CN113430060A - Tungsten compatible cleaning solution for removing hard mask, preparation method and application thereof - Google Patents

Tungsten compatible cleaning solution for removing hard mask, preparation method and application thereof Download PDF

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CN113430060A
CN113430060A CN202010208618.2A CN202010208618A CN113430060A CN 113430060 A CN113430060 A CN 113430060A CN 202010208618 A CN202010208618 A CN 202010208618A CN 113430060 A CN113430060 A CN 113430060A
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ammonium
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CN113430060B (en
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王溯
蒋闯
徐锦波
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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
    • C11D3/02—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
    • C11D3/33—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
    • C11D3/3947—Liquid compositions
    • 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
    • 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
    • H01L21/02082—Cleaning product to be cleaned
    • 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 tungsten compatible cleaning solution for removing a hard mask, and a preparation method and application thereof. The invention provides a cleaning solution which is prepared from the following raw materials in parts by mass: 0.5-20% of oxidant, 0.01-30% of oxidant stabilizer, 0.1-20% of fluoride, 0.1-20% of organic alkali, 0.001-10% of chelating agent, 0.001-10% of corrosion inhibitor, 0.01-15% of ammonium carboxylate, 0.001-1.5% of surfactant, 0.001-2.5% of passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials; wherein the surfactant is EO-PO polymer L42. The cleaning solution can selectively remove the hard mask and other residues, has strong compatibility to tungsten and various metals and dielectrics, and has good cleaning effect.

Description

Tungsten compatible cleaning solution for removing hard mask, preparation method and application thereof
Technical Field
The invention relates to a tungsten compatible cleaning solution for removing a hard mask, and a preparation method and application thereof.
Background
In the chip manufacturing technology, the cleaning solution for residues after copper interconnection plasma etching is mainly fluorine-containing cleaning solution. 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 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., 28-14nm), 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) needs to be removed after etching protection, and other metal and dielectric materials need to be protected during the cleaning process for removing the hardmask material, thereby challenging compatibility of conventional fluorine-containing cleaning solutions 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 provides a tungsten compatible cleaning solution for removing a hard mask, a preparation method and application thereof, aiming at overcoming the defects of poor compatibility and corrosion inhibition performance of the existing cleaning solution for removing a hard mask material on other metals and dielectric materials, poor cleaning effect and the like. The cleaning liquid of the present invention mayFor selectively removing hardmask and other residues from Integrated Circuit (IC) wet process cleaning processes, and in particular for selectively removing TiN, TaN, TiN from such chips or wafers comprising low-k dielectric materials, TEOS, copper, cobalt, and other low-k dielectric materialsxOyCompositions and methods of Ti hardmask and hardmask including alloys of the above, and other residues. Moreover, the cleaning solution has strong compatibility to tungsten, various metals and dielectrics and good cleaning effect.
The present invention solves the above technical problems by the following technical solutions.
The invention provides a cleaning solution which is prepared from the following raw materials in parts by mass: 0.5-20% of oxidant, 0.01-30% of oxidant stabilizer, 0.1-20% of fluoride, 0.1-20% of organic alkali, 0.001-10% of chelating agent, 0.001-10% of corrosion inhibitor, 0.01-15% of ammonium carboxylate, 0.001-1.5% of surfactant, 0.001-2.5% of passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials;
wherein the surfactant is EO-PO polymer L42.
In the cleaning solution, the oxidizing agent may be an oxidizing agent conventionally used in the art, 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 chlorous acid [ (N (CH))3)4)ClO2]Tetramethylammonium chlorate [ (N (CH))3)4)ClO3]Tetramethylammonium iodate[(N(CH3)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]、[(CO(NH2)2)H2O2]And peroxyacetic acid [ CH3(C＝O)OOH]More preferably hydrogen peroxide and/or peracetic acid.
In the cleaning solution, the mass fraction of the oxidizing agent may be 0.5% to 10%, preferably 1% to 5% (e.g., 1%, 2.5%, 5%), and the mass fraction is the percentage of the mass of the oxidizing agent in the total mass of the raw materials.
In the cleaning solution, the oxidant stabilizer may be an oxidant stabilizer conventionally used in the art, preferably one or more of N-methylmorpholine oxide (NMMO or NMO), pyrimidine N-oxide, pyridine N-oxide, pyridazine N-oxide, quinoline N-oxide and trimethylamine N-oxide, more preferably one or more of N-methylmorpholine oxide, pyridine N-oxide and trimethylamine N-oxide.
In the cleaning solution, the mass fraction of the oxidant stabilizer may be 0.5% to 20%, preferably 1% to 10% (e.g., 1%, 5%, 10%), and the mass fraction is the mass percentage of the oxidant stabilizer in the total mass of the raw materials.
In the cleaning liquid, the fluoride may be a fluoride conventionally used 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, and more preferably hydrogen fluoride and/or fluoroboric acid.
In the cleaning solution, the mass fraction of the fluoride may be 0.5% to 10%, preferably 1% to 5% (e.g., 1%, 2.5%, 5%), and the mass fraction is the percentage of the mass of the fluoride in the total mass of the raw materials.
In the cleaning solution, the organic base may be an organic base conventionally used in the art, preferably one or more of tetramethylammonium hydroxide (TMAH), 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) and tetramethylguanidine, and more preferably tetramethylammonium hydroxide and/or choline.
In the cleaning solution, the mass fraction of the organic base may be 0.5% to 10%, preferably 1% to 5% (e.g., 1%, 2.5%, 5%), and the mass fraction is the percentage of the mass of the organic base in the total mass of the raw materials.
In the cleaning solution, the chelating agent may be one or more chelating agents conventionally used 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 ', N ' -tetraacetic acid, N- {2- [ bis (carboxymethyl) amino ] ethyl } -N- (2-hydroxyethyl) glycine (HEDTA), ethylenediamine-N, N ' -bis (2-hydroxyphenylacetic acid) (EDDHA), dioxaoctamethylenediazepinetetraacetic acid (DOCTA) and triethylenetetraminehexaacetic acid (TTHA), more preferably ethylenediaminetetraacetic acid and/or 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid.
In the cleaning solution, the mass fraction of the chelating agent can be 0.005% -5%, preferably 0.01% -2% (e.g. 0.01%, 1%, 2%), and the mass fraction is the percentage of the mass of the chelating agent in the total mass of the raw materials.
In the cleaning solution, the corrosion inhibitor may be a corrosion inhibitor conventionally used in the art, 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, benzotriazole derivatives thereof, and the like, 5-benzenethiol-benzotriazole, halo-benzotriazole (halogen ═ F, Cl, Br or I), naphthotriazole, 2-Mercaptobenzimidazole (MBI), 2-mercaptobenzothiazole, 4-methyl-2-phenylimidazole, 2-mercaptothiazoline, 5-aminotetrazole monohydrate, 5-amino-1, 3, 4-thiadiazole-2-thiol, 2, 4-diamino-6-methyl-1, 3, 5-triazine, thiazole, triazine, methyltetrazole, 1, 3-dimethyl-2-imidazolidinone, 1, 5-pentamethylenetetrazole, 1-phenyl-5-mercaptotetrazole, diaminomethyltriazine, imidazolidinethione, mercaptobenzimidazole, thiobenzole, thiole, and the like, 4-methyl-4H-1, 2, 4-triazole-3-thiol, 5-amino-1, 3, 4-thiadiazole-2-thiol and benzothiazole, more preferably benzotriazole and/or tolyltriazole.
In the cleaning solution, the mass fraction of the corrosion inhibitor may be 0.005% to 5%, preferably 0.01% to 2% (e.g., 0.01%, 0.5%, 2%), and the mass fraction is the mass percentage of the corrosion inhibitor in the total mass of the raw materials.
In the cleaning solution, the ammonium carboxylate may be ammonium carboxylate conventionally used in the art, 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 cleaning solution, the mass fraction of the ammonium carboxylate may be 0.1% to 5%, preferably 0.5% to 3% (e.g., 0.5%, 1%, 3%), and the mass fraction is a percentage of the mass of the ammonium carboxylate to the total mass of the raw materials.
In the cleaning solution, the mass fraction of the surfactant can be 0.01% -1.5%, preferably 0.01% -1% (e.g. 0.01%, 0.05%, 1%), and the mass fraction is the percentage of the mass of the surfactant in the total mass of the raw materials.
In the cleaning solution, the passivating agent can be a passivating agent conventionally used in the field, and preferably 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole). The preparation method of the 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) is conventional in the field, and is referred to patent application CN 106188103A.
In the cleaning solution, the mass fraction of the passivating agent can be 0.01% -2.5%, preferably 0.01% -2% (e.g. 0.01%, 0.7%, 1%, 1.5%, 2%), and the mass fraction is the percentage of the mass of the passivating agent in the total mass of the raw materials.
In the cleaning liquid, the water is preferably one or more of deionized water, pure water and ultrapure water, and is more preferably deionized water.
In certain preferred embodiments of the present invention, the cleaning solution is prepared from the following raw materials, wherein the raw materials comprise the following components in parts by mass: 0.5-10% of an oxidizing agent, 0.5-20% of an oxidizing agent stabilizer, 0.5-10% of fluoride, 0.5-10% of organic alkali, 0.005-5% of a chelating agent, 0.005-5% of a corrosion inhibitor, 0.1-5% of ammonium carboxylate, 0.01-1.5% of a surfactant, 0.01-2.5% of a passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials.
In certain preferred embodiments of the present invention, the cleaning solution is prepared from the following raw materials, wherein the raw materials comprise the following components in parts by mass: 1-5% of oxidant, 1-10% of oxidant stabilizer, 1-5% of fluoride, 1-5% of organic alkali, 0.01-2% of chelating agent, 0.01-2% of corrosion inhibitor, 0.5-3% of ammonium carboxylate, 0.01-1% of surfactant, 0.01-2% of passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials.
In certain preferred embodiments of the present invention, the cleaning solution is prepared from the following raw materials, wherein the raw materials comprise the following components in parts by mass: 0.5-20% of oxidant, 0.01-30% of oxidant stabilizer, 0.1-20% of fluoride, 0.1-20% of organic alkali, 0.001-10% of chelating agent, 0.001-10% of corrosion inhibitor, 0.01-15% of ammonium carboxylate, 0.001-1.5% of surfactant, 0.001-2.5% of passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials.
In certain preferred embodiments of the present invention, the cleaning solution is prepared from the following raw materials, wherein the raw materials comprise the following components in parts by mass: 0.5-10% of an oxidizing agent, 0.5-20% of an oxidizing agent stabilizer, 0.5-10% of fluoride, 0.5-10% of organic alkali, 0.005-5% of a chelating agent, 0.005-5% of a corrosion inhibitor, 0.1-5% of ammonium carboxylate, 0.01-1.5% of a surfactant, 0.01-2.5% of a passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials.
In certain preferred embodiments of the present invention, the cleaning solution is prepared from the following raw materials, wherein the raw materials comprise the following components in parts by mass: 1-5% of oxidant, 1-10% of oxidant stabilizer, 1-5% of fluoride, 1-5% of organic alkali, 0.01-2% of chelating agent, 0.01-2% of corrosion inhibitor, 0.5-3% of ammonium carboxylate, 0.01-1% of surfactant, 0.01-2% of passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials.
The invention also provides a preparation method of the cleaning solution, which comprises the following steps: and mixing the raw materials to obtain the cleaning solution.
Wherein, the solid component in the raw material components is preferably added into the liquid component and stirred uniformly.
Wherein the temperature of the mixing may be room temperature.
The invention also provides application of the cleaning solution in cleaning a semiconductor device with a hard mask and/or after plasma etching.
Wherein, the material of the hard mask can be titanium-containing or tantalum-containing material; the titanium-containing material can be one or more of titanium, titanium nitride and titanium oxynitride; the tantalum-containing material may be tantalum nitride.
The substrate for plasma etching can be a copper interconnection substrate.
Wherein the temperature of the washing may be room temperature, preferably 35 ℃ to 50 ℃ (e.g., 40 ℃). The washing time may be 5min to 30min (e.g., 20 min).
In the present invention, "room temperature" means 10 to 40 ℃ unless otherwise specified.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows: the cleaning solutions of the present invention are useful for selectively removing hard masks and other residues from Integrated Circuit (IC) wet process cleaning processes, and in particular for selectively removing TiN, TaN, TiN, from such chips or wafers comprising low-k dielectric materials, TEOS, copper, cobalt, and other low-k dielectric materialsxOyCompositions and methods of Ti hardmask and hardmask including alloys of the above, and other residues. Moreover, the cleaning solution has strong compatibility to tungsten, various metals and dielectrics and good cleaning effect.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Abbreviations referred to in the examples are as follows:
TMAH: tetramethyl ammonium hydroxide; a BTA: benzotriazole; NMO: n-methylmorpholine oxide; CDTA: 1, 2-cyclohexanediamine-N, N' -tetraacetic acid;
AlNxOy: aluminum oxynitride; AlN: aluminum nitride; w: tungsten; cu: copper; LP-TEOS: low pressure deposition of ethyl orthosilicate; co: cobalt; BD 2: low-k dielectric materials commonly used in the art, under the trade name BLACK DIAMOND; SiCN: silicon carbon nitrogen; ti: titanium; TiN: titanium nitride, according to the inventionTiN is PVD TiN, wherein PVD refers to (Physical Vapor Deposition); TaN-tantalum nitride; TiN (titanium nitride)xOy-titanium oxynitride.
1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole) was prepared according to CN106188103A and shown by D in the following Table.
The EO-PO products in the examples were obtained from Nantong Koilai chemical Co.
Examples 1 to 13
The cleaning solution comprises the following raw material components: the kinds and contents of the oxidizing agent, the oxidizing agent stabilizer, the fluoride, the organic base, the chelating agent, the corrosion inhibitor, the ammonium carboxylate, the surfactant, and the passivating agent are listed in tables 1 and 2; the water in the cleaning solution is deionized water, and the balance is made up by the deionized water.
In the following examples, the cleaning solution was prepared by adding the solid components of the raw material components in the examples to the liquid components and stirring them uniformly.
In the following examples, the specific operation temperature is not limited, and all the operations are carried out at room temperature.
TABLE 1 kinds of raw material components of cleaning solution
Figure BDA0002422041730000081
Figure BDA0002422041730000091
TABLE 2 mass fractions of the respective raw material components of the cleaning liquid
Figure BDA0002422041730000092
Figure BDA0002422041730000101
Application examples 1 to 13
(1) Etch Rate determination
Etching rate of a sample to be detected: dummy wafers of a single material, such as aluminum, copper, titanium nitride, tungsten, cobalt, dielectric materials (low-k or high-k), etc., are deposited on a silicon wafer.
Etching experiment: statically dipping a sample to be detected in a cleaning solution for 30min at 40 ℃, cleaning by using deionized water and drying by using nitrogen.
Method for measuring etch rate (A/min): the thickness of the sample before and after etching was measured, respectively, with a metal sample being measured for thickness using a four-point probe apparatus (createst-e of Napson, japan) and a non-metal sample being measured for thickness using an optical film thickness measuring apparatus (filmmetrics F20, usa).
The corrosion effect is classified into four grades: good A-compatibility without undercutting; b-there is very slight undercut; c-there is little undercut; d-undercut is more pronounced and severe.
(2) Measurement of cleaning Effect
Cleaning effect to detect samples: patterned wafers with post plasma etch and post ash residues with pattern features (metal lines, vias via, metal pads pad, trench, etc.).
The cleaning effect experiment method comprises the following steps: the sample is statically immersed in a cleaning solution for 20min at 40 ℃, and then cleaned by deionized water and dried by nitrogen. The cleaning and corrosion effects were observed by electron microscope SEM.
The cleaning effect is divided into four grades: a-no residue was observed; b-very little residue was observed; C-Small residue observed; d-significantly more residue was observed.
The etching rate (A/min), etching effect and cleaning effect of the cleaning liquids of examples 1 to 13 are shown in Table 3.
Figure BDA0002422041730000111
As can be seen from Table 3, the cleaning solution of the present invention was applied to AlNxOyAlN, W, Cu, LP-TEOS, Co, BD2, SiCN and the like have lower etching rates, which shows that the corrosion inhibition performance of the materials is better;for Ti, TiN, TaN, TiNxOyThe high etch rate indicates that it is effective in removing such materials as the hard mask. And after the cleaning solution of the invention is used for cleaning the patterned wafer with the through hole characteristic and the patterned wafer with the metal wire characteristic, almost no undercut phenomenon is observed, which shows that the cleaning solution has good compatibility to various metals and dielectrics.
In addition, after the patterned wafer with the through hole characteristic and the patterned wafer with the metal wire characteristic are cleaned by the cleaning solution of the invention, almost no residue is observed, which shows that the cleaning effect is good.
Comparative examples 1 to 11
The preparation process is as in examples 1 to 13.
TABLE 4 kinds of raw material components of cleaning solution
Figure BDA0002422041730000121
Figure BDA0002422041730000131
TABLE 5 mass fractions of respective raw material components of the cleaning liquids
Figure BDA0002422041730000132
The cleaning liquids of comparative examples 1 to 11 were subjected to the etching rate (A/min), the etching effect and the cleaning effect in the same manner as in application examples 1 to 13, and the results are shown in Table 6.
Figure BDA0002422041730000141
As can be seen from Table 6, the cleaning solutions of comparative examples 1 to 11 were applied to AlN as compared with those of examples 1 to 13xOyThe etching rate of AlN, W, Cu, LP-TEOS, Co, BD2, SiCN and the like is obviously increased, and the corrosion inhibition performance is poor. For Ti、TiN、TaN、TiNxOyThe reduced etch rate of (a) indicates that it is less effective in removing such materials as hard masks.
Also, after the patterned wafers having the via hole features and the patterned wafers having the metal line features were cleaned with the cleaning solutions of comparative examples 1 to 11, a severe undercut phenomenon occurred with more residues.

Claims (10)

1. The cleaning solution is characterized by being prepared from the following raw materials in parts by mass: 0.5-20% of oxidant, 0.01-30% of oxidant stabilizer, 0.1-20% of fluoride, 0.1-20% of organic alkali, 0.001-10% of chelating agent, 0.001-10% of corrosion inhibitor, 0.01-15% of ammonium carboxylate, 0.001-1.5% of surfactant, 0.001-2.5% of passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials;
wherein the surfactant is EO-PO polymer L42.
2. The cleaning solution according to claim 1,
the mass fraction of the oxidant is 0.5-10%, and the mass fraction is the mass percentage of the oxidant in the total mass of the raw materials;
and/or the mass fraction of the oxidant stabilizer is 0.5-20%, and the mass fraction is the percentage of the mass of the oxidant stabilizer in the total mass of the raw materials;
and/or the mass fraction of the fluoride is 0.5-10%, and the mass fraction is the percentage of the mass of the fluoride in the total mass of the raw materials;
and/or the mass fraction of the organic alkali is 0.5-10%, and the mass fraction is the percentage of the mass of the organic alkali in the total mass of the raw materials;
and/or the mass fraction of the chelating agent is 0.005-5%, and the mass fraction is the percentage of the mass of the chelating agent in the total mass of the raw materials;
and/or the mass fraction of the corrosion inhibitor is 0.005-5%, and the mass fraction is the percentage of the mass of the corrosion inhibitor in the total mass of the raw materials;
and/or the mass fraction of the ammonium carboxylate is 0.1-5%, and the mass fraction is the percentage of the mass of the ammonium carboxylate in the total mass of the raw materials;
and/or the mass fraction of the surfactant is 0.01-1.5%, and the mass fraction is the percentage of the mass of the surfactant in the total mass of the raw materials;
and/or the mass fraction of the passivating agent is 0.01-2.5%, and the mass fraction is the mass percentage of the passivating agent in the total mass of the raw materials.
3. The cleaning solution according to claim 2,
the mass fraction of the oxidant is 1% -5%, and the mass fraction is the mass percentage of the oxidant in the total mass of the raw materials;
and/or the mass fraction of the oxidant stabilizer is 1-10%, and the mass fraction is the percentage of the mass of the oxidant stabilizer in the total mass of the raw materials;
and/or the mass fraction of the fluoride is 1-5%, and the mass fraction is the percentage of the mass of the fluoride in the total mass of the raw materials;
and/or the mass fraction of the organic alkali is 1-5%, and the mass fraction is the percentage of the mass of the organic alkali in the total mass of the raw materials;
and/or the mass fraction of the chelating agent is 0.01-2%, and the mass fraction is the percentage of the mass of the chelating agent in the total mass of the raw materials;
and/or the mass fraction of the corrosion inhibitor is 0.01-2%, and the mass fraction is the mass percentage of the corrosion inhibitor in the total mass of the raw materials;
and/or the mass fraction of the ammonium carboxylate is 0.5-3%, and the mass fraction is the percentage of the mass of the ammonium carboxylate in the total mass of the raw materials;
and/or the mass fraction of the surfactant is 0.01-1%, and the mass fraction is the percentage of the mass of the surfactant in the total mass of the raw materials;
and/or the mass fraction of the passivating agent is 0.01-2%, and the mass fraction is the percentage of the mass of the passivating agent in the total mass of the raw materials.
4. The cleaning solution according to claim 1,
the oxidizing agent is hydrogen peroxide, benzoyl peroxide, tetrabutylammonium peroxymonosulfate, ozone, ferric chloride, permanganate, perborate, perchlorate, persulfate, ammonium peroxydisulfate, peracetic acid, urea peroxide, nitric acid, ammonium chlorite, ammonium chlorate, ammonium iodate, ammonium perborate, ammonium perchlorate, ammonium periodate, ammonium persulfate, tetramethylammonium chlorite, tetramethylammonium chlorate, tetramethylammonium iodate, tetramethylammonium perborate, tetramethylammonium perchlorate, tetramethylammonium periodate, tetramethylammonium persulfate, [ (CO (NH)2)2)H2O2]And peroxyacetic acid;
and/or the oxidant stabilizer is one or more of N-methylmorpholine oxide, pyrimidine N-oxide, pyridine N-oxide, pyridazine N-oxide, quinoline N-oxide and trimethylamine N-oxide;
and/or the fluoride is 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/or the organic base is one or more of tetramethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, tetraethylammonium hydroxide, benzyltrimethylammonium hydroxide, choline, (2-hydroxyethyl) trimethylammonium hydroxide, tris (2-hydroxyethyl) methylammonium hydroxide, monoethanolamine, diglycolamine, triethanolamine, isobutanolamine, isopropanolamine, tetrabutylphosphonium hydroxide and tetramethylguanidine;
and/or the chelating agent is one or more of 1, 2-cyclohexanediamine-N, N, N ', N ' -tetraacetic acid, ethylenediaminetetraacetic acid, nitrilotriacetic acid, diethylenetriaminepentaacetic acid, 1,4,7, 10-tetraazacyclododecane-1, 4,7, 10-tetraacetic acid, ethyleneglycol tetraacetic acid, 1, 2-bis (o-aminophenoxy) ethane-N, N, N ', N ' -tetraacetic acid, N- {2- [ bis (carboxymethyl) amino ] ethyl } -N- (2-hydroxyethyl) glycine, ethylenediamine-N, N ' -bis (2-hydroxyphenylacetic acid), dioxaoctamethylenediazepine tetraacetic acid, and triethylenetetramine hexaacetic acid;
and/or the corrosion inhibitor is benzotriazole, 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-benzenethiol-benzotriazole, halo-benzotriazole, or a salt thereof, Naphthotriazole, 2-mercaptobenzimidazole, 2-mercaptobenzothiazole, 4-methyl-2-phenylimidazole, 2-mercaptothiazoline, 5-aminotetrazole monohydrate, 5-amino-1, 3, 4-thiadiazole-2-thiol, 2, 4-diamino-6-methyl-1, 3, 5-triazine, thiazole, triazine, methyltetrazole, 1, 3-dimethyl-2-imidazolidinone, 1, 5-pentamethylenetetrazole, 1-phenyl-5-mercaptotetrazole, diaminomethyltriazine, imidazolidinethione, mercaptobenzimidazole, 4-methyl-4H-1, 2, 4-triazole-3-thiol, thiohydrabamine, thiobenzoguanamine, thioamine, thiobenzoguanamine, 2-methyl-4H-1, 2, 4-triazole-3-thiol, thioamine, thio, One or more of 5-amino-1, 3, 4-thiadiazole-2-thiol and benzothiazole;
and/or the ammonium carboxylate is one or more of ammonium oxalate, ammonium lactate, ammonium tartrate, triammonium citrate, ammonium acetate, ammonium carbamate, ammonium carbonate, ammonium benzoate, ammonium ethylenediaminetetraacetic acid, diammonium ethylenediaminetetraacetic acid, triammonium ethylenediaminetetraacetic acid, tetraammonium ethylenediaminetetraacetic acid, ammonium succinate, ammonium formate and 1-H-pyrazole-3-ammonium formate;
and/or the passivating agent is 1- (benzotriazole-1-methyl) -1- (2-methylbenzimidazole);
and/or the water is one or more of deionized water, pure water and ultrapure water.
5. The cleaning solution according to claim 4,
the oxidant is hydrogen peroxide and/or peroxyacetic acid;
and/or the oxidant stabilizer is one or more of N-methylmorpholine oxide, pyridine N-oxide and trimethylamine N-oxide;
and/or the fluoride is hydrogen fluoride and/or fluoroboric acid;
and/or the organic base is tetramethyl ammonium hydroxide and/or choline;
and/or the chelating agent is ethylenediamine tetraacetic acid and/or 1, 2-cyclohexanediamine-N, N, N ', N' -tetraacetic acid;
and/or the corrosion inhibitor is benzotriazole and/or tolyltriazole;
and/or the ammonium carboxylate is ammonium oxalate and/or triammonium citrate;
and/or the water is deionized water.
6. The cleaning solution according to any one of claims 1 to 5, wherein the cleaning solution is any one of the following solutions,
scheme 1:
the raw materials comprise the following components in percentage by mass: 0.5-10% of an oxidizing agent, 0.5-20% of an oxidizing agent stabilizer, 0.5-10% of fluoride, 0.5-10% of organic alkali, 0.005-5% of a chelating agent, 0.005-5% of a corrosion inhibitor, 0.1-5% of ammonium carboxylate, 0.01-1.5% of a surfactant, 0.01-2.5% of a passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials;
scheme 2:
the cleaning solution is prepared from the following raw materials in parts by mass: 1-5% of an oxidant, 1-10% of an oxidant stabilizer, 1-5% of fluoride, 1-5% of organic alkali, 0.01-2% of a chelating agent, 0.01-2% of a corrosion inhibitor, 0.5-3% of ammonium carboxylate, 0.01-1% of a surfactant, 0.01-2% of a passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials;
scheme 3:
the cleaning solution is prepared from the following raw materials in parts by mass: 0.5-20% of oxidant, 0.01-30% of oxidant stabilizer, 0.1-20% of fluoride, 0.1-20% of organic alkali, 0.001-10% of chelating agent, 0.001-10% of corrosion inhibitor, 0.01-15% of ammonium carboxylate, 0.001-1.5% of surfactant, 0.001-2.5% of passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials;
scheme 4:
the cleaning solution is prepared from the following raw materials in parts by mass: 0.5-10% of an oxidizing agent, 0.5-20% of an oxidizing agent stabilizer, 0.5-10% of fluoride, 0.5-10% of organic alkali, 0.005-5% of a chelating agent, 0.005-5% of a corrosion inhibitor, 0.1-5% of ammonium carboxylate, 0.01-1.5% of a surfactant, 0.01-2.5% of a passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials;
scheme 5:
the cleaning solution is prepared from the following raw materials in parts by mass: 1-5% of oxidant, 1-10% of oxidant stabilizer, 1-5% of fluoride, 1-5% of organic alkali, 0.01-2% of chelating agent, 0.01-2% of corrosion inhibitor, 0.5-3% of ammonium carboxylate, 0.01-1% of surfactant, 0.01-2% of passivating agent and the balance of water, wherein the mass fraction is the percentage of the mass of each component in the total mass of the raw materials.
7. A method for preparing a cleaning fluid according to any one of claims 1 to 6, comprising the steps of: and mixing the raw materials to obtain the cleaning solution.
8. A method for producing the cleaning liquid according to claim 7,
the mixing is to add the solid component in the raw material components into the liquid component and stir the mixture evenly;
and/or the temperature of the mixing is room temperature.
9. Use of a cleaning solution according to any one of claims 1 to 6 for cleaning a semiconductor device having a hard mask and/or after plasma etching.
10. Use of an cleaning solution according to claim 9 for cleaning a semiconductor device having a hard mask and/or a plasma etched,
the material of the hard mask is titanium-containing or tantalum-containing material; the titanium-containing material can be one or more of titanium, titanium nitride and titanium oxynitride; the tantalum-containing material can be tantalum nitride;
and/or the plasma etching substrate is a copper interconnection substrate;
and/or the temperature of the cleaning is room temperature, preferably 35-50 ℃;
and/or the cleaning time is 5min-30 min.
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