CN102277242B - Cleaning agent composition - Google Patents

Cleaning agent composition Download PDF

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Publication number
CN102277242B
CN102277242B CN201110170337.3A CN201110170337A CN102277242B CN 102277242 B CN102277242 B CN 102277242B CN 201110170337 A CN201110170337 A CN 201110170337A CN 102277242 B CN102277242 B CN 102277242B
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Prior art keywords
acid
methyl
cleansing composition
phosphonic acid
benzotriazole
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CN102277242A (en
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尹嚆重
金圣植
房淳洪
金炳默
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Dongwoo Fine Chem Co Ltd
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Dongwoo Fine Chem Co Ltd
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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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/36—Organic compounds containing phosphorus
    • 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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0094—Process for making liquid detergent compositions, e.g. slurries, pastes or gels
    • 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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/26—Organic compounds containing oxygen
    • C11D7/261—Alcohols; Phenols
    • 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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/26—Organic compounds containing oxygen
    • C11D7/266—Esters or carbonates
    • 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
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/32—Organic compounds containing nitrogen
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/1316—Methods for cleaning the liquid crystal cells, or components thereof, during manufacture: Materials therefor
    • 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
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10—Objects to be cleaned
    • C11D2111/14—Hard surfaces
    • C11D2111/22—Electronic devices, e.g. PCBs or semiconductors

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nonlinear Science (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Detergent Compositions (AREA)
  • Liquid Crystal (AREA)
  • Cleaning By Liquid Or Steam (AREA)

Abstract

The invention discloses a cleaning agent composition containing no basic compounds. The composition comprises, based on the total weight of the composition, 0.1-15 weight percent of C1-C5 low alcohol, 0.1-15 weight percent of water-soluble glycol ether compounds, 0.01-10 weight percent of organic phosphoric acid, 0.001-10 weight percent of pyrrolyl compounds and the remaining water.

Description

Cleansing composition
Technical field
The present invention relates to a kind of cleansing composition.
This application claims the rights and interests of the korean patent application 10-2010-0055632 that on June 1st, 2010 submits to, by quoting, it being incorporated in the application in full.
Background technology
Usually, in the manufacture of liquid crystal cells, polyimide (PI) is painted on two patterned substrates with electrode pattern so that is endowed the function of oriented layer and insulation layer, and its upper surface stands friction in predetermined direction, thus forms oriented layer.Afterwards, be used for controlling the sealing tackiness agent of liquid crystal cell thickness and barrier sheet is configured between the substrates, so this two plate base combines togather.According to this, if pollutent remains on oriented layer substrate, inject liquid crystal thereon, very difficult acquisition display screen clearly, and packaging defect undesirably may produce.Therefore, need by cleaning to remove pollutent from substrate.
When manufacturing the liquid crystal cells of liquid-crystal display (LCDs), the contamination sources of substrate may be included in the impurity be separated in the friction cloth used in the friction process before two panels PI substrate or PI particle being combined, and may be attached on substrate, undesirably cause defect.The removing of this pollutent produced in process is by solvent ratio as Virahol or isopropanol water solution traditionally, or pure water has come.But, use solvent cleaning to be disadvantageous, because solvent may remain in after substrate, and from concerning the security of environment with to comprise flammable chemical stability aspect also may be undesirably debatable.In addition, along with the arrival of Waste Era of Oil, solvent cleaning is used may to cause the process costs increasing proportional increase with cost of material.And, use pure water cleaning also not demonstrate the cleansing power of removing pollutent fully, and therefore produce the decline of producing productive rate together.
In addition, the clean-out system containing basic cpd may undesirably damage PI oriented layer.
Further, the flat 3-62018 of publication number Japanese patent discloses a kind of ultrasonic cleaning using pure water to carry out rubbed substrate, stably to form the method for high tilt angle.But it is very difficult for introducing in the technique manufacturing indicating meter by ultrasonic wave, and use pure water cleaning can not meet the performance of recently required clean-out system.The flat 3-81730 of publication number Japanese patent discloses a kind of method on surface using brush to clean rubbed substrate, but is again attached on substrate, so can not expect desirable cleaning performance from the secondary pollutant of brush and pollutent owing to producing.
In above-mentioned Japanese Patent, the equipment of the cleansing power bestowing physics is employed in cleaning, undesirably add the cost of cleaning, and also inevitably have problem, comprise due to use Virahol or pure water and make dissolvent residual on substrate, rinse not good, the attachment again etc. of particle.
Therefore, in order to solve above-mentioned problem, in human-body safety and work safety, the superior and research that can be shown the various aqueous cleaning systems of high cleansing power and flushing characteristics by additional various tensio-active agent is constantly being carried out,
Summary of the invention
Therefore, the present invention aims to provide a kind of cleansing composition, and it has superior wetting and osmotic effect, and it is very effective for removing pollutent from the upper surface of oriented layer substrate thus.
In addition, the present invention aims to provide a kind of cleansing composition not damaging oriented layer.
In addition, the present invention aims to provide a kind of cleansing composition, and it has uninflammability, is therefore safe with environment amenable, and has low foaming.
In addition, the present invention aims to provide a kind of cleansing composition, and it does not corrode the metal level comprising copper and the metal level comprising aluminium.
One aspect of the present invention provides a kind of cleansing composition of alkali-free compound, it comprises, based on the gross weight of composition, the lower alcohol of the C1 ~ C5 of 0.1 ~ 15 % by weight, the water-soluble glycol ether compound of 0.1 ~ 15 % by weight, the organic phosphoric acid of 0.01 ~ 10 % by weight, the pyrrolyl compound of 0.001 ~ 10 % by weight, and residuum is water.
Another aspect of the present invention providing package is containing the liquid crystal cells of the oriented layer of cleaning with above-mentioned cleansing composition.
Further aspect of the present invention providing package is containing the LCD of above-mentioned liquid crystal cells.
Accompanying drawing explanation
More clearly the features and advantages of the present invention will be understood by the following detailed description in conjunction with respective drawings, wherein:
Fig. 1 show when use-case 1 cleansing composition cleaning Cu/Ti circuit board time Cu surface;
Fig. 2 show when use-case 2 cleansing composition cleaning Mo/Al/Mo circuit board time Al surface;
Fig. 3 shows the surface of the Al when using the cleansing composition cleaning Mo/Al/Mo circuit board of comparative example 1; With
Fig. 4 shows the surface of the Cu when using the cleansing composition cleaning Cu/Ti circuit board of comparative example 1;
Embodiment
Provide detailed description of the present invention hereinafter.
Cleansing composition according to alkali-free compound of the present invention comprises C1 ~ C5 lower alcohol, water-soluble glycol ether compound, organic phosphoric acid, pyrrolyl compound, and water.
Usually, basic cpd is used to remove the pollutent from air or organic substance.But, when basic cpd is used in the liquid crystal cells process manufacturing LCDs, may liquid crystal aligning layer be damaged, particularly, PI oriented layer.Therefore, according to cleansing composition of the present invention not containing such basic cpd, thus the damage to liquid crystal aligning layer is stoped.
In addition, cleansing composition according to the present invention is favourable, because C1 ~ C5 lower alcohol, water-soluble glycol ether compound, with the combination of organic phosphoric acid, thus show superior effect in removing pollutent and prevention oriented layer are damaged, and in the liquid crystal cells process manufacturing indicating meter, before or after the liquid crystal aligning layer that rubs during cleaning base plate, demonstrate uninflammability and low foaming.And, said composition cleaning liquid crystal aligning layer particularly, in PI oriented layer to removing pollutent be very effective.And, due to pyrrolyl compound, do not damage the metal level comprising Cu and the metal level comprising Al according to cleansing composition of the present invention, so that be positioned at the electrode at the capped place of liquid crystal aligning layer or wire does not also corrode.
Enhance clean-out system to the wetting of substrate and penetrating power according to C1 ~ C5 lower alcohol contained in cleansing composition of the present invention, and improve prevention pollutent by the ability of again adhering to, thus easily remove pollutent from substrate.
Lower alcohol can according to based on composition gross weight 0.1 ~ 15 % by weight amount use, and preferably 0.5 ~ 10 % by weight.If the amount of lower alcohol is less than 0.1 % by weight, surface tension does not reduce, and makes it be difficult to show wetting and penetrating power.On the contrary, if the amount of lower alcohol is more than 15 % by weight, lower alcohol may be stayed after substrate, undesirably causes defect.
The kind of C1 ~ C5 lower alcohol is not particularly limited, but based on to the consideration comprising water miscible characteristic, preferably includes C1 ~ C4 lower alcohol, such as, methyl alcohol, ethanol, n-propyl alcohol, Virahol, ethylene glycol, 1,2-PD, 1,3-PD, 1,2 butyleneglycols, 1,3 butyleneglycols, BDO, glycerol and 1,2,4-trihydroxybutane, can be used alone or use the mixture of two kinds or more.
The water-soluble glycol ether compound comprised in cleansing composition works in the solvability in water at removing oily components and raising, and described oily components is considered to, by means of only use aqueous lower alcoholic solutions, be difficult to remove from the surface of rubbed substrate.
Water-soluble glycol ether compound can according to based on composition gross weight, and the amount of 0.1 ~ 15 % by weight uses, and preferably 0.5 ~ 10 % by weight.If the amount of water-soluble glycol ether compound is less than 0.1 % by weight, be difficult to from rubbed substrate surface removing oily components.On the contrary, if the amount of water-soluble glycol ether compound is more than 15 % by weight, therefore obtained clean-out system may become very thickness, thus in cleaning its to the wetting of substrate and penetrating power possible deviation.
The water-soluble glycol ether of the preferred C1 ~ C10 of water-soluble glycol ether compound.The example of the water-soluble glycol ether of C1 ~ C10 can comprise ethylene glycol monomethyl ether (MG), diethylene glycol monomethyl ether (MDG), triethylene glycol monomethyl ether (MTG), poly glycol monomethyl ether (MPG), ethylene glycol monoethyl ether (EG), diethylene glycol monoethyl ether (EDG), ethylene glycol monobutyl ether (BG), diethylene glycol monobutyl ether (BDG), triethylene glycol butyl ether (BTG), propylene glycol monomethyl ether (MFG), dipropylene glycol monomethyl ether (MFDG), and it can be used alone or use the mixture of two kinds or more.
Play disperse contaminants particle according to organic phosphoric acid contained in cleansing composition of the present invention, make it the effect do not assembled, and also play a part to improve the wetting of substrate and penetrating power in cleaning, and then improve cleaning performance.In addition, organic phosphoric acid can remove metallics effectively, and also can stop the corrosion of the metal level comprising Cu and the metal level comprising Al.
Organic phosphoric acid can according to based on composition gross weight, and the amount of 0.01 ~ 10 % by weight uses, and preferably 0.1 ~ 5 % by weight.If the amount of organic phosphoric acid is lower than 0.01 % by weight, can not increase by the wetting and penetrating power on the surface of substrate rubbed.On the contrary, if the amount of organic phosphoric acid is more than 10 % by weight, this component may remain in after substrate, undesirably causes defect.
The example of organic phosphoric acid is not particularly limited, comprise Amino Trimethylene Phosphonic Acid, ethylidene diphosphonic acid, 1-hydroxy ethylene-1, 1-di 2 ethylhexyl phosphonic acid, 1-hydroxy propylidene-1, 1-di 2 ethylhexyl phosphonic acid, 1-hydroxy butylidene-1, 1-di 2 ethylhexyl phosphonic acid, ethylamino dimethylene-phosphonic acid, 1, 2-propylene diamine tetramethylene phosphonic acid, dodecylamino dimethylene-phosphonic acid, nitrotrimethylene phosphonic acids (nitrotris (methylenephosphonic acid)), quadrol dimethylene-phosphonic acid, ethylenediamine tetramethylene phosphonic acid, hexamethylenediamire tetramethylene phosphonic acid, diethylenetriamine pentamethylene phosphonic acids, cyclohexanediamine tetramethylene phosphonic acid, hydroxyl phosphonoacetic acid and 2-phosphonic acids-butane-1, 2, 4-tricarboxylic acid.Useful especially is HEDP, hydroxyl phosphonoacetic acid, Amino Trimethylene Phosphonic Acid or 2-phosphonic acids-butane-1,2,4-tricarboxylic acid.
According to pyrrolyl compound contained in cleansing composition of the present invention, the corrosion of the metal level comprising Cu with the metal level comprising Al is minimized.
Pyrrolyl compound can according to based on composition gross weight, and the amount of 0.001 ~ 10 % by weight uses, and preferably 0.01 ~ 3 % by weight.When the consumption of this component falls in above-mentioned scope, to comprising the metal level of Cu and comprising the damage of metal level of Al, namely, its corrosion can be reduced to minimum, and can produce economic benefit.
Preferably with the pyrrolyl compound that molecular formula 1 below represents.
Molecular formula 1
In molecular formula 1, R 1, R 2and R 3it is the group of the independently unit price of hydrogen atom, halogen atom, C1 ~ C6 alkyl, C3 ~ C6 cycloalkyl, allyl group, aryl, amino, C1 ~ C6 alkylamino, nitro, cyano group, sulfydryl (mercapto group), C1 ~ C6 alkane sulfydryl, hydroxyl, C1 ~ C6 hydroxyalkyl, carboxyl, C1 ~ C6 carboxyalkyl, acyl group, C1 ~ C6 alkoxyl group or heterocycle separately.
Pyrrolyl compound representated by molecular formula 1 can be selected from by N-[(benzotriazole) methyl] diethanolamine, N-[(methyl isophthalic acid H-benzotriazole-1-base) methyl] dimethanolamine, N-[(ethyl-1H-benzotriazole-1-base) methyl] diethanolamine, N-[(methyl isophthalic acid H-benzotriazole-1-base) methyl] dipropanolamine, 2, 2 '-[[(methyl isophthalic acid H-benzotriazole-1-base) methyl] imino-] dicarboxylic acid, 2, 2 '-[[(methyl isophthalic acid H-benzotriazole-1-base) methyl] imino-] dimethylamine, with the group of N-[(amine-1H-benzotriazole-1-base) methyl] diethanolamine composition.
In addition, the water according to comprising in cleansing composition of the present invention is not particularly limited, but can comprise the deionized water being suitable for semiconductor technology, and has the resistivity of at least 18M Ω cm.The amount of water can adjust according to the amount of other component.Based on composition gross weight, add water as residuum, to make total weight percentage of composition for 100.
According in cleansing composition of the present invention not containing organic acid be preferred.Reason is when using after friction orientation layer in LCDs manufactures containing organic acid cleansing composition, and metallics can by effectively from oriented layer, the particularly surface removing of PI oriented layer, but the corrosion of metal electrode or wire also may be accelerated.
In order to improve cleaning performance, common additive known in the art can be comprised further according to cleansing composition of the present invention, such as, inhibitor, wetting/permeate agent, dispersion agent, surface-modifying agent etc.
Known method preparation can be used usually according to the component of cleansing composition of the present invention, and preferably there is the purity of applicable semiconductor technology.
In addition, the invention provides the liquid crystal cells comprising the oriented layer using the cleaning of above-mentioned cleansing composition, in addition, the invention provides the LCD comprising above-mentioned liquid crystal cells.
When using according to cleansing composition of the present invention, the pollutent recrement on oriented layer substrate can be completely removed, and the liquid crystal cells comprising such oriented layer thus has high quality.And the LCD comprising such liquid crystal cells can provide display screen clearly.
Use the purging method according to cleansing composition of the present invention, be not particularly limited.Its example can comprise immersion, stirring, ultrasonic degradation, sprinkling (shower spraying), smash slurry (puddling), brush etc.
Cleansing composition according to the present invention has superior wetting and osmotic effect, and the pollutent be therefore present on oriented layer substrate can be removed efficiently.Do not damage the oriented layer comprised in an lcd according to cleansing composition of the present invention, therefore in the liquid crystal cells process manufacturing LCD, the cleaning base plate before or after friction liquid crystal aligning layer is very effective.Particularly, when this cleansing composition is used in manufacture LCD technique, metallics can be removed by the upper surface effectively from oriented layer.And cleansing composition according to the present invention does not fire, be safe and environment amenable thus and can not bubble problem be caused.The metal level comprising Cu and the metal level comprising Al is not corroded according to cleansing composition of the present invention yet.
Can be obtained by following example and better understand the present invention, these examples are used to elaborate, instead of it is of the present invention to be interpreted as restriction.
Example 1 ~ 11 and comparison example 1 ~ 8: the preparation of cleansing composition
Adding the component of display in following table 1 to one with predetermined amount is equipped with in the mixing vessel of agitator, at room temperature stirs 1 hour with the speed of 500rpm, thus prepares cleansing composition.
Table 1
A-1: ethanol
A-2: Virahol
A-3: glycerol
B-1: diethylene glycol monomethyl ether (MDG)
B-2: diethylene glycol monoethyl ether (EDG)
B-3: diethylene glycol monobutyl ether (BDG)
C-1:1-hydroxy ethylene-1,1-di 2 ethylhexyl phosphonic acid (HEDP)
C-2:2-phosphonic acids-butane-1,2,4-tricarboxylic acid (PBTC)
C-3: hydroxyl phosphonoacetic acid (HPA)
D-1:N-[(ethyl-1H-benzotriazole-1-base) methyl] diethanolamine
D-2:N-[(amine-1H-benzotriazole-1-base) methyl] diethanolamine
TMAH: Tetramethylammonium hydroxide
E-1: oxalic acid
Test examples: the assessment of cleansing power and the damage to oriented layer
1. the damage of pair PI oriented layer and the assessment of removing particle ability
A substrate (5cm x 5cm x 0.7cm), its PI oriented layer is rubbed, it is made to be in air 24 hours, so that it is by pollutions such as various organism, inorganics, particles, then use the glass substrate washing device spraying type, at room temperature clean 2 minutes with each cleansing composition of example 1 ~ 11 and comparison example 1 ~ 8.After cleaning, use nitrogen drying with ultrapure water substrate 30 seconds.Observe thus obtained substrate by scanning electronic microscope (SEM) (S-4700 is provided by Hitachi, Ltd), evaluate PI oriented layer whether damaged and evaluate cleansing power according to the number of the gritty particle remained in after substrate.
Result is presented in following table 2, and wherein ◎ is superior, and zero is good, and △ is medium, and × be poor.When PI oriented layer is stripped, can not measure result, this situation represents with "-".
2. remove the assessment of organic pollutant ability
A glass substrate, make it locate 24 hours in atmosphere, so that it is by pollutions such as various organism, inorganics, particles, backward its drip the ultrapure water of 0.5 μ l, measure contact angle before washing with confirmation form surface pollution.Particularly, each cleansing composition 100ml of example 1 ~ 11 and comparison example 1 ~ 8 is joined in a 250ml beaker, at room temperature glass substrate is soaked wherein 2 minutes and clean.Afterwards, nitrogen drying is used with ultrapure water substrate 30 seconds.The ultrapure water of 0.5 μ l is added drop-wise on glass substrate and measures the contact angle after cleaning.
Result is presented in following table 2, wherein be judged to be ◎ when the change of contact angle is 30 ° or larger after cleaning, the change of contact angle is judged to be zero from 15 ° to when being less than 30 °, the change of contact angle is judged to be △ from 5 ° to when being less than 15 °, and the change of contact angle be 5 ° or less time be judged to be ×.
3. the assessment of the damage of couple Al, Cu
For the damage of assessment to wire, use the damage of Mo/Al/Mo circuit board assessment to Al, and use the damage of Cu/Ti circuit board assessment to Cu.Particularly, each cleansing composition 100ml of example 1 ~ 11 and comparison example 1 ~ 8 is joined in 250ml beaker, and at room temperature glass substrate is soaked wherein 30 minutes and clean by (25 °).Afterwards, nitrogen drying is used with ultrapure water substrate 30 seconds.Whether Al and Cu observing substrate with SEM (S-4700 is provided by Hitachi, Ltd) be damaged.Result is presented in following table 2.
The assessment result of the damage of wire is also shown in Fig. 1 to 4.
Table 2
Ex. To the damage of PI oriented layer Removing particle ability Removing organism ability To the damage of Al To the damage of Cu
1 No ◎ ○ No No
2 No ◎ ○ No No
3 No ◎ ○ No No
4 No ○ ○ No No
5 No ◎ ○ No No
6 No ◎ ○ No No
7 No ◎ ○ No No
8 No ○ ○ No No
9 No ◎ ○ No No
10 No ○ ◎ No No
11 No ○ ◎ No No
C.1 Be stripped - ◎ Be Be
C.2 No △ ○ No No
C.3 No × × No No
C.4 No ○ ○ No Be
C.5 Be stripped - ◎ No No
C.6 No ◎ ○ No Be
C.7 No △ × No No
C.8 No ○ ○ No Be
Just as seen from Table 2, all cleansing compositions of embodiment according to the present invention 1 ~ 11 show superior cleansing power and do not cause the damage to PI oriented layer.And, do not observe the damage to Al and Cu.
But, cleansing composition containing a small amount of basic cpd in comparison example 1 completely removes PI oriented layer and has damaged the metal level comprising Al and Cu, and the cleansing composition of comparison example 2 is effective for removing impurity, what but cause organic materials to remain in substrate below forms dirt thus, undesirably produces defect.The cleansing composition of comparison example 3 does not cause the damage to oriented layer, but has the cleansing power of low removing impurity.The cleansing composition of comparison example 4 does not cause the damage of oriented layer and shows superior cleansing power, has but damaged copper; Except component of the present invention, the cleansing composition of the comparison example 5 also further containing basic cpd undesirably makes PI oriented layer peel off; Cleansing composition not containing the comparison example 6 of pyrrolyl compound has undesirably damaged Cu.Only do not cause the damage of PI oriented layer containing the cleansing composition of comparison example 7 of pure water but undesirably demonstrate low cleansing power, and undesirably having damaged Cu containing organic acid comparison example 8 cleansing composition.
Simultaneously, the picture on Cu surface when Fig. 1 is the cleansing composition cleaning Cu/Ti circuit board of display use-case 1, the photo on Al surface when Fig. 2 is the cleansing composition cleaning Mo/Al/Mo circuit board of display use-case 2, the photo on Al surface when Fig. 3 is the cleansing composition cleaning Mo/Al/Mo-circuit board of display use comparison example 1, the photo on Cu surface when Fig. 4 is the cleansing composition cleaning Cu/Ti circuit board of display use comparison example 1.
About Fig. 1 to 4, the cleansing composition of embodiment according to the present invention 1 and 2 does not cause the damage to Cu/Ti wire and Mo/Al/Mo wire.But the cleansing composition of comparison example 1 has damaged the whole of Cu/Ti wire and Mo/Al/Mo wire.
Described in above, the invention provides the cleansing composition with outstanding wetting and osmotic effect and be very effective in oriented layer upper surface of base plate removing pollutent.Do not damage the oriented layer comprised in an lcd according to cleansing composition of the present invention, and therefore, it is possible to demonstrate the superior effect in the liquid crystal cells process manufacturing LCDs before or after friction liquid crystal aligning layer in the base-plate cleaning implemented.Particularly, when cleansing composition according to the present invention is used to manufacture LCD, the ability of the metallics that its removing is positioned in oriented layer is high.Cleansing composition according to the present invention does not fire, and is therefore safe and environment amenable, and does not produce air bubble problem.And, do not corrode the metal level comprising Cu and the metal level comprising Al according to cleansing composition of the present invention.
Preferred embodiment be disclosed for illustrative purposes although of the present invention, but those skilled in the art can know not to be needed to depart from from scope of invention and purport disclosed in subsidiary claim, it is possible for carrying out various amendment, increase and substituting.

Claims (4)

1. a cleansing composition for alkali-free compound, comprises, based on described composition gross weight,
C1 ~ C5 lower alcohol of 0.1 ~ 15 % by weight;
The water-soluble glycol ether compound of 0.1 ~ 15 % by weight, described water-soluble glycol ether compound be selected from the group that is made up of ethylene glycol monomethyl ether, diethylene glycol monomethyl ether, triethylene glycol monomethyl ether, ethylene glycol monoethyl ether, diethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monobutyl ether, triethylene glycol butyl ether, propylene glycol monomethyl ether and dipropylene glycol monomethyl ether one or more;
The organic phosphoric acid of 0.01 ~ 10 % by weight, described organic phosphoric acid is selected from by Amino Trimethylene Phosphonic Acid, ethylidene diphosphonic acid, 1-hydroxy ethylene-1, 1-di 2 ethylhexyl phosphonic acid, 1-hydroxy propylidene-1, 1-di 2 ethylhexyl phosphonic acid, 1-hydroxy butylidene-1, 1-di 2 ethylhexyl phosphonic acid, ethylamino dimethylene-phosphonic acid, 1, 2-propylene diamine tetramethylene phosphonic acid, dodecylamino dimethylene-phosphonic acid, nitrotrimethylene phosphonic acids, quadrol dimethylene-phosphonic acid, ethylenediamine tetramethylene phosphonic acid, hexamethylenediamire tetramethylene phosphonic acid, diethylenetriamine pentamethylene phosphonic acids, cyclohexanediamine tetramethylene phosphonic acid, hydroxyl phosphonoacetic acid and 2-phosphonic acids-butane-1, 2, 4-tricarboxylic acid composition group in one or more,
The pyrrolyl compound of 0.001 ~ 10 % by weight, described pyrrolyl compound is selected from by N-[(benzotriazole) methyl] diethanolamine, N-[(methyl isophthalic acid H-benzotriazole-1-base) methyl] dimethanolamine, N-[(ethyl-1H-benzotriazole-1-base) methyl] diethanolamine, N-[(methyl isophthalic acid H-benzotriazole-1-base) methyl] dipropanolamine, 2, 2 '-[[(methyl isophthalic acid H-benzotriazole-1-base) methyl] imino-] dicarboxylic acid, 2, 2 '-[[(methyl isophthalic acid H-benzotriazole-1-base) methyl] imino-] dimethylamine, with N-[(amine-1H-benzotriazole-1-base) methyl] diethanolamine composition group in one or more, be water with residuum.
2. cleansing composition as claimed in claim 1, it is used in manufacture liquid-crystal display, cleaning base plate before or after the friction process of oriented layer.
3. cleansing composition as claimed in claim 1, wherein said C1 ~ C5 lower alcohol is selected from by methyl alcohol, ethanol, n-propyl alcohol, Virahol, ethylene glycol, 1,2-propylene glycol, 1, ammediol, 1,2-butyleneglycol, 1,3 butylene glycol, BDO, glycerol and 1, the group of 2,4-trihydroxybutane composition.
4. cleansing composition as claimed in claim 1, it does not comprise organic acid.
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