CN108235741A - Anticorrosive additive stripping liquid controlling - Google Patents
Anticorrosive additive stripping liquid controlling Download PDFInfo
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- CN108235741A CN108235741A CN201680042942.3A CN201680042942A CN108235741A CN 108235741 A CN108235741 A CN 108235741A CN 201680042942 A CN201680042942 A CN 201680042942A CN 108235741 A CN108235741 A CN 108235741A
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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
- 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
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Exposure Of Semiconductors, Excluding Electron Or Ion Beam Exposure (AREA)
- Photosensitive Polymer And Photoresist Processing (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
In the manufacturing process of semiconductor device etc., cured under high-temperature all the time, the curing 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, it includes：As at least one of the primary amine of amine or secondary amine；Diethylene glycol monoethyl ether (EDG) and propylene glycol (PG) and water as polar solvent；And the hydrazine as additive, aforementioned amine is more than 3.0 mass % and is below 20.0 mass %, aforementioned diethylene glycol monoethyl ether is more than 39.5 mass % and is below 59.5 mass %, aforementioned water is more than 5.18 mass % and less than 28.18 mass %, more than 0.064 mass % and for 1.28% hereinafter, the anticorrosive additive stripping liquid controlling can remove the resist film baked through high temperature the corrosion of metallic film surface, section will not occur for aforementioned hydrazine, in addition, regeneration efficiency when recycling is good.
Description
Technical field
The present invention relates to a kind of strippers, are used to remove in manufacture liquid crystal, organic EL when display equipment, semiconductor when institute
The resist film used more specifically, is related to even if for that can be removed resist film through baking firmly, and then can be with
Say the anticorrosive additive stripping liquid controlling that will not substantially corrode to aluminium film and copper film.
Background technology
The flat-panel monitors (FPD) such as liquid crystal, organic EL (Electro-Luminescence) require large screen.It is another
Aspect, as notebook PC, tablet PC, smart mobile phone purposes, it is desirable that small-sized fine screen.As large screen purposes, can make
With being utilized, Cu is connected up or wiring (hereinafter referred to as " Cu wirings " is laminated in Cu/Mo.) thin film transistor (TFT) (TFT：Thin Film
Transistor).In addition, as small-sized fine screen purposes, the TFT that Al wirings are utilized can be used.It should be noted that
Following 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 that Cu wirings have been produced and used in a factory and make Cu wirings and Al
Connect up the situation of TFT being mixed in.When production makes the TFT that Cu wirings and Al wirings are mixed in, in the stripping of resist film
In process, as long as anticorrosive additive stripping liquid controlling can be shared when Al is used to connect up and when Cu is used to connect up, it will be able to reduce production
Cost and equipment.
Water-based positive light anti-etching agent typically includes the composition of alkanolamine, polar solvent, water with stripper, anti-
40 DEG C or more and less than 50 DEG C Zuo You are heated to use in erosion agent stripping off device.
Alkanolamine is the DNQ of alkali insolubilizing agent for making to be used as in positive light anti-etching agent film by nucleation
The carbonyl of (diazo naphthoquinone) compound ingredient necessary to solubilising in polar solvent and water.Alkanolamine according to nitrogen knot
The number of substituent group other than the hydrogen of conjunction and be divided into primary amine, secondary amine, tertiary amine.It is known that the smaller then alkaline stronger, nucleophilic of series
Property is also stronger.
Therefore, the small alkanolamine of series, makes the DNQ compounds as alkali insolubilizing agent in polar solvent, water
The ability of solubilising is stronger, plays the resist stripping performance of strength (also referred to as " resist peeling force ".).
On the other hand, it is known that alkanolamine has chelation to Cu.Make Cu solubilized, therefore meeting the chelation of Cu
Corrode Cu films.The smaller chelation for Cu of series of alkanolamine is stronger in the same manner as alkalinity, nucleophilicity.Therefore,
The small alkanolamine of series more consumingly corrodes Cu films.
At non-crystalline 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 ".) as semiconductor fine in the production technology of TFT, have in dry etch sequence
When resist is modified when impaired, becomes difficult to stripping resist.It is believed that this is because form the DNQization of positive-workingresist film
Conjunction object polymerize with novolac resin caused by excessively carrying out.
Al wirings will not be by the corrosiveness (chelation) of alkanolamine.Therefore, in order to remove modified resist,
Usually using the alkanolamine of the primary amine of the resist stripping performance with strength.
On the other hand, the situation of Cu wirings, if using primary amine or the alkanolamine of secondary amine, the corruption of most cases Cu wirings
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 films 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 shortcomings that agent peeling force is weak such.
Under such technical background, need and used the Al wirings of alkanolamine of primary amine to have with anticorrosive additive stripping liquid controlling
There is equal and above degree stripping performance, and can be used in the anticorrosive additive stripping liquid controlling composition of both Cu wirings, Al wirings.
In addition, the anticorrosive additive stripping liquid controlling comprising (1) formula compound represented and solvent is disclosed in patent document 1.This is anti-
Losing agent stripper can also share in the resist stripping process that Cu is connected up and Al is connected up.
In addition, it is disclosed in patent document 2：Although using the alkanolamine of tertiary amine, but still with having used primary amine
Alkanolamine the equal peeling force of Al wiring anticorrosive additive stripping liquid controllings anticorrosive additive stripping liquid controlling.The stripper include tertiary amine,
Polar solvent, water, cyclic amine, sugar alcohol and reducing agent, the five-membered cyclic amine have nafoxidine or in 3 substds
The composition of nafoxidine.
Existing technical literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 2012-514765 bulletins (patent 5279921)
Patent document 2：Japanese Unexamined Patent Publication 2016-085378 bulletins (patent 5885041)
Invention content
Problems to be solved by the invention
The stripper of patent document 2 can be connected up in Cu and (wiring be laminated comprising Cu/Mo) and the resist stripping of Al wirings
It is shared in process.In addition, even if implementing hard baking to resist film, resist film can be also removed.
However, at the scene for using resist manufacture semiconductor device, FPD, disposably to be handled more massive
Substrate.Therefore, the failure in 1 photo-mask process can cause disposably to generate a large amount of substandard products.Therefore, each work of photoetching
Sequence runs operating parameter with secure context.
Specifically, carrying out curing at a higher temperature in the curing process of resist, consolidating for resist is avoided
Change bad this problem.However, at the same time, it is meant that the resist stronger than previous resist peeling force is needed to remove
Liquid.
The solution to the problem
The present invention be in view of the above subject and complete, even if provide for baked at higher than previous temperature form it is anti-
Lose agent film, the anticorrosive additive stripping liquid controlling that can also remove.Certainly much less, do not require nothing more than that resist peeling force is strong but also requirement pair
It is low in corrosivity as Cu, Mo and Al.
More specifically, the anticorrosive additive stripping liquid controlling about the present invention, which is characterized in that include：
As at least one of the primary amine of amine or secondary amine；
As polar solvent,
Diethylene glycol monoethyl ether (EDG) and
Propylene glycol (PG) and
Water；And
As the hydrazine of additive,
Aforementioned amine more than 3.0 mass % and for 20.0 mass % hereinafter,
Aforementioned diethylene glycol monoethyl ether more than 39.5 mass % and for 59.5 mass % hereinafter,
Aforementioned water is more than 5.18 mass % and is less than 28.18 mass %,
Aforementioned hydrazine is more than 0.064 mass % and is less than 1.28%.It should be noted that much less these ratio of components be with
It is prepared by the 100 mass % of total of each material.
The effect of invention
The anticorrosive additive stripping liquid controlling of the present invention has used secondary amine or primary amine, therefore even if for being baked higher than previous high temperature
Into resist, also can reliably be removed.And then anticorrosive additive stripping liquid controlling of the invention is made comprising diethylene glycol monoethyl ether
For polar solvent, therefore regardless of whether containing secondary amine or primary amine, can inhibit to corrosion of metal as Cu, Mo, Al.
In addition, the amine and the boiling point of organic polar solvent that are used in the anticorrosive additive stripping liquid controlling of the present invention are used higher than water
After can be recycled.And then for can suitable for by the use of amine and as polar solvent diethylene glycol monoethyl ether with
Propylene glycol, respective boiling point differs 5 degree or more, therefore can also individually be detached, and can effectively be recycled.
In addition, the bath service life of the anticorrosive additive stripping liquid controlling of the present invention is excellent, even if being placed 12 hours under atmosphere opening state
Above or even if closed preserve 4 days, resist stripping ability will not change.
Description of the drawings
Fig. 1 is the cone angle for illustrating Cu/Mo stacked films and the figure of Mo undercutting.
Specific embodiment
The anticorrosive additive stripping liquid controlling of the present 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 following embodiment party
Formula and embodiment are changed.It should be noted that in this specification, represent to use during range " more than " and " following " be
Refer to " comprising the value and more than (or " being more than ") value " and " comprising the value and less than (or " being less than ") value ".In addition, " being less than "
Refer to " not including the value and less than the value ".In addition, " being more than " refers to " not including the value and more than the value ".
The resist film that the anticorrosive additive stripping liquid controlling of the present invention is removed is assumed to positive-workingresist.It is included in positive-workingresist
The resin of novolaks system uses diazo naphthoquinone (DNQ) compound as resin as emulsion.When being etched, in substrate
Upper formation resist film, is exposed across pattern.
DNQ compounds is made to become indone by the exposure.When indone associates with water, become 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 compounds.DNQ chemical combination
Object goes bad due to exposure, is dissolved in the developer solution comprising water, so as to also dissolve out novolac resin.Thus resist is completed
The patterning of film.
Patterned substrate warp is completed by resist film to bake later and implement wet etching or dry etching is handled.
Bake afterwards be in order to make the novolac resin in resist film and DNQ compounds polymerize be able to carry out to a certain extent and
Implement.The heat treatment of 5 minutes or so is carried out typically at 140 DEG C.Hard bake refers at 170 DEG C in the present specification
The heating condition of 30 minutes or more.When stoving temperature rises, novolac resin and DNQ compounds can polymerize rapidly and secured
Ground is bonded to the metal film of substrate, becomes to not readily dissolve.The anticorrosive additive stripping liquid controlling of the present invention will also pass through this hard bake
Resist film as object.
The anticorrosive additive stripping liquid controlling of the present invention includes：The amine of primary amine or secondary amine without cyclic structure, polar solvent and
Reducing agent as additive.As amine, it is expected that boiling point is higher than water, and not azeotrope with water.The reason is that, stripper is carried out
During recycling, detached with water.As such substance, as primary amine it is preferable to use monoethanolamine (hereinafter also referred to
“MEA”.Boiling point is 170 DEG C.CAS model 141-43-5).
In addition, as secondary amine, it is preferable to use N- methylethanolamines (hereinafter also referred to " MMA ".Boiling point is 155 DEG C.
CAS model 109-83-1), N- ehtylethanolamines (hereinafter also referred to " EEA ".170 DEG C of boiling point.CAS model 110-73-6).Also may be used
To mix them.
In addition, relative to stripper total amount, the composition ratio of amine is more than 3.0 mass % and for below 20.0 mass %
Preferably, it is preferably more than 5.0 mass % and below 20.0 mass %, most preferably more than 10.0 mass % and below 20.0 mass %
It is advisable.When amine is few, the resist baked firmly can not be removed.On the other hand, when excessive, damaged metal becomes larger.
As polar solvent, it is preferable to use water and affinity organic solvent are (referred to as water-soluble organic molten
Agent.).In addition, if the Combination of above-mentioned primary amine and secondary amine well if it is more suitable.
As such water-miscible organic solvent, it is preferable to use diethylene glycol monoethyl ether (hereinafter also referred to " EDG ".
Boiling point is 202 DEG C.CAS model 111-90-0) and propylene glycol (hereinafter also referred to " PG ".Boiling point is 188 DEG C.CAS models 57-55-
6) mixed liquor.Polar solvent is made of water-miscible organic solvent and water.
After the composition ratio of polar solvent is the amount that amine and aftermentioned reducing agent are eliminated relative to stripper total amount
Amount.
The composition ratio of each material in polar solvent has desired range as follows.First, relative to resist
Stripper total amount, water are suitably more than 5.18 mass % and less than 28.18 mass %.If more than 10.0 mass % and 25.0 matter
It is then more suitable to measure below %.During dilutional hyponatremia, metal film can occur to corrode Al this problems when being Al.
Relative to anticorrosive additive stripping liquid controlling total amount, diethylene glycol monoethyl ether is suitably more than 39.5 mass % and 59.5 mass %
Below.If more than 44.5 mass % and below 50.0 mass % it is then more suitable.In addition, propylene glycol can be polar solvent
Surplus.
It (is also denoted as below " HN " as hydrazine of the additive it is preferable to use reducing agent.CAS model 302-01-2).Also
The addition of former agent inhibits Mo undercutting and the surface corrosion of metal film as caused by amine (evaluation assessment is aftermentioned).It is shelled relative to resist
Chaotropic total amount, reducing agent are desired for the range more than 0.064 mass % and below 1.28 mass %.More preferably 0.128 matter
Measure the range of more than % and below 0.64 mass %.It should be noted that from the viewpoint of safety operation, hydrazine can also use
Water and object (one water of hydrazine and object：It is denoted as " HNH2O”.).When being converted with one water of hydrazine and object, the range of above-mentioned hydrazine is desired for more
In the range of 0.1 mass % and below 2.0 mass %, if the range of more than 0.2 mass % and below 1.0 mass % then more
It is preferred that.
[embodiment]
The embodiment and comparative example of the anticorrosive additive stripping liquid controlling of the present 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 fissilities ＞
The silicon thermal oxidation film of 100nm is formed on a silicon substrate, and 300nm thickness is formed on silicon thermal oxidation film using sputtering method
Copper film.Positive-workingresist liquid is coated on by rotary coating and has made resist film on the copper film.Do resist film
After dry, it is exposed using the mask of wiring pattern.Then the resist of photosensitive part is removed by developer solution.That is, it is copper film
The state of part that the upper remaining part of resist film and copper film with wiring pattern are exposed.Then to silicon substrate at 170 DEG C
Plate integrally carries out the rear baking of 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, using the sample anticorrosive additive stripping liquid controlling just prepared (in aftermentioned table " new liquid ".) to against corrosion on the pattern of remaining copper
Agent film is removed.It is set as 15 minutes, is measured until the time of stripping for the processing time of stripping.With light microscope side into
Row interference edges see whether to remove, and are thus judged.
Even across 15 minutes, the remaining situation of resist film is also confirmed on copper film as "×" (fork), is confirmed
It is "○" (" circle " or " circle evaluation ") to the remaining situation of resist film.In the case, also record stripping complete when
Between.It should be noted that "○" (circle) represents successfully or qualified, "×" (" fork " or " fork evaluation ") represents failure or does not conform to
Lattice.Following evaluation is also identical.
The corrosivity ＞ of ＜ metal films
The corrosivity (metal membrane damage) of metal film is evaluated as follows.First, 100nm thickness is formed on a silicon substrate
Silicon thermal oxidation film.Then, the molybdenum film of 20nm thickness is formed on silicon thermal oxidation film on a silicon substrate, is then formed on
The copper film of 300nm thickness has made the stacking membrane sample of Cu/Mo.It is denoted as " Cu/Mo ".In addition, silicon heat on a silicon substrate
The aluminium film of 300nm thickness is formed on oxidation film, has made Al membrane samples.It is denoted as " Al ".
The resist film of patterned wiring shape, the base as erosion analysis are formed on these evaluation samples
Material.That is, erosion analysis base material includes appointing in the Cu/Mo films formed on silicon thermal oxidation film on a silicon substrate, Al films
The layer of one；And it is formed on the resist layer for wiring shape.
Copper film with or the etchant of aluminium film in these erosion analysis are carried out with base material with accurately etching during make
It is impregnated, etching.Then the erosion analysis after etching with base material is immersed in sample anticorrosive additive stripping liquid controlling 4 minutes, removed
Resist film.The erosion analysis for being immersed in 4 minutes in sample anticorrosive additive stripping liquid controlling with base material is cleaned, is dried, so
After observe film surface.In addition, it cuts off wiring portion and observes 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 during film.
The observation of film surface and section uses scanning electron microscope (SEM：Scanning Electron
Microscope) (Hitachi's system：SU8020 types), it is carried out under conditions of accelerating potential 1kV, 30000~50000 times.
The signal of section shape is illustrated in Fig. 1.(a) of Fig. 1 shows the section shape of the situation of " Al ".Accurate erosion
The section shape of the part at quarter is formd almost relative to substrate 1 into 30 ° of cone angles 5 to 60 ° of angles.Film portion 2 is Al films.
(b) of Fig. 1 shows the situation of " Cu/Mo ".The film portion 2 (Cu) of the situation of " Cu/Mo ", at least upper strata has cone angle 5.
It is expected to be etched basal layer 3 (Mo) along the taper surface 6 in film portion 2.However, as shown in (b) of Fig. 1, basal layer 3 and film portion
2 compare, and etch residue is also possible.
About corrosive evaluation, the situation of " Cu/Mo " is known as " Cu/Mo damages ", and the situation of " Al " is known as " Al damages ".
They are referred to as " metal membrane damage ".In addition, by observing above-mentioned cross sectional shape, observe film portion 2, film portion 2 surface 4 or
Any one of basal layer 3 does not observe that there is a situation where corrode to be judged as circle there is a situation where corroding to be judged as pitching (×)
(○)。
The particularly situation of " Cu/Mo " as shown in (c) of Fig. 1, is 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 dissolving, Mo (basal layer 3) is earlier than layers of copper
(film portion 2) is selectively etched.Therefore, the situation that gap 10 will be confirmed between basal layer 3 and film portion 2 is evaluated as
It pitches (×).
＜ 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 reacts as carbonate bicarbonate ion or with amine in stripper and generates carbamate ions, ties
Tab phenolphthaleinum causes peeling force reduction or damaged metal to become larger.
Particularly 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 bath short life,
It then needs frequently to replace or supplement anticorrosive additive stripping liquid controlling.
As test method, with after each anticorrosive additive stripping liquid controlling is just prepared (=0 hour), place under room temperature atmospheric environment
The experiment of resist fissility is carried out after 6 hours, after 12 hours, " Cu/Mo ", the surface of " Al " and section shape are observed by SEM
State.Evaluation method is identical with for ＜ resist fissility ＞ and ＜ the corrosivity ＞ in the case of.It should be noted that 0
Hour refers to (i.e. " new liquid ") immediately after preparation.
In addition, anticorrosive additive stripping liquid controlling is put into and is moved in container.However, if container preservation cannot be carried out at normal temperatures,
Then the availability in factory becomes very poor.Therefore, it also studied the composition transfer preserved by closed room temperature.
It about evaluation method, is put into closed container, places 4 days at normal temperatures, determine the stability of hydrazine.With just preparing
After compare, the situation that hydrazine reduces more than 1% is " × (fork evaluation) ", is " zero (circle evaluation) " if less than 1%.
These evaluations are carried out successively.However, situation of the result before also with good grounds without carrying out subsequent evaluation.It will
The situation is not carried out as evaluation and is denoted as "-".
＜ sample anticorrosive additive stripping liquid controllings ＞
Sample anticorrosive additive stripping liquid controlling is prepared for by following main points.
(embodiment 1)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of embodiment 1 is mixed and is made to more than ingredient.
It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.One water of hydrazine and object are remaining
The amount of 0.18 mass % is water.It therefore, can be with when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
It says as 20.18 mass %.In following all embodiment and comparative example, the situation of hydrazine monohydrate is used to contain to be identical
Justice.
(embodiment 2)
The N- ehtylethanolamines of secondary amine are used as amine.
20.0 mass % of N- ehtylethanolamines (EEA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
Hydrazine is used as reducing agent.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of embodiment 2 is mixed and is made to more than ingredient.
Embodiment 2 is that the N- methylethanolamines (MMA) of embodiment 1 are changed to the composition of N- ehtylethanolamines (EEA).It needs
It is noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.0.18 mass % of one water of hydrazine and object remnants
Amount be water.Therefore, it may be said that for 20.18 matter when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
Measure %.
(embodiment 3)
The monoethanolamine of primary amine is used as amine.
20.0 mass % of monoethanolamine (MEA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
Hydrazine is used as reducing agent.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of embodiment 3 is mixed and is made to more than ingredient.
Embodiment 3 is that the N- methylethanolamines (MMA) of embodiment 1 are changed to the composition of monoethanolamine (MEA).It needs
Bright, 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.The amount of the 0.18 mass % of one water of hydrazine and object remnants
For water.Therefore, it may be said that for 20.18 matter when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
Measure %.
(embodiment 4)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.8 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
Hydrazine is used as reducing agent.
One water of hydrazine and object (HNH2O) 0.2 mass %
The sample anticorrosive additive stripping liquid controlling of embodiment 4 is mixed and is made to more than ingredient.
Embodiment 4 is to reduce one water of hydrazine and object (HNH in embodiment 12O the composition of composition ratio).HN·H2O's
Increase EDG with reducing partial response.It should be noted that 0.2 mass % of one water of hydrazine and object is equivalent to 0.128 mass % of hydrazine.
The amount of the 0.072 mass % of one water of hydrazine and object remnants are water.Therefore, the ratio of components of above-mentioned water is also included with the shape of hydrazine monohydrate
During the amount of formula input it may be said that for 20.072 mass %.
(embodiment 5)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
48.0 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
Hydrazine is used as reducing agent.
One water of hydrazine and object (HNH2O) 2.0 mass %
The sample anticorrosive additive stripping liquid controlling of embodiment 5 is mixed and is made to more than ingredient.
Embodiment 5 is the increase in one water of hydrazine of embodiment 1 and object (HNH2O the composition of composition ratio).With HNH2O
Increase partial response reduce EDG.It should be noted that 2.0 mass % of one water of hydrazine and object are equivalent to 1.28 mass % of hydrazine.
The amount of the 0.72 mass % of one water of hydrazine and object remnants are water.Therefore, the ratio of components of above-mentioned water is also included with the shape of hydrazine monohydrate
During the amount of formula input it may be said that for 20.72 mass %.
(embodiment 6)
The N- methylethanolamines of secondary amine are used as amine.
5.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
54.5 mass % of diethylene glycol monoethyl ether (EDG)
20.0 mass % of propylene glycol (PG)
20.0 mass % of water
Hydrazine is used as reducing agent.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of embodiment 6 is mixed and is made to more than ingredient.
Embodiment 6 is the composition for the composition ratio for reducing N- methylethanolamines (MMA) in embodiment 1.The reduction portion of MMA
Dividing correspondingly increases EDG and PG.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.Hydrazine one
The amount of the 0.18 mass % of water and object remnants are water.Therefore, the ratio of components of above-mentioned water is also included and is thrown in the form of hydrazine monohydrate
During the amount entered it may be said that for 20.18 mass %.
(embodiment 7)
The N- methylethanolamines of secondary amine are used as amine.
10.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
20.0 mass % of propylene glycol (PG)
20.0 mass % of water
Hydrazine is used as reducing agent.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of embodiment 7 is mixed and is made to more than ingredient.
Embodiment 7 is the composition for the composition ratio for reducing N- methylethanolamines (MMA) in embodiment 1.The reduction portion of MMA
Dividing correspondingly increases PG.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.One water of hydrazine and
The amount of the 0.18 mass % of object remnants is water.Therefore, the ratio of components of above-mentioned water is also comprising the input in the form of hydrazine monohydrate
During amount it may be said that for 20.18 mass %.
(embodiment 8)
The monoethanolamine of primary amine is used as amine.
5.0 mass % of monoethanolamine (MEA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
25.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of embodiment 8 is mixed and is made to more than ingredient.
Embodiment 8 is that the N- methylethanolamines (MMA) of embodiment 1 are changed to the monoethanolamine (MEA) of primary amine, are reduced
The composition of composition ratio.Increase PG to the reduction partial response of MEA.It should be noted that 0.5 mass % phases of one water of hydrazine and object
When in 0.32 mass % of hydrazine.The amount of the 0.18 mass % of one water of hydrazine and object remnants are water.Therefore, the ratio of components of above-mentioned water also includes
During the amount put into the form of hydrazine monohydrate it may be said that for 20.18 mass %.
(embodiment 9)
The monoethanolamine of primary amine is used as amine.
10.0 mass % of monoethanolamine (MEA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
20.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of embodiment 9 is mixed and is made to more than ingredient.
Embodiment 9 is that the N- methylethanolamines (MMA) of embodiment 1 are changed to the monoethanolamine (MEA) of primary amine, are reduced
The composition of composition ratio.Increase PG to the reduction partial response of MEA.It should be noted that 0.5 mass % phases of one water of hydrazine and object
When in 0.32 mass % of hydrazine.The amount of the 0.18 mass % of one water of hydrazine and object remnants are water.Therefore, the ratio of components of above-mentioned water also includes
During the amount put into the form of hydrazine monohydrate it may be said that for 20.18 mass %.
(embodiment 10)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
44.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
25.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of embodiment 10 is mixed and is made to more than ingredient.
Embodiment 10 is the increase in the composition of the composition ratio of the water of embodiment 1.Reduce to the increase partial response of water
EDG.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.The 0.18 of one water of hydrazine and object remnants
The amount of quality % is water.Therefore, it may be said that being when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
25.18 quality %.
(embodiment 11)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
59.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
10.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of embodiment 11 is mixed and is made to more than ingredient.
Embodiment 11 is the composition for the composition ratio for reducing water in embodiment 1.Increase to the reduction partial response of water
EDG.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.The 0.18 of one water of hydrazine and object remnants
The amount of quality % is water.Therefore, it may be said that being when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
10.18 quality %.
(comparative example 1)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monobutyl ether (hereinafter also referred to " BDG ".CAS model 112-34-5) and third
Glycol.
49.5 mass % of diethylene glycol monobutyl ether (BDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 1 is mixed and is made to more than ingredient.
Comparative example 1 is that the polar solvent diethylene glycol monoethyl ether (EDG) of embodiment 1 is changed to diethylene glycol monobutyl ether
(BDG) composition.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.One water of hydrazine and object are residual
The amount of 0.18 remaining mass % is water.Therefore, when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
It may be said that for 20.18 mass %.
(comparative example 2)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water and diethylene glycol monoethyl ether.
59.5 mass % of diethylene glycol monoethyl ether (EDG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 2 is mixed and is made to more than ingredient.
Comparative example 2 is the composition that polar solvent propylene glycol (PG) is eliminated in embodiment 1.Increase EDG and replace PG parts.It needs
It is noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.0.18 mass % of one water of hydrazine and object remnants
Amount be water.Therefore, it may be said that for 20.18 matter when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
Measure %.
(comparative example 3)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
39.5 mass % of diethylene glycol monoethyl ether (EDG)
20.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 3 is mixed and is made to more than ingredient.
Comparative example 3 is the composition for the composition ratio for reducing polar solvent diethylene glycol monoethyl ether (EDG) in embodiment 1.
Increase PG to the reduction partial response of EDG.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 matter of hydrazine
Measure %.The amount of the 0.18 mass % of one water of hydrazine and object remnants are water.Therefore, the ratio of components of above-mentioned water is also included with hydrazine monohydrate
Form input amount when it may be said that for 20.18 mass %.
(comparative example 4)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, N-METHYLFORMAMIDE (hereinafter also referred to " NMF ".CAS model 123-39-7) and the third two
Alcohol.
49.5 mass % of N-METHYLFORMAMIDE (NMF)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 4 is mixed and is made to more than ingredient.
Comparative example 4 is that the polar solvent diethylene glycol monoethyl ether (EDG) of embodiment 1 is changed to N-METHYLFORMAMIDE
(NMF) composition.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.One water of hydrazine and object are residual
The amount of 0.18 remaining mass % is water.Therefore, when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
It may be said that for 20.18 mass %.
(comparative example 5)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, N,N-dimethylformamide (hereinafter also referred to " DMF ".CAS model 68-12-2) and third
Glycol.
49.5 mass % of N,N-dimethylformamide (DMF)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 5 is mixed and is made to more than ingredient.
Comparative example 5 is that the polar solvent diethylene glycol monoethyl ether (EDG) of embodiment 1 is changed to N,N-dimethylformamide
(DMF) composition.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.One water of hydrazine and object are residual
The amount of 0.18 remaining mass % is water.Therefore, when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
It may be said that for 20.18 mass %.
(comparative example 6)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent be mixed with water, ethylene carbonate (：Ethylene carbonate, hereinafter also referred to " EC ".CAS models 96-49-
And propylene glycol 1).
49.5 mass % of ethylene carbonate (EC)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 6 is mixed and is made to more than ingredient.
Comparative example 6 is that the polar solvent diethylene glycol monoethyl ether (EDG) of embodiment 1 is changed to ethylene carbonate (EC)
Composition.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.One water of hydrazine and object are remaining
The amount of 0.18 mass % is water.It therefore, can be with when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
It says as 20.18 mass %.
(comparative example 7)
The nafoxidine (hereinafter also referred to " PRL " of cyclic amine is used as amine.CAS model 123-75-1).
20.0 mass % of nafoxidine (PRL)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 7 is mixed and is made to more than ingredient.
Comparative example 7 is the nafoxidine that the N- methylethanolamines (MMA) of the secondary amine of embodiment 1 are changed to cyclic amine
(PRL) composition.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.One water of hydrazine and object are residual
The amount of 0.18 remaining mass % is water.Therefore, when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
It may be said that for 20.18 mass %.
(comparative example 8)
As amine use cyclic amine hydroxyethyl piperazine (：1- (2- ethoxys) piperazine, hereinafter also referred to " OH-PIZ ".
CAS model 103-76-4).
20.0 mass % of hydroxyethyl piperazine (OH-PIZ)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 8 is mixed and is made to more than ingredient.
Comparative example 8 is the hydroxyethyl piperazine that the N- methylethanolamines (MMA) of the secondary amine of embodiment 1 are changed to cyclic amine
(OH-PIZ) composition.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.One water of hydrazine and
The amount of the 0.18 mass % of object remnants is water.Therefore, the ratio of components of above-mentioned water is also comprising the input in the form of hydrazine monohydrate
During amount it may be said that for 20.18 mass %.
(comparative example 9)
The N methyldiethanol amine (hereinafter also referred to " MDEA " of tertiary amine is used as amine.CAS model 105-59-9).
20.0 mass % of N methyldiethanol amine (MDEA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 9 is mixed and is made to more than ingredient.
Comparative example 9 is the N methyldiethanol amine that the N- methylethanolamines (MMA) of the secondary amine of embodiment 1 are changed to tertiary amine
(MDEA) composition.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.One water of hydrazine and object
The amount of 0.18 remaining mass % is water.Therefore, the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
When it may be said that for 20.18 mass %.
(comparative example 10)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.9 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.1 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 10 is mixed and is made to more than ingredient.
Comparative example 10 is to reduce one water of hydrazine and object (HNH in embodiment 12O the composition of composition ratio).It needs to illustrate
, 0.1 mass % of one water of hydrazine and object is equivalent to 0.064 mass % of hydrazine.The amount of the 0.036 mass % of one water of hydrazine and object remnants
For water.Therefore, it may be said that for 20.036 matter when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
Measure %.
(comparative example 11)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
50.0 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
It is not added as the hydrazine reducing agent of additive.
The sample anticorrosive additive stripping liquid controlling of comparative example 11 is mixed and is made to more than ingredient.Comparative example 11 is from reality
It applies and one water of hydrazine and object (HNH is eliminated in the composition of example 12O composition).
(comparative example 12)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
As additive use saccharin (：O-benzoic sulfimide, CAS model 81-07-2).
0.5 mass % of saccharin
The sample anticorrosive additive stripping liquid controlling of comparative example 12 is mixed and is made to more than ingredient.Comparative example 12 is by reality
Apply the additive (reducing agent of example 1：One water of hydrazine and object (HNH2O)) it is changed to the composition of saccharin.
(comparative example 13)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
D-sorbite (hereinafter referred to as " Stol " is used as additive.CAS model 50-70-4).
0.5 mass % of D-sorbite (Stol)
The sample anticorrosive additive stripping liquid controlling of comparative example 13 is mixed and is made to more than ingredient.Comparative example 13 is by reality
Apply the additive (reducing agent of example 1：One water of hydrazine and object (HNH2O)) it is changed to the composition of D-sorbite (Stol).
(comparative example 14)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
20.0 mass % of water
As additive use diglycerol (：Diglycerol, CAS model 627-82-7).
0.5 mass % of diglycerol
The sample anticorrosive additive stripping liquid controlling of comparative example 14 is mixed and is made to more than ingredient.Comparative example 14 is by reality
Apply the additive (reducing agent of example 1：One water of hydrazine and object (HNH2O)) it is changed to the composition of diglycerol.
(comparative example 15)
The N- methylethanolamines of secondary amine are used as amine.
3.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
27.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 15 is mixed and is made to more than ingredient.
Comparative example 15 is the composition for the composition ratio for reducing N- methylethanolamines (MMA) in embodiment 1.The reduction of MMA
Increase 2P to partial response.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.One water of hydrazine
Amount with the 0.18 mass % of object remnants 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 for 20.18 mass %.
(comparative example 16)
The monoethanolamine of primary amine is used as amine.
3.0 mass % of monoethanolamine (MEA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
49.5 mass % of diethylene glycol monoethyl ether (EDG)
27.0 mass % of propylene glycol (PG)
20.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 16 is mixed and is made to more than ingredient.
Comparative example 16 is that the N- methylethanolamines (MMA) of embodiment 1 are changed to the monoethanolamine (MEA) of primary amine, are reduced
The composition of composition ratio.Increase PG to the reduction partial response of MEA.It should be noted that 0.5 mass % of one water of hydrazine and object
It is equivalent to 0.32 mass % of hydrazine.The amount of the 0.18 mass % of one water of hydrazine and object remnants are water.Therefore, the ratio of components of above-mentioned water also wraps
During containing the amount put into the form of hydrazine monohydrate it may be said that for 20.18 mass %.
(comparative example 17)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
64.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
5.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 17 is mixed and is made to more than ingredient.
Comparative example 17 is the composition for the composition ratio for reducing water in embodiment 1.Increase to the reduction partial response of water
EDG.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.The 0.18 of one water of hydrazine and object remnants
The amount of quality % is water.Therefore, it may be said that being when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
5.18 quality %.
(comparative example 18)
The N- methylethanolamines of secondary amine are used as amine.
20.0 mass % of N- methylethanolamines (MMA)
Polar solvent is mixed with water, diethylene glycol monoethyl ether and propylene glycol.
41.5 mass % of diethylene glycol monoethyl ether (EDG)
10.0 mass % of propylene glycol (PG)
28.0 mass % of water
The hydrazine of reducing agent is used as additive.
One water of hydrazine and object (HNH2O) 0.5 mass %
The sample anticorrosive additive stripping liquid controlling of comparative example 18 is mixed and is made to more than ingredient.
Comparative example 18 is the composition for the composition ratio that water is increased in embodiment 1.Reduce to the increase partial response of water
EDG.It should be noted that 0.5 mass % of one water of hydrazine and object is equivalent to 0.32 mass % of hydrazine.The 0.18 of one water of hydrazine and object remnants
The amount of quality % is water.Therefore, it may be said that being when the ratio of components of above-mentioned water is also comprising the amount put into the form of hydrazine monohydrate
28.18 quality %.
By the composition of embodiment 1 and comparative example 1~6 and evaluation result is shown in table 1, in addition, by Examples 1 to 3 and comparing
The composition of example 7~9 and evaluation result is shown in table 2.In addition, the composition and evaluation of embodiment 1,4~5 and comparative example 10~14 are tied
Fruit is shown in table 3.In addition, by embodiment 1,6~9 and the composition and evaluation result is shown in table 4 of comparative example 15~16.It in addition, will be real
Apply the composition and evaluation result is shown in table 5 of example 1,10~11 and comparative example 17~18.
[table 1]
Table 1 shows the composition and result of embodiment 1 and comparative example 1~4.With reference to the embodiment 1 of table 1.Made by being used as amine
With the N- methylethanolamines (MMA) of secondary amine, diethylene glycol monoethyl ether (EDG), propylene glycol (PG) and water are used as polar solvent
Mixed liquor, so as in 3 minutes stripping the resist of (hard bake) is baked under the conditions of as 170 DEG C, 30 minutes
Film.In addition, the damage of " Cu/Mo " and " Al " film is also evaluated for circle.
In addition, for placing bath service life during stripper under atmosphere opening state, even across 12 hours peeling forces
It does not change.And then the reduction of hydrazine is not observed in the case of closed preserve 4 days yet.
Comparative example 1~6 is the type for changing water-miscible organic solvent.Comparative example 1 is by the polar solvent two of embodiment 1
Ethylene glycol monoethyl ether (EDG) is changed to the composition of diethylene glycol monobutyl ether (BDG).Comparative example 1 can not even be removed immediately after preparation
The resist film that (new liquid) extremely bakes under conditions of 170 DEG C, 30 minutes.For comparative example 1, as amine and 1 phase of embodiment
N- methylethanolamines (MMA) have been used together.I.e., it is known that the resist through baking firmly not can be removed as long as secondary amine is used
Film, the combination with polar solvent are necessary.
Comparative example 2 is the composition that polar solvent propylene glycol (PG) is eliminated in embodiment 1.For comparative example 2, immediately after preparation
The resist peeling force of (new liquid), in an atmosphere place after be " circle " to the evaluation of the damage of Cu/Mo and Al.However,
In the case of closed placement 4 days, the reduction of hydrazine is observed.As described above, the presence of propylene glycol (PG) has the stabilization for improving hydrazine
The effect of property.
Comparative example 3 is to reduce the amount of the polar solvent diethylene glycol monoethyl ether of embodiment 1 to 39.5 from 49.5 mass %
The composition of quality %.Comparative example 3 fails to remove the resist film through baking firmly from (new liquid) immediately after preparation.Therefore, for bath
Service life is not tested.When diethylene glycol monoethyl ether (EDG) is below 39.5 mass %, relative to the resist through baking firmly
The resist peeling force of film reduces.
Comparative example 4 is that the polar solvent diethylene glycol monoethyl ether (EDG) of embodiment 1 is changed to N-METHYLFORMAMIDE
(NMF) composition.For comparative example 4, problem does not occur for the resist peeling force of (new liquid), metal membrane damage immediately after preparation,
It is evaluated for circle.However, placing the situation of 6 hours in an atmosphere, resist peeling force reduces, and is evaluated for fork.In addition, due to
It is placed 6 hours in air, and evaluates the fork that is evaluated as of the damage on the surface and section of Cu/Mo.It should be noted that Al is damaged
It does not observe.In addition, in the case of closed place 4 days, the reduction of hydrazine is observed.
Comparative example 5 is that the polar solvent diethylene glycol monoethyl ether (EDG) of embodiment 1 is changed to N,N-dimethylformamide
(DMF) composition.For comparative example 5, problem does not occur for the resist peeling force of (new liquid), metal membrane damage immediately after preparation,
It is evaluated for circle.However, placing the situation of 6 hours in an atmosphere, resist peeling force reduces, and is evaluated for fork.In addition, due to
It is placed 6 hours in air, and evaluates the fork that is evaluated as of the damage on the surface and section of Cu/Mo.It should be noted that it does not observe
To the damage to Al.In addition, in the case of closed place 4 days, the reduction of hydrazine is observed.
Comparative example 6 is that the polar solvent diethylene glycol monoethyl ether (EDG) of embodiment 1 is changed to ethylene carbonate (EC)
Composition.Comparative example 6 is also to fail to remove the resist film through baking firmly from (new liquid) immediately after preparation.Therefore, for bathing the service life,
It is not tested.
As knowen from these results, as polar solvent, by combine diethylene glycol monoethyl ether (EDG), propylene glycol (PG) and
Water so as to remove the resist film through baking firmly, will not damage metal, and the hydrazine when bathing service life, closed keeping 4 days is steady
Qualitative aspect also obtains circle evaluation.
[table 2]
Table 2 shows the composition and evaluation result of Examples 1 to 3 and comparative example 7~9.Embodiment 1 is discloses again, therefore
It is represented with bracket.Embodiment 2 is that the N- methylethanolamines (MMA) of embodiment 1 are changed to the group of N- ehtylethanolamines (EEA)
Into.Embodiment 2 also similarly to Example 1 resist peeling force, damaged metal and bathe the service life whole assessment items in be round
Circle evaluation.
Embodiment 3 is the composition for the monoethanolamine (MEA) that the N- methylethanolamines (MMA) of embodiment 1 are changed to primary amine.
Embodiment 3 also in resist peeling force and damaged metal and whole assessment items in bath service life is similarly to Example 1 circle
Evaluation.
It can be seen from the above result that as secondary amine, N- ehtylethanolamines (EEA) can be used.In addition it can not only use secondary
Amine can also use the monoethanolamine (MEA) of primary amine.
Comparative example 7~9 is the composition for having used other amines.Comparative example 7 is the nafoxidine (PRL) for having used cyclic amine
Situation.In addition, comparative example 8 is the situation for the hydroxyethyl piperazine (OH-PIZ) for having used cyclic amine, comparative example 9 is to have used uncle
The situation of the N methyldiethanol amine (MDEA) of amine.
Comparative example 7,8,9 fails to remove the resist film baked firmly.In addition, these comparative examples observed on surface for
The damage of Cu/Mo.However, the damage for Al is not observed.It should be noted that due to failing to remove the resist baked firmly
Film, therefore for bathing the service life, do not tested.It can be seen from the above result that even if as secondary amine, for the amine with cyclic structure and
The situation of tertiary amine can not also remove the resist film through baking firmly.
[table 3]
Table 3 shows the composition and evaluation result of embodiment 1,4~5 and comparative example 10~14.Embodiment 1 is to disclose again,
Therefore it is represented with bracket.Embodiment 4 is to reduce the composition ratio of the hydrazine of embodiment 1 to the group of 0.2 mass % from 0.5 mass %
Into.Increase EDG to the reduction partial response of hydrazine.Embodiment 4 also similarly to Example 1 in resist peeling force and damaged metal and
It bathes in whole assessment items in service life and is evaluated for circle.
Embodiment 5 is that the composition ratio of the hydrazine of embodiment 1 is increased to the composition of 2.0 mass % from 0.5 mass %.Hydrazine
Reduce EDG with increasing partial response.Embodiment 5 is also similarly to Example 1 in resist peeling force and damaged metal and bath service life
Whole assessment items in for circle evaluate.
Comparative example 10 is by one water of hydrazine and object (HNH of embodiment 12O composition ratio) from 0.5 mass % reduce to
The composition of 0.1 mass %.The resist peeling force of (new liquid) immediately after preparation for comparative example 10 is placed 6 hours in an atmosphere
Afterwards problem is not occurred to metal membrane damage.However, resist peeling force reduces after placing 12 hours in an atmosphere, evaluated for fork.
In addition, due to evaluating the fork that is evaluated as of the damage on the surface and section of Cu/Mo after placing in an atmosphere 12 hours.It needs
It is bright, do not observe that Al is damaged.In addition, in the case of closed preserve 4 days, the reduction of hydrazine is not observed yet.
Comparative example 11 is not add in hydrazine (one water of hydrazine and object (HNH2O composition)).Comparative example 11 is certainly (new immediately after preparation
Liquid) rise fail to remove the resist film baked firmly.In addition, the membrane damage of " Cu/Mo " occurs.It should be noted that it does not observe
Al is damaged.For bathing the service life, it is not carried out testing.
Comparative example 12 is to add in saccharin to replace example of the hydrazine of embodiment 1 as additive.Comparative example 13 is to add in sorb
Sugar alcohol (Stol) is instead of example of the hydrazine of embodiment 1 as additive.In addition, comparative example 14 is to add in diglycerol to replace embodiment
Example of 1 hydrazine as additive.Comparative example 12, comparative example 13, comparative example 14 fail from (new liquid) immediately after preparation the moment
Remove the resist film baked firmly.In addition, Cu/Mo damages occur.It should be noted that do not observe that Al is damaged.For bathing the longevity
Life, is not carried out testing.
By result above, it can be said that hydrazine (one water of hydrazine and object (HNH2O)) it is the necessary material of stripper of the invention,
Ratio of components be 0.064 mass % (one water of hydrazine and object be 0.1 mass %) below when, by stripping performance, the gold of bathing life test
Circle evaluation can not be obtained in terms of belonging to damage.On the other hand, at least in the hydrazine comprising 1.28 mass %, (one water of hydrazine and object are 2.0
Quality %) in the case of, characteristic will not be had an impact.
[table 4]
Table 4 shows embodiment 1,6~9 and the 15 of comparative example, 16 composition and evaluation result.Embodiment 1 is to disclose again,
Therefore it is represented with bracket.Embodiment 6 is to subtract the composition ratio of the N- methylethanolamines (MMA) of embodiment 1 from 20.0 mass %
The as little as composition of 5.0 mass %.Increase EDG and PG to the reduction partial response of MMA.Embodiment 6 passes through (new liquid) immediately after preparation
The resist film through baking firmly can be removed in 8 minutes.In addition, also there is no problem and is circle metal membrane damage and bath service life
Evaluation.In addition, closed situation about placing 4 days does not observe the reduction of hydrazine yet.
Embodiment 7 is to reduce the composition ratio of the N- methylethanolamines (MMA) of embodiment 1 to 10.0 from 20.0 mass %
The composition of quality %.Increase PG to the reduction partial response of MMA.Embodiment 7 is by the way that (new liquid) can be in 5 minutes immediately after preparation
Remove the resist film through baking firmly.In addition, also there is no problem and is circle evaluation metal membrane damage and bath service life.Closed placement
The situation of 4 days does not observe the reduction of hydrazine yet.
Embodiment 8 is that the N- methylethanolamines (MMA) of embodiment 1 are changed to monoethanolamine (MEA), the ratio of components of primary amine
Rate is also reduced from 20.0 mass % to the composition of 5.0 mass %.Increase PG to the reduction partial response of MEA.Embodiment 8 is by firm
(new liquid) can remove the resist film through baking firmly in 5 minutes after preparation.In addition, metal membrane damage and bath service life do not have yet
Problem and be circle evaluation.Closed situation about placing 4 days does not observe the reduction of hydrazine yet.
Embodiment 9 is that the N- methylethanolamines (MMA) of embodiment 1 are changed to monoethanolamine (MEA), the ratio of components of primary amine
Rate is also reduced from 20.0 mass % to the composition of 10.0 mass %.Increase PG to the reduction partial response of MEA.Embodiment 9 passes through
(new liquid) can remove the resist film through baking firmly in 2 minutes immediately after preparation.In addition, metal membrane damage and bath service life do not have yet
It is problematic and be circle evaluation.In addition, closed situation about placing 4 days does not observe the reduction of hydrazine yet.
Comparative example 15 is to reduce the composition ratio of the N- methylethanolamines (MMA) of embodiment 1 to 3.0 from 20.0 mass %
The composition of quality %.Increase PG to the reduction partial response of MMA.Comparative example 15 fails stripping through hard by (new liquid) immediately after preparation
The resist film of baking.Therefore, it for bathing the service life, is not carried out testing.It follows that the ratio of components of N- methylethanolamines (MMA)
During for below 3.0 mass %, circle evaluation cannot be obtained about peeling force.
Comparative example 16 is monoethanolamine (MEA), the composition that the N- methylethanolamines (MMA) of embodiment 1 are changed to primary amine
Ratio is reduced from 20.0 mass % to the composition of 3.0 mass %.Increase PG to the reduction partial response of MEA.Comparative example 16 passes through
(new liquid) fails to remove the resist film through baking firmly immediately after preparation.Therefore, it for bathing the service life, is not carried out testing.Thus can recognize
Even if the monoethanolamine (MEA) as primary amine, when composition ratio is below 3.0 mass %, also to become not removing through drying firmly
The anticorrosive additive stripping liquid controlling of roasting.
[table 5]
Table 5 shows the composition and evaluation result of embodiment 1,10~11 and comparative example 17~18.Embodiment 1 is takes off again
Show, therefore represented with bracket.Embodiment 10 is that the composition ratio of the water of embodiment 1 is increased to 25.0 matter from 20.0 mass %
Measure the composition of %.Reduce EDG to the increase partial response of water.Embodiment 10 can be by (new liquid) immediately after preparation in 5 minutes
Remove the resist film through baking firmly.In addition, also there is no problem and is circle evaluation metal membrane damage and bath service life.It is in addition, close
Close the reduction that situation about placing 4 days does not observe hydrazine yet.
Embodiment 11 is to reduce the composition ratio of the water of embodiment 1 to the composition of 10.0 mass % from 20.0 mass %.
Increase EDG to the reduction partial response of water.Embodiment 11 can stripping be baked through hard in 3 minutes by (new liquid) immediately after preparation
Resist film.In addition, also there is no problem and is circle evaluation metal membrane damage and bath service life.In addition, the closed feelings for placing 4 days
Condition does not observe the reduction of hydrazine yet.
Comparative example 17 is to reduce the composition ratio of the water of embodiment 1 to the composition of 5.0 mass % from 20.0 mass %.Water
Reduction partial response increase EDG.Comparative example 17 fails to remove the resist film through baking firmly by (new liquid) immediately after preparation.
Therefore, it for bathing the service life, is not carried out testing.It follows that when the composition ratio of water is below 5.18 mass %, for peeling force
It can not obtain circle evaluation.
Comparative example 18 is the composition that the composition ratio of the water of embodiment 1 is increased to 28.0 mass % from 20.0 mass %.
Water is 28.18 mass % after counting the water of one water of hydrazine and object in.Reduce EDG to the increase partial response of water.Comparative example 18 can lead to
It crosses and removes the resist film through baking firmly in 5 minutes immediately after preparation (new liquid).In addition, the damage to Cu/Mo is also commented for circle
Valency.However, Al is damaged.It follows that when the composition ratio of water is more than 28.18 mass %, in terms of the damage of Al films
It can not obtain circle evaluation.
Industrial availability
The anticorrosive additive stripping liquid controlling of the present invention can be reliably peeled the especially resist film through baking firmly, can suitably use
In the situation for using photoresist.
Reference sign
1 substrate
2 film portions
3 basal layers
4 (film portion) surfaces
5 cone angles
10 (between the Mo layers of substrate and Cu layers) gaps
Claims (2)
1. a kind of anticorrosive additive stripping liquid controlling, it includes：
As at least one of the primary amine of amine or secondary amine；
As polar solvent,
Diethylene glycol monoethyl ether (EDG),
Propylene glycol (PG) and
Water；And
As the hydrazine of additive,
The amine more than 3.0 mass % and for 20.0 mass % hereinafter,
The diethylene glycol monoethyl ether more than 39.5 mass % and for 59.5 mass % hereinafter,
The water is more than 5.18 mass % and is less than 28.18 mass %,
The hydrazine is more than 0.064 mass % and is less than 1.28%.
2. anticorrosive additive stripping liquid controlling according to claim 1, wherein,
When the amine includes primary amine, the primary amine is monoethanolamine (MEA),
When the amine includes secondary amine, the secondary amine in N- methylethanolamines (MMA) and N- ehtylethanolamines (EEA) at least
One.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/JP2016/089014 WO2018122992A1 (en) | 2016-12-28 | 2016-12-28 | Resist removal solution |
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| CN108235741A true CN108235741A (en) | 2018-06-29 |
| CN108235741B CN108235741B (en) | 2019-05-28 |
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|---|---|
| JP (1) | JP6213803B1 (en) |
| CN (1) | CN108235741B (en) |
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| WO (1) | WO2018122992A1 (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030083215A1 (en) * | 2001-10-25 | 2003-05-01 | Hynix Semiconductor Inc. | Cleaning solution for removing photoresist |
| CN103975052A (en) * | 2011-10-05 | 2014-08-06 | 安万托特性材料股份有限公司 | Microelectronic substrate cleaning compositions having copper/azole polymer inhibition |
| CN104946429A (en) * | 2014-03-26 | 2015-09-30 | 安集微电子科技(上海)有限公司 | Low-etching detergent for removing photoresist etching residues |
| JP2016095413A (en) * | 2014-11-14 | 2016-05-26 | パナソニックＩｐマネジメント株式会社 | Resist removal liquid |
| CN105676602A (en) * | 2010-12-02 | 2016-06-15 | Ltc有限公司 | Photoresist stripping composition comprising primary alkanolamine for liquid crystal display manufacturing process |
| KR20160108109A (en) * | 2015-03-05 | 2016-09-19 | 동우 화인켐 주식회사 | Resist stripper composition |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6300021B2 (en) * | 2014-06-23 | 2018-03-28 | 株式会社豊田自動織機 | Positive electrode for lithium ion secondary battery and lithium ion secondary battery |
-
2016
- 2016-12-28 CN CN201680042942.3A patent/CN108235741B/en active Active
- 2016-12-28 WO PCT/JP2016/089014 patent/WO2018122992A1/en active Application Filing
- 2016-12-28 JP JP2017542203A patent/JP6213803B1/en active Active
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030083215A1 (en) * | 2001-10-25 | 2003-05-01 | Hynix Semiconductor Inc. | Cleaning solution for removing photoresist |
| CN105676602A (en) * | 2010-12-02 | 2016-06-15 | Ltc有限公司 | Photoresist stripping composition comprising primary alkanolamine for liquid crystal display manufacturing process |
| CN103975052A (en) * | 2011-10-05 | 2014-08-06 | 安万托特性材料股份有限公司 | Microelectronic substrate cleaning compositions having copper/azole polymer inhibition |
| CN104946429A (en) * | 2014-03-26 | 2015-09-30 | 安集微电子科技(上海)有限公司 | Low-etching detergent for removing photoresist etching residues |
| JP2016095413A (en) * | 2014-11-14 | 2016-05-26 | パナソニックＩｐマネジメント株式会社 | Resist removal liquid |
| KR20160108109A (en) * | 2015-03-05 | 2016-09-19 | 동우 화인켐 주식회사 | Resist stripper composition |
Also Published As
| Publication number | Publication date |
|---|---|
| JP6213803B1 (en) | 2017-10-18 |
| WO2018122992A1 (en) | 2018-07-05 |
| TWI640842B (en) | 2018-11-11 |
| JPWO2018122992A1 (en) | 2018-12-27 |
| TW201827952A (en) | 2018-08-01 |
| CN108235741B (en) | 2019-05-28 |
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