 3 ... glass substrate, 4 ... washing nozzle, 5 ... acidic cleaning solution, 6 ... rotating brush, 7 ... alkaline cleaning fluid.
Claims (10)
1. the purging method of glass substrate, it is characterized in that, glass substrate after grinding for the abrasive utilized containing cerium oxide particles, cleans with the water system scavenging solution containing organic acid acidity, then cleans with the water system scavenging solution of the alkalescence containing alkali.
2. the purging method of glass substrate as claimed in claim 1, it is characterized in that, the water system scavenging solution of described acidity is the water system scavenging solution of below pH5.
3. the purging method of glass substrate as claimed in claim 1 or 2, it is characterized in that, the water system scavenging solution of described acidity is the water system scavenging solution containing (A) organic phospho acid, (B) polycarboxylate, (C) aromatic sulphonic acid and (D) amine-oxirane affixture.
4. the purging method of glass substrate as claimed in claim 3, it is characterized in that, each composition of described (A) ~ (D) in the water system scavenging solution of described acidity containing the proportional total amount 100 quality % relative to (A) ~ (D) respectively: (A) organic phospho acid is 0.01 ~ 50 quality %, (B) polycarboxylate is 0.01 ~ 10 quality %, (C) aromatic sulphonic acid is 0.01 ~ 50 quality %, and (D) amine-oxirane affixture is 0.02 ~ 10 quality %.
5. the purging method of the glass substrate according to any one of Claims 1 to 4, is characterized in that, the water system scavenging solution of described alkalescence is the water system scavenging solution of more than pH10.
6. the purging method of the glass substrate according to any one of Claims 1 to 5, is characterized in that, the water system scavenging solution of described alkalescence is the water system scavenging solution containing alkali, sequestrant and tensio-active agent.
7. the purging method of glass substrate as claimed in claim 6, it is characterized in that, it is alkali that the described alkali in the water system scavenging solution of described alkalescence and the quality of described sequestrant and described tensio-active agent contain ratio: sequestrant: tensio-active agent=1 ~ 10:1 ~ 10:1 ~ 10.
8. the purging method of the glass substrate according to any one of claim 1 ~ 7, is characterized in that, described glass substrate is the glass substrate be made up of alumina silicate glass.
9. the purging method of glass substrate as claimed in claim 8, it is characterized in that, described alumina silicate glass is the aluminium borosilicate glass of alkali-free metal ingredient in fact.
10. the purging method of the glass substrate according to any one of claim 1 ~ 9, is characterized in that, described glass substrate is the glass substrate of the liquid crystal indicator forming resene black matrix film thereon.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2012-256714 | 2012-11-22 | ||
| JP2012256714 | 2012-11-22 | ||
| PCT/JP2013/081203 WO2014080917A1 (en) | 2012-11-22 | 2013-11-19 | Glass substrate cleaning method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104781204A true CN104781204A (en) | 2015-07-15 |
Family
ID=50776097
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201380059747.8A Pending CN104781204A (en) | 2012-11-22 | 2013-11-19 | Glass substrate cleaning method |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JPWO2014080917A1 (en) |
| KR (1) | KR20150087224A (en) |
| CN (1) | CN104781204A (en) |
| TW (1) | TW201433373A (en) |
| WO (1) | WO2014080917A1 (en) |
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| CN106946465A (en) * | 2015-11-20 | 2017-07-14 | 旭硝子株式会社 | glass substrate and glass plate package body |
| CN109517676A (en) * | 2017-09-20 | 2019-03-26 | 蓝思科技（长沙）有限公司 | For cleaning the cleaning agent of glass anti-reflection film and the cleaning process of glass anti-reflection film |
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| CN110767534A (en) * | 2019-10-28 | 2020-02-07 | 苏师大半导体材料与设备研究院(邳州)有限公司 | Wafer cleaning method |
| CN111073767A (en) * | 2019-12-25 | 2020-04-28 | 东莞市晶博光电有限公司 | Glass cover plate cleaning agent and cleaning method thereof |
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| CN114845966A (en) * | 2020-03-25 | 2022-08-02 | 日本电气硝子株式会社 | Method for manufacturing glass plate |
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Also Published As
| Publication number | Publication date |
|---|---|
| JPWO2014080917A1 (en) | 2017-01-05 |
| TW201433373A (en) | 2014-09-01 |
| KR20150087224A (en) | 2015-07-29 |
| WO2014080917A1 (en) | 2014-05-30 |
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Application publication date: 20150715 |