CN103308654B - For testing the method for moisture in photoresistance stripper - Google Patents
For testing the method for moisture in photoresistance stripper Download PDFInfo
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- CN103308654B CN103308654B CN201310232747.5A CN201310232747A CN103308654B CN 103308654 B CN103308654 B CN 103308654B CN 201310232747 A CN201310232747 A CN 201310232747A CN 103308654 B CN103308654 B CN 103308654B
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- 238000012360 testing method Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims description 30
- -1 aromatic organic acid Chemical class 0.000 claims abstract description 54
- 150000001412 amines Chemical class 0.000 claims abstract description 47
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 46
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical group NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 27
- 239000005711 Benzoic acid Substances 0.000 claims abstract description 24
- 239000002253 acid Substances 0.000 claims abstract description 20
- 235000010233 benzoic acid Nutrition 0.000 claims abstract description 18
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 9
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229960004889 salicylic acid Drugs 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 73
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 238000007086 side reaction Methods 0.000 abstract description 4
- 239000012085 test solution Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 13
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 229920002120 photoresistant polymer Polymers 0.000 description 7
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000007530 organic bases Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 125000002723 alicyclic group Chemical group 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000005234 chemical deposition Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003196 chaotropic effect Effects 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 125000001309 chloro group Chemical class Cl* 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012453 solvate Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
- G03F7/422—Stripping or agents therefor using liquids only
- G03F7/425—Stripping or agents therefor using liquids only containing mineral alkaline compounds; containing organic basic compounds, e.g. quaternary ammonium compounds; containing heterocyclic basic compounds containing nitrogen
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Exposure Of Semiconductors, Excluding Electron Or Ion Beam Exposure (AREA)
- Photosensitive Polymer And Photoresist Processing (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a kind of for testing the solution of moisture in photoresistance stripper, including organic fat amine in described photoresistance stripper, described test solution is aromatic organic acid, wherein, by in aromatic organic acid and organic fat amine so that photoresistance stripper is faintly acid.The quality of aromatic organic acid is 1.2～1.5 times of its equivalent quality, and described organic fat amine is monoethanolamine, and described aromatic organic acid is benzoic acid or salicylic acid.The aromatic organic acid class of excess is added in the stripper of organic fatty amine, control the ratio of aromatic organic acid and stripper, pre-neutralized organic fat amine in atent solvent, both can guarantee that organic fat amine can react completely with aromatic organic acid, aromatic organic acid excess will not be made again too many to such an extent as to affect the pH value of solution, the aromatic organic acid of excess will not destroy the balance of system, avoid the generation of side reaction, measure the most quickly, easy and simple to handle quickly, testing cost and testing time-effectiveness can be saved.
Description
Technical field
The present invention relates to TFT technology, refer in particular in TFT applies, the solution of moisture in test photoresistance stripper
And method of testing.
Background technology
TFT technology is to use new material and the large-scale semiconductive integrated circuit technique of new technology, and it is at glass or to mould
On the on-monocrystalline sheets such as material substrate, by the atomic thin various films of the multi-section technical constructions such as sputtering, chemical deposition, and by etching,
Strippings etc. are to film processing and manufacturing integrated circuit.Prior to forming oxide insulating film or aluminum by sputtering or chemical deposition on substrate
The conducting films such as alloy, then it is uniformly coated with photoresist on above film layer, photoresist is exposed/develop after forming given pattern,
Using photoresist as mask, by wet etching or dry etching, film layer obtains required pattern, then with peeling off
Liquid removes the photoetching agent pattern as mask.
For removing photoetching agent pattern, at the TFT industry development initial stage, have employed by phenol and its derivatives and alkyl benzene sulphonate
And the solution that chloride series organic solvent is constituted, but this remover contains phenol series compound and chlorine series is organic
Solvent, therefore has toxicity, and can corrode the metal level under it, and its waste liquid is difficult to process, and due to water-insoluble and
The cleaning work after stripping is made to become complicated unavoidably.For solving the deficiency of problem above, at present use by organic fat amine and
The water soluble debonding agent that solvent is constituted, wherein, the stripper that monoethanolamine (MEA) the is key component combination of organic fatty amine
Thing is widely used.
The composition of stripper formula mainly determines according to the photoresist character used, but basic principle has two, one
Being fissility, it is desirable to do not have photoresist to remain after stripping, another is that requirement can not occur chemical reaction with graphic films layer, prevents
Metal electrode is corroded.The effect of monoethanolamine is the interface being impregnated with photoresist/film, makes photoresist depart from and dissolves.But peel off
In liquid, monoethanolamine is dissolved in water, generates alkaline matter, is susceptible to the reaction that aluminum in gate wirings is corroded, causes this distribution
Impedance becomes big, uses middle meeting to cause broken string due to heating.Be deteriorated it addition, aluminum corrosion also results in gate shapes, under the influence of together
The step coverage of film forming in operation, causes the defect ware such as point defect and line defect.Therefore, measure and monitored in stripper
Water content plays vital effect to the quality of stripping technology and the manufacture of TFT.
In actual production, there is employing online infrared spectrum analyser that the moisture in stripper is measured and supervised
Control.But this method condition controls strict, result accuracy and poor reliability, and is easily affected by other volatile component, often
Chang Buneng really meets in actual production the actual requirement of moisture in stripper.Karl-Fischer method (being called for short KF) is one
Planting the chemical method of exclusive mensuration moisture, it is extremely low that it measures detection limit, the accuracy height of measurement result and favorable reproducibility, makes
Obtain its field of micro-moisture in terms of stripper this needs accurately mensuration and have the biggest application space.
Traditional Ka Shi reagent consist of SO2、I2, organic base and alcohols solvent, its reaction principle is as follows:
CH3OH+SO2+RN→[RNH]SO3CH3
H2O+I2+[RNH]SO3CH3+2RN→[RNH]SO4CH3+2[RNH]I
RN=organic base, such as pyridine, imidazoles
According to above-mentioned reaction equation, I2With the H in system2O reacts quantitatively, and this chemical relationship is that in system, moisture is surveyed
The quantitative basis of examination.Substantial amounts of research shows, only the PH of measurement system is between 5～7, and KF reaction quickly and meets chemistry meter
Magnitude relation.But the monoethanolamine in stripper is a kind of stronger organic base, along with the addition of monoethanolamine in reaction, can make anti-
The pH value answering system increases, and when pH value is more than 7, can destroy balance and the quantitative relation of system, cause the generation of side reaction, with
Time also can cause the infinite delay of test, even can not accurately find out test terminal, as shown in Figure 1.
Therefore, it is necessary to provide that a kind of test accuracy is high, can reduce testing cost for testing in photoresistance stripper
The test solution of moisture and method of testing.
Summary of the invention
The invention provides a kind of for testing the solution of moisture in photoresistance stripper, described photoresistance stripper wraps
Containing organic fat amine, described test solution is aromatic organic acid, wherein, by aromatic organic acid and organic fatty
Amine so that photoresistance stripper is faintly acid.
The equivalent quality of described aromatic organic acid isWOrganic fat amine% is organic
The mass concentration of fatty amine, mStripperFor the quality of stripper, MAromatic organic acidFor the molal weight of aromatic organic acid, MOrganic fat amineFor
The molal weight of organic fat amine, mAromatic organic acidQuality for aromatic organic acid, it is preferable that mAromatic organic acidFor its equivalent quality
1.2～1.5 times, mAromatic organic acidFor its equivalent quality 1.3 times.
Preferably, described organic fat amine is monoethanolamine, and described aromatic organic acid is benzoic acid or salicylic acid.
A kind of method that present invention also offers moisture used in solution testing photoresistance stripper, it includes following
Step:
Step 1) sampling, measure V1Ml stripper, wherein, in stripper, the mass concentration of organic fatty amine is
WOrganic fat amine%, quality is mStripperg；
Step 2) measure in appropriate volume absolute methanol addition stripper, the volume of described absolute methanol is described stripper
2～3 times of volume V1；
Step 3) to step 2) in dilution after stripper in add aromatic organic acid, the quality of aromatic organic acid is
mAromatic organic acidG, stirs, and wherein, the equivalent quality of aromatic organic acid is
mAromatic organic acidFor 1.2～1.5 times of its equivalent quality, WStripper% is the mass concentration of stripper, mPeel offLiquid is the quality of stripper,
MAromatic organic acidFor the molal weight of aromatic organic acid, MOrganic fat amineMolal weight for organic fat amine；
Step 4) by step 3) in acquired solution to be transferred to volume be V2In the volumetric flask of ml, use absolute methanol profit
Wash, and described solution is settled to V2ml；
Step 5) from above-mentioned solution, take V by Ka Shi sample introduction needle3The solution of ml volume, surveys on Ka Shi moisture analyser
The absolute content trying out moisture therein is m3g；
Step 6) take steps 1)-step 5) and same procedure measure the absolute mass of moisture in absolute methanol solvent
m4G, is used for deducting blank, to deduct moisture background value in absolute methanol；
Step 7) moisture in stripper is calculated by following computing formula:
Preferably, described benzoic purity is more than 99.5%.
In step 3) before, described benzoic acid is heated in the baking oven of 105 DEG C 20-24h, is subsequently placed in exsiccator cold
But at least 1 hour.In step 2) in, the volume of absolute methanol is less than step 4) constant volume volumetric flask volume V22/3.
PH value during determination of moisture in described stripper is 5-7.
Compared with prior art, testing for the moisture in organic fatty amine stripper, by the present invention's
In photoresistance stripper, the measuring method of moisture have employed pre-neutralized measuring method, instead of original online infrared
Method for measurement or directly Karl-Fischer method, add the aromatic organic acid of excess in the stripper containing organic fatty amine
Class, such as benzoic acid or salicylic acid, controls the ratio of aromatic organic acid and stripper, pre-neutralized alicyclic organic in atent solvent
Fat amine, both can guarantee that organic fat amine can react completely with aromatic organic acid, will not make aromatic organic acid excess too again
Many to such an extent as to affect the pH value of solution, pH value is controlled between faintly acid 5-7, excessive aromatic organic acid will not destroy body
The balance of system, it is to avoid the generation of side reaction, measures accurately quickly, easy and simple to handle quickly can save testing cost and testing time-effectiveness,
Ka Shi reagent need not be replaced as frequently as, can be greatly saved the cost of test, improve accuracy and the repeatability of test, can be
TFT industry widelys popularize application.
Accompanying drawing explanation
Fig. 1 is existing a kind of for testing the response curve of the solution of moisture in photoresistance stripper；
Fig. 2 is that the present invention is a kind of for testing the response curve of the solution of moisture in photoresistance stripper.
Detailed description of the invention
When measuring for moisture in organic fatty amine stripper, the membership that adds of organic fat amine destroys Ka Shi reagent
Balance causes testing the inaccurate and phenomenon of test delay, the invention provides one and contains for testing moisture in photoresistance stripper
The solution of amount, wherein, includes organic fat amine and aromatic organic acid, and wherein, the quality of described aromatic organic acid is more than
Organic fat amine.The present invention uses the aromatic organic acid class adding excess before the reaction, pre-in atent solvent (such as methanol)
The method first neutralizing organic fatty amine, overcomes owing to the change measuring system PH causes measuring the deficiency of difficulty, the method
Measuring accurately quickly, the aromatic organic acid of excess will not destroy the balance of system, the most easy and simple to handle quickly, survey can be saved
Examination cost and testing time-effectiveness.Preferably, described organic fat amine is monoethanolamine, and described aromatic organic acid is benzoic acid or water
Poplar acid.Wherein, by aromatic organic acid and organic fat amine so that photoresistance stripper is faintly acid.
Aromatic organic acid is as a example by benzoic acid, and organic fat amine is as a example by monoethanolamine MEA, and chemical equation is as follows:
C5H5-COOH+OHCH2-CH2NH2→C5H5-COONH2CH2-CH2OH
By excess benzoic acid in and monoethanolamine MEA so that it is the pH value before test reaction is 5-7 so that system protect
Maintain an equal level weighing apparatus and quantitative relation.
Wherein, the equivalent quality of described aromatic organic acid is
WOrganic fat amine% is the mass concentration of organic fat amine, mStripperFor the quality of stripper, MAromatic organic acidFor aromatic organic acid mole
Quality, MOrganic fat amineMolal weight for organic fat amine.Preferably, mAromatic organic acidFor 1.2～1.5 times of its equivalent quality,
mAromatic organic acidFor quality is its equivalent quality 1.2～1.5 times of the quality of aromatic organic acid, i.e. aromatic organic acid, pass through
Organic fat amine is neutralized by the aromatic organic acid of excess, can either ensure that organic fat amine and aromatic organic acid are complete
Reaction, will not make again the amount excess of aromatic organic acid too much to such an extent as to affect the pH value of stripper.
With reference to shown in Fig. 2, by pre-neutralized method for measurement, after controlling the pH value in photoresistance stripper, carry out moisture
The test of content so that the reaction end of test is controlled, it is to avoid regularly change Ka Shi reagent, cause carrying of testing cost
High.
A kind of method that present invention also offers moisture used in solution testing photoresistance stripper, it includes following
Step:
As a example by stripper the most frequently used in TFT industry and the most frequently used aromatic organic acid benzoic acid, wherein, stripper
In main formula dimethyl sulfoxide (Dimethyl sulfoxide or DMSO) and the ratio of monoethanolamine MEA be DMSO: MEA
=3: 7, described monoethanolamine MEA is the one of organic fat amine.
Step 1) sampling, use liquid-transfering gun accurately to measure V1Ml stripper, wherein, organic fatty amine monoethanolamine MEA
Mass concentration be WMEA%, weighs described stripper and puts in 100ml small beaker, and accurately claims it with electronics fraction analysis balance
Quality is mStripperg；
Step 2) measure in appropriate absolute methanol addition stripper and stir, add methanol solvate reaction medium, with
Time play diluting effect so that uniformly, the volume of described absolute methanol is regarding step 1 in stripper dilution) in stripper volume depending on,
Preferably, the volume of described absolute methanol is described stripper volume V12～3 times of ml, wherein, the moisture of absolute methanol
≤ 0.05%；
Step 3) to step 2) in dilution after stripper in add aromatic organic acid benzoic acid, aromatic organic acid
Quality is mBenzoic acidG, stirs, and wherein, the equivalent quality of described aromatic organic acid is
WMEA% is the mass concentration of monoethanolamine MEA, MBenzoic acidFor benzoic molal weight, MMEAMole matter for monoethanolamine MEA
Amount.Preferably, mBenzoic acidFor 1.2～1.5 times of its equivalent quality, mBenzoic acidFor benzoic quality, mStripperFor the quality of stripper,
Add monoethanolamine MEA reaction in benzoic acid, and stripper, be equivalent to neutralize alkali, reduce the pH value of solution.
Benzoic acid equivalent quality calculation specifications: benzoic acid C6H5-COOH and monoethanolamine MEA OHCH2-CH2NH2Reaction, instead
The relation answering coefficient to be 1: 1, MBenzoic acidAnd MMEARepresenting the molal weight of benzoic acid and monoethanolamine MEA respectively, both are when reaction
Relative mass ratio should be identical with absolute mass ratio.The quality of stripper is mStripper, wherein the quality of monoethanolamine MEA is dense
Degree is WMEA%, mStripper*WMEA% is the quality of monoethanolamine MEA in stripper.Benzoic equivalent quality is unknown number to be asked,
Be set to x, establish an equation into:
MBenzoic acid∶MMEA=x: (mStripper*WMEA%), solve equation, obtain
Step 4) by step 3) in acquired solution to be transferred to volume be V2In the volumetric flask of ml, use absolute methanol profit
Washing above-mentioned weighing small beaker and stirring peels off rod at least 3 times, rinse liquid is also transferred in same volumetric flask, and by described solution constant volume
To V2Ml, is transferred to above solution in volumetric flask and shakes up, the volume V of volumetric flask2For it is known that the total of solution can accurately be known
Volume, prepares for next step；
Step 5) from volumetric flask, take a part of sample examination with computer, from above-mentioned solution, take V by Ka Shi sample introduction needle3ml
The solution of volume, the absolute content testing out moisture therein on Ka Shi moisture analyser is m3g；
Step 6) because absolute methanol also contains the moisture of trace, need to deduct moisture background value in methanol, take steps
1)-step 5) same procedure measure absolute mass m of moisture in absolute methanol solvent4G, is used for deducting blank；
Step 7) moisture in stripper is calculated by following computing formula:
Calculation specifications:
m3For V3Total moisture content in volume stripper, m4For the water content in same volume absolute methanol, m3-m4For V3Body
The clean water content of long-pending stripper.Stripper gross mass is m1, in volumetric flask, constant volume is to V2Volume,Be equivalent to unit volume
Middle stripper quality, by stripper quality in unit volumeIt is multiplied by sample volume V3, i.e. obtain in step 5 for upper machine
The gross mass of the stripper of testBy V3Clean water content in volume stripper, divided by sampling gross mass, obtains stripping
Water content percentage in chaotropic.
Wherein, described organic fat amine is monoethanolamine, and described aromatic organic acid is benzoic acid or salicylic acid.Described benzene
The purity of formic acid is more than 99.5%.
In step 2) in, the volume of absolute methanol is less than step 4) constant volume volumetric flask volume V22/3.
In step 3) before, described benzoic acid is heated in the baking oven of 105 DEG C 20-24h, is subsequently placed in exsiccator cold
But at least 1 hour.
PH value during determination of moisture in described stripper is 5-7.
Testing for the moisture in organic fatty amine stripper, by moisture in the photoresistance stripper of the present invention
The measuring method of content have employed pre-neutralized measuring method, instead of original online infrared method for measurement or directly blocks
Er Feixiu method, adds the aromatic organic acid class of excess in the stripper of organic fatty amine, such as benzoic acid or salicylic acid,
Control the ratio of aromatic organic acid and stripper, pre-neutralized organic fat amine in atent solvent, both can guarantee that alicyclic organic
Fat amine can react completely with aromatic organic acid, aromatic organic acid excess will not be made again too many to such an extent as to affect the PH of solution
Value, controls pH value between faintly acid 5-7, and the aromatic organic acid of excess will not destroy the balance of system, it is to avoid side reaction
Generation, measure accurately quickly, easy and simple to handle quickly, testing cost and testing time-effectiveness can be saved, it is not necessary to be replaced as frequently as Ka Shi
Reagent, can be greatly saved the cost of test, improves accuracy and the repeatability of test, and can widely popularize in TFT industry should
With.
Claims (7)
1. the method for the moisture tested in photoresistance stripper, it is characterised in that comprise the following steps:
Step 1) sampling, measure V1Ml stripper, wherein, in stripper, the mass concentration of organic fat amine is WOrganic fat amine%, quality
For mStripperg；
Step 2) measure in appropriate volume absolute methanol addition stripper, the volume of described absolute methanol is described stripper volume
V12～3 times；
Step 3) to step 2) in dilution after stripper in add aromatic organic acid, the quality of aromatic organic acid is mAromatic organic acid
G, stirs, and wherein, the equivalent quality of aromatic organic acid ismAromatic organic acidFor
1.2～1.5 times of its equivalent quality, WOrganic fat amine% is the mass concentration of organic fat amine, mStripperFor the quality of stripper,
MAromatic organic acidFor the molal weight of aromatic organic acid, MOrganic fat amineMolal weight for organic fat amine；
Step 4) by step 3) in acquired solution to be transferred to volume be V2In the volumetric flask of ml, use absolute methanol rinse, and
Described solution is settled to V2ml；
Step 5) from above-mentioned solution, take V by Ka Shi sample introduction needle3The solution of ml volume, tests out on Ka Shi moisture analyser
The absolute content of moisture therein is m3g；
Step 6) take steps 1) step 5) and same procedure measure absolute mass m of moisture in absolute methanol solvent4G, uses
In deduction blank, to deduct moisture background value in absolute methanol；
Step 7) moisture in stripper is calculated by following computing formula:
2. according to the method for the moisture in the test photoresistance stripper described in claim 1, it is characterised in that: described
mAromatic organic acidFor 1.3 times of the equivalent quality of aromatic organic acid, mAromatic organic acidQuality for aromatic organic acid.
3. according to the method for the moisture in the test photoresistance stripper described in claim 2, it is characterised in that have described in:
Machine fatty amine is monoethanolamine, and described aromatic organic acid is benzoic acid or salicylic acid.
4. according to the method for the moisture in the test photoresistance stripper described in claim 3, it is characterised in that: described benzene
The purity of formic acid is more than 99.5%.
5. according to the method for the moisture in the test photoresistance stripper described in claim 3, it is characterised in that: in step
3) before, described benzoic acid is heated 20-24 hour in the baking oven of 105 DEG C, be subsequently placed in exsiccator that to cool down at least 1 little
Time.
6. according to the method for the moisture in the test photoresistance stripper described in claim 1, it is characterised in that: in step
2), in, the volume of absolute methanol is less than step 4) constant volume volumetric flask volume V22/3.
7., according to the method for the moisture in the test photoresistance stripper according to any one of claim 1-6, its feature exists
In: pH value during determination of moisture in described stripper is 5-7.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310232747.5A CN103308654B (en) | 2013-06-13 | 2013-06-13 | For testing the method for moisture in photoresistance stripper |
| PCT/CN2013/078542 WO2014198078A1 (en) | 2013-06-13 | 2013-06-30 | Solution for testing moisture content in photoresist stripping solution and testing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310232747.5A CN103308654B (en) | 2013-06-13 | 2013-06-13 | For testing the method for moisture in photoresistance stripper |
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| CN103308654B true CN103308654B (en) | 2016-08-10 |
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| CN106645556A (en) * | 2016-12-13 | 2017-05-10 | 深圳市华星光电技术有限公司 | Method for detecting moisture content of photoresist |
| CN107121522A (en) * | 2017-06-06 | 2017-09-01 | 深圳市华星光电技术有限公司 | A kind of method for detecting photoresistance acid-base value |
| CN107328729B (en) * | 2017-08-28 | 2021-01-29 | Tcl华星光电技术有限公司 | Method and system for measuring components of stripping liquid medicine |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0036487A1 (en) * | 1980-03-19 | 1981-09-30 | MERCK PATENT GmbH | Karl Fischer reagent without pyridine and method for the determination of water using this reagent |
| CN1403877A (en) * | 2001-06-25 | 2003-03-19 | 株式会社平间理化研究所 | Nonaqueous protective film stripping liquid handling apparatus and nonaqueous protective film stripping liquid handling method |
| KR20030059842A (en) * | 2001-12-28 | 2003-07-12 | 대정화금주식회사 | One-component reagent for karl-fisher coulometric titration |
| KR20090080206A (en) * | 2008-01-21 | 2009-07-24 | 동우 화인켐 주식회사 | Photoresist stripper composition and exfoliation method of a photoresist using the same |
| KR20110019027A (en) * | 2009-08-19 | 2011-02-25 | 동우 화인켐 주식회사 | Stripper composition for photoresist or photoresist ashing residue and stripping method of photoresists using the same |
| CN102004399A (en) * | 2009-08-31 | 2011-04-06 | 气体产品与化学公司 | Water-rich stripping and cleaning formulation and method for using same |
| CN102472985A (en) * | 2009-08-11 | 2012-05-23 | 东友Fine-Chem股份有限公司 | Resist stripping solution composition, and method for stripping resist by using same |
| CN102590443A (en) * | 2012-03-07 | 2012-07-18 | 江苏永华精细化学品有限公司 | Safe stable type Karl Fischer reagent and preparation method thereof |
| CN102880017A (en) * | 2012-09-28 | 2013-01-16 | 京东方科技集团股份有限公司 | Stripping liquid composition for photoresist and preparation and applications of stripping liquid composition |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5597420A (en) * | 1995-01-17 | 1997-01-28 | Ashland Inc. | Stripping composition having monoethanolamine |
| JP3093975B2 (en) * | 1996-07-02 | 2000-10-03 | 株式会社平間理化研究所 | Resist stripper management system |
| KR101266897B1 (en) * | 2006-03-03 | 2013-05-23 | 주식회사 동진쎄미켐 | A recycling method for resist stripper scrapped and a recycling device for same |
-
2013
- 2013-06-13 CN CN201310232747.5A patent/CN103308654B/en not_active Expired - Fee Related
- 2013-06-30 WO PCT/CN2013/078542 patent/WO2014198078A1/en active Application Filing
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0036487A1 (en) * | 1980-03-19 | 1981-09-30 | MERCK PATENT GmbH | Karl Fischer reagent without pyridine and method for the determination of water using this reagent |
| CN1403877A (en) * | 2001-06-25 | 2003-03-19 | 株式会社平间理化研究所 | Nonaqueous protective film stripping liquid handling apparatus and nonaqueous protective film stripping liquid handling method |
| KR20030059842A (en) * | 2001-12-28 | 2003-07-12 | 대정화금주식회사 | One-component reagent for karl-fisher coulometric titration |
| KR20090080206A (en) * | 2008-01-21 | 2009-07-24 | 동우 화인켐 주식회사 | Photoresist stripper composition and exfoliation method of a photoresist using the same |
| CN102472985A (en) * | 2009-08-11 | 2012-05-23 | 东友Fine-Chem股份有限公司 | Resist stripping solution composition, and method for stripping resist by using same |
| KR20110019027A (en) * | 2009-08-19 | 2011-02-25 | 동우 화인켐 주식회사 | Stripper composition for photoresist or photoresist ashing residue and stripping method of photoresists using the same |
| CN102004399A (en) * | 2009-08-31 | 2011-04-06 | 气体产品与化学公司 | Water-rich stripping and cleaning formulation and method for using same |
| CN102590443A (en) * | 2012-03-07 | 2012-07-18 | 江苏永华精细化学品有限公司 | Safe stable type Karl Fischer reagent and preparation method thereof |
| CN102880017A (en) * | 2012-09-28 | 2013-01-16 | 京东方科技集团股份有限公司 | Stripping liquid composition for photoresist and preparation and applications of stripping liquid composition |
Non-Patent Citations (4)
| Title |
|---|
| 几种卡尔费休氏水分测定法;王晨 等;《药物分析杂志》;20081231;第28卷(第12期);第2145页右栏第2段、第2146页左栏第1-2段 * |
| 卡尔费休容量滴定法测定混胺燃料中水含量;王菊香等;《化学分析计量》;20130131;第22卷(第1期);第67-69页 * |
| 卡尔费休滴定法测定液体推进剂混胺燃料中水分;王菊香 等;《理化检验(化学分册)》;20110218;第47卷(第2期);第219页左栏第2-7段和右栏第1-3段 * |
| 用尿素作为基本成分的无吡啶卡尔-费休试剂;M·波斯;《湖南化工》;19861231(第2期);第59-61页 * |
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| CN103308654A (en) | 2013-09-18 |
| WO2014198078A1 (en) | 2014-12-18 |
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