CN116042331B - Application of cleaning liquid - Google Patents

Application of cleaning liquid Download PDF

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Publication number
CN116042331B
CN116042331B CN202211414101.4A CN202211414101A CN116042331B CN 116042331 B CN116042331 B CN 116042331B CN 202211414101 A CN202211414101 A CN 202211414101A CN 116042331 B CN116042331 B CN 116042331B
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water
soluble polymer
mass fraction
deionized water
diaminomaleonitrile
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CN116042331A (en
Inventor
王溯
蒋闯
刘金霞
任发强
刘文奇
刘超勇
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Shanghai Xinyang Semiconductor Material Co Ltd
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Shanghai Xinyang Semiconductor Material Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/32—Organic compounds containing nitrogen
    • C11D7/3218—Alkanolamines or alkanolimines
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/26—Organic compounds containing oxygen
    • C11D7/265—Carboxylic acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/32—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/32—Organic compounds containing nitrogen
    • C11D7/3209—Amines or imines with one to four nitrogen atoms; Quaternized amines
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/32—Organic compounds containing nitrogen
    • C11D7/3245—Aminoacids
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/32—Organic compounds containing nitrogen
    • C11D7/3281—Heterocyclic compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/34—Organic compounds containing sulfur
    • 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
    • H01L21/02041—Cleaning
    • 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
    • H01L21/02041—Cleaning
    • H01L21/02057—Cleaning during device manufacture
    • H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
    • H01L21/02071—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a delineation, e.g. RIE, of conductive layers
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10—Objects to be cleaned
    • C11D2111/14—Hard surfaces
    • C11D2111/22—Electronic devices, e.g. PCBs or semiconductors

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Emergency Medicine (AREA)
  • Health & Medical Sciences (AREA)
  • Detergent Compositions (AREA)

Abstract

The invention discloses application of a cleaning solution. The cleaning liquid can be used for removing residues after etching or ashing in the cleaning process of the integrated circuit wet process; the cleaning solution is prepared from the following raw materials in percentage by mass: alcohol amine, 5-20% hydroxylamine, cysteine, 0.01-0.05% water-soluble polymer, organic base, chelating agent, corrosion inhibitor, ammonium carboxylate, 0.01-1% EO-PO polymer L81, 0.01-2%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and water, wherein the balance is water. The cleaning liquid disclosed by the invention has a wide range of residues which can be cleaned, is generally non-corrosive to exposed substrate materials (such as exposed low-k dielectric materials, metal oxides, metals, metal nitrides and alloys thereof), and has a good application prospect.

Description

Application of cleaning liquid
Technical Field
The invention relates to application of a cleaning solution.
Background
In the chip manufacturing technology, the residual cleaning liquid after the plasma etching of the copper interconnection is mainly fluorine-containing cleaning liquid. With the continuous advancement of technology nodes, more and more materials are introduced, such as cobalt, titanium, tungsten, titanium nitride and other metal materials, low-k dielectric materials and the like, so that the compatibility of the traditional fluorine-containing cleaning solution with various materials is challenging.
Plasma dry etching is commonly used to fabricate vertical sidewall trenches and anisotropic interconnect vias in copper (Cu)/low dielectric constant dual damascene manufacturing processes. As technology nodes evolve to 45nm and smaller (e.g., 7 nm), the shrinking dimensions of semiconductor devices makes achieving precise profile control of vias and trenches more challenging. Integrated circuit manufacturers are researching the use of various hard masks to improve etch selectivity to low dielectric constant materials for better profile control. In post-etch residue cleaning processes, more and more types of metal and dielectric materials are protected, and thus compatibility of conventional cleaning fluids with a variety of materials is challenging.
Development of a cleaning solution with high compatibility is a problem to be solved in the art.
Disclosure of Invention
The invention aims to solve the technical problem of poor compatibility in the traditional cleaning solution, and provides application of the cleaning solution. The cleaning solution of the present invention has at least one or more of the following advantages: the range of the cleanable residues is wide; generally, the method has good application prospect without corrosiveness to exposed substrate materials (such as exposed low-k dielectric materials, metal oxides (such as AlOx)), metals (such as aluminum, aluminum/copper alloys, copper, titanium, tantalum, tungsten and cobalt), metal nitrides (such as aluminum nitride, aluminum oxide nitride, titanium nitride, tantalum nitride and tungsten nitride), and alloys thereof.
The invention solves the technical problems through the following technical proposal.
The invention provides application of a cleaning solution, which can be used for removing residues after etching or ashing in a cleaning process of a wet manufacturing process of an integrated circuit, wherein the cleaning solution is prepared from the following raw materials in percentage by mass: alcohol amine, 5-20% of hydroxylamine, cysteine, 0.01-0.05% of water-soluble polymer, organic base, chelating agent, corrosion inhibitor, ammonium carboxylate, 0.01-1% of EO-PO polymer L81, 0.01-2%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and water, wherein the balance is water, and the sum of the mass fractions of the components is 100%;
the corrosion inhibitor is amidoximated diaminomaleonitrile or a mixture of tolutriazole and amidoximated diaminomaleonitrile;
the water-soluble polymer is prepared by a preparation method which comprises the following steps:
step (1): dissolving acrylamide, amphoteric monomer methacryloyloxyethyl-N, N-dimethyl propane sulfonate and hydrophobic monomer docosane polyoxyethylene ether methacrylate in water to obtain a mixture I;
the molar ratio of the acrylamide to the amphoteric monomer is (18-19): 1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is (20-200): 1;
Step (2): adding an initiator into the mixture I obtained in the step (1) to remove oxygen to obtain a mixture II;
the initiator is a mixture of potassium persulfate, sodium bisulphite and azodiisobutylamidine hydrochloride, and the molar ratio of the sodium bisulphite to the potassium persulfate is 2:1; the molar ratio of the azo diisobutylamidine hydrochloride to the potassium persulfate is 6:1; the addition amount of potassium persulfate is 0.11 to 0.3mol.L relative to the volume of the polymerization system -1 ；
Step (3): and (3) reacting the mixture II obtained in the step (2) at 70-85 ℃ to obtain the water-soluble polymer.
The mass fraction of each component is the mass percentage of the mass of each component in the total mass of all components in the cleaning liquid.
In the application of the cleaning solution, the wafer used for manufacturing the integrated circuit is a silicon wafer.
In the application of the cleaning solution, the integrated circuit is preferably immersed in the cleaning solution. The time of the impregnation may be 5 to 30 minutes, preferably 20 minutes. The temperature of the impregnation may be 45-60 ℃, preferably 50 ℃.
The mass fraction of the alcohol amine in the cleaning solution may be in the range of from 5 to 20%, preferably 5%,10% or 20% of the mass fraction conventional in cleaning solutions in the art.
Among the cleaning solutions, the alcohol amine can be alcohol amine conventional in the cleaning solutions in the field, preferably one or more of methanol amine, monoethanolamine, diethanolamine, triethanolamine, N-methylethanolamine, N-dimethylethanolamine, diglycolamine, methyldiethanolamine, aminoethylethanolamine, N-methylaminoethanol, isopropanolamine and isobutolamine; more preferably one or more of diglycolamine, monoethanolamine and triethanolamine.
In the cleaning solution, the mass fraction of the hydroxylamine may be 5%,10% or 20%.
In the washing liquid, the mass fraction of the cysteine may be a mass fraction conventional in washing liquids in the art, preferably 0.001 to 0.25%, more preferably 0.15 to 0.25%, for example 0.15% or 0.25%.
In the cleaning solution, the mass fraction of the water-soluble polymer can be 0.025%,0.01% or 0.05%.
In the cleaning solution, the water-soluble polymer can be one or more of a water-soluble polymer A1, a water-soluble polymer A2, a water-soluble polymer A3, a water-soluble polymer A4, a water-soluble polymer A5 and a water-soluble polymer A6;
wherein the water-soluble polymer A1 is prepared by the preparation method; in step (1), the molar ratio of the acrylamide to the amphoteric monomer is 18.98:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 20:1; in the step (2), the potassium persulfate was added in an amount of 0.11mol.L based on the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step (3), the temperature of the reaction is 70 ℃; preferably, the reaction temperature is replaced by 70 ℃ with reference to the preparation method in the example 1 of the patent CN104140507A, and other conditions and operations are the same as in the example 1 of the CN 104140507A;
the water-soluble polymer A2 is prepared by the preparation method; in step (1), the molar ratio of the acrylamide to the amphoteric monomer is 18.9:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 100:1; in the step (2), the potassium persulfate was added in an amount of 0.3mol.L based on the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step (3), the temperature of the reaction is 80 ℃; preferably, the reaction temperature is changed from 50 ℃ to 80 ℃ by referring to the preparation method in the example 3 of the patent CN104140507A, and other conditions and operations are the same as in the example 3 of the CN 104140507A;
the water-soluble polymer A3 is prepared by the preparation method; in step (1), the molar ratio of the acrylamide to the amphoteric monomer is 18.94:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 60:1; in the step (2)The amount of potassium persulfate added was 0.11mol.L relative to the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step (3), the temperature of the reaction is 70 ℃; preferably, the reaction temperature is changed from 45 ℃ to 70 ℃ by referring to the preparation method in the example 2 of the patent CN104140507A, and other conditions and operations are the same as in the example 2 of the CN 104140507A;
The water-soluble polymer A4 is prepared by the preparation method; in step (1), the molar ratio of the acrylamide to the amphoteric monomer is 18.76:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 200:1; in the step (2), the potassium persulfate was added in an amount of 0.11mol.L based on the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step (3), the temperature of the reaction is 70 ℃; preferably, the reaction temperature is replaced by 70 ℃ with reference to the preparation method in the example 5 of the patent CN104140507A, and other conditions and operations are the same as in the example 5 of the CN 104140507A;
the water-soluble polymer A5 is prepared by the preparation method; in step (1), the molar ratio of the acrylamide to the amphoteric monomer is 18.98:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 20:1; in the step (2), the potassium persulfate was added in an amount of 0.11mol.L based on the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step (3), the temperature of the reaction is 75 ℃; preferably, the reaction temperature is changed from 45 ℃ to 75 ℃ by referring to the preparation method in the example 1 of the patent CN104140507A, and other conditions and operations are the same as in the example 1 of the CN 104140507A;
the water-soluble polymer A6 is prepared by the preparation method; in step (1), the molar ratio of the acrylamide to the amphoteric monomer is 18.9:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 100:1; in the step (2), the potassium persulfate was added in an amount of 0.3mol.L based on the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step (3), the temperature of the reaction is 85 ℃; preferably, the reaction temperature was changed from 50℃to 85℃by the preparation method described in example 3 of the patent CN104140507A, and the other conditions and operations were the same as in example 3 of the patent CN 104140507A.
In the cleaning solution, the mass fraction of the organic base may be a mass fraction conventional in cleaning solutions in the art, preferably 1-5%, such as 1%,2.5% or 5%.
In the cleaning solution, the organic base may be an organic base conventional in the art, preferably one or more of tetramethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, tetraethylammonium hydroxide (TEAH), benzyltrimethylammonium hydroxide (BTAH), choline, (2-hydroxyethyl) trimethylammonium hydroxide, tris (2-hydroxyethyl) methylammonium hydroxide, tetrabutylphosphonium hydroxide (TBPH) and tetramethylguanidine; more preferably tetramethylammonium hydroxide and/or choline.
The chelating agent may be present in the cleaning solution in an amount conventional in the art, preferably in an amount of 0.01 to 2.0%, for example 0.01%, 1.0% or 2.0%.
In the cleaning solution, the chelating agent may be a chelating agent conventional in the art, preferably one or more of 1, 2-cyclohexanediamine-N, N ' -tetraacetic acid (CDTA), ethylenediamine tetraacetic acid, nitrilotriacetic acid, diethylenetriamine pentaacetic acid, 1,4,7, 10-tetraazacyclododecane-1, 4,7, 10-tetraacetic acid, ethylene Glycol Tetraacetic Acid (EGTA), 1, 2-bis (o-aminophenoxy) ethane-N, N ' -tetraacetic acid, N- {2- [ bis (carboxymethyl) amino ] ethyl } -N- (2-hydroxyethyl) glycine (HEDTA), ethylenediamine-N, N ' -bis (2-hydroxyphenylacetic acid) (EDDHA), dioxaoctamethylenediazatetraacetic acid (dotta), and triethylenetetramine hexaacetic acid (TTHA); more preferably ethylenediamine tetraacetic acid and/or 1, 2-cyclohexanediamine-N, N' -tetraacetic acid (CDTA).
The mass fraction of the corrosion inhibitor in the cleaning solution may be in an amount conventional in the art, preferably 0.01-2.0%, for example 0.01%, 0.5% or 2.0%.
The amidoximated diamino Ma Laijing of the amidoximated diamino maleonitrile and the tolyltriazole-amidoximated diamino maleonitrile is preferably prepared by a process comprising the steps of:
at K 2 CO 3 NH is added in the presence of a catalyst at a temperature of 75-95 DEG C 2 OH-HCl and diaminomaleonitrile react in aqueous ethanol to give amidoximated diaminomaleonitrile.
In the mixture of tolyltriazole and amidoximated diaminomaleonitrile, the mass ratio of the amidoximated diaminomaleonitrile to the tolyltriazole is preferably 1:1.
The mass fraction of the ammonium carboxylate in the cleaning solution may be in an amount conventional in the art, and may be 0.5-3%, for example 0.5%, 1.0% or 3.0%.
In the cleaning solution, the ammonium carboxylate may be one or more of ammonium oxalate, ammonium lactate, ammonium tartrate, ammonium citrate, ammonium acetate, ammonium carbamate, ammonium carbonate, ammonium benzoate, ammonium ethylenediamine tetraacetate, ammonium succinate, ammonium formate and ammonium 1-H-pyrazole-3-carboxylate, more preferably ammonium oxalate and/or ammonium citrate, which are conventional in the art.
In the cleaning solution, the mass fraction of the EO-PO polymer L81 may be 0.05%, 0.01% or 1.0%.
In the cleaning solution, the mass fraction of the 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) can be 0.01%, 0.7% or 2.0%.
In the cleaning solution, the water is preferably deionized water.
In one embodiment, the cleaning solution is prepared from the following raw materials in parts by mass:
the alcohol amine is one or more of diglycolamine, monoethanolamine and triethanolamine;
the mass fraction of the alcohol amine is 5-20%;
the mass fraction of the hydroxylamine is 5-20%;
the mass fraction of the cysteine is 0.15-0.25%;
the water-soluble polymer is one or more of the water-soluble polymer A1, the water-soluble polymer A2, the water-soluble polymer A3, the water-soluble polymer A4, the water-soluble polymer A5 and the water-soluble polymer A6;
the mass fraction of the water-soluble polymer is 0.01-0.05%;
the organic base is tetramethyl ammonium hydroxide and/or choline;
the mass fraction of the organic alkali is 1-5%;
The chelating agent is ethylenediamine tetraacetic acid and/or 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid (CDTA);
the mass fraction of the chelating agent is 0.01-2%;
the corrosion inhibitor is the amidoximated diaminomaleonitrile or the amidoximated diaminomaleonitrile-tolyltriazole mixture; the mass ratio of the amidoximated diaminomaleonitrile to the tolyltriazole in the amidoximated diaminomaleonitrile-tolyltriazole mixture is preferably 1:1;
the mass fraction of the corrosion inhibitor is 0.01-2%;
the ammonium carboxylate is ammonium oxalate and/or ammonium citrate;
the mass fraction of the ammonium carboxylate is 0.5-3%;
the mass fraction of the EO-PO polymer L81 is 0.01-1%;
the mass fraction of the 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) is 0.01-2%;
the water is deionized water; the deionized water is used for supplementing the balance.
In one embodiment, the cleaning solution is prepared from the following raw materials in parts by mass:
the alcohol amine is diglycolamine;
the mass fraction of the alcohol amine is 5-20%;
the mass fraction of the hydroxylamine is 5-20%;
The mass fraction of the cysteine is 0.15-0.25%;
the water-soluble polymer is the water-soluble polymer A1;
the mass fraction of the water-soluble polymer is 0.01-0.05%;
the organic base is tetramethyl ammonium hydroxide;
the mass fraction of the organic alkali is 1-5%;
the chelating agent is ethylenediamine tetraacetic acid;
the mass fraction of the chelating agent is 0.01-2%;
the corrosion inhibitor is diamino Ma Laijing of the amidoxime;
the mass fraction of the corrosion inhibitor is 0.01-2%;
the ammonium carboxylate is ammonium oxalate;
the mass fraction of the ammonium carboxylate is 0.01-1%;
the mass fraction of the EO-PO polymer L81 is 0.01-1%;
the mass fraction of the 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) is 0.01-2%;
the water is deionized water; the deionized water is used for supplementing the balance.
In one embodiment, the cleaning solution is prepared from the following raw materials in parts by mass:
the alcohol amine is one or more of diglycolamine, monoethanolamine and triethanolamine;
the mass fraction of the alcohol amine is 5%;
The mass fraction of the hydroxylamine is 5%;
the mass fraction of the cysteine is 0.25%;
the water-soluble polymer is one or more of the water-soluble polymer A1, the water-soluble polymer A2, the water-soluble polymer A3, the water-soluble polymer A4, the water-soluble polymer A5 and the water-soluble polymer A6;
the mass fraction of the water-soluble polymer is 0.025%;
the organic base is tetramethyl ammonium hydroxide and/or choline;
the mass fraction of the organic alkali is 2.5%;
the chelating agent is ethylenediamine tetraacetic acid and/or 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid (CDTA);
the mass fraction of the chelating agent is 1%;
the corrosion inhibitor is the amidoximated diaminomaleonitrile or the amidoximated diaminomaleonitrile-tolyltriazole mixture; the mass ratio of the amidoximated diaminomaleonitrile to the tolyltriazole in the amidoximated diaminomaleonitrile-tolyltriazole mixture is preferably 1:1;
the mass fraction of the corrosion inhibitor is 0.5%;
the ammonium carboxylate is ammonium oxalate and/or ammonium citrate;
the mass fraction of the ammonium carboxylate is 1%;
The mass fraction of the EO-PO polymer L81 is 0.05%;
the mass fraction of the 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) is 0.7%;
the water is deionized water; the deionized water is used for supplementing the balance.
In a certain preferred technical scheme, in the cleaning solution, the raw materials are any combination of the following components in percentage by mass:
combination 1:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 2:10.0% diglycolamine, 10.000% hydroxylamine, 0.15% cysteine, 0.010% water-soluble polymer A1, 1.00% tetramethylammonium hydroxide, 0.01% ethylenediamine tetraacetic acid, 0.01% amidoximated diaminomaleonitrile, 0.50% ammonium oxalate, 0.01% EO-PO polymer L81, 0.01%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
Combination 3:20.0% diglycolamine, 10.000% hydroxylamine, 0.25% cysteine, 0.050% water-soluble polymer A1, 5.0% tetramethylammonium hydroxide, 2.0% ethylenediamine tetraacetic acid, 2.0% amidoximated diaminomaleonitrile, 3.0% ammonium oxalate, 1.0% EO-PO polymer L81, 2.0%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 4:10.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% eo-PO polymer L81, 0.70%1- (benzotriazol-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 5:20.0% diglycolamine, 20.000% hydroxylamine, 0.15% cysteine, 0.025% water-soluble polymer A1, 5.0% tetramethylammonium hydroxide, 2.0% ethylenediamine tetraacetic acid, 2.0% amidoximated diaminomaleonitrile, 3.0% ammonium oxalate, 1.0% EO-PO polymer L81, 2.0%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
Combination 6:5.0% monoethanolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% eo-PO polymer L81, 0.70%1- (benzotriazol-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 7:5.0% triethanolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70%1- (benzotriazol-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 8:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% choline, 1.00% ethylenediamine tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70%1- (benzotriazol-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
Combination 9:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00%1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70%1- (benzotriazol-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 10:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% 50% tolyltriazole+50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 11:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% tri-ammonium citrate, 0.05% EO-PO polymer L81, 0.70%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
Combination 12:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A2, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 13:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A3, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 14:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A4, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
Combination 15:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A5, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 16:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A6, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70%1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
the water-soluble polymers A1-A6 are the same as the above;
the amidoximated diaminomaleonitrile is as described above.
In one embodiment, the cleaning solution comprises the following raw materials in percentage by mass: the balance of the alcohol amine, the hydroxylamine, the cysteine, the water-soluble polymer, the organic base, the chelating agent, the corrosion inhibitor, the ammonium carboxylate, the polymer L81, the 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and the water;
Wherein the mass fraction of each component is as described above;
the alcohol amine, the water-soluble polymer, the organic base, the chelating agent, the corrosion inhibitor and the ammonium carboxylate are as described above.
The invention also provides the cleaning liquid.
The components of the cleaning liquid can be packaged and temporarily mixed when in use.
The invention also provides a kit comprising in one or more containers, said alcohol amine, said hydroxylamine, said cysteine, said water-soluble polymer, said organic base, said chelating agent, said corrosion inhibitor, said ammonium carboxylate, said EO-PO polymer L81, said 1- (benzotriazol-1-methyl) -1- (2-methylbenzimidazole) and said water, in one or more containers.
The invention also provides a preparation method of the cleaning liquid, which comprises the following steps: and mixing the components to obtain the cleaning liquid.
Wherein, the mixing is preferably to add the solid component in the components into the liquid component and stir the mixture uniformly.
Wherein the temperature of the mixing may be room temperature.
As used herein, "room temperature" refers to 10-30deg.C.
The "volume of the polymerization system" in the present invention refers to the volume of acrylamide, the amphoteric monomer methacryloyloxyethyl-N, N-dimethylpropanesulfonate and the hydrophobic monomer docosapolyoxyethylene ether methacrylate when dissolved in water.
The above preferred conditions can be arbitrarily combined on the basis of not deviating from the common knowledge in the art, and thus, each preferred embodiment of the present invention can be obtained.
Other reagents and starting materials for the present invention, except 1- (benzotriazol-1-methyl) -1- (2-methylbenzimidazole) and amidoximated diaminomaleonitrile, are commercially available, wherein EO-PO polymer L81, EO-PO polymer L42, EO-PO polymer L62 and EO-PO polymer L31 are all available from Nantong brocade chemical Co.
The invention has the positive progress effects that: the cleaning solution of the present invention can clean a wide range of residues, is generally non-corrosive to exposed substrate materials (e.g., exposed low-k dielectric materials, metal oxides (such as AlOx), metals (such as aluminum, aluminum/copper alloys, copper, titanium, tantalum, tungsten, and cobalt), metal nitrides (such as aluminum nitride, aluminum oxide nitride, titanium nitride, tantalum nitride, and tungsten nitride), and alloys thereof), and has good application prospects.
Detailed Description
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
1- (benzotriazol-1-methyl) -1- (2-methylbenzimidazole)
In the present invention 1- (benzotriazol-1-methyl) -1- (2-methylbenzimidazole) was self-made, which was prepared according to example 2 in patent CN 106188103B.
Amidoximated diamino Ma Laijing
Preparation of amidoximated diaminomaleonitrile: NH is added to 2 OH HCl and K 2 CO 3 Dissolving in ethanol water solution to obtain mixed solution, adding diaminomaleonitrile into the mixed solution, heating to 75-95 ℃ under the protection of nitrogen gas for reaction for 4-8h, centrifuging after the reaction, collecting samples, washing with ethanol and water respectively, and freeze-drying to obtain amidoximated diaminomaleonitrile.
Water-soluble polymers A1 to A6
The water-soluble polymer A1 in the embodiment of the invention is self-made and is prepared by referring to the conditions and the operation in the embodiment 1 in the patent CN104140507A, wherein the reaction temperature is replaced by 70 ℃ from 45 ℃, and other conditions and the operation are the same as those in the embodiment 1 in the CN 104140507A;
The water-soluble polymer A2 in the embodiment of the invention is self-made and is prepared by referring to the conditions and the operation in the embodiment 3 in the patent CN104140507A, wherein the reaction temperature is replaced by 80 ℃ from 50 ℃, and other conditions and the operation are the same as those in the embodiment 3 in the CN 104140507A;
the water-soluble polymer A3 in the embodiment of the invention is self-made and is prepared by referring to the conditions and the operation in the embodiment 2 in the patent CN104140507A, wherein the reaction temperature is changed from 45 ℃ to 70 ℃, and other conditions and the operation are the same as those in the embodiment 2 in the CN 104140507A;
the water-soluble polymer A4 in the embodiment of the invention is self-made and is prepared by referring to the conditions and the operation in the embodiment 5 of the patent CN104140507A, wherein the reaction temperature is changed from 45 ℃ to 70 ℃, and other conditions and the operation are the same as those in the embodiment 5 of the CN 104140507A;
the water-soluble polymer A5 in the embodiment of the invention is self-made and is prepared by referring to the conditions and the operation in the embodiment 1 in the patent CN104140507A, wherein the reaction temperature is replaced by 75 ℃ from 45 ℃, and other conditions and the operation are the same as those in the embodiment 1 in the CN 104140507A;
the water-soluble polymer A6 in the embodiment of the invention is self-made and is prepared by referring to the conditions and the operation in the embodiment 3 in the patent CN104140507A, wherein the reaction temperature is replaced by 85 ℃ from 50 ℃, and other conditions and the operation are the same as those in the embodiment 3 in the CN 104140507A.
Comparative example Water-soluble Polymer
The comparative example water-soluble polymer 1 of the present invention was self-made, which was prepared according to example 1 of CN104140507 a;
the comparative example of the water-soluble polymer 2 of the present invention was self-made and was prepared according to example 2 of CN104140507 a;
the comparative example water-soluble polymer 3 of the present invention was self-made, which was prepared according to example 3 of CN104140507 a;
the comparative example 4 of the present invention was self-made and was prepared according to example 4 of CN104140507 a;
comparative example Water-soluble Polymer 5 in the present invention was self-made, which was prepared according to example 5 of patent CN 104140507A.
In the following examples and comparative examples, the preparation method of the cleaning liquid includes the following steps: adding the solid component into the liquid component, and stirring uniformly.
In the following examples, the specific operating temperatures are not limited, and all refer to being conducted under room temperature conditions.
The types of raw material components in the cleaning liquid of each example are the raw material components and deionized water as shown in table 1.
Table 1: examples kinds of raw material components in cleaning liquid
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The contents of the raw material components in the cleaning liquid of each example are shown in Table 2.
Table 2: example content of each raw material component in the cleaning liquid
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Comparative examples 1 to 19 below are screens based on the kinds or contents of components performed in example 1.
Comparative example 1
The hydroxylamine component of example 1 was removed, the others being unchanged.
Comparative example 2
The component hydroxylamine of example 1 was replaced with oxidized glutathione and the cysteine was removed, the others being unchanged.
Comparative example 3
The component water-soluble polymer A1 in example 1 was replaced with the comparative water-soluble polymer 1, the others being unchanged.
Comparative example 4
The component water-soluble polymer A1 in example 1 was replaced with the comparative water-soluble polymer 2, the others being unchanged.
Comparative example 5
The component water-soluble polymer A1 in example 1 was replaced with the comparative water-soluble polymer 3, the others being unchanged.
Comparative example 6
The component water-soluble polymer A1 in example 1 was replaced with the comparative water-soluble polymer 4, the others being unchanged.
Comparative example 7
The component water-soluble polymer A1 in example 1 was replaced with the comparative water-soluble polymer 5, the others being unchanged.
Comparative example 8
The component EO-PO polymer L81 in example 1 was replaced with EO-PO polymer L42, the others being unchanged.
Comparative example 9
The component EO-PO polymer L81 in example 1 was replaced with EO-PO polymer L62, the others being unchanged.
Comparative example 10
The component EO-PO polymer L81 in example 1 was replaced with EO-PO polymer L31, the others being unchanged.
Comparative example 11
The water-soluble polymer was removed from the composition of example 1, and the other was unchanged.
Comparative example 12
The content of the water-soluble polymer in example 1 was replaced with 0.005%, and the other was unchanged.
Comparative example 13
The hydroxylamine content in example 1 was replaced with 4.5% and the others were unchanged.
Comparative example 14
The content of the water-soluble polymer in example 1 was replaced with 0.06%, and the other was unchanged.
Comparative example 15
The EO-PO polymer L81 content of example 1 was replaced with 0.0005% and the others were unchanged.
Comparative example 16
The content of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) in example 1 was replaced with 0.0005%, and the others were unchanged.
Comparative example 17
The EO-PO polymer L81 content of example 1 was replaced with 1.1% and the others were unchanged.
Comparative example 18
The content of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) in example 1 was replaced with 2.1% with the other ones unchanged.
Comparative example 19
The component corrosion inhibitors of example 1 were replaced by a mixture of 50% benzotriazole and 50% amidoximated diaminomaleonitrile, the others being unchanged.
Effect examples
ER (Corrosion Rate) detection
Etching rate sample to be detected: a dummy wafer (dummy wafer) of a single material such as copper, cobalt, titanium nitride, titanium, dielectric material (low-k or high-k), etc. is deposited on the silicon wafer.
Etching experiment: and (3) statically soaking the sample to be detected in a cleaning solution for 30min at 50 ℃, and then cleaning with deionized water and drying with nitrogen.
Method of measuring etch rate (a/min): the thickness of the samples before and after etching was measured, respectively, wherein the metal samples were tested for thickness using a four-point probe instrument (CRESTEST-e of Napson, japan), and the non-metal samples were tested for thickness using an optical film thickness measuring instrument (Filmetrics F20, USA), and the test results are shown in Table 3.
TABLE 3 Table 3
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The TiN is PVD TiN. Wherein PVD refers to (Physical Vapor Deposition) physical vapor deposition.
In the table, the cleaning solution of the present invention is used for cleaning the substrate material exposed on the silicon wafer, such as AlNxOy, alN,The etching rates of W, cu, LP-TEOS, BD2, siCN, co, ti, tiN, taN and TiNxOy are extremely low and are all smaller thanHardly corroding the interconnection material on the device; the etching rate of the comparative cleaning solution on the above materials is slightly higher and can reach 192.84 +.>It is possible to etch the interconnect material on the device.
2. Cleaning effect and corrosion effect
Cleaning effect sample to be detected: patterned wafers with post plasma etch residues and post ash residues with patterned features (metal lines, holes via, metal pad or trench, etc.).
The cleaning effect experimental method comprises the following steps: the sample is statically immersed in a cleaning solution for 20min at 50 ℃, and then is cleaned by deionized water and then dried by nitrogen. The cleaning and corrosion effects were observed by electron microscope SEM and the test results are shown in table 4.
The cleaning effect is classified into four grades: a-no residue was observed; b-very little residue was observed; c-small residues were observed; d-significantly more residue was observed.
The corrosion effects are rated in four classes: a-compatibility is good, and undercut is avoided; b-very slight undercut; c-having a small undercut; d-undercut is more pronounced and severe.
TABLE 4 Table 4
Therefore, the cleaning solution has good cleaning effect on residues after etching or ashing in the cleaning process of the Integrated Circuit (IC) wet process.

Claims (20)

1. The application of the cleaning liquid is characterized in that the cleaning liquid can be used for removing residues after etching or ashing in the cleaning process of the wet manufacturing process of the integrated circuit, and the cleaning liquid is prepared from the following raw materials in percentage by mass: 5-20% of alcohol amine, 5-20% of hydroxylamine, 0.15-0.25% of cysteine, 0.01-0.05% of water-soluble polymer, 1-5% of organic base, 0.01-2% of chelating agent, 0.01-2% of corrosion inhibitor, 0.5-3% of ammonium carboxylate, 0.01-1% of EO-PO polymer L81, 0.01-2% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and water, wherein the balance is water, and the sum of the mass fractions of the components is 100%;
The alcohol amine is one or more of diglycolamine, monoethanolamine and triethanolamine;
the organic base is tetramethyl ammonium hydroxide and/or choline;
the chelating agent is ethylenediamine tetraacetic acid and/or 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid;
the ammonium carboxylate is ammonium oxalate and/or ammonium citrate;
the corrosion inhibitor is amidoximated diaminomaleonitrile or a mixture of tolutriazole and amidoximated diaminomaleonitrile;
the water-soluble polymer is prepared by a preparation method which comprises the following steps:
step (1): dissolving acrylamide, amphoteric monomer methacryloyloxyethyl-N, N-dimethyl propane sulfonate and hydrophobic monomer docosane polyoxyethylene ether methacrylate in water to obtain a mixture I;
the molar ratio of the acrylamide to the amphoteric monomer is (18-19): 1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is (20-200): 1;
step (2): adding an initiator into the mixture I obtained in the step (1) to remove oxygen to obtain a mixture II;
the initiator is a mixture of potassium persulfate, sodium bisulphite and azodiisobutylamidine hydrochloride, and the molar ratio of the sodium bisulphite to the potassium persulfate is 2:1; the mole of the azo diisobutylamidine hydrochloride and the mole of the potassium persulfate The ratio is 6:1; the addition amount of potassium persulfate is 0.11 to 0.3mol.L relative to the volume of the polymerization system -1 ；
Step (3): reacting the mixture II obtained in the step (2) at 70-85 ℃ to obtain the water-soluble polymer;
the mass fraction of each component is the mass percentage of the mass of each component in the total mass of all components in the cleaning liquid.
2. The use of the cleaning solution of claim 1, wherein the wafer used to fabricate the integrated circuit is a silicon wafer; the application adopts a mode of immersing the integrated circuit in the cleaning liquid; the soaking time is 5-30min; the temperature of the impregnation is 45-60 ℃.
3. The use of a cleaning solution as claimed in claim 2,
the soaking time is 20min;
and/or, the temperature of the impregnation is 50 ℃.
4. The use of a cleaning solution according to claim 1,
the mass fraction of the hydroxylamine is 5%,10% or 20%.
5. The use of a cleaning solution according to claim 1,
the mass fraction of the water-soluble polymer is 0.025%,0.01% or 0.05%.
6. The use of a cleaning solution according to claim 1,
The water-soluble polymer is one or more of a water-soluble polymer A1, a water-soluble polymer A2, a water-soluble polymer A3, a water-soluble polymer A4, a water-soluble polymer A5 and a water-soluble polymer A6;
wherein the water-soluble polymer A1 is prepared by the preparation method of claim 1; in step (1), theThe molar ratio of the acrylamide to the amphoteric monomer is 18.98:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 20:1; in the step (2), the potassium persulfate was added in an amount of 0.11mol.L based on the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step (3), the temperature of the reaction is 70 ℃;
the water-soluble polymer A2 is prepared by the preparation method of claim 1; in step (1), the molar ratio of the acrylamide to the amphoteric monomer is 18.9:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 100:1; in the step (2), the potassium persulfate was added in an amount of 0.3mol.L based on the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step (3), the temperature of the reaction is 80 ℃;
the water-soluble polymer A3 is prepared by the preparation method of claim 1; in step (1), the molar ratio of the acrylamide to the amphoteric monomer is 18.94:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 60:1; in the step (2), the potassium persulfate was added in an amount of 0.11mol.L based on the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step (3), the temperature of the reaction is 70 ℃;
the water-soluble polymer A4 is prepared by the preparation method of claim 1; in step (1), the molar ratio of the acrylamide to the amphoteric monomer is 18.76:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 200:1; in the step (2), the potassium persulfate was added in an amount of 0.11mol.L based on the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step (3), the temperature of the reaction is 70 ℃;
the water-soluble polymer A5 is prepared by the preparation method of claim 1; in step (1), the molar ratio of the acrylamide to the amphoteric monomer is 18.98:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 20:1; in the step (2), the potassium persulfate was added in an amount of 0.11mol.L based on the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step (3), the temperature of the reaction is 75 ℃;
the water-soluble polymer A6 is prepared by the preparation method of claim 1; in step (1), the molar ratio of the acrylamide to the amphoteric monomer is 189:1; the molar ratio of the hydrophobic monomer to the amphoteric monomer is 100:1; in the step (2), the potassium persulfate was added in an amount of 0.3mol.L based on the volume of the polymerization system -1 The method comprises the steps of carrying out a first treatment on the surface of the In step (3), the temperature of the reaction was 85 ℃.
7. The use of a cleaning solution according to claim 1,
the amidoximated diaminomaleonitrile and the amidoximated diaminomaleonitrile of the tolyltriazole-amidoximated diaminomaleonitrile are prepared by a method comprising the steps of:
at K 2 CO 3 NH is added in the presence of a catalyst at a temperature of 75-95 DEG C 2 OH ∙ HCl and diaminomaleonitrile are reacted in aqueous ethanol to give amidoximated diaminomaleonitrile.
8. The use of a cleaning solution according to claim 1,
in the mixture of the tolyltriazole and the amidoximation diaminomaleonitrile, the mass ratio of the amidoximation diaminomaleonitrile to the tolyltriazole is 1:1.
9. The use of a cleaning solution according to claim 1,
the mass fraction of the EO-PO polymer L81 is 0.05%, 0.01% or 1.0%.
10. The use of a cleaning solution according to claim 1,
the mass fraction of the 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) is 0.01%, 0.7% or 2.0%.
11. The use of a cleaning solution according to claim 1,
The water is deionized water.
12. The use of a cleaning solution according to claim 1,
the mass fraction of the alcohol amine is 5%,10% or 20%.
13. The use of a cleaning solution according to claim 1,
the mass fraction of the organic alkali is 1%,2.5% or 5%.
14. The use of a cleaning solution according to claim 1,
the mass fraction of the chelating agent is 0.01%, 1.0% or 2.0%.
15. The use of a cleaning solution according to claim 1,
the mass fraction of the corrosion inhibitor is 0.01%, 0.5% or 2.0%.
16. The use of a cleaning solution according to claim 1,
the mass fraction of the ammonium carboxylate is 0.5%, 1.0% or 3.0%.
17. The use of the washing liquid according to claim 1, wherein the mass fraction of the cysteine in the washing liquid is 0.15% or 0.25%.
18. The use of a cleaning solution according to claim 1, characterized in that the cleaning solution is prepared from the following raw materials, which consist of the following components in mass fraction:
the alcohol amine is diglycolamine;
the mass fraction of the alcohol amine is 5-20%;
The mass fraction of the hydroxylamine is 5-20%;
the mass fraction of the cysteine is 0.15-0.25%;
the water-soluble polymer is the water-soluble polymer A1 as defined in claim 6;
the mass fraction of the water-soluble polymer is 0.01-0.05%;
the organic base is tetramethyl ammonium hydroxide;
the mass fraction of the organic alkali is 1-5%;
the chelating agent is ethylenediamine tetraacetic acid;
the mass fraction of the chelating agent is 0.01-2%;
the corrosion inhibitor is diamino Ma Laijing of the amidoxime;
the mass fraction of the corrosion inhibitor is 0.01-2%;
the ammonium carboxylate is ammonium oxalate;
the mass fraction of the ammonium carboxylate is 0.01-1%;
the mass fraction of the EO-PO polymer L81 is 0.01-1%;
the mass fraction of the 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) is 0.01-2%;
the water is deionized water; the deionized water is used for supplementing the balance.
19. The method for preparing the cleaning fluid according to claim 1, wherein the cleaning fluid is prepared from the following raw materials in parts by mass:
the alcohol amine is one or more of diglycolamine, monoethanolamine and triethanolamine;
The mass fraction of the alcohol amine is 5%;
the mass fraction of the hydroxylamine is 5%;
the mass fraction of the cysteine is 0.25%;
the water-soluble polymer is one or more of a water-soluble polymer A1, a water-soluble polymer A2, a water-soluble polymer A3, a water-soluble polymer A4, a water-soluble polymer A5 and a water-soluble polymer A6; the water-soluble polymer A1-A6 is as defined in claim 6;
the mass fraction of the water-soluble polymer is 0.025%;
the organic base is tetramethyl ammonium hydroxide and/or choline;
the mass fraction of the organic alkali is 2.5%;
the chelating agent is ethylenediamine tetraacetic acid and/or 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid;
the mass fraction of the chelating agent is 1%;
the corrosion inhibitor is the amidoximated diaminomaleonitrile or the amidoximated diaminomaleonitrile-tolyltriazole mixture; the mass ratio of the amidoximated diaminomaleonitrile to the tolyltriazole in the amidoximated diaminomaleonitrile-tolyltriazole mixture is 1:1;
the mass fraction of the corrosion inhibitor is 0.5%;
the ammonium carboxylate is ammonium oxalate and/or ammonium citrate;
The mass fraction of the ammonium carboxylate is 1%;
the mass fraction of the EO-PO polymer L81 is 0.05%;
the mass fraction of the 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) is 0.7%;
the water is deionized water; the deionized water is used for supplementing the balance.
20. The use of a cleaning fluid according to claim 1, wherein the cleaning fluid is prepared from the following raw materials, the raw materials comprising any combination of the following components in mass fraction:
combination 1:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% of the amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 2:10.0% diglycolamine, 10.000% hydroxylamine, 0.15% cysteine, 0.010% water-soluble polymer A1, 1.00% tetramethylammonium hydroxide, 0.01% ethylenediamine tetraacetic acid, 0.01% of the amidoximated diaminomaleonitrile, 0.50% ammonium oxalate, 0.01% EO-PO polymer L81, 0.01% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
Combination 3:20.0% diglycolamine, 10.000% hydroxylamine, 0.25% cysteine, 0.050% water-soluble polymer A1, 5.0% tetramethylammonium hydroxide, 2.0% ethylenediamine tetraacetic acid, 2.0% of the amidoximated diaminomaleonitrile, 3.0% ammonium oxalate, 1.0% EO-PO polymer L81, 2.0% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 4:10.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% of the amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 5:20.0% diglycolamine, 20.000% hydroxylamine, 0.15% cysteine, 0.025% water-soluble polymer A1, 5.0% tetramethylammonium hydroxide, 2.0% ethylenediamine tetraacetic acid, 2.0% of the amidoximated diaminomaleonitrile, 3.0% ammonium oxalate, 1.0% EO-PO polymer L81, 2.0% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 6:5.0% monoethanolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% of the amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
Combination 7:5.0% triethanolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% of said amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 8:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% choline, 1.00% ethylenediamine tetraacetic acid, 0.50% of the amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 9:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% 1, 2-cyclohexanediamine-N, N' -tetraacetic acid, 0.50% of said amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazol-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
Combination 10:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% 50% tolyltriazole+50% of the amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 11:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A1, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% of the amidoximated diaminomaleonitrile, 1.00% triammonium citrate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 12:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A2, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% of the amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
Combination 13:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A3, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% of the amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 14:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A4, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% of the amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
combination 15:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A5, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% of the amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
Combination 16:5.0% diglycolamine, 5.000% hydroxylamine, 0.25% cysteine, 0.025% water-soluble polymer A6, 2.50% tetramethylammonium hydroxide, 1.00% ethylenediamine tetraacetic acid, 0.50% of the amidoximated diaminomaleonitrile, 1.00% ammonium oxalate, 0.05% EO-PO polymer L81, 0.70% 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, the balance being deionized water;
the water-soluble polymer A1-A6 is as defined in claim 6.
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