CN113186043B - Fluorine-containing cleaning fluid composition and application thereof - Google Patents

Fluorine-containing cleaning fluid composition and application thereof Download PDF

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CN113186043B
CN113186043B CN202110459918.2A CN202110459918A CN113186043B CN 113186043 B CN113186043 B CN 113186043B CN 202110459918 A CN202110459918 A CN 202110459918A CN 113186043 B CN113186043 B CN 113186043B
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fluorine
containing cleaning
ammonium
deionized water
polymer
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CN113186043A (en
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王溯
蒋闯
冯强强
史筱超
于仙仙
王亮
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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
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble 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
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/08—Acids
    • 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
    • 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
    • C11D7/3245—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
    • C11D7/3272—Urea, guanidine or derivatives 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
    • C11D7/3281—Heterocyclic compounds

Abstract

The invention discloses a fluorine-containing cleaning fluid composition and application thereof. The fluorine-containing cleaning fluid composition comprises the following components in percentage by mass: 10-30% of oxidant, 0.001-0.01% of reduced glutathione, 0.001-0.25% of cysteine, 1-5% of fluoride, 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%9-anthracene formaldehyde-1, 1-diphenyl hydrazone and water, and the balance being water. The fluorine-containing cleaning fluid composition can selectively remove the hard mask on the microelectronic device, and has good application prospect.

Description

Fluorine-containing cleaning fluid composition and application thereof
Technical Field
The present invention relates to a fluorine-containing cleaning fluid composition and application thereof, and more particularly to a composition for selectively removing a hard mask containing a TiN, taN, tiNxOy or Ti hard mask and Ti alloy, as well as other residues, from such chips or wafers containing low dielectric constant dielectric materials, TEOS, copper and cobalt using the fluorine-containing cleaning fluid composition.
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., 28-14 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. The hard mask material (e.g., ti, tiN, silicon oxynitride, or the like) is removed after the etch protection, and other metals and dielectric materials are protected during the cleaning process to remove the hard mask material, thus challenging the compatibility of conventional fluorine-containing cleaning fluids with a variety of materials.
Developing a compatible cleaning solution to selectively remove the hard mask is a problem in the art.
Disclosure of Invention
The invention aims to overcome the defect that the existing fluorine-containing cleaning solution is poor in selectively removing a hard mask, and provides a fluorine-containing cleaning solution composition and application thereof. The fluorine-containing cleaning solution of the invention has good compatibility between interlayer dielectric materials and metal interconnection materials, good cleaning effect on residues after plasma etching and residues after ashing, and excellent selectivity to hard masks.
The invention solves the technical problems through the following technical proposal.
The invention provides a fluorine-containing cleaning fluid composition which comprises the following components in percentage by mass: 10-30% of oxidant, 0.001-0.01% of reduced glutathione, 0.001-0.25% of cysteine, 1-5% of fluoride, 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%9-anthracene formaldehyde-1, 1-diphenyl hydrazone and water, and the balance being water; the sum of the mass fractions of the components is 100 percent.
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 fluorine-containing cleaning liquid composition.
The fluorine-containing cleaning fluid composition preferably does not contain an amine-containing substance oxidant stabilizer. The amine-containing oxidant stabilizer may be an amine compound (e.g., primary amine, secondary amine, tertiary amine, or an alcohol compound containing such an amine), an alcohol amine compound (e.g., triethanolamine, N-methylethanolamine, N-dimethyldiglycolamine), or an amine-N-oxide compound (e.g., N-methylmorpholine oxide).
In the fluorine-containing cleaning fluid composition, the mass fraction of the oxidant can be 10-15%, and can also be 15-30%.
The oxidizing agent in the fluorine-containing cleaning liquid composition may be an oxidizing agent conventional in the art, preferably hydrogen peroxide (H) 2 O 2 ) Benzoyl peroxide, tetrabutylammonium peroxymonosulfate, ozone, ferric chloride, permanganate, perborate, perchlorate, persulfate, ammonium peroxydisulfate, peracetic acid, carbamide peroxide, nitric acid (HNO) 3 ) Ammonium chlorite (NH) 4 ClO 2 ) Ammonium chlorate (NH) 4 ClO 3 ) Ammonium iodate (NH) 4 IO 3 ) Ammonium perborate (NH) 4 BO 3 ) Ammonium perchlorate (NH) 4 ClO 4 ) Ammonium periodate (NH) 4 IO 3 ) Ammonium persulfate ((NH) 3 ) 2 S 2 O 8 ) Tetramethylammonium chlorite ((N (CH) 3 ) 4 ClO 2 ) Tetramethyl ammonium chlorate ((N (CH) 3 ) 4 ClO 3 ) Tetramethyl ammonium iodate (N (CH) 3 ) 4 IO 3 ) Tetramethyl ammonium perborate ((N (CH) 3 ) 4 BO 3 ) Tetramethyl ammonium perchlorate ((N (CH) 3 ) 4 )ClO 4 ) Tetramethyl ammonium periodate ((N (CH) 3 ) 4 IO 4 ) Tetramethyl ammonium persulfate ((N (NH) 4 ) 4 S 2 O 8 ) Urea peroxide ((CO (NH) 2 ) 2 )H 2 O 2 ) And peracetic acid (CH) 3 (CO) OOH), more preferably one or more of hydrogen peroxide, urea peroxide and peracetic acid, more preferably hydrogen peroxide and/or peracetic acid.
In the fluorine-containing cleaning liquid composition, the mass fraction of the reduced glutathione can be 0.005-0.01%.
In the fluorine-containing cleaning fluid composition, the mass fraction of the cysteine can be 0.15-0.25%.
The mass fraction of the fluoride in the fluorine-containing cleaning liquid composition can be 1.0-2.5%, and can also be 2.5-5.0%.
The fluoride may be any fluoride conventional in the art, preferably one or more of hydrogen fluoride, ammonium fluoride, potassium fluoride, alkali metal fluoride, tetraalkylammonium fluoride, fluoroboric acid, ammonium tetrafluoroborate, alkali metal tetrafluoroborate, tetraalkylammonium tetrafluoroborate and trimethyloxonium tetrafluoroborate, preferably hydrogen fluoride.
In the fluorine-containing cleaning liquid composition, the mass fraction of the organic alkali can be 1.0-2.5%, and can also be 2.5-5.0%.
In the fluorine-containing cleaning liquid composition, the organic base may be one or more of conventional organic bases in the art, preferably tetramethyl ammonium hydroxide, tetrapropyl ammonium hydroxide, tetrabutyl ammonium hydroxide, tetraethyl ammonium hydroxide (TEAH), benzyl Trimethyl Ammonium Hydroxide (BTAH), choline, (2-hydroxyethyl) trimethyl ammonium hydroxide, tris (2-hydroxyethyl) methyl ammonium hydroxide, monoethanolamine (MEA), diglycolamine (DGA), triethanolamine (TEA), isobutolamine, isopropanolamine, tetrabutyl ammonium hydroxide (TBPH) phosphonium and tetramethyl guanidine, more preferably one or more of tetramethyl ammonium hydroxide, tetrapropyl ammonium hydroxide, tetrabutyl ammonium hydroxide, tetraethyl ammonium hydroxide and choline, and most preferably tetramethyl ammonium hydroxide.
In the fluorine-containing cleaning liquid composition, the mass fraction of the chelating agent can be 0.01-1.0%, and can also be 1.0-2.0%.
The chelating agent in the fluorine-containing cleaning liquid composition may be a chelating agent conventional in the art, preferably 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid (CDTA), ethylenediamine tetraacetic acid (EDTA), 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, N ', one or more of N' -tetraacetic acid, N- {2- [ bis (carboxymethyl) amino ] ethyl } -N- (2-hydroxyethyl) glycine (HEDTA), ethylenediamine-N, N '-bis (2-hydroxyphenylacetic acid) (EDDHA), dioxaoctamethylenediaza tetraacetic acid (dotta) and triethylenetetramine hexaacetic acid (TTHA), more preferably 1, 2-cyclohexanediamine-N, N' -tetraacetic acid and/or ethylenediamine tetraacetic acid, most preferably ethylenediamine tetraacetic acid.
In the fluorine-containing cleaning fluid composition, the mass fraction of the corrosion inhibitor can be 0.01-0.5%, and can also be 0.5-2.0%.
In the fluorine-containing cleaning fluid composition, the corrosion inhibitor can be a conventional corrosion inhibitor in the field, preferably Benzotriazole (BTA), tolyltriazole, 5-phenyl-benzotriazole, 5-nitro-benzotriazole, 3-amino-5-mercapto-1, 2, 4-triazole, 1-amino-1, 2, 4-triazole, hydroxybenzotriazole, 2- (5-amino-pentyl) -benzotriazole, 1-amino-1, 2, 3-triazole, 1-amino-5-methyl-1, 2, 3-triazole, 3-amino-1, 2, 4-triazole, 3-mercapto-1, 2, 4-triazole, 3-isopropyl-1, 2, 4-triazole, 5-thiophen-benzotriazole, halo-benzotriazole (halogen = F, cl, br or I), naphthazole, 2-Mercaptobenzimidazole (MBI), 2-mercaptobenzothiazole, 4-methyl-2-phenylimidazole, 2-mercaptothiazoline, 5-aminotetrazole monohydrate, 5-amino-1, 3, 4-thiadiazole, 2-dithiol, 2, 4-triazine, 5-mercapto-1, 2, 4-mercapto-triazole, 3-mercapto-1, 2, 4-triazole, 3-isopropyl-1, 2, 4-triazole, 5-mercapto-benzotriazole, mercapto-benzothiazole, 2, mercapto-thiotetrazole, 2-methyl-thiotetrazole, 2-thiotetrazole, one or more of 4-methyl-4H-1, 2, 4-triazole-3-thiol, 5-amino-1, 3, 4-thiadiazole-2-thiol and benzothiazole, preferably benzotriazole and/or tolyltriazole, more preferably tolyltriazole.
In the fluorine-containing cleaning liquid composition, the mass fraction of the ammonium carboxylate can be 0.5-1.0%, and can also be 1.0-3.0%.
In the fluorine-containing cleaning liquid composition, the ammonium carboxylate may be one or more of ammonium carboxylate, preferably 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, and most preferably ammonium citrate.
In the fluorine-containing cleaning fluid composition, the mass fraction of the EO-PO polymer L81 can be 0.01-0.05%, and can also be 0.05-1.0%.
In the fluorine-containing cleaning liquid composition, the mass fraction of the 9-anthracene formaldehyde-1, 1-diphenyl hydrazone can be 0.01-0.9%, and can also be 0.9-2.0%.
In the fluorine-containing cleaning liquid composition, the water is preferably deionized water.
In a certain preferred technical scheme, the fluorine-containing cleaning liquid composition comprises the following components in percentage by mass: 10-30% of oxidant, 0.005-0.01% of reduced glutathione, 0.15-0.25% of cysteine, 1-5% of hydrogen fluoride, 1-5% of organic base, 0.01-2% of chelating agent, 0.01-2% of corrosion inhibitor, 0.5-3% of ammonium carboxylate, 0.05-1% of EO-PO polymer L81, 0.01-2%9-anthracene formaldehyde-1, 1-diphenyl hydrazone and water, and the balance being water;
the oxidant is one or more of hydrogen peroxide, peracetic acid and carbamide peroxide;
the organic base is tetramethyl ammonium hydroxide and/or choline;
the chelating agent is 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid and/or ethylenediamine tetraacetic acid;
the corrosion inhibitor is benzotriazole and/or tolyltriazole;
the ammonium carboxylate is ammonium oxalate and/or ammonium citrate.
In a certain preferred technical scheme, the fluorine-containing cleaning liquid composition comprises the following components in percentage by mass: 10-15% of oxidant, 0.005-0.01% of reduced glutathione, 0.15-0.25% of cysteine, 1-5% of hydrogen fluoride, 1-5% of organic base, 0.01-2% of chelating agent, 0.01-2% of corrosion inhibitor, 0.5-3% of ammonium carboxylate, 0.05-1% of EO-PO polymer L81, 0.01-2%9-anthracene formaldehyde-1, 1-diphenyl hydrazone and water, and the balance being water;
the oxidant is hydrogen peroxide and/or peracetic acid;
the organic base is tetramethyl ammonium hydroxide;
the chelating agent is 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid and/or ethylenediamine tetraacetic acid;
the corrosion inhibitor is benzotriazole and/or tolyltriazole;
the ammonium carboxylate is ammonium oxalate and/or ammonium citrate.
In a certain preferred technical scheme, the fluorine-containing cleaning liquid composition comprises the following components in percentage by mass: 10-15% of peracetic acid, 0.005-0.01% of reduced glutathione, 0.15-0.25% of cysteine, 1-5% of hydrogen fluoride, 1-5% of tetramethylammonium hydroxide, 0.01-2% of ethylenediamine tetraacetic acid, 0.01-2% of benzotriazole, 0.5-3% of ammonium oxalate, 0.01-1% of EO-PO polymer L81, 0.01-2%9-anthracene formaldehyde-1, 1-diphenylhydrazone and water, and the balance being water.
In a certain preferred technical scheme, the fluorine-containing cleaning liquid composition is any combination of the following components in percentage by mass:
combination 1:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and deionized water, the balance being deionized water;
combination 2:10% hydrogen peroxide, 0.01% reduced glutathione, 0.15% cysteine, 1.0% hydrogen fluoride, 1.0% tetramethylammonium hydroxide, 0.01% ethylenediamine tetraacetic acid, 0.01% benzotriazole, 0.5% ammonium oxalate, 0.01% EO-PO polymer L81, 0.1% 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and deionized water, the balance being deionized water;
combination 3:30% hydrogen peroxide, 0.01% reduced glutathione, 0.25% cysteine, 5.0% hydrogen fluoride, 5.0% tetramethylammonium hydroxide, 2.0% ethylenediamine tetraacetic acid, 2.0% benzotriazole, 3.0% ammonium oxalate, 1.0% eo-PO polymer L81, 2.0% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and water, the balance being deionized water;
combination 4:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and deionized water, the balance being deionized water;
combination 5:30% hydrogen peroxide, 0.01% reduced glutathione, 0.15% cysteine, 2.5% hydrogen fluoride, 5.0% tetramethylammonium hydroxide, 2.0% ethylenediamine tetraacetic acid, 2.0% benzotriazole, 3.0% ammonium oxalate, 1.0% EO-PO polymer L81, 2.0% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and deionized water, the balance being deionized water;
combination 6:15% carbamide peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and deionized water, the balance being deionized water;
combination 7:15% peracetic acid, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% eo-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone, and deionized water, the balance being deionized water;
combination 8:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% choline, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and deionized water, the balance being deionized water;
combination 9:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0%1, 2-cyclohexanediamine-N, N' -tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% eo-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone, and deionized water, the balance being deionized water;
combination 10:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% tolyltriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and deionized water, the balance being deionized water;
combination 11:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% tri-ammonium citrate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenyl hydrazone, and deionized water, the balance being deionized water.
In a certain preferred technical scheme, the fluorine-containing cleaning liquid composition comprises the following components: the above-mentioned oxidizing agent, the above-mentioned reduced glutathione, the above-mentioned cysteine, the above-mentioned fluoride, the above-mentioned organic base, the above-mentioned chelating agent, the above-mentioned corrosion inhibitor, the above-mentioned ammonium carboxylate, the above-mentioned EO-PO polymer L81, the above-mentioned 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and the above-mentioned water.
Wherein the above-mentioned oxidizing agent, the above-mentioned fluoride, the above-mentioned organic base, the above-mentioned chelating agent, the above-mentioned corrosion inhibitor, the above-mentioned ammonium carboxylate and the above-mentioned water all refer to the kinds and contents of these components.
The components of the invention can be in split charging mode, and can be temporarily mixed when in use; the above-mentioned oxidizing agent is preferably separately packaged as component A, and the components other than the above-mentioned oxidizing agent are mixed and packaged as component B, and when in use, AB is mixed.
The invention also provides a kit comprising one or more containers containing a component, a plurality of components, or a plurality of components that separate from each other or that divide each component into a plurality of groups, that are mixed to form the composition of the fluorine-containing cleaning fluid;
the components are the oxidant, the reduced glutathione, the cysteine, the fluoride, the organic base, the chelating agent, the corrosion inhibitor, the ammonium carboxylate, the EO-PO polymer L81, the 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and the water.
Wherein the above-mentioned oxidizing agent, the above-mentioned fluoride, the above-mentioned organic base, the above-mentioned chelating agent, the above-mentioned corrosion inhibitor, the above-mentioned ammonium carboxylate and the above-mentioned water all refer to the kinds and contents of these components.
Preferably, the oxidizing agent is placed in the container alone.
The invention also provides a preparation method of the fluorine-containing cleaning fluid composition, which comprises the following steps of mixing the components to obtain the fluorine-containing cleaning fluid composition.
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.
The invention also provides the use of a substance A for cleaning one or more of post plasma etch residues, post plasma ash residues and hard masks on microelectronic devices, said substance A being a fluorine-containing cleaning fluid composition as described above or a kit as described above.
The microelectronic device is preferably a silicon wafer.
The microelectronic device preferably comprises a low-k material and the hard mask is disposed over the low-k material.
The hard mask material is preferably a Ti-containing material, a TiN-containing material, a TaN-containing material, a TiNxOy-containing material, or a Ti alloy.
In such applications, it is preferred to impregnate the microelectronic device in the fluorine-containing cleaning fluid composition. The time of the soaking can be 20-30min. The temperature of the impregnation may be 40-60 ℃, for example 50 ℃.
In the application, the Ti alloy is conventional in the art.
In the present invention, the "low dielectric material" means a material having a dielectric constant of 3.5 or less.
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.
The 9-anthracene-formaldehyde-1, 1-diphenylhydrazone of the present invention was self-made, which was prepared according to example 2 of patent CN106366017 a; other reagents and starting materials were commercially available, with EO-PO polymer L81, EO-PO polymer L42, EO-PO polymer L62, and EO-PO polymer L31 all purchased from Nantong Jinlai chemical Co.
The invention has the positive progress effects that: the fluorine-containing cleaning liquid composition of the present invention has a high degree of selectivity for removing TiN, taN, tiNxOy, ti hard masks and Ti alloy hard masks, and is excellent in cleaning effect for post plasma etching residues and post ashing residues.
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.
In the following examples, the specific operating temperatures are not limited, and all refer to being conducted under room temperature conditions. Room temperature is 10-30 ℃.
The components of the fluorine-containing cleaning fluid composition of the invention: the types and amounts of oxidizing agent, reduced glutathione, cysteine, fluoride, organic base, chelating agent, corrosion inhibitor, ammonium carboxylate, EO-PO polymer L81, 9-anthracene formaldehyde-1, 1-diphenyl hydrazone, and deionized water are listed in tables 1 and 2, respectively.
The fluorine-containing cleaning liquid composition of the present invention was obtained by adding a solid component to a liquid component in accordance with the components and contents in tables 1 and 2 and stirring uniformly.
TABLE 1
Figure BDA0003042037730000091
/>
Figure BDA0003042037730000101
TABLE 2
Figure BDA0003042037730000102
/>
Figure BDA0003042037730000111
The following comparative examples 1 to 19 were fluorine-containing cleaning liquid compositions obtained by adding the solid component to the liquid component in accordance with the following components and contents, and stirring uniformly.
Comparative examples 1 to 15 below are screens based on the kinds or contents of components performed in example 1.
Comparative example 1
The component reduced glutathione of example 1 was replaced with oxidized glutathione, the others being unchanged.
Comparative example 2
The component reduced glutathione of example 1 was removed, the others being unchanged.
Comparative example 3
The component cysteine was removed from example 1, the others being unchanged.
Comparative example 4
The component cysteine in example 1 was replaced with arginine, the others being unchanged.
Comparative example 5
The component cysteine in example 1 was replaced with histidine, the others being unchanged.
Comparative example 6
Component EO-PO polymer L81 was removed as in example 1, the others being unchanged.
Comparative example 7
The component 9-anthracenecarbaldehyde-1, 1-diphenylhydrazone of example 1 was removed, the others being unchanged.
Comparative example 8
The ammonium carboxylate component of example 1 was removed, the others being unchanged.
Comparative example 9
The components other than EO-PO polymer L81 in example 1 were replaced with EO-PO polymer L42.
Comparative example 10
The components other than EO-PO polymer L81 in example 1 were replaced with EO-PO polymer L62.
Comparative example 11
The components other than EO-PO polymer L81 in example 1 were replaced with EO-PO polymer L31.
Comparative example 8
The component corrosion inhibitor of example 1 was removed, the others being unchanged.
Comparative example 13
The content of the oxidizing agent in example 1 was replaced with 9%, and the others were unchanged.
Comparative example 14
The content of reduced glutathione in example 1 was replaced with 0.02%, and the others were unchanged.
Comparative example 15
The cysteine content of example 1 was replaced with 0.40% and the others were unchanged.
Comparative example 16
The EO-PO polymer L81 content in example 1 was replaced with 1.10% and the others were unchanged.
Comparative example 17
The content of 9-anthracene-formaldehyde-1, 1-diphenylhydrazone in example 1 was replaced with 2.10%, and the others were unchanged.
Comparative example 18
The EO-PO polymer L81 content in example 1 was replaced with 0.0005%, otherwise unchanged.
Comparative example 19
The content of 9-anthracenecarbaldehyde-1, 1-diphenylhydrazone in example 1 was replaced with 0.0005%, otherwise unchanged.
Effect examples
1. Etch rate
Figure BDA0003042037730000131
TABLE 3 Table 3
Figure BDA0003042037730000132
/>
Figure BDA0003042037730000141
TABLE 4 Table 4
Figure BDA0003042037730000142
/>
Figure BDA0003042037730000151
/>
Figure BDA0003042037730000161
Remarks: the "TiN" in the table is PVD (Physical Vapor Deposition) physical vapor deposition TiN.
In Table 3, the fluorine-containing cleaning liquid composition of the present invention has extremely low etching rates for AlNxOy, aluminum nitride, W, copper, TEOS, BD2, siCN and cobalt on silicon wafers, which are all smaller than
Figure BDA0003042037730000163
While the fluorine-containing cleaning solution not in the scope of the application can etch the above materials at a rate up to about +.>
Figure BDA0003042037730000164
In Table 4, the fluorine-containing cleaning liquid composition of the present invention has extremely high etching rates to Ti, tiN, taN and TiNxOy on silicon wafers, which are both greater than
Figure BDA0003042037730000165
The hard mask can be removed rapidly; while the fluorine-containing cleaning solution not in the scope of the application has extremely low etching rate to the above-mentioned materials, the lowest is only +.>
Figure BDA0003042037730000166
In combination with tables 3 and 4, the fluorine-containing cleaning fluid composition of the present invention has a high etching selectivity to Ti, tiN, taN and TiNxOy on silicon wafers, and a selectivity ratio of at least 279:1, preferably as high as 18075, relative to the interconnect material on the device in table 3, for example TiN/Cu. In particular examples 1,2,4, 7, 9, 10 and 11, the TiN/Cu ratio was above 983 and the etching rate to copper was less than
Figure BDA0003042037730000167
2. Cleaning effect
Figure BDA0003042037730000162
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 5
Figure BDA0003042037730000171
/>
Figure BDA0003042037730000181
It can be seen that the fluorine-containing cleaning liquid composition of the present invention has good wafer cleaning effect and good compatibility with metal wires after plasma etching and patterning of post-ashing residues.

Claims (10)

1. The fluorine-containing cleaning fluid composition is characterized by comprising the following components in percentage by mass: 10-30% of oxidant, 0.001-0.01% of reduced glutathione, 0.001-0.25% of cysteine, 1-5% of fluoride, 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 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and water, and the balance being water; the sum of the mass fractions of the components is 100 percent;
the oxidant is hydrogen peroxide and/or peracetic acid;
the fluoride is hydrogen fluoride;
the organic base is tetramethyl ammonium hydroxide and/or choline;
the chelating agent is 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid and/or ethylenediamine tetraacetic acid;
the corrosion inhibitor is benzotriazole and/or tolyltriazole;
the ammonium carboxylate is ammonium oxalate and/or ammonium citrate.
2. The fluorine-containing cleaning liquid composition according to claim 1, wherein the mass fraction of the oxidizing agent in the fluorine-containing cleaning liquid composition is 10 to 30%;
and/or, in the fluorine-containing cleaning liquid composition, the mass fraction of the reduced glutathione is 0.005% -0.01%;
and/or, in the fluorine-containing cleaning fluid composition, the mass fraction of the cysteine is 0.15-0.25%;
and/or, the mass fraction of the fluoride in the fluorine-containing cleaning liquid composition is 1.0-5.0%;
and/or, in the fluorine-containing cleaning liquid composition, the mass fraction of the organic base is 1.0-5.0%;
and/or, in the fluorine-containing cleaning liquid composition, the mass fraction of the chelating agent is 0.01-2.0%;
and/or, in the fluorine-containing cleaning fluid composition, the mass fraction of the corrosion inhibitor is 0.01-2.0%;
and/or, in the fluorine-containing cleaning liquid composition, the mass fraction of the ammonium carboxylate is 0.5-3.0%;
and/or, in the fluorine-containing cleaning liquid composition, the mass fraction of the EO-PO polymer L81 is 0.01-1.0%;
and/or, in the fluorine-containing cleaning liquid composition, the mass fraction of the 9-anthracene formaldehyde-1, 1-diphenyl hydrazone is 0.01-2.0%.
3. The fluorine-containing cleaning liquid composition according to claim 1, wherein the fluorine-containing cleaning liquid composition does not contain an amine compound, an alcohol amine compound or an amine-N-oxide compound; the alcohol amine compound is triethanolamine, N-methylethanolamine and N, N-dimethyl diglycolamine; the amine-N-oxide compound is N-methylmorpholine oxide;
and/or, in the fluorine-containing cleaning liquid composition, the organic base is tetramethyl ammonium hydroxide;
and/or, in the fluorine-containing cleaning liquid composition, the chelating agent is ethylenediamine tetraacetic acid;
and/or, in the fluorine-containing cleaning fluid composition, the corrosion inhibitor is tolyltriazole;
and/or, in the fluorine-containing cleaning liquid composition, the ammonium carboxylate is tri-ammonium citrate;
and/or, the water is deionized water.
4. The fluorine-containing cleaning fluid composition as claimed in claim 1, wherein the fluorine-containing cleaning fluid composition comprises the following components in mass fraction: 10-30% of oxidant, 0.005-0.01% of reduced glutathione, 0.15-0.25% of cysteine, 1-5% of hydrogen fluoride, 1-5% of organic base, 0.01-2% of chelating agent, 0.01-2% of corrosion inhibitor, 0.5-3% of ammonium carboxylate, 0.05-1% of EO-PO polymer L81, 0.01-2% of 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and water, and the balance being water;
the oxidant is hydrogen peroxide and/or peracetic acid;
the organic base is tetramethyl ammonium hydroxide and/or choline;
the chelating agent is 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid and/or ethylenediamine tetraacetic acid;
the corrosion inhibitor is benzotriazole and/or tolyltriazole;
the ammonium carboxylate is ammonium oxalate and/or ammonium citrate.
5. The fluorine-containing cleaning fluid composition as claimed in claim 1, wherein the fluorine-containing cleaning fluid composition comprises the following components in mass fraction: 10-15% of oxidant, 0.005-0.01% of reduced glutathione, 0.15-0.25% of cysteine, 1-5% of hydrogen fluoride, 1-5% of organic base, 0.01-2% of chelating agent, 0.01-2% of corrosion inhibitor, 0.5-3% of ammonium carboxylate, 0.05-1% of EO-PO polymer L81, 0.01-2% of 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and water, and the balance being water;
the oxidant is hydrogen peroxide and/or peracetic acid;
the organic base is tetramethyl ammonium hydroxide;
the chelating agent is 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid and/or ethylenediamine tetraacetic acid;
the corrosion inhibitor is benzotriazole and/or tolyltriazole;
the ammonium carboxylate is ammonium oxalate and/or ammonium citrate.
6. The fluorine-containing cleaning fluid composition as claimed in claim 1, wherein the fluorine-containing cleaning fluid composition comprises the following components in mass fraction: 10-15% of peracetic acid, 0.005-0.01% of reduced glutathione, 0.15-0.25% of cysteine, 1-5% of hydrogen fluoride, 1-5% of tetramethylammonium hydroxide, 0.01-2% of ethylenediamine tetraacetic acid, 0.01-2% of benzotriazole, 0.5-3% of ammonium oxalate, 0.01-1% of EO-PO polymer L81, 0.01-2% of 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and water, and the balance being water.
7. The fluorine-containing cleaning fluid composition as claimed in claim 1, wherein the fluorine-containing cleaning fluid composition comprises any combination of the following components in mass fraction:
combination 1:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and deionized water, the balance being deionized water;
combination 2:10% hydrogen peroxide, 0.01% reduced glutathione, 0.15% cysteine, 1.0% hydrogen fluoride, 1.0% tetramethylammonium hydroxide, 0.01% ethylenediamine tetraacetic acid, 0.01% benzotriazole, 0.5% ammonium oxalate, 0.01% EO-PO polymer L81, 0.1% 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and deionized water, the balance being deionized water;
combination 3:30% hydrogen peroxide, 0.01% reduced glutathione, 0.25% cysteine, 5.0% hydrogen fluoride, 5.0% tetramethylammonium hydroxide, 2.0% ethylenediamine tetraacetic acid, 2.0% benzotriazole, 3.0% ammonium oxalate, 1.0% EO-PO polymer L81, 2.0% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and water, the balance being deionized water;
combination 4:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and deionized water, the balance being deionized water;
combination 5:30% hydrogen peroxide, 0.01% reduced glutathione, 0.15% cysteine, 2.5% hydrogen fluoride, 5.0% tetramethylammonium hydroxide, 2.0% ethylenediamine tetraacetic acid, 2.0% benzotriazole, 3.0% ammonium oxalate, 1.0% EO-PO polymer L81, 2.0% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and deionized water, the balance being deionized water;
combination 6:15% carbamide peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and deionized water, the balance being deionized water;
combination 7:15% peracetic acid, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone, and deionized water, the balance being deionized water;
combination 8:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% choline, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and deionized water, the balance being deionized water;
combination 9:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0%1, 2-cyclohexanediamine-N, N' -tetraacetic acid, 0.5% benzotriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone, and deionized water, the balance being deionized water;
combination 10:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% tolyltriazole, 1.0% ammonium oxalate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenylhydrazone and deionized water, the balance being deionized water;
combination 11:15% hydrogen peroxide, 0.005% reduced glutathione, 0.25% cysteine, 2.5% hydrogen fluoride, 2.5% tetramethylammonium hydroxide, 1.0% ethylenediamine tetraacetic acid, 0.5% benzotriazole, 1.0% tri-ammonium citrate, 0.05% EO-PO polymer L81, 0.9% 9-anthracene formaldehyde-1, 1-diphenyl hydrazone, and deionized water, the balance being deionized water.
8. A fluorochemical cleaning fluid composition according to any of claims 1 to 7 wherein said fluorochemical cleaning fluid composition comprises the following components: the oxidant, the reduced glutathione, the cysteine, the fluoride, the organic base, the chelating agent, the corrosion inhibitor, the ammonium carboxylate, the EO-PO polymer L81, the 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and the water.
9. A kit comprising one or more containers containing a single component, separate components or multiple components that form the components of the fluorine cleaning fluid composition of any of claims 1-8;
the components are the oxidant, the reduced glutathione, the cysteine, the fluoride, the organic base, the chelating agent, the corrosion inhibitor, the ammonium carboxylate, the EO-PO polymer L81, the 9-anthracene formaldehyde-1, 1-diphenyl hydrazone and the water.
10. Use of a substance a for cleaning one or more of post plasma etch residues, post plasma ash residues and hard masks on microelectronic devices, said substance a being a fluorine-containing cleaning fluid composition according to any of claims 1-8 or a kit according to claim 9.
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