CN115710536B - Preparation method of cleaning liquid - Google Patents

Preparation method of cleaning liquid Download PDF

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CN115710536B
CN115710536B CN202211413424.1A CN202211413424A CN115710536B CN 115710536 B CN115710536 B CN 115710536B CN 202211413424 A CN202211413424 A CN 202211413424A CN 115710536 B CN115710536 B CN 115710536B
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water
soluble polymer
mass fraction
diaminomaleonitrile
amidoximated
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CN115710536A (en
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王溯
蒋闯
冯强强
张怡
任发强
邢乃观
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Shanghai Xinyang Semiconductor Material Co Ltd
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Shanghai Xinyang Semiconductor Material Co Ltd
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Abstract

The invention discloses a preparation method of a cleaning liquid. The preparation method comprises the following steps: mixing all the components in the cleaning solution to obtain the cleaning solution; 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 fluids prepared by the cleaning fluid preparation method of the present invention can clean a wide range of residues and are generally non-corrosive to exposed substrate materials (e.g., exposed low k dielectric materials, metal oxides, metals, metal nitrides, and alloys thereof).

Description

Preparation method of cleaning liquid
Technical Field
The invention relates to a preparation method of a cleaning liquid.
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 a preparation method of the cleaning solution. The cleaning solution prepared by the preparation method of the cleaning solution has at least one or more of the following advantages: the range of cleanable residues is wide; and are 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).
The invention solves the technical problems through the following technical proposal.
The invention provides a preparation method of cleaning liquid, which comprises the following steps of mixing all components in the cleaning liquid to obtain the cleaning liquid;
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 preparation method of the cleaning liquid, the mixing mode is preferably to add the solid component in the components into the liquid component and stir the mixture uniformly.
In the preparation method of the cleaning solution, the mixing temperature can be room temperature.
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, refer to patent CN104140507AThe preparation in example 1 was carried out by replacing the reaction temperature with 70℃from 45℃under the same conditions and operation as in example 1 of 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 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 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 step (2), relative to the polymerizationThe system volume, the addition amount of potassium persulfate is 0.11mol.L -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 EO-PO 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 application of the cleaning liquid in removing residues after etching or ashing in a cleaning process of an Integrated Circuit (IC) wet process.
In such applications, it is preferred to impregnate the integrated circuit 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 "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.
As used herein, "room temperature" refers to 10-30deg.C.
The invention has the positive progress effects that: the cleaning fluids made using the cleaning fluid preparation methods of the present invention can clean a wide range of residues and are 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, titanium nitride, tantalum nitride, and tungsten nitride), and alloys thereof).
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: will NH 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 solutions of the present invention have very low etch rates for exposed substrate materials on silicon wafers, such as AlNxOy, alN, W, cu, LP-TEOS, BD2, siCN, co, ti, tiN, taN, and TiNxOy, all less thanHardly corroding the interconnection material on the device; the comparative cleaning solution has a slightly higher etching rate for the above-mentioned materials, up to +.> 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 the residues after etching or ashing in the cleaning process of the Integrated Circuit (IC) wet process.

Claims (20)

1. The preparation method of the cleaning liquid is characterized by comprising the following steps: mixing all the components in the cleaning solution to obtain the cleaning solution; the cleaning solution 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, 0.01-2.0% of chelating agent, 0.01-2.0% of corrosion inhibitor, 0.5-3.0% of 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 alcohol amine is diglycolamine, monoethanolamine and/or 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 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): 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 method for preparing a cleaning solution according to claim 1, wherein the mixing is carried out by adding the solid component of the components to the liquid component and stirring uniformly;
the temperature of the mixing is room temperature.
3. A process for preparing a cleaning liquid according to claim 1,
the mass fraction of the hydroxylamine is 5%,10% or 20%.
4. The method for preparing a cleaning liquid according to claim 1, wherein the mass fraction of the water-soluble polymer is 0.025%,0.01% or 0.05%.
5. The method for preparing a cleaning liquid according to claim 1, wherein the water-soluble polymer is one or more of water-soluble polymer A1, water-soluble polymer A2, water-soluble polymer A3, water-soluble polymer A4, water-soluble polymer A5 and water-soluble polymer A6;
wherein the water-soluble polymer A1 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 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 step (2), potassium persulfate is present in the polymerization system in terms of volumeThe addition amount of (C) was 0.11mol.L -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 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 step (3), the temperature of the reaction was 85 ℃.
6. The method for preparing a cleaning liquid according to claim 1, wherein 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 react in aqueous ethanol to give amidoximated diaminomaleonitrile.
7. The method of preparing a cleaning solution according to claim 1, wherein the mass ratio of the amidoximated diaminomaleonitrile to the tolyltriazole in the mixture of tolyltriazole and amidoximated diaminomaleonitrile is 1:1.
8. The method for preparing a cleaning liquid according to claim 1, wherein the mass fraction of the EO-PO polymer L81 is 0.05%, 0.01% or 1.0%.
9. The method for preparing a cleaning solution according to claim 1, wherein the mass fraction of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) is 0.01%, 0.7% or 2.0%.
10. The method of preparing a cleaning solution as recited in claim 1, wherein the water is deionized water.
11. A process for preparing a cleaning liquid according to claim 1,
the mass fraction of the alcohol amine is 5%,10% or 20%.
12. The method for preparing a cleaning liquid according to claim 1, wherein the mass fraction of the organic base is 1%,2.5% or 5%.
13. The method for preparing a cleaning liquid according to claim 1, wherein the chelating agent is 0.01%, 1.0% or 2.0% by mass.
14. The method for preparing a cleaning solution according to claim 1, wherein the corrosion inhibitor is 0.01%, 0.5% or 2.0% by mass.
15. The method according to claim 1, wherein the mass fraction of the ammonium carboxylate is 0.5%, 1.0% or 3.0%.
16. The method for preparing a cleaning solution according to claim 1, wherein the mass fraction of the cysteine in the cleaning solution is 0.15% or 0.25%.
17. 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 5-20%;
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 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 5;
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;
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 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.
18. 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 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 claimed in claim 5;
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 0.5-3%;
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.
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 5;
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 method for preparing the cleaning fluid according to claim 1, wherein the cleaning fluid is prepared from the following raw materials, and 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% 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- (benzotriazol-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 to A6 as defined in claim 5.
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