CN113150885B - Fluorine-containing cleaning liquid composition - Google Patents

Fluorine-containing cleaning liquid composition Download PDF

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CN113150885B
CN113150885B CN202110459926.7A CN202110459926A CN113150885B CN 113150885 B CN113150885 B CN 113150885B CN 202110459926 A CN202110459926 A CN 202110459926A CN 113150885 B CN113150885 B CN 113150885B
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fluorine
percent
containing cleaning
benzotriazole
cleaning liquid
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CN113150885A (en
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王溯
蒋闯
冯强强
史筱超
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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/722—Ethers of polyoxyalkylene glycols having mixed oxyalkylene groups; Polyalkoxylated fatty alcohols or polyalkoxylated alkylaryl alcohols with mixed oxyalkylele groups
    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/0005—Other compounding ingredients characterised by their effect
    • C11D3/0073—Anticorrosion compositions
    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/042—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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2075—Carboxylic acids-salts thereof
    • C11D3/2082—Polycarboxylic acids-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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/26—Organic compounds containing nitrogen
    • C11D3/28—Heterocyclic compounds containing nitrogen in the ring
    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/26—Organic compounds containing nitrogen
    • C11D3/30—Amines; Substituted amines ; Quaternized amines
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/26—Organic compounds containing nitrogen
    • C11D3/32—Amides; Substituted amides
    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/26—Organic compounds containing nitrogen
    • C11D3/33—Amino carboxylic 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3942—Inorganic per-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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3945—Organic per-compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02041—Cleaning
    • H01L21/02057—Cleaning during device manufacture
    • H01L21/0206—Cleaning during device manufacture during, before or after processing of insulating layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02041—Cleaning
    • H01L21/02057—Cleaning during device manufacture
    • H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
    • H01L21/02071—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a delineation, e.g. RIE, of conductive layers
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10—Objects to be cleaned
    • C11D2111/14—Hard surfaces
    • C11D2111/22—Electronic devices, e.g. PCBs or semiconductors

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Abstract

The invention discloses a fluorine-containing cleaning liquid composition. The fluorine-containing cleaning liquid composition comprises the following components in percentage by mass: 10 to 30 percent of oxidant, 0.001 to 0.01 percent of reduced glutathione, 0.001 to 0.25 percent of cysteine, 1 to 5 percent of fluoride, 1 to 5 percent of organic alkali, 0.01 to 2 percent of chelating agent, 0.01 to 2 percent of corrosion inhibitor, 0.5 to 3 percent of ammonium carboxylate, 0.01 to 1 percent of EO-PO polymer L31, 0.01 to 2 percent of passivating agent and water, and the balance is water; the sum of the mass fractions of the components is 100 percent. The fluorine-containing cleaning solution composition can selectively remove the hard mask on the microelectronic device and has good application prospect.

Description

Fluorine-containing cleaning liquid composition
Technical Field
The present invention relates to a fluorine-containing cleaning solution composition, and more particularly to a composition for selectively removing a hard mask containing TiN, taN, tiNxOy, or Ti, and an alloy of Ti, and other residues from such a chip or wafer comprising a low dielectric constant dielectric material, TEOS, copper, cobalt, and other low dielectric constant dielectric materials, using a cleaning solution composition.
Background
In the chip manufacturing technology, the cleaning solution of residues after copper interconnection plasma etching is mainly fluorine-containing cleaning solution composition. With the continuous advance of technology nodes, more and more materials are introduced, such as metal materials of cobalt, titanium, tungsten, titanium nitride, and the like, and low-k dielectric materials, and the compatibility of the conventional fluorine-containing cleaning solution composition with various materials is challenged.
Plasma dry etching is commonly used to fabricate vertical sidewall trenches and anisotropic interconnect vias in a copper (Cu)/low dielectric constant dual damascene fabrication process. As technology nodes evolve to 45nm and smaller (e.g., 28-14 nm), the shrinking of semiconductor device dimensions makes it more challenging to achieve precise profile control of vias and trenches. Integrated circuit manufacturing companies are investigating the use of various hard masks to improve etch selectivity to low dielectric constant materials for better profile control. The hardmask material (e.g., ti, tiN, silicon oxynitride, or the like) is removed after etch protection, and other metals and dielectric materials are protected during the cleaning process to remove the hardmask material, thereby challenging compatibility of conventional fluorine-containing cleaning solution compositions with a variety of materials.
Developing a highly compatible cleaning solution for selectively removing the hard mask is a problem to be solved in the art.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defect of poor selectivity of removing a hard mask by the conventional fluorine-containing cleaning liquid composition, and provides the fluorine-containing cleaning liquid composition. Compared with an interlayer dielectric material and a metal interconnection material of a microelectronic device, the fluorine-containing cleaning solution composition has excellent selectivity on a hard mask and has good cleaning effect on post-plasma etching residues and post-ashing residues.
The present invention solves the above technical problems by the following technical solutions.
The invention provides a fluorine-containing cleaning liquid composition which comprises the following components in percentage by mass: 10 to 30 percent of oxidant, 0.001 to 0.01 percent of reduced glutathione, 0.001 to 0.25 percent of cysteine, 1 to 5 percent of fluoride, 1 to 5 percent of organic alkali, 0.01 to 2 percent of chelating agent, 0.01 to 2 percent of corrosion inhibitor, 0.5 to 3 percent of ammonium carboxylate, 0.01 to 1 percent of EO-PO polymer L31, 0.01 to 2 percent of passivator and water, and the balance is 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 the components in the fluorine-containing cleaning liquid composition.
The fluorine-containing cleaning solution composition preferably does not contain an amine-containing oxidizing agent stabilizer. The amine-containing oxidant stabilizer can be an amine compound (such as primary amine, secondary amine, tertiary amine or alcohol compounds containing these amines), an alcohol amine compound (such as triethanolamine, N-methylethanolamine, N-dimethyldiglycolamine) or an amine-N-oxide compound (such as N-methylmorpholine oxide).
In the fluorine-containing cleaning liquid composition, the mass fraction of the oxidizing agent can be 10-15%, and can also be 15-30%.
In the fluorine-containing cleaning liquid composition, the oxidizing agent can be an oxidizing agent conventional in the art, and is preferably hydrogen peroxide (H)2O2) Benzoyl peroxide, tetrabutylammonium peroxymonosulfate, ozone, ferric chloride, permanganate, perborate, perchlorate, persulfate, ammonium peroxydisulfate, peracetic acid, urea peroxide, nitric acid (HNO)3) Ammonium chlorite (NH)4ClO2) Ammonium chlorate (NH)4ClO3) Ammonium iodate (NH)4IO3) Ammonium perborate (NH)4BO3) Ammonium perchlorate (NH)4ClO4) Ammonium periodate (NH)4IO3) Ammonium persulfate ((NH)4)2S2O8) Tetramethylammonium chlorite ((N (CH)3)4)ClO2) Tetramethylammonium chlorate ((N (CH))3)4)ClO3) Tetramethylammonium iodate ((N (CH)3)4)IO3) Tetramethylammonium perborate ((N (CH)3)4)BO3) Tetramethylammonium perchlorate ((N (CH)3)4)ClO4) Tetramethylammonium periodate ((N (CH)3)4)IO4) Tetramethylammonium persulfate ((N (CH))3)4)S2O8) Urea peroxide ((CO (NH))2)2)H2O2) And peroxyAcetic acid (CH)3(CO) OOH); more preferably one or more of hydrogen peroxide, carbamide peroxide and peroxyacetic acid; most preferred is peroxyacetic 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 liquid composition, the mass fraction of the cysteine may be 0.15 to 0.25%.
In the fluorine-containing cleaning liquid composition, the mass fraction of the fluoride can be 1-2.5%, and can also be 2.5-5%.
In the fluorine-containing cleaning liquid composition, the fluoride may be a fluoride which is conventional in the art, and is 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, and is more preferably hydrogen fluoride.
In the fluorine-containing cleaning liquid composition, the mass fraction of the organic base can be 1.0-2.5%, and can also be 2.5% -5%.
In the fluorine-containing cleaning solution composition, the organic base may be one or more of organic bases conventional in the art, preferably tetramethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, tetraethylammonium hydroxide (TEAH), benzyltrimethylammonium hydroxide (BTAH), choline, (2-hydroxyethyl) trimethylammonium hydroxide, tris (2-hydroxyethyl) methylammonium hydroxide, monoethanolamine (MEA), diglycolamine (DGA), triethanolamine (TEA), isobutanol amine, isopropanolamine, tetrabutylphosphonium hydroxide (TBPH), tetramethylguanidine; more preferably one or more of tetramethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, tetraethylammonium hydroxide and choline, most preferably tetramethylammonium hydroxide and/or choline.
In the fluorine-containing cleaning liquid composition, the chelating agent may be present in an amount of 0.01 to 1% by mass or 1 to 2% by mass.
In the fluorine-containing cleaning liquid composition, the chelating agent may be a chelating agent conventional in the art, preferably 1, 2-cyclohexanediamine-N, N, N ', N ' -tetraacetic acid (CDTA), ethylenediaminetetraacetic acid, nitrilotriacetic acid, diethylenetriaminepentaacetic acid, 1,4,7, 10-tetraazacyclododecane-1, 4,7, 10-tetraacetic acid, ethyleneglycol 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), dioxaoctamethylenediazepine tetraacetic acid (DOCTA), and triethylenetetraminehexaacetic acid (TTHA), more preferably 1, 2-cyclohexanediamine-N, N, N ', N ' -tetraacetic acid and/or ethylenediaminetetraacetic acid.
In the fluorine-containing cleaning liquid composition, the mass fraction of the corrosion inhibitor can be 0.01-0.5%, and can also be 0.5-2%.
<xnotran> , , (BTA), ,5- - ,5- - ,3- -5- -1,2,4- , 1- -1,2,4- , ,2- (5- - ) - , 1- -1,2,3- , 1- -5- -1,2,3- ,3- -1,2,4- ,3- -1,2,4- ,3- -1,2,4- ,5- - , - ( = F, cl, br I), ,2- (MBI), 2- ,4- -2- ,2- ,5- ,5- ,5- -1,3,4- -2- ,2,4- -6- -1,3,5- , , , ,1,3- -2- ,1,5- , 1- -5- , , , ,4- -4H-1,2,4- -3- , </xnotran> One or more of 5-amino-1, 3, 4-thiadiazole-2-thiol and benzothiazole, more preferably benzotriazole and/or tolyltriazole; benzotriazole is most preferred.
In the fluorine-containing cleaning liquid composition, the mass fraction of the ammonium carboxylate may be 0.5 to 1%, and may be 1 to 3%.
In the fluorine-containing cleaning liquid composition, the ammonium carboxylate may be an ammonium carboxylate which is conventional in the art, and is preferably one or more of ammonium oxalate, ammonium lactate, ammonium tartrate, triammonium citrate, ammonium acetate, ammonium carbamate, ammonium carbonate, ammonium benzoate, ammonium ethylenediaminetetraacetate, diammonium ethylenediaminetetraacetate, triammonium ethylenediaminetetraacetate, tetraammonium ethylenediaminetetraacetate, ammonium succinate, ammonium formate and 1-H-pyrazole-3-ammonium formate, and more preferably ammonium oxalate and/or triammonium citrate.
In the fluorine-containing cleaning liquid composition, the mass fraction of the EO-PO polymer L31 can be 0.01-0.05%, and can also be 0.05-1.0%.
In the fluorine-containing cleaning liquid composition, the passivating agent can be 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole).
In the fluorine-containing cleaning liquid composition, the mass fraction of the passivating agent can be 0.01-0.7%, and can also be 0.7-2%.
In the fluorine-containing cleaning liquid composition, the water is preferably deionized water.
In a preferred technical scheme, the fluorine-containing cleaning liquid composition comprises the following components in percentage by mass: 10-30% of oxidant, 0.05-0.01% 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, 0.01-1% of EO-PO polymer L31, 0.01-2% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and water, and the balance is made up by water;
the oxidant is one or more of hydrogen peroxide, carbamide peroxide and peroxyacetic acid;
the organic alkali is tetramethyl ammonium hydroxide and/or choline;
the chelating agent is 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid and/or ethylene diamine tetraacetic acid;
the corrosion inhibitor is benzotriazole and/or tolyltriazole;
the ammonium carboxylate is ammonium oxalate and/or triammonium citrate.
In a preferred technical scheme, the fluorine-containing cleaning liquid composition comprises the following components in percentage by mass: 10-20% of peroxyacetic acid, 0.001-0.01% of reduced glutathione, 0.02-0.25% of cysteine, 1.5-3.5% of hydrogen fluoride, 1.5-3.5% of tetramethylammonium hydroxide, 0.5-1.5% of ethylenediamine tetraacetic acid, 0.1-1% of benzotriazole, 0.5-1.5% of ammonium oxalate, 0.01-0.1% of EO-PO polymer L31, 0.1-1% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and water, and the balance being water.
In a preferred embodiment, the fluorine-containing cleaning liquid composition comprises any combination of the following components in parts by mass:
combination 1:15% of hydrogen peroxide, 0.005% of reduced glutathione, 0.25% of cysteine, 2.5% of hydrogen fluoride, 2.5% of tetramethylammonium hydroxide, 1.0% of ethylenediamine tetraacetic acid, 0.5% of benzotriazole, 1.0% of ammonium oxalate, 0.05% of EO-PO polymer L31, 0.7% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, wherein the balance is deionized water;
and (3) combination 2:10% of hydrogen peroxide, 0.01% of reduced glutathione, 0.15% of cysteine, 1.0% of hydrogen fluoride, 1.0% of tetramethylammonium hydroxide, 0.01% of ethylenediamine tetraacetic acid, 0.01% of benzotriazole, 0.5% of ammonium oxalate, 0.01% of EO-PO polymer L31, 0.01% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, wherein the balance is deionized water;
and (3) combination: 30% of hydrogen peroxide, 0.01% of reduced glutathione, 0.25% of cysteine, 5.0% of hydrogen fluoride, 5.0% of tetramethylammonium hydroxide, 2.0% of ethylenediamine tetraacetic acid, 2.0% of benzotriazole, 3.0% of ammonium oxalate, 1.0% of EO-PO polymer L31, 2.0% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and water, and the balance of deionized water is supplemented;
and (4) combination: 15% of hydrogen peroxide, 0.005% of reduced glutathione, 0.25% of cysteine, 2.5% of hydrogen fluoride, 2.5% of tetramethylammonium hydroxide, 1.0% of ethylenediamine tetraacetic acid, 0.5% of benzotriazole, 1.0% of ammonium oxalate, 0.05% of EO-PO polymer L31, 0.7% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, wherein the balance is made up by deionized water;
and (4) combination 5:30% of hydrogen peroxide, 0.01% of reduced glutathione, 0.15% of cysteine, 2.5% of hydrogen fluoride, 5.0% of tetramethylammonium hydroxide, 2.0% of ethylenediamine tetraacetic acid, 2.0% of benzotriazole, 3.0% of ammonium oxalate, 1.0% of EO-PO polymer L31, 2.0% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, wherein the balance is deionized water;
and (4) combination 6:15% of carbamide peroxide, 0.005% of reduced glutathione, 0.25% of cysteine, 2.5% of hydrogen fluoride, 2.5% of tetramethylammonium hydroxide, 1.0% of ethylenediamine tetraacetic acid, 0.5% of benzotriazole, 1.0% of ammonium oxalate, 0.05% of EO-PO polymer L31, 0.7% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, wherein the balance is deionized water;
and (3) combination 7:15% of peroxyacetic acid, 0.005% of reduced glutathione, 0.25% of cysteine, 2.5% of hydrogen fluoride, 2.5% of tetramethylammonium hydroxide, 1.0% of ethylenediamine tetraacetic acid, 0.5% of benzotriazole, 1.0% of ammonium oxalate, 0.05% of EO-PO polymer L31, 0.7% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, wherein the balance is the balance;
and (4) combination 8:15% of hydrogen peroxide, 0.005% of reduced glutathione, 0.25% of cysteine, 2.5% of hydrogen fluoride, 2.5% of choline, 1.0% of ethylenediamine tetraacetic acid, 0.5% of benzotriazole, 1.0% of ammonium oxalate, 0.05% of EO-PO polymer L31, 0.7% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, wherein the balance is the rest;
combination 9:15% of hydrogen peroxide, 0.005% of reduced glutathione, 0.25% of cysteine, 2.5% of hydrogen fluoride, 2.5% of tetramethylammonium hydroxide, 1.0% of 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid, 0.5% of benzotriazole, 1.0% of ammonium oxalate, 0.05% of EO-PO polymer L31, 0.7% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, wherein the balance is made up by deionized water;
combination 10:15% of hydrogen peroxide, 0.005% of reduced glutathione, 0.25% of cysteine, 2.5% of hydrogen fluoride, 2.5% of tetramethylammonium hydroxide, 1.0% of ethylenediamine tetraacetic acid, 0.5% of tolyltriazole, 1.0% of ammonium oxalate, 0.05% of EO-PO polymer L31, 0.7% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, wherein the balance is deionized water;
combination 11:15% of hydrogen peroxide, 0.005% of reduced glutathione, 0.25% of cysteine, 2.5% of hydrogen fluoride, 2.5% of tetramethylammonium hydroxide, 1.0% of ethylenediamine tetraacetic acid, 0.5% of benzotriazole, 1.0% of triammonium citrate, 0.05% of EO-PO polymer L31, 0.7% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, and the balance is made up by deionized water.
The fluorine-containing cleaning liquid composition comprises the following components in percentage by mass: 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 L31, the above-mentioned 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and the above-mentioned water.
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 L31, the above-mentioned 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and the above-mentioned water all include the kind and content of the component. The components of the invention can adopt a split charging mode, and can be mixed temporarily when in use; it is preferable that the above-mentioned oxidizing agent is separately packaged as component A, the components other than the above-mentioned oxidizing agent are mixed and packaged as component B, and AB is mixed at the time of use.
The invention also provides a kit comprising one or more containers containing a component from which the components forming the fluorine-containing cleaning fluid composition are mixed, separate components or components that separate the components into groups;
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 L31, the 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and the water.
Preferably, the oxidizing agent is separately placed in one of the vessels.
The invention also provides a preparation method of the fluorine-containing cleaning liquid composition, which comprises the following steps of mixing the components to obtain the fluorine-containing cleaning liquid composition.
Preferably, the mixing mode is to add the solid component in the components into the liquid component and stir the mixture evenly.
Wherein the temperature of the mixing may be room temperature.
The invention also provides application of the fluorine-containing cleaning solution composition in cleaning one or more of post-plasma etching residues, post-ashing residues and hard mask materials on microelectronic devices.
The microelectronic device is preferably a silicon wafer.
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 immerse the microelectronic device in the fluorine-containing cleaning solution composition. The dipping time can be 5-30min. The temperature of the impregnation may be 45-60 ℃.
The above preferred conditions can be arbitrarily combined to obtain preferred embodiments of the present invention without departing from the common general knowledge in the art.
The 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) is prepared by self-made according to example 2 in patent CN 106188103B; other reagents and starting materials are commercially available, with EO-PO polymer L81, EO-PO polymer L42, EO-PO polymer L62, and EO-PO polymer L31 all being purchased from Nantong Koilai chemical Co.
The positive progress effects of the invention are as follows: the fluorine-containing cleaning solution composition has the advantages of highly selectively removing TiN, taN, tiNxOy, ti hard mask and Ti alloy hard mask, and has good cleaning effect on residues after plasma etching and ashing.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. Experimental procedures without specifying specific conditions in the following examples were selected in accordance with conventional procedures and conditions, or in accordance with commercial instructions.
In the following examples, the specific operation temperature is not limited, and all the operations are carried out at room temperature. The room temperature means 10-30 ℃.
The fluorine-containing cleaning liquid composition comprises the following components: the kinds and contents of the oxidant, reduced glutathione, cysteine, fluoride, organic base, chelating agent, corrosion inhibitor, ammonium carboxylate, EO-PO polymer L31, 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole), and deionized water are listed in tables 1 and 2, respectively.
According to the components and contents in the tables 1 and 2, the fluorine-containing cleaning liquid composition of the invention is prepared by adding the solid component into the liquid component and uniformly stirring.
TABLE 1
Figure BDA0003042041110000091
Figure BDA0003042041110000101
TABLE 2
Figure BDA0003042041110000102
Figure BDA0003042041110000111
The fluorine-containing cleaning liquid compositions of comparative examples 1 to 15 were obtained by adding the solid component to the liquid component in the following composition and content and stirring them uniformly.
Comparative examples 1 to 15 below are screens of the kinds or contents of components based on example 1.
Comparative example 1
The component reduced glutathione in example 1 was replaced by oxidized glutathione, and the others were not changed.
Comparative example 2
The component reduced glutathione in example 1 was removed, and the others were unchanged.
Comparative example 3
The cysteine component of example 1 was removed and the others were unchanged.
Comparative example 4
The cysteine component in example 1 was replaced with arginine, and the others were not changed.
Comparative example 5
The cysteine component in example 1 was replaced by histidine, and the others were unchanged.
Comparative example 6
The EO-PO polymer L31 of example 1 was removed and the rest was unchanged.
Comparative example 7
The component 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) in example 1 was removed, and the others were unchanged.
Comparative example 8
The ammonium carboxylate component of example 1 was removed and the rest was unchanged.
Comparative example 9
The EO-PO polymer L31 was replaced by the EO-PO polymer L42 in addition to the component in example 1, but otherwise was not changed.
Comparative example 10
The EO-PO polymer L31 was replaced with the EO-PO polymer L62 in example 1, but the other components were not changed.
Comparative example 11
The EO-PO polymer L31 of example 1, a component, was replaced by the EO-PO polymer L81, and the rest was unchanged.
Comparative example 12
The corrosion inhibitor of the composition in example 1 was removed, and the others were 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 in example 1 was replaced with 0.40%, and the others were unchanged.
Comparative example 16
The EO-PO polymer L31 content in example 1 was replaced by 0.0005%, the rest being unchanged.
Comparative example 17
The content of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) in example 1 was changed to 0.0005%, and the rest was unchanged.
Comparative example 18
The EO-PO polymer L31 content in example 1 was replaced by 1.1%, the other being unchanged.
Comparative example 19
The content of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) in example 1 was replaced with 2.1%, and the others were unchanged.
Effects of the embodiment
1. Etch rate
Figure BDA0003042041110000131
TABLE 3
Figure BDA0003042041110000132
Figure BDA0003042041110000141
TABLE 4
Figure BDA0003042041110000142
Figure BDA0003042041110000151
Remarking: "TiN" in the table is PVD (Physical Vapor Deposition) TiN.
In Table 3, the fluorine-containing cleaning liquid composition of the present invention has extremely low etching rates of less than all of AlNxOy, aluminum nitride, W, copper, TEOS, BD2, siCN and cobalt on a silicon wafer
Figure BDA0003042041110000152
Hardly corroding interconnection materials on the device; fluorine-containing cleaning fluid compositions not within the scope of the present application etch such materials at rates up to about the maximum rate
Figure BDA0003042041110000153
In Table 4, the fluorine-containing cleaning liquid composition of the present invention has extremely high etching rates of Ti, tiN, taN and TiNxOy on silicon wafers, which are all higher than those of Ti, tiN, taN and TiNxOy
Figure BDA0003042041110000154
The hard mask can be removed quickly; the fluorine-containing cleaning liquid composition which is not in the scope of the application has extremely low etching rate and highest etching rate on the materials
Figure BDA0003042041110000155
At the lowest, only
Figure BDA0003042041110000156
With reference to tables 3 and 4, the fluorine-containing cleaning solution composition of the present invention has a high etching selectivity to Ti, tiN, taN and TiNxOy on a silicon wafer, and the selectivity of TiN/Cu is at least 242 or more, compared with the interconnect material on the device in table 3, for example, tiN/Cu.
2. Cleaning effect
Figure BDA0003042041110000161
The cleaning effect is divided into four grades: a-no residue was observed; b-very little residue was observed; C-A small residue was observed; d-significantly more residue was observed.
The corrosion effect is classified into four grades: a-compatibility is good, and no undercut is formed; b-there is very slight undercut; c-there is a small amount of undercutting; d-undercut is more pronounced and severe.
TABLE 5
Figure BDA0003042041110000162
Figure BDA0003042041110000171
Therefore, the fluorine-containing cleaning solution composition has good cleaning effect on patterned wafers of residues after plasma etching and ashing and good compatibility with metal wires.

Claims (2)

1. A fluorine-containing cleaning liquid composition comprises the following components in parts by mass: 15% of hydrogen peroxide, 0.005% of reduced glutathione, 0.25% of cysteine, 2.5% of hydrogen fluoride, 2.5% of tetramethylammonium hydroxide, 1.0% of ethylenediamine tetraacetic acid, 0.5% of benzotriazole, 1.0% of ammonium oxalate, 0.05% of EO-PO polymer L31, 0.7% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, and the balance is made up by deionized water.
2. A kit comprising one or more containers containing a component that forms a mixture of components comprising the fluorine containing cleaning solution composition of claim 1, separate components, or a plurality of components that separate components into groups;
the components comprise 15% of hydrogen peroxide, 0.005% of reduced glutathione, 0.25% of cysteine, 2.5% of hydrogen fluoride, 2.5% of tetramethylammonium hydroxide, 1.0% of ethylenediamine tetraacetic acid, 0.5% of benzotriazole, 1.0% of ammonium oxalate, 0.05% of EO-PO polymer L31, 0.7% of 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) and deionized water, and the balance is made up by deionized water.
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