CN107995960B - Anticorrosive additive stripping liquid controlling - Google Patents
Anticorrosive additive stripping liquid controlling Download PDFInfo
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- CN107995960B CN107995960B CN201680034620.4A CN201680034620A CN107995960B CN 107995960 B CN107995960 B CN 107995960B CN 201680034620 A CN201680034620 A CN 201680034620A CN 107995960 B CN107995960 B CN 107995960B
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
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- Exposure Of Semiconductors, Excluding Electron Or Ion Beam Exposure (AREA)
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Abstract
In the manufacturing process of semiconductor device etc., solidified under high-temperature all the time, the solidification for avoiding resist is bad.Therefore, it is necessary to the strippers stronger than previous peeling force.A kind of anticorrosive additive stripping liquid controlling is, characterized by comprising: secondary amine；It include 1,3- dimethyl-2-imidazolinone (DMI) and water as polar solvent；As the hydrazine of additive, aforementioned water is 10.0 mass % more than or lower than 31.0 mass %, can remove the resist baked through high temperature, the corrosion of film surface, section will not occur.
Description
Technical field
The present invention relates to a kind of stripper, it is used to remove in the display equipment, semiconductor when institute such as manufacture liquid crystal, organic EL
The resist used is more specifically related to even if for that can remove resist resist film through baking firmly, and then can be with
It says to aluminium film and copper film substantially also incorrosive anticorrosive additive stripping liquid controlling.
Background technique
The flat-panel monitors (FPD) such as liquid crystal, organic EL (Electro-Luminescence) require large screen.It is another
Aspect is used, it is desirable that small-sized fine screen as notebook PC, tablet PC, smart phone.It is used as large screen, benefit can be used
With Cu wiring or Cu/Mo stacking wiring (hereinafter referred to as " Cu wiring ".) thin film transistor (TFT) (TFT:Thin Film
Transistor).In addition, using as small-sized fine screen, the TFT that Al wiring is utilized can be used.It should be noted that with
Lower Cu is also referred to as copper, Mo is also referred to as molybdenum, Al is also referred to as aluminium.
In panel manufacturing plant quotient, also there is the TFT for having produced and used Cu wiring in a factory and make Cu wiring and Al
The case where TFT made of wiring is mixed in.When TFT made of production is mixed in Cu wiring and Al wiring, in the removing of resist film
In process, as long as anticorrosive additive stripping liquid controlling can be shared when being routed using Al and when being routed using Cu, it will be able to reduce production
Cost and equipment.
Water-based positive light anti-etching agent is usually the composition for including alkanolamine, polar solvent, water with stripper, anti-
40 or more and 50 DEG C or less Zuo You are heated in erosion agent stripping off device to use.
Alkanolamine is for being made by nucleation as the alkali insolubilizing agent in positive light anti-etching agent stripper
The carbonyl of DNQ (diazo naphthoquinone) compound ingredient necessary to solubilising in polar solvent and water.Alkanolamine is according to first with nitrogen
Element in conjunction with hydrogen other than substituent group number and be divided into primary amine, secondary amine, tertiary amine.In these, it is known that series is smaller then alkaline
It is stronger, nucleophilicity is also stronger.
Therefore, the small alkanolamine of series, makes the DNQ compound as alkali insolubilizing agent in polar solvent, water
The ability of solubilising is stronger, plays the resist stripping performance of strength.
On the other hand, it is known that alkanolamine has chelation to Cu.Keep Cu solubilized the chelation of Cu, therefore meeting
Corrode Cu film.The series of alkanolamine is smaller stronger for the chelation of Cu in the same manner as alkalinity, nucleophilicity.Therefore,
The small alkanolamine of series more consumingly corrodes Cu film.
At amorphous silicon (hereinafter also referred to " a-Si ".), low temperature polycrystalline silicon (hereinafter also referred to " LTPS ".), oxide partly leads
Body (hereinafter also referred to " IGZO ".) etc semiconductor fine in the production technology of TFT, resist in dry etch sequence
Erosion agent is modified because impaired, becomes difficult to removing resist sometimes.It is believed that this is because constituting the DNQization of positive-workingresist film
Conjunction object polymerize caused by excessively carrying out with novolac resin.
Al wiring not will receive the corrosiveness as caused by alkanolamine (chelation).Therefore, modified in order to remove
Resist, usually using the alkanolamine of the primary amine of the stripping performance with strength.
On the other hand, the case where Cu is routed, if using primary amine or the alkanolamine of secondary amine, the corruption of most cases Cu wiring
Erosion can reach unacceptable degree.Therefore, it is proposed to the stripper of the alkanolamine using tertiary amine.The alkanolamine pair of tertiary amine
The chelation of Cu is weak, can inhibit the corrosion of Cu film in the range of not going wrong in practical.However, alkalinity, nucleophilic
Property is also weak in the same manner as chelation, and compared with having used the anticorrosive additive stripping liquid controlling of alkanolamine of primary amine or secondary amine, there are anti-
Lose the weak such disadvantage of agent peeling force.
Under such technical background, needs and the Al wiring of the alkanolamine of primary amine has been used to have with anticorrosive additive stripping liquid controlling
There is the stripping performance of the same and above degree, and can be used in the anticorrosive additive stripping liquid controlling composition of both Cu wiring, Al wiring.
In addition, disclosing the anticorrosive additive stripping liquid controlling comprising (1) formula compound represented and solvent in patent document 1.This is anti-
Losing agent stripper can also share in the resist stripping process that Cu is routed and Al is routed.
In addition, disclosing in patent document 2: the alkanolamine of tertiary amine all has and has used primary amine whether or not using
The anticorrosive additive stripping liquid controlling of the same peeling force of the Al wiring anticorrosive additive stripping liquid controlling of alkanolamine.The stripper includes tertiary amine, pole
Property solvent, water, cyclic amine, sugar alcohol and reducing agent, the five-membered cyclic amine is that have nafoxidine or the four of 3 substds
The composition of hydrogen pyrroles.
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2012-514765 bulletin (patent 5279921)
Patent document 2: Japanese Unexamined Patent Publication 2016-085378 bulletin (patent 5885041)
Summary of the invention
Problems to be solved by the invention
The stripper of patent document 2 can be routed in Cu (comprising Cu/Mo stacking wiring) and the resist removing of Al wiring
It is shared in process.In addition, can also remove resist film even if implementing hard baking to resist film.
However, disposably to be handled more massive substrate at the scene using resist manufacture semiconductor device.
Therefore, the failure in 1 photo-mask process, which will lead to, disposably generates a large amount of substandard products.Therefore, in each process of photoetching
Using secure context operation as operating parameter.
Specifically, carrying out solidification at a higher temperature in the curing process of resist, consolidating for resist is avoided
Change bad such problems.However, at the same time, it is meant that need the stripper stronger than previous peeling force.
The solution to the problem
The present invention is expected in view of the above subject, is provided even if being to be higher than made of previous high-temperature bakes and resist
Agent is lost, the anticorrosive additive stripping liquid controlling of removing is also able to carry out.Certainly much less, do not require nothing more than peeling force it is strong but also require for
Corrosivity as Cu, Mo and Al is low.
More specifically, about anticorrosive additive stripping liquid controlling of the invention, characterized by comprising:
Secondary amine；
It include 1,3- dimethyl-2-imidazolinone (DMI) and water as polar solvent；And
As the hydrazine of additive,
Aforementioned water is 10.0 mass % more than or lower than 31.0 mass %.
The effect of invention
Anticorrosive additive stripping liquid controlling of the invention has used secondary amine, therefore even if to be resisted with being higher than made of previous high temperature bakes
Agent is lost, also can reliably be removed.In turn, anticorrosive additive stripping liquid controlling of the invention includes 1,3-Dimethyl-2-imidazolidinone
(DMI) it is used as polar solvent, therefore regardless of whether contain secondary amine, can inhibit to corrosion of metal as Cu, Mo, Al.
In addition, the secondary amine that anticorrosive additive stripping liquid controlling of the invention has used boiling point high, therefore be able to carry out after use again sharp
With.
In addition, the bath service life of anticorrosive additive stripping liquid controlling of the invention is excellent, even if placing 12 hours under atmosphere opening state
Above or even if closed save 4 days, resist stripping ability will not change.
Detailed description of the invention
Fig. 1 is the cone angle for illustrating Cu/Mo stacked film and the figure of Mo undercutting.
Specific embodiment
Anticorrosive additive stripping liquid controlling of the invention is illustrated below.It should be noted that the following description shows the present invention
Photoresist stripper an embodiment, without departing from the scope of the subject in the invention can be to embodiment party below
Formula and embodiment are changed.It should be noted that in the present specification, indicate to use when range " more than " and " following " be
Refer to " comprising the value and being greater than the value " and " comprising the value and being less than the value "." not comprising the value and it is less than in addition, " being lower than " refers to
The value ".
The resist film that anticorrosive additive stripping liquid controlling of the invention is removed is assumed to positive-workingresist.In positive-workingresist, make
Include the resin of novolaks system for resin, uses diazo naphthoquinone (DNQ) compound as emulsion.When being etched, in base
Resist film is formed on plate, is exposed across pattern.
DNQ compound is set to become indone by the exposure.When indone and water associate, becomes indene carboxylic acid and be dissolved in water.Phenol
The resin of Novolac system has the property for being dissolved in aqueous slkali originally, but protects dissolved click by DNQ compound.DNQ chemical combination
Object goes bad due to exposure, is dissolved in the developer solution comprising water, to also novolac resin be made to dissolve out.Thus resist is completed
The patterning of film.
Patterned substrate warp, which is completed, by resist film bakes and implement later wet etching or dry etching processing.
Bake afterwards be in order to make the novolac resin in resist film and DNQ compound polymerize be able to carry out to a certain extent and
Implement.Heat treatment in 5 minutes or so is carried out usually at 140 DEG C.Hard bake refers at 170 DEG C in the present specification
30 minutes or more heating conditions.When stoving temperature rises, novolac resin and DNQ compound can promptly polymerize and firm
Admittedly be bonded to the metal film of substrate, it becomes difficult to dissolve.Anticorrosive additive stripping liquid controlling of the invention will also pass through such hard baking
Made of resist film as object.
Anticorrosive additive stripping liquid controlling of the invention includes secondary amine, polar solvent and reducing agent.As secondary amine, it is expected that boiling point is higher than
Water, and and secondary amine of the water without azeotropic.The reason is that, being separated when being recycled to stripper with water.As in this way
Substance, N- methylethanolamine (hereinafter also referred to " MMA " can be properly used.Boiling point is 155 DEG C.CAS model 109-83-
1), N- ehtylethanolamine (hereinafter also referred to " EEA ".170 DEG C of boiling point.CAS model 110-73-6).Them can also be mixed.
In addition, mentioned component is advisable, preferably relative to stripper total amount with 0.5 mass % or more and 9.0 mass % or less
For 1.0 mass % or more and 8.0 mass % or less, most preferably 2.0 mass % or more and 7.0 mass % or less.When secondary amine is few,
The resist baked firmly can not be removed.On the other hand, when excessive, damaged metal becomes larger.It should be noted that as performance,
It confirmed to go wrong for required performance even if containing 9.0 mass %.
As polar solvent, as long as organic solvent (the referred to as water-miscible organic solvent affinity with water.).
In addition, if with the Combination of above-mentioned secondary amine well if it is more suitable.
As such water-miscible organic solvent, it is (following to be also referred to as that 1,3-Dimethyl-2-imidazolidinone can be properly used
For " DMI ".CAS model 80-73-9).Polar solvent is made of water-miscible organic solvent and water.
It is the amount after the amount for eliminating secondary amine and aftermentioned reducing agent relative to stripper total amount as polar solvent.Specifically
For, it is 90.60 mass % or more and 99.47 mass % or less.
Each material in polar solvent has desired range as follows.Firstly, relative to anticorrosive additive stripping liquid controlling total amount,
Water is suitably 10.0 mass % more than or lower than 31.0 mass %.When dilutional hyponatremia, metal film can occur to corrode Al for the case where Al
Such problems.1,3- dimethyl-2-imidazolinone (DMI) can be the surplus of polar solvent.Only pass through 1,3- dimethyl -2-
Imidazolone (DMI) enables hydrazine stabilization, mitigates secondary amine and hydrazine to the damage on the surface and section of metal film.
As additive, the hydrazine that can properly use reducing agent (is also denoted as " HN " below.CAS model 302-01-2).
The addition of reducing agent inhibits the undercutting of the Mo as caused by secondary amine.Relative to anticorrosive additive stripping liquid controlling total amount, reducing agent is desired for 0.03 matter
Measure % or more and 0.4 mass % range below.More preferably 0.06 mass % or more and 0.2 mass % range below.It needs
It is noted that hydrazine also can be used hydrate and (hydrazine monohydrate: be denoted as " HN from the viewpoint of safely operating
H2O”。)。
[embodiment]
The embodiment and comparative example of anticorrosive additive stripping liquid controlling of the invention described below.For " resist fissility ", " metal
The corrosivity of film " and this 3 points of " bath service life " have rated anticorrosive additive stripping liquid controlling.
< resist fissility >
The silicon thermal oxidation film for forming 100nm on a silicon substrate, forms 300nm thickness using sputtering method on silicon thermal oxidation film
Copper film.Positive-workingresist liquid is coated on the copper film by rotary coating and has made resist film.Keep resist film dry
After dry, it is exposed using the mask of wiring pattern.Then the resist of photosensitive part is removed by developer solution.That is, being in copper
There is the state of the part for the resist film for having remained wiring pattern and the part of copper film exposing on film.Then right at 170 DEG C
Silicon substrate integrally carries out rear baking in 30 minutes.
Then, using the etchant of the copper of hydrogen peroxide system, the copper film of exposing is etched, is removed.The etching of copper film
After, the resist film on the pattern of remaining copper is removed using sample anticorrosive additive stripping liquid controlling.Place for removing
The reason time is set as 15 minutes, measures the time until removing.Carrying out that interference edges see whether with optical microscopy side can
Removing, is thus judged.
Even across 15 minutes, it is the case where also confirming the residual of resist film on copper film "×" (fork), not
The case where confirming the residual of resist film is "○" (circle).In the case, the time that also record removing is completed.It needs
Bright, "○" (circle) indicates successfully or qualified, and "×" (fork) indicates failure or unqualified.Evaluation below is also identical.
The corrosivity > of < metal film
The corrosivity of metal film is evaluated as follows.Firstly, forming the silicon thermal oxidation of 100nm thickness on a silicon substrate
Film.Then, the molybdenum film that 20nm thickness is formed on silicon thermal oxidation film on a silicon substrate, is then formed on 300nm thickness
Copper film has made the stacking membrane sample of Cu/Mo.It is denoted as " Cu/Mo ".In addition, shape on silicon thermal oxidation film on a silicon substrate
At the aluminium film of 300nm thickness, Al membrane sample has been made.It is denoted as " Al ".
The resist that patterned wiring shape is formed on these evaluation samples, the substrate as erosion analysis.
That is, any one for being formed by Cu/Mo film, Al film on the silicon thermal oxidation film that substrate includes on a silicon substrate of erosion analysis
Layer；And the resist layer being formed on as wiring shape.
Copper film with or the etchant of aluminium film in these erosion analysis with substrate carry out accurately etching during make
It impregnates, etches.Then the erosion analysis after etching is immersed in sample anticorrosive additive stripping liquid controlling 4 minutes with substrate, is removed
Resist film.The erosion analysis for being immersed in 4 minutes in sample anticorrosive additive stripping liquid controlling is cleaned with substrate, is dried, so
After observe film surface.In addition, cutting off wiring portion and observing section.
It should be noted that the judgement accurately etched is to play to be able to confirm that by visual observation to silicon thermal oxidation since etching
At the time of when film.
The observation of film surface and section uses scanning electron microscope (SEM:Scanning Electron
Microscope) (Hitachi's system: SU8020 type) carries out under conditions of acceleration voltage 1kV, 30000~50000 times.
The signal of section shape is illustrated in Fig. 1.(a) of Fig. 1 shows the section shape of the case where " Al ".Accurate erosion
The section shape of the part at quarter forms the almost cone angle 5 at 30 ° to 60 ° angles relative to substrate 1.Film portion 2 is Al film.
(b) of Fig. 1 shows the case where " Cu/Mo ".The case where " Cu/Mo ", at least the film portion 2 (Cu) on upper layer, have cone angle 5.
It is expected that the tapered surface 6 along film portion 2 is etched basal layer 3 (Mo).However, film portion 2 can also have as shown in (b) of Fig. 1
Etch residue.
Corrosive evaluation is evaluated as follows by the observation of the cross sectional shape: by the surface 4 in film portion 2, film portion 2 or
The case where the case where 3 any portion of basal layer confirms corrosion is judged as fork (×), does not observe corrosion is judged as circle
(○)。
Especially " Cu/Mo " the case where, as shown in (c) of Fig. 1, sent out between basal layer 3 (Mo) and film portion 2 (Cu) sometimes
Raw corrosion.That is, sometimes since film portion 2 and the interface of basal layer 3 the Mo of basal layer 3 dissolution, Mo (basal layer 3) is earlier than layers of copper
(film portion 2) is selectively etched.Therefore, the case where gap 10 will be confirmed between basal layer 3 and film portion 2, is judged as
Fork (×).
< bathes service life >
Anticorrosive additive stripping liquid controlling is the blend compositions of amine, organic solvent, material as reducing agent.Titanium dioxide in air
Carbon dissolution becomes carbonic acid bicarbonate ion in stripper or reacts with amine and generate carbamate ions, as a result
Lead to that peeling force reduces or damaged metal becomes larger.
Especially in large-scale factory, a large amount of anticorrosive additive stripping liquid controlling is used under atmosphere opening environment.In addition, due to
Anticorrosive additive stripping liquid controlling is recycled, therefore the chance that anticorrosive additive stripping liquid controlling associates with air increases.Therefore, if the bath service life is short,
It then needs to be replaced as frequently as or supplement anticorrosive additive stripping liquid controlling.
As test method, after preparing each anticorrosive additive stripping liquid controlling, placed in the environment of room temperature atmosphere 0 hour, it is 6 small
When, 12 hours time, carry out the test of resist fissility, pass through SEM observation " Cu/Mo ", the surface of " Al " and section shape
State.The case where evaluation method is with for < resist fissility > and < corrosivity > is identical.
In addition, anticorrosive additive stripping liquid controlling is put into and is moved in container.However, if container cannot be saved at normal temperature,
Availability when factory becomes very poor.Therefore, it also studied through the closed composition transfer being stored at room temperature.
Evaluation method is as follows: it is put into closed container, places 4 days at normal temperature, determine the stability of hydrazine.With rigid preparation
It is compared after hydrazine, it is "○" if lower than 1% that the situation for reducing 1% or more, which is "×",.
< sample anticorrosive additive stripping liquid controlling >
Sample anticorrosive additive stripping liquid controlling is prepared for by following main points.
(embodiment 1)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
74.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of embodiment 1.
It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.Hydrazine monohydrate it is residual
The amount of 0.036 remaining mass % is water.Therefore, when the ratio of components of above-mentioned water also includes the amount put into the form of hydrazine monohydrate
It may be said that being 20.036 mass %.In following all embodiment and comparative example, the case where having used hydrazine monohydrate is phase
Same meaning.
(embodiment 2)
N- ehtylethanolamine is used as secondary amine.
5.0 mass % of N- ehtylethanolamine (EEA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
74.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of embodiment 2.
Embodiment 2 is by the N- methylethanolamine (MMA) as the secondary amine of embodiment 1) it is changed to N- ehtylethanolamine
(EEA) composition.It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.Hydrazine monohydrate
The amount of 0.036 remaining mass % be water.Therefore, the ratio of components of above-mentioned water is also included and is put into the form of hydrazine monohydrate
It may be said that being 20.036 mass % when amount.
(embodiment 3)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
70.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
24.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of embodiment 3.
Embodiment 3 is the composition changed to the DMI of the polar solvent of embodiment 1 and the ratio of water.It needs to illustrate
, 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.The 0.036 remaining mass %'s of hydrazine monohydrate
Amount is water.Therefore, when the ratio of components of above-mentioned water also includes the amount put into the form of hydrazine monohydrate it may be said that for 24.036 matter
Measure %.
(embodiment 4)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
68.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
26.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of embodiment 4.
Embodiment 4 is the composition changed to the DMI of the polar solvent of embodiment 1 and the ratio of water.It needs to illustrate
, 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.The 0.036 remaining mass %'s of hydrazine monohydrate
Amount is water.Therefore, when the ratio of components of above-mentioned water also includes the amount put into the form of hydrazine monohydrate it may be said that for 26.036 matter
Measure %.
(embodiment 5)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
66.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
28.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of embodiment 5.
Embodiment 5 is the composition changed to the DMI of the polar solvent of embodiment 1 and the ratio of water.It needs to illustrate
, 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.The 0.036 remaining mass %'s of hydrazine monohydrate
Amount is water.Therefore, when the ratio of components of above-mentioned water also includes the amount put into the form of hydrazine monohydrate it may be said that for 28.036 matter
Measure %.
(embodiment 6)
N- methylethanolamine is used as secondary amine.
2.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
73.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
24.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of embodiment 6.
Embodiment 6 is the reduction of the composition of the amount of the secondary amine of embodiment 1.It should be noted that 0.1 matter of hydrazine monohydrate
Amount % is equivalent to 0.064 mass % of hydrazine.The amount of the 0.036 remaining mass % of hydrazine monohydrate is water.Therefore, the group of above-mentioned water
It may be said that being 24.036 mass % when at than also including the amount put into the form of hydrazine monohydrate.
(embodiment 7)
N- methylethanolamine is used as secondary amine.
3.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
72.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
24.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of embodiment 7.
Embodiment 7 is the reduction of the composition of the amount of the secondary amine of embodiment 1.It should be noted that 0.1 matter of hydrazine monohydrate
Amount % is equivalent to 0.064 mass % of hydrazine.The amount of the 0.036 remaining mass % of hydrazine monohydrate is water.Therefore, the group of above-mentioned water
It may be said that being 24.036 mass % when at than also including the amount put into the form of hydrazine monohydrate.
(embodiment 8)
N- methylethanolamine is used as secondary amine.
4.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
71.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
24.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of embodiment 8.
Embodiment 8 is the reduction of the composition of the amount of the secondary amine of embodiment 1.It should be noted that 0.1 matter of hydrazine monohydrate
Amount % is equivalent to 0.064 mass % of hydrazine.The amount of the 0.036 remaining mass % of hydrazine monohydrate is water.Therefore, the group of above-mentioned water
It may be said that being 24.036 mass % when at than also including the amount put into the form of hydrazine monohydrate.
(embodiment 9)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
70.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
24.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of embodiment 9.
Embodiment 9 is and the same amount of composition of the amount of the secondary amine of embodiment 1.But the amount of water is different from embodiment 1.It needs
It is noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.The 0.036 remaining matter of hydrazine monohydrate
The amount for measuring % is water.Therefore, it may be said that being when the ratio of components of above-mentioned water also includes the amount put into the form of hydrazine monohydrate
24.036 quality %.
(embodiment 10)
N- methylethanolamine is used as secondary amine.
6.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
69.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
24.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of embodiment 10.
Embodiment 10 is the composition for increasing the amount of secondary amine of embodiment 1.It should be noted that the 0.1 of hydrazine monohydrate
Quality % is equivalent to 0.064 mass % of hydrazine.The amount of the 0.036 remaining mass % of hydrazine monohydrate is water.Therefore, above-mentioned water
When ratio of components also includes the amount put into the form of hydrazine monohydrate it may be said that for 24.036 mass %.
(embodiment 11)
N- methylethanolamine is used as secondary amine.
7.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
68.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
24.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of embodiment 11.
Embodiment 11 is the composition for increasing the amount of secondary amine of embodiment 1.It should be noted that the 0.1 of hydrazine monohydrate
Quality % is equivalent to 0.064 mass % of hydrazine.The amount of the 0.036 remaining mass % of hydrazine monohydrate is water.Therefore, above-mentioned water
When ratio of components also includes the amount put into the form of hydrazine monohydrate it may be said that for 24.036 mass %.
(comparative example 1)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and N-METHYLFORMAMIDE.
74.9 mass % of N-METHYLFORMAMIDE (NMF:CAS model 123-39-7)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 1.
Comparative example 1 is that the 1,3- dimethyl-2-imidazolinone (DMI) of the polar solvent of embodiment 1 is changed to N- methyl
The composition of formamide (NMF).It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.Hydrazine one
The amount of the 0.036 remaining mass % of hydrate is water.Therefore, the ratio of components of above-mentioned water also includes in the form of hydrazine monohydrate
It may be said that being 20.036 mass % when the amount of investment.
(comparative example 2)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and N,N-dimethylformamide.
74.9 mass % of N,N-dimethylformamide (DMF:CAS model 68-12-2)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 2.
Comparative example 2 is that the 1,3- dimethyl-2-imidazolinone (DMI) of the polar solvent of embodiment 1 is changed to N, N- bis-
The composition of methylformamide (DMF).It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.
The amount of the 0.036 remaining mass % of hydrazine monohydrate is water.Therefore, the ratio of components of above-mentioned water also includes with hydrazine monohydrate
It may be said that being 20.036 mass % when the amount of form investment.
(comparative example 3)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 2-Pyrrolidone.
74.9 mass % of 2-Pyrrolidone (2P:CAS model 616-45-5)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 3.
Comparative example 3 is that the 1,3- dimethyl-2-imidazolinone (DMI) of the polar solvent of embodiment 1 is changed to 2- pyrroles
The composition of alkanone (2P).It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.Hydrazine one is hydrated
The amount of the 0.036 remaining mass % of object is water.Therefore, the ratio of components of above-mentioned water is also included and is put into the form of hydrazine monohydrate
Amount when it may be said that be 20.036 mass %.
(comparative example 4)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1-Methyl-2-Pyrrolidone.
74.9 mass % of 1-Methyl-2-Pyrrolidone (NMP:CAS model 872-50-4)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 4.
Comparative example 4 is that the 1,3- dimethyl-2-imidazolinone (DMI) of the polar solvent of embodiment 1 is changed to 1- methyl-
The composition of 2-Pyrrolidone (NMP).It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.
The amount of the 0.036 remaining mass % of hydrazine monohydrate is water.Therefore, the ratio of components of above-mentioned water also includes with hydrazine monohydrate
It may be said that being 20.036 mass % when the amount of form investment.
(comparative example 5)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and NEP.
74.9 mass % of 1- ethyl-2-pyrrolidone (NEP:CAS model 2687-91-4)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 5.
Comparative example 5 is that the 1,3- dimethyl-2-imidazolinone (DMI) of the polar solvent of embodiment 1 is changed to 1- ethyl-
The composition of 2-Pyrrolidone (NEP).It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.
The amount of the 0.036 remaining mass % of hydrazine monohydrate is water.Therefore, the ratio of components of above-mentioned water also includes with hydrazine monohydrate
It may be said that being 20.036 mass % when the amount of form investment.
(comparative example 6)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and gamma butyrolactone.
74.9 mass % of gamma butyrolactone (GBL:CAS model 96-48-0)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 6.
Comparative example 6 is that the 1,3- dimethyl-2-imidazolinone (DMI) of the polar solvent of embodiment 1 is changed in γ fourth
The composition of ester (GBL).It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.Hydrazine one is hydrated
The amount of the 0.036 remaining mass % of object is water.Therefore, the ratio of components of above-mentioned water is also included and is put into the form of hydrazine monohydrate
Amount when it may be said that be 20.036 mass %.
(comparative example 7)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and ethylene carbonate.
74.9 mass % of ethylene carbonate (EC:CAS model 96-49-1)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 7.
Comparative example 7 is that the 1,3- dimethyl-2-imidazolinone (DMI) of the polar solvent of embodiment 1 is changed to carbonic acid Asia
The composition of ethyl ester (EC).It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.Hydrazine one is hydrated
The amount of the 0.036 remaining mass % of object is water.Therefore, the ratio of components of above-mentioned water is also included and is put into the form of hydrazine monohydrate
Amount when it may be said that be 20.036 mass %.
(comparative example 8)
The N methyldiethanol amine of tertiary amine is used as amine.
5.0 mass % of N methyldiethanol amine (MDEA:CAS model 105-59-9)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
74.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 8.
Comparative example 8 is the N methyldiethanol amine that the N- methylethanolamine (MMA) of the secondary amine of embodiment 1 is changed to tertiary amine
(MDEA) composition.It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.Hydrazine monohydrate
The amount of 0.036 remaining mass % be water.Therefore, the ratio of components of above-mentioned water is also included and is put into the form of hydrazine monohydrate
It may be said that being 20.036 mass % when amount.
(comparative example 9)
The nafoxidine of cyclic amine is used as amine.
1.5 mass % of nafoxidine (PRL:CAS model 123-75-1)
Polar solvent is mixed with water and DMI.
78.4 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 9.
Comparative example 9 is the nafoxidine that the N- methylethanolamine (MMA) of the secondary amine of embodiment 1 is changed to cyclic amine
(PRL) composition.It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.Hydrazine monohydrate
The amount of 0.036 remaining mass % be water.Therefore, the ratio of components of above-mentioned water is also included and is put into the form of hydrazine monohydrate
It may be said that being 20.036 mass % when amount.
(comparative example 10)
The hydroxyethyl piperazine of cyclic amine is used as amine.
5.0 mass % of hydroxyethyl piperazine (OH-PIZ:CAS model 103-76-4)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
74.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 10.
Comparative example 10 is the hydroxyethyl piperazine that the N- methylethanolamine (MMA) of the secondary amine of embodiment 1 is changed to cyclic amine
(OH-PIZ) composition.It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.Hydrazine one is hydrated
The amount of the 0.036 remaining mass % of object is water.Therefore, the ratio of components of above-mentioned water is also included and is put into the form of hydrazine monohydrate
Amount when it may be said that be 20.036 mass %.
(comparative example 11)
The monoethanolamine of primary amine is used as amine.
5.0 mass % of monoethanolamine (MEA:CAS model 141-43-5)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
74.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
20.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 11.
Comparative example 11 is the monoethanolamine (MEA) that the N- methylethanolamine (MMA) of the secondary amine of embodiment 1 is changed to primary amine
Composition.It should be noted that 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.The remnants of hydrazine monohydrate
0.036 mass % amount be water.It therefore, can when the ratio of components of above-mentioned water also includes the amount put into the form of hydrazine monohydrate
To say as 20.036 mass %.
(comparative example 12)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
75.0 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
20.0 mass % of water
Reducing agent is not added.
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 12.Comparative example 12 is to remove
The composition of the hydrazine reducing agent (HN) of embodiment 1.
(comparative example 13)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
74.5 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
20.0 mass % of water
D-sorbite is used as additive.
0.5 mass % of D-sorbite (Stol:CAS model 50-70-4)
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 13.Comparative example 13 is by reality
The additive (reducing agent: hydrazine (HN)) for applying example 1 is changed to the composition of D-sorbite.
(comparative example 14)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
74.5 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
20.0 mass % of water
Diglycerol is used as additive.
0.5 mass % of diglycerol (CAS model 627-82-7)
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 14.Comparative example 14 is by reality
The additive (reducing agent: hydrazine (HN)) for applying example 1 is changed to the composition of diglycerol.
(comparative example 15)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
74.5 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
20.0 mass % of water
Saccharin is used as additive.
0.5 mass % of saccharin (CAS model 81-07-2)
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 15.Comparative example 15 is by reality
The additive (reducing agent: hydrazine (HN)) for applying example 1 is changed to the composition of saccharin.
(comparative example 16)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
74.5 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
20.0 mass % of water
Polyethylene glycol 400 (PEG400) is used as additive.
0.5 mass % of polyethylene glycol 400 (PEG400:CAS model 25322-68-3)
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 16.Comparative example 16 is by reality
The additive (reducing agent: hydrazine (HN)) for applying example 1 is changed to the composition of polyethylene glycol 400.
(comparative example 17)
N- methylethanolamine is used as secondary amine.
5.0 mass % of N- methylethanolamine (MMA)
Polar solvent is mixed with water and 1,3- dimethyl-2-imidazolinone.
63.9 mass % of 1,3- dimethyl-2-imidazolinone (DMI)
31.0 mass % of water
Hydrazine is used as reducing agent.
Hydrazine monohydrate (HNH2O) 0.1 mass %
The above ingredient is mixed and is made the sample anticorrosive additive stripping liquid controlling of comparative example 17.
Comparative example 17 is the composition that the amount of the water of embodiment 1 is increased to 31.0 mass % from 20.0 mass %.It needs
Bright, 0.1 mass % of hydrazine monohydrate is equivalent to 0.064 mass % of hydrazine.The 0.036 remaining mass % of hydrazine monohydrate
Amount be water.Therefore, it may be said that being 31.036 when the ratio of components of above-mentioned water also includes the amount put into the form of hydrazine monohydrate
Quality %.
By the composition and evaluation result is shown in table 1 of embodiment 1 and comparative example 1~7.In addition, by Examples 1 and 2 and comparing
The composition of example 8~11 and evaluation result is shown in table 2.In addition, the composition and evaluation result of embodiment 1 and comparative example 12~16 are shown
In table 3.In addition, by the composition and evaluation result is shown in table 4 of embodiment 1,3~5 and comparative example 17.In addition, by embodiment 6~11
Composition and evaluation result is shown in table 5.[table 1]
Table 1 shows the composition and evaluation result of embodiment 1 and comparative example 1~7.Referring to embodiment 1.Secondary amine is used as amine
N- methylethanolamine (MMA), the mixed liquor of only 1,3-Dimethyl-2-imidazolidinone (DMI) and water is used as polar solvent,
The resist baked is removed under the conditions of thus, it is possible to as 170 DEG C, 30 minutes in 4 minutes.In addition, " Cu/Mo " and
The damage of the film of " Al " is also good.
In addition, bath service life when stripper is placed under atmosphere opening state, even across 12 hours, peeling force is not yet
It changes.In turn, in the case where closed save 4 days, the reduction of hydrazine is not observed yet.
Comparative example 1 replaces the 1,3- dimethyl-2-imidazolinone (DMI) of the polar solvent of embodiment 1 to use N- methyl
Formamide (NMF).
Comparative example 2 has used N,N-dimethylformamide (DMF) instead of DMI.
Comparative example 3 has used 2-Pyrrolidone (2P) instead of DMI.
Comparative example 4 has used 1-Methyl-2-Pyrrolidone (NMP) instead of DMI.
Comparative example 5 has used 1- ethyl-2-pyrrolidone (NEP) instead of DMI.
Comparative example 6 has used gamma butyrolactone (GBL) instead of DMI.
Comparative example 7 has used ethylene carbonate (EC) instead of DMI.
Comparative example 1 is removed well for fissility immediately after preparation.However, if putting in an atmosphere in advance
It sets, is then damaged in the section of " Cu/Mo " and surface.In addition, observing the reduction of hydrazine if placing 4 days closed.
Comparative example 2 is also removed well for fissility immediately after preparation.However, if in advance in an atmosphere
It places, is then damaged after 12h in the section of " Cu/Mo " and surface.In addition, being observed if being placed 4 days closed
The reduction of hydrazine.
Fissility immediately after preparation does not occur for comparative example 3, place 12 hours in atmosphere after the problem of damaging metal film.So
And if being placed 4 days closed, observe the reduction of hydrazine.
Fissility immediately after preparation does not occur yet for comparative example 4, place 12 hours in atmosphere after the problem of damaging metal film.So
And if being placed 4 days closed, observe the reduction of hydrazine.
Fissility immediately after preparation does not occur yet for comparative example 5, place 12 hours in atmosphere after the problem of damaging metal film.So
And if being placed 4 days closed, observe the reduction of hydrazine.
Comparative example 6 is removed well for fissility immediately after preparation.However, the section of " Cu/Mo " and
Surface is damaged.Therefore, it for bathing the service life, is not tested.
Comparative example 7 cannot remove the resist film baked firmly immediately after preparation.Therefore, it for bathing the service life, is not tested.
As described above, the N- methylethanolamine (MMA) for using secondary amine of embodiment 1, using only 1,3- as polar solvent
The mixed liquor of dimethyl-2-imidazolinone (DMI) and water, the stripper comprising hydrazine obtain stripping ability and bath service life
Good result.
[table 2]
Table 2 shows the composition and evaluation result of Examples 1 and 2 and comparative example 8~11.Embodiment 1 be disclose again, so
It is indicated with bracket.Embodiment 2 is the feelings for replacing N- methylethanolamine (MMA) to use N- ehtylethanolamine (EEA) as secondary amine
Condition.Embodiment 2 is also good similarly to Example 1 for peeling force and to the damage of metal and bath service life.
Comparative example 8~11 is the case where changing amine.Comparative example 8 is the N methyldiethanol amine that tertiary amine has been used as amine
(MDEA) the case where.In addition, the case where comparative example 9 is nafoxidine (PRL) for having used cyclic amine, comparative example 10 is to use
The case where hydroxyethyl piperazine (OH-PIZ) of cyclic amine.Comparative example 11 is the example for having used the monoethanolamine (MEA) of primary amine.
Comparative example 8,9,10 fails to remove the resist baked firmly.Therefore, it for bathing the service life, is not tested.In addition,
The monoethanolamine (MEA) of primary amine can remove the resist baked firmly immediately after preparation, but make " Cu/Mo " surface and section by
Damage.Therefore, the test in relation to bathing the service life is not carried out for comparative example 11 yet.
[table 3]
Table 3 shows the composition and evaluation result of embodiment 1 and comparative example 12~16.Embodiment 1 be show again, so with
Bracket indicates.Comparative example 12 is that hydrazine (hydrazine monohydrate (HNH is not added2O composition)).Comparative example 12 immediately after preparation can
Remove the resist baked firmly.However, the membrane damage of " Cu/Mo " occurs.
Comparative example 13 joined D-sorbite (Stol) as additive.In addition, comparative example 14 joined as additive
Diglycerol.Comparative example 13, comparative example 14 are failing to remove the resist baked firmly immediately after preparation.
Comparative example 15 joined saccharin as additive.In addition, comparative example 16 joined polyethylene glycol 400 as additive
(PEG400).Comparative example 15 and comparative example 16 can remove the resist baked firmly immediately after preparation.However, two comparative examples are equal
Damage is generated to the section of " Cu/Mo ".
According to result above it can be said that hydrazine (hydrazine monohydrate (HNH2It O)) is material needed for stripper of the invention.
[table 4]
Table 4 shows the composition and evaluation result of embodiment 1,3~5 and comparative example 17.Embodiment 1 be show again, so
It is indicated with bracket.Table 4 is the quantifier elimination for water.Amount of moisture is set as 24.0 mass % by embodiment 3, and embodiment 4 is by moisture
Amount is set as 26.0 mass %, and amount of moisture is set as 28.0 mass % by embodiment 5.On the other hand, comparative example 17 increases amount of moisture
To 31.0 mass %.
Other compositions are same as Example 1.Therefore, for peeling force, bath service life, all samples do not go wrong.So
And the comparative example 17 that amount of moisture increases to 31.0 mass % is corroded on the surface of " Al " and section.It can by result above
Know, amount of moisture has to be lower than 31.0 mass %.
[table 5]
Table 5 shows the composition and evaluation result of embodiment 6~11.Embodiment 6~11 has studied the amount of amine.The amount of water is complete
Portion is unified for 24.0 mass %.In addition, the composition arrangement formed at most that the amount of table arrangement from amine is few.The N- methyl of embodiment 6
Ethanol amine (MMA) is 2.0 mass %, and embodiment 7 is 3.0 mass %, embodiment 8 is 4.0 mass %.These are amine less than implementation
The composition of the ratio of components (5.0 mass %) of the N- methylethanolamine (MMA) of example 1.It should be noted that the amount of the amine of embodiment 9
Ratio of components with the MMA of embodiment 1 is all 5.0 mass %.
Embodiment 10 is the case where N- methylethanolamine (MMA) is 6.0 mass %, and embodiment 11 is N- methylethanolamine
(MMA) be 7.0 mass % the case where.Embodiment 10 and 12 is that the amount of N- methylethanolamine (MMA) is more than the composition of embodiment 1.
For peeling force, the damage to metal surface and bath service life, the Arbitrary Samples of embodiment 6~11 shown in table 5 are equal
It is good similarly to Example 1.That is, even if N- methylethanolamine (MMA) is modulated with the high concentration of 7.0 mass %, property
It can will not go wrong.That is, the case where composition of the invention, for amine, even if blending ratio as defined in deviateing, performance
It is not in problem.
Industrial availability
Anticorrosive additive stripping liquid controlling of the invention can be reliably peeled the especially resist through baking firmly, can suitably use
In using photoresist the case where.
Description of symbols
1 substrate
2 film portions
3 basal layers
4 (film portion) surfaces
5 cone angles
10 (between the Mo layer of substrate and Cu layers) gaps
Claims (1)
1. a kind of anticorrosive additive stripping liquid controlling, which is characterized in that it is the anticorrosive additive stripping liquid controlling for removing resist,
The anticorrosive additive stripping liquid controlling is constituted as follows:
0.5 mass % or more and 9.0 mass % secondary amine below,
0.03 mass % or more and 0.4 mass % hydrazine below,
Water of the 10.0 mass % more than or lower than 31.0 mass % and
The 1,3- dimethyl-2-imidazolinone (DMI) of surplus.
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| PCT/JP2016/004436 WO2018061064A1 (en) | 2016-09-30 | 2016-09-30 | Resist removal liquid |
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| KR100718527B1 (en) * | 2006-04-12 | 2007-05-16 | 테크노세미켐 주식회사 | Stripper composition for negative photoresist |
| CN101681129A (en) * | 2007-05-15 | 2010-03-24 | 长瀬化成株式会社 | Photoresist remover composition |
| CN105659167A (en) * | 2013-10-18 | 2016-06-08 | 松下知识产权经营株式会社 | Resist-stripping liquid |
| CN105723284A (en) * | 2013-09-02 | 2016-06-29 | 松下知识产权经营株式会社 | Resist remover liquid |
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Also Published As
| Publication number | Publication date |
|---|---|
| JPWO2018061064A1 (en) | 2018-10-04 |
| CN107995960A (en) | 2018-05-04 |
| JP6160893B1 (en) | 2017-07-12 |
| WO2018061064A1 (en) | 2018-04-05 |
| TWI629353B (en) | 2018-07-11 |
| TW201814036A (en) | 2018-04-16 |
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