CN112859554B - Preparation method of vanadium oxide corrosion inhibition fluorine-containing stripping liquid - Google Patents

Preparation method of vanadium oxide corrosion inhibition fluorine-containing stripping liquid Download PDF

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CN112859554B
CN112859554B CN202110156148.4A CN202110156148A CN112859554B CN 112859554 B CN112859554 B CN 112859554B CN 202110156148 A CN202110156148 A CN 202110156148A CN 112859554 B CN112859554 B CN 112859554B
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organic solvent
mass fraction
ether
fluoride
acid
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CN112859554A (en
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王溯
冯强强
蒋闯
刘超勇
赖鑫
翟俊杰
邢乃观
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Shanghai Xinyang Semiconductor Material Co Ltd
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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26—Processing photosensitive materials; Apparatus therefor
    • G03F7/42—Stripping or agents therefor
    • G03F7/422—Stripping or agents therefor using liquids only
    • G03F7/425—Stripping or agents therefor using liquids only containing mineral alkaline compounds; containing organic basic compounds, e.g. quaternary ammonium compounds; containing heterocyclic basic compounds containing nitrogen
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26—Processing photosensitive materials; Apparatus therefor
    • G03F7/42—Stripping or agents therefor
    • G03F7/422—Stripping or agents therefor using liquids only
    • G03F7/426—Stripping or agents therefor using liquids only containing organic halogen compounds; containing organic sulfonic acids or salts thereof; containing sulfoxides

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  • General Physics & Mathematics (AREA)
  • Detergent Compositions (AREA)
  • Cleaning Or Drying Semiconductors (AREA)

Abstract

The invention discloses a vanadium oxide corrosion inhibition fluorine-containing stripping solution, a preparation method and application thereof. The preparation method of the vanadium oxide corrosion inhibition fluorine-containing stripping liquid comprises the steps of mixing raw materials, wherein the raw materials comprise the following components: fluoride, alkanolamine, corrosion inhibitor, complexing agent, linear amide organic solvent, sulfone and/or sulfoxide organic solvent, alcohol ether organic solvent, alkanone organic solvent, PO-EO-vinyl diamine copolymer and the balance of water, wherein the PO-EO-vinyl diamine copolymer is one or more of Tetronic 901, tetronic 904 and Tetronic908. The vanadium oxide corrosion inhibition fluorine-containing stripping liquid can effectively remove materials to be stripped, and has low corrosiveness to photoresist materials such as VOX/PI/Ni and the like.

Description

Preparation method of vanadium oxide corrosion inhibition fluorine-containing stripping liquid
Technical Field
The invention relates to a vanadium oxide corrosion inhibition fluorine-containing stripping solution, a preparation method and application thereof.
Background
In the field of infrared sensing chips, chip fabrication mainly relies on MEMS technology. At present, the technology is advanced and foresight, the domestic technology is not behind the foreign technology, and the technology is almost synchronously developed. Because of the newer technology, the development of materials and equipment related to the chip preparation also needs to be synchronously followed, and no mature foreign technology can learn.
In the MEMS process, a photoresist stripping liquid is required to strip and clean the chip. Photoresists involved in MEMS processing include G-line/I-line, DUV photoresists, and the like. Therefore, when stripping and cleaning a photoresist using a photoresist stripper, it is necessary to protect the photoresist material, such as VOX/PI/Ni, in particular, with a strict protection (i.e., low corrosiveness to the photoresist material) in addition to effectively removing photoresist residues, which is a higher requirement for the photoresist stripper.
There is therefore a need in the art to develop a stripping solution that is effective in removing photoresist residues and that is less corrosive to photoresist materials (e.g., VOX/PI/Ni materials).
Disclosure of Invention
The invention provides a vanadium oxide corrosion inhibition fluorine-containing stripping solution, a preparation method and application thereof. The vanadium oxide corrosion inhibition fluorine-containing stripping liquid can effectively remove materials to be stripped, and has low corrosiveness to photoresist materials, such as VOX/PI/Ni and the like.
The invention mainly solves the technical problems by the following technical means.
The invention provides a vanadium oxide corrosion inhibition fluorine-containing stripping solution, which comprises the following raw materials in percentage by mass:
0.05% -15% of fluoride, 18% -40% of alkanolamine, 0.5% -5% of corrosion inhibitor, 0.5% -5% of complexing agent, 10% -20% of linear amide organic solvent, 5% -15% of sulfone and/or sulfoxide organic solvent, 5% -10% of alcohol ether organic solvent, 5% -10% of alkanone organic solvent, 0.05% -1.5% of PO-EO-vinyl diamine copolymer and the balance of water, wherein the sum of the mass fractions of the components is 100%, and the PO-EO-vinyl diamine copolymer is one or more of Tetronic 901, tetronic 904 and Tetronic908.
In some embodiments, the mass fraction of fluoride may be 2.0% -10.00%. In some preferred embodiments, the mass fraction of fluoride may be 2.0% -6.0%. In some more preferred embodiments, the mass fraction of fluoride may be 5.3%.
In particular, in some embodiments, the mass fraction of fluoride may be 0.05%, 2.0%, 5.3%, 6.0%, 9.0%, 10.0%, 13.0%, or 15%.
In some embodiments, the alkanolamine may be 18.0% to 35.0% by mass. In some preferred embodiments, the alkanolamine may be 20.0% to 29.0% by mass. In some more preferred embodiments, the alkanolamine may be 25.4% by mass.
Specifically, in some embodiments, the alkanolamine may be 18%, 20.0%, 25.0%, 25.4%, 29.0%, 30.0%, 35.0%, or 40% by mass.
In some embodiments, the corrosion inhibitor may be 1.2% -4.3% by mass. In some preferred embodiments, the corrosion inhibitor may be 1.8% -3.5% by mass. In some more preferred embodiments, the corrosion inhibitor may be 2.2% by mass.
Specifically, in some embodiments, the corrosion inhibitor may be 0.50%, 1.20%, 1.80%, 2.00%, 2.20%, 3.50%, 4.30%, or 5.00% by mass.
In some embodiments, the complexing agent may be present in an amount of 0.80% to 4.5% by mass. In some preferred embodiments, the complexing agent may be present in a mass fraction of 1.10% to 3.6%. In some more preferred embodiments, the complexing agent may be present at a mass fraction of 1.50%.
In particular, in some embodiments, the complexing agent may be 0.50%, 0.80%, 1.10%, 1.30%, 1.50%, 3.60%, 4.50%, or 5.00% by mass.
In some embodiments, the linear amide-based organic solvent may be 13% -18% by mass. In some preferred embodiments, the linear amide-based organic solvent may be 15% -18% by mass. In some more preferred embodiments, the linear amide-based organic solvent may have a mass fraction of 17.8%.
Specifically, in some embodiments, the linear amide-based organic solvent may be 10%, 13%, 15%, 16%, 17.8%, 18%, or 20% by mass.
In some embodiments, the mass fraction of the sulfone-based and/or sulfoxide-based organic solvent may be 6.70% -15%. In some preferred embodiments, the mass fraction of the sulfone-based and/or sulfoxide-based organic solvent may be 7.50% -12.4%. In some more preferred embodiments, the mass fraction of the sulfone-based and/or sulfoxide-based organic solvent may be 12.4%.
In particular, in some embodiments, the mass fraction of the sulfone-and/or sulfoxide-based organic solvent may be 5.0%, 6.70%, 7.50%, 10%, 12.4%, or 15%.
In some embodiments, the mass fraction of the alcohol ether organic solvent may be 6.70% -9.6%. In some preferred embodiments, the mass fraction of the alcohol ether organic solvent may be 7.50% -8.2%. In some more preferred embodiments, the mass fraction of the alcohol ether organic solvent may be 7.8%.
In particular, in some embodiments, the mass fraction of the alcohol ether organic solvent may be 5%, 6.70%, 7.50%, 7.8%, 8.2%, 9.6%, or 10%.
In some embodiments, the mass fraction of the alkanone organic solvent may be 6.70% -10%. In some preferred embodiments, the mass fraction of the alkanone organic solvent may be 7.50% -9.1%. In some more preferred embodiments, the mass fraction of the alkanone organic solvent may be 9.1%.
In particular, in some embodiments, the mass fraction of the alkanone organic solvent may be 5%, 6.70%, 7.50%, 8.20%, 9.1%, or 10%.
In some embodiments, the PO-EO-vinyl diamine copolymer can be from 0.56% to 1.5%. In some preferred embodiments, the PO-EO-vinyl diamine copolymer can be from 0.73% to 1.2%. In some more preferred embodiments, the PO-EO-vinyl diamine copolymer may be 1.2%.
Specifically, in some embodiments, the PO-EO-vinyl diamine copolymer may be 0.05%, 0.10%, 0.56%, 0.73%, 1.08%, 1.2%, or 1.50%.
Wherein the fluoride can be selected from one or more of hydrogen fluoride and salts formed by hydrogen fluoride and alkali; preferably one or more of ammonium bifluoride, ammonium fluoride, hydrogen fluoride, tetramethyl ammonium fluoride, tetraethyl ammonium fluoride, tetrapropyl ammonium fluoride, tetrabutyl ammonium fluoride, benzyl trimethyl ammonium fluoride and choline fluoride; more preferably one or more of ammonium bifluoride, ammonium fluoride, hydrogen fluoride, tetramethylammonium fluoride, tetraethylammonium fluoride, tetrapropylammonium fluoride, benzyltrimethylammonium fluoride and choline fluoride; further preferred is ammonium fluoride.
The alkanolamine may be a conventional alkanolamine in the art; preferably aminoethylethanolamine, dimethylaminoethanol, monoethanolamine, N-methylethanolamine, N-ethylethanolamine, N-propylethanolamine, N-butylethanolamine, diethanolamine, triethanolamine, N-methyldiethanolamine, N-ethyldiethanolamine, isopropanolamine, diisopropanolamine, triisopropanolamine, N-methylisopropanolamine, N-propylisopropanolamine, 2-aminopropane-1-ol, N-methyl-2-aminopropane-1-ol, N-ethyl-2-aminopropane-1-ol, 1-aminopropane-3-ol, N-methyl-1-aminopropane-3-ol, N-ethyl-1-aminopropane-3-ol, 1-aminobutan-2-ol, N-methyl-1-aminobutan-2-ol, N-ethyl-1-aminobutan-2-ol, 2-aminobutan-1-ol, N-methyl-2-aminobutan-1-ol, N-ethyl-2-aminobutan-1-ol, 3-methylbutan-1-ol, N-methyl-3-aminopropane-1-ol, N-methyl-1-aminobutan-1-ol, N-ethyl-1-aminobutan-4-1-aminobutan-1-ol, one or more of N-methyl-1-aminobutan-4-ol, N-ethyl-1-aminobutan-4-ol, 1-amino-2-methylpropan-2-ol, 2-amino-2-methylpropan-1-ol, 1-aminopentan-4-ol, 2-amino-4-methylpentan-1-ol, 2-aminohexane-1-ol, 3-aminoheptane-4-ol, 1-aminooctane-2-ol, 5-aminooctane-4-ol, 1-aminopropane-2, 3-diol, 2-aminopropane-1, 3-diol, tris (hydroxymethyl) aminomethane, 1, 2-diaminopropane-3-ol, 1, 3-diaminopropane-2-ol and 2- (2-aminoethoxy) ethanol; more preferably one or more of monoethanolamine, diethanolamine, triethanolamine, isopropanolamine, N-methyldiethanolamine, 1-aminobutan-2-ol, N-ethylisopropanolamine, 1-aminooctan-2-ol and tris (hydroxymethyl) aminomethane; further preferred is monoethanolamine.
When the alkanolamine is plural, the plural is preferably two, for example, N-ethylisopropanolamine and tris (hydroxymethyl) aminomethane. When two alkanolamines are mentioned, the mass ratio of the two can be 0.5-2.0, for example, 1:1. For example, the mass ratio of N-ethylisopropanolamine to tris (hydroxymethyl) aminomethane may be 0.5-2.0, e.g., 1:1.
The corrosion inhibitor may be a conventional corrosion inhibitor in the art, preferably one or more of 1-thioglycerol, 2-mercaptopropionic acid, benzotriazole, catechol, gallic acid and pyrogallol, more preferably 1-thioglycerol.
When the corrosion inhibitor is plural, the plural is preferably two, for example, gallic acid and pyrogallol. When two corrosion inhibitors are used, the mass ratio of the two corrosion inhibitors can be 0.5-2.0, for example, 1:1. For example, the mass ratio of gallic acid to pyrogallol may be 0.5-2.0, e.g., 1:1.
The complexing agent can be one or more of glycolic acid, malonic acid, citric acid, iminodiacetic acid, nitrilotriacetic acid, ethylenediamine tetraacetic acid, salicylic acid, pentamethyldiethylenetriamine, sulfamic acid and sulfosalicylic acid; preferably one or more of glycolic acid, malonic acid, citric acid, iminodiacetic acid, pentamethyldiethylenetriamine, sulfamic acid and sulfosalicylic acid; more preferably ethanolamine.
When the corrosion inhibitor is plural, the plural is preferably two, for example, malonic acid and citric acid. When two corrosion inhibitors are used, the mass ratio of the two corrosion inhibitors can be 0.5-2.0, for example, 1:1. For example, the mass ratio of malonic acid to citric acid can be 0.5-2.0, e.g., 1:1.
The linear amide organic solvent may be a conventional linear amide organic solvent in the art, preferably one or more of N-methylformamide, N-ethylformamide, N-dimethylformamide, N-diethylformamide, acetamide, N-methylacetamide, N-dimethylacetamide, N- (2-hydroxyethyl) acetamide, N-dimethylpropionamide, 3-methoxy-N, N-dimethylpropionamide, 3- (2-ethylhexyl oxy) -N, N-dimethylpropionamide and 3-butoxy-N, N-dimethylpropionamide; more preferably one or more of N-methylformamide, N-ethylformamide, N-diethylformamide, N-methylacetamide, 3- (2-ethylhexyl oxy) -N, N-dimethylpropionamide and 3-butoxy-N, N-dimethylpropionamide; n-methylformamide is further preferred.
When the linear amide-based organic solvent is plural, the plural is preferably three, for example, a mixed solvent of N-methylformamide, N-methylacetamide and 3-butoxy-N, N-dimethylpropionamide. When the number of the linear amide organic solvents is three, the mass ratio of the two organic solvents is (0.5-2.0): (0.5-2.0), e.g., 1:1.
The sulfone organic solvent can be a conventional sulfone organic solvent in the field; preferably one or more of methylsulfonic acid, sulfolane and dipropyl sulfone, more preferably sulfolane. The sulfoxide organic solvent can be a conventional sulfoxide organic solvent in the field, and is preferably one or more of dimethyl sulfoxide and methyl ethyl sulfoxide, diphenyl sulfoxide, thionyl chloride and benzyl sulfoxide.
When the sulfone-based organic solvent and the sulfoxide-based organic solvent are mixed, the mass ratio of the sulfone-based organic solvent to the sulfoxide-based organic solvent may be 0.5 to 2.0, for example, 1:1.
The alcohol ether organic solvent can be a conventional alcohol ether organic solvent in the field; preferably one or more of ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monoisopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monoisopropyl ether, diethylene glycol monobutyl ether, triethylene glycol monomethyl ether, triethylene glycol monoethyl ether, triethylene glycol monoisopropyl ether, triethylene glycol monobutyl ether, polyethylene glycol, polypropylene glycol, polyethylene glycol monomethyl ether, polyethylene glycol monobutyl ether, propylene glycol monomethyl ether, dipropylene glycol monomethyl ether, tripropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, dipropylene glycol monopropyl ether and dipropylene glycol monobutyl ether; more preferably one or more of ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monoisopropyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, propylene glycol monomethyl ether, tripropylene glycol monomethyl ether and dipropylene glycol monobutyl ether; more preferred is ethylene glycol monomethyl ether.
When the alcohol ether type organic solvent is plural, the plural is preferably two, for example, ethylene glycol monomethyl ether and dipropylene glycol monobutyl ether. When the alcohol ether type organic solvent is two, the mass ratio of the two can be 0.5-2.0, for example, 1:1. For example, the mass ratio of ethylene glycol monomethyl ether to dipropylene glycol monobutyl ether may be 0.5-2.0, e.g., 1:1.
The alkanone organic solvent may be a conventional alkanone organic solvent in the art; preferred are imidazolidinone and/or pyrrolidone type organic solvents, and more preferred are imidazolidinone type organic solvents. The imidazolidinone organic solvent is preferably 2-imidazolidinone and/or 1, 3-dimethyl-2-imidazolidinone, more preferably 2-imidazolidinone. The pyrrolidone type organic solvent is preferably one or more of N-ethyl pyrrolidone, N-methyl pyrrolidone and N-cyclohexyl pyrrolidone.
When the alkanone organic solvent is a mixture of an imidazolidinone and a pyrrolidone organic solvent, the mass ratio of the imidazolidinone organic solvent to the pyrrolidone organic solvent may be 0.5 to 2.0, for example, 1:1. For example, the mass ratio of 2-imidazolidinone to N-ethyl pyrrolidone may be 0.5-2.0, e.g., 1:1.
The PO-EO-vinyl diamine copolymer is preferably Tetronic908.
In some preferred embodiments of the present invention, the raw material components of the vanadium oxide corrosion inhibition fluorine-containing stripping solution comprise the fluoride, the alkanolamine, the corrosion inhibitor, the complexing agent, the linear amide organic solvent, the sulfone and/or sulfoxide organic solvent, the alcohol ether organic solvent, the alkanone organic solvent, the PO-EO-vinyl diamine copolymer and the balance of water, wherein the sum of the mass percentages of the components is 100%.
The invention also provides a preparation method of the vanadium oxide corrosion inhibition fluorine-containing stripping liquid, which comprises the following steps: mixing the raw materials. The mixing is preferably carried out by adding the solid component in the raw material components into the liquid component and stirring uniformly. The temperature of the mixing is room temperature. The mixing is preferably followed by a shaking and filtering operation. The purpose of the shaking is to thoroughly mix the raw material components, and the shaking speed and time are not limited. Filtration is to remove insoluble materials.
The invention also provides application of the vanadium oxide corrosion inhibition fluorine-containing stripping liquid in stripping and cleaning of materials to be stripped in semiconductor devices. The semiconductor device is preferably one or more of a logic chip, a memory chip, a microelectromechanical chip (i.e., MEMS chip), an optoelectronic chip, and a power chip (e.g., IGBT, etc.). The material to be peeled is preferably: positive photoresist, photoresist residue, hardened cross-linked photoresist, and polymers. The photoresist residue can be the self-residue of the photoresist after dry etching and/or dry photoresist stripping. The hardened and crosslinked photoresist can be the reaction product of the photoresist and plasma or oxygen and other gases after dry etching and/or dry photoresist stripping. The polymer can be the reaction product of light and a dielectric layer, a metal layer and the like on a wafer under the action of plasma in the dry etching and/or dry photoresist removing process. The material to be peeled can be specifically: positive photoresist RZJ-5701 from su state reddish company; AZ MIR 701 from AZ corporation. The application preferably comprises the steps of: and (3) contacting the material to be stripped with stripping liquid. The contacting is preferably by impregnation.
The temperature of the contacting is preferably 55-85 ℃, more preferably 60-75 ℃.
The contact time is preferably 10 to 65min, more preferably 30 to 60min.
In the present invention, room temperature is 10-30 ℃.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred examples of the invention.
The reagents and materials used in the present invention are commercially available, wherein the PO-EO-vinyl diamine copolymer selected from Tetronic908, tetronic 904, tetronic 901 is derived from Shanghai Taijin International trade company.
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 and comparative examples, the preparation method of the vanadium oxide corrosion inhibition fluorine-containing stripping solution comprises the following steps: mixing the corresponding raw materials.
In the following examples, the specific operating temperatures are not limited, and all refer to being conducted under room temperature conditions.
1. Preparation method example of vanadium oxide corrosion inhibition fluorine-containing stripping solution
The raw material components of table 1 were uniformly mixed according to the mass fractions in table 2. Wherein, the mixing is generally to add the solid component in the raw material components into the liquid component and stir the mixture uniformly. The mixing is generally carried out by adding the solid component in the raw material components into the liquid component and stirring uniformly. The temperature of the mixing is room temperature. The mixing is typically followed by a shaking and filtering operation. The purpose of the shaking is to thoroughly mix the raw material components, and the shaking speed and time are not limited. Filtration is to remove insoluble materials.
Table 1 kinds of components in examples
Table 2 mass fraction (%)
Wherein, the comparative example 1 is to examine the mass fraction boundary value of fluoride;
comparative example 2 is to examine the mass fraction boundary value of alkanolamine;
comparative example 3 is to examine the mass fraction boundary value of the PO-EO-vinyl diamine copolymer;
comparative examples 4 to 19 are for examining the kind of PO-EO-vinyl diamine copolymer.
2. Effect examples
1. Sheet metal corrosion test
Titanium (Ti) sheet, aluminum sheet (Al sheet) and nickel sheet deposited with a certain thickness are immersed in a stripping solution (60 ℃ for 30 minutes) to be subjected to corrosion treatment, and then rinsed with pure water. The corrosion rate was calculated by measuring the change in resistivity before and after corrosion using a four-point probe instrument.
2. Dielectric layer corrosion test
The silicon oxide wafer, the silicon nitride wafer, the vanadium oxide wafer and the polyimide wafer deposited with certain thickness are soaked in stripping liquid (60 ℃ for 30 minutes), subjected to corrosion treatment, and then rinsed with pure water. The thickness of the dielectric layer before and after etching was measured by a film thickness meter.
3. Photoresist residue cleaning effect test
The display master wafer containing the material to be peeled was immersed in a cleaning liquid (60 ℃ C., 30 minutes), subjected to a peeling treatment, and then subjected to a rinsing treatment with pure water. Then SEM observation and evaluation are carried out, and the A grade is that the cleaning rate reaches 100 percent; the class B is to wash 50% -99.9%; grade C is 20% -49.9% of cleaning; grade D is a rinse off of only 19.9% or less.
4. Test of cleaning effect of hardened crosslinked photoresist
The display master wafer containing the material to be peeled was immersed in a cleaning liquid (60 ℃ C., 30 minutes), subjected to a peeling treatment, and then subjected to a rinsing treatment with pure water. Then SEM observation and evaluation are carried out, and the A grade is that the cleaning rate reaches 100 percent; the class B is to wash 50% -99.9%; grade C is 20% -49.9% of cleaning; grade D is a rinse off of only 19.9% or less
5. Polymer cleaning effect test
The display master wafer containing the material to be peeled was immersed in a cleaning liquid (60 ℃ C., 30 minutes), subjected to a peeling treatment, and then subjected to a rinsing treatment with pure water. Then SEM observation and evaluation are carried out, and the A grade is that the cleaning rate reaches 100 percent; the class B is to wash 50% -99.9%; grade C is 20% -49.9% of cleaning; grade D is a rinse off of only 19.9% or less.
TABLE 3 Effect example results
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According to the embodiment 1 and the comparative example 1, the vanadium oxide corrosion inhibition fluorine-containing stripping liquid provided by the invention uses 0.05% -15% of fluoride in mass fraction, so that the cleaning effect can be effectively improved, and the VOX and PI corrosion rates can be effectively reduced.
According to the embodiment 1 and the comparative example 2, the vanadium oxide corrosion inhibition fluorine-containing stripping liquid provided by the invention can effectively reduce Al, ti, VOX, PI, ni, siO and SiN corrosion rates by using 18-40% of alkanolamine by mass.
According to the embodiment 1 and the comparative example 3, the vanadium oxide corrosion inhibition fluorine-containing stripping liquid provided by the invention uses 0.05% -1.5% of PO-EO-vinyl diamine copolymer by mass fraction, so that the cleaning effect can be effectively improved, and the corrosion rates of Al, ti, PI, ni, siO and SiN can be effectively reduced.
According to the embodiment 1 and the comparative examples 4-19, it can be found that the vanadium oxide corrosion inhibition fluorine-containing stripping liquid provided by the invention adopts one or more of Tetronic 901, tetronic 904 and Tetronic908 as the PO-EO-vinyl diamine copolymer, so that the cleaning effect can be effectively improved, or the corrosion rates of Al, ti, VOX, PI, ni, siO and SiN can be effectively reduced.
In summary, according to Table 3, the vanadium oxide corrosion inhibition fluorine-containing stripping solution provided by the invention has low corrosiveness to various materials and has a strong removal effect on photoresist residues, hardened and crosslinked photoresist and polymers compared with the stripping solutions in comparative examples 1 to 19.

Claims (10)

1. The preparation method of the vanadium oxide corrosion inhibition fluorine-containing stripping liquid is characterized in that the raw materials of the vanadium oxide corrosion inhibition fluorine-containing stripping liquid are mixed, wherein the raw materials comprise the following components in percentage by mass: 0.05% -15% of fluoride, 18% -40% of alkanolamine, 0.5% -5% of corrosion inhibitor, 0.5% -5% of complexing agent, 10% -20% of linear amide organic solvent, 5% -15% of sulfone and/or sulfoxide organic solvent, 5% -10% of alcohol ether organic solvent, 5% -10% of alkanone organic solvent, 0.05% -1.5% of PO-EO-vinyl diamine copolymer and the balance of water, wherein the sum of the mass fractions of the components is 100%, and the PO-EO-vinyl diamine copolymer is one or more of Tetronic 901, tetronic 904 and Tetronic908.
2. The method of claim 1, wherein,
the mass fraction of the fluoride is 2.0% -10.00%;
and/or, the mass fraction of the complexing agent is 0.80% -4.5%;
and/or, the alkanolamine has a mass fraction of 18.0% to 35.0%;
and/or, the PO-EO-vinyl diamine copolymer is 0.56% -1.5%;
and/or, the mass fraction of the corrosion inhibitor is 1.2% -4.3%;
and/or, the mass fraction of the linear amide organic solvent is 13% -18%;
and/or, the mass fraction of the sulfone and/or sulfoxide organic solvent is 6.70% -15%;
and/or the mass fraction of the alcohol ether organic solvent is 6.70% -9.6%;
and/or the mass fraction of the alkane organic solvent is 6.70% -10%.
3. The method of claim 2, wherein,
the mass fraction of the fluoride is 2.0% -6.0%;
and/or the mass fraction of the complexing agent is 1.10% -3.6%;
and/or, the alkanolamine has a mass fraction of 20.0% to 29.0%;
and/or, the PO-EO-vinyl diamine copolymer is 0.73% -1.2%;
and/or, the mass fraction of the corrosion inhibitor is 1.8% -3.5%;
and/or, the mass fraction of the linear amide organic solvent is 15% -18%;
and/or, the mass fraction of the sulfone and/or sulfoxide organic solvent is 7.50% -12.4%;
and/or the mass fraction of the alcohol ether organic solvent is 7.50% -8.2%;
and/or, the mass fraction of the alkane organic solvent is 7.50% -9.1%.
4. The method according to claim 3, wherein,
the mass fraction of the fluoride is 5.3%;
and/or, the mass fraction of the complexing agent is 1.50%;
and/or, the alkanolamine is 25.4% by mass;
and/or, the PO-EO-vinyl diamine copolymer is 1.2%;
and/or, the mass fraction of the corrosion inhibitor is 2.2%;
and/or, the mass fraction of the linear amide type organic solvent is 17.8%;
and/or, the mass fraction of the sulfone and/or sulfoxide organic solvent is 12.4%;
and/or the mass fraction of the alcohol ether organic solvent is 7.8%;
and/or, the mass fraction of the alkanone organic solvent is 9.1%.
5. The method of claim 1, wherein,
the fluoride is selected from one or more of hydrogen fluoride and salts formed by the hydrogen fluoride and alkali;
and/or the alkanolamine is aminoethylethanolamine, dimethylaminoethanol, monoethanolamine, N-methylethanolamine, N-ethylethanolamine, N-propylethanolamine, N-butylethanolamine, diethanolamine, triethanolamine, N-methyldiethanolamine, N-ethyldiethanolamine, isopropanolamine, diisopropanolamine, triisopropanolamine, N-methylisopropanolamine, N-ethylisopropanolamine, N-propylisopropanolamine, 2-aminopropane-1-ol, N-methyl-2-aminopropane-1-ol, N-ethyl-2-aminopropane-1-ol, 1-aminopropane-3-ol, N-methyl-1-aminopropane-3-ol, N-ethyl-1-aminopropane-3-ol, 1-aminobutan-2-ol, N-methyl-1-aminobutan-2-ol, N-ethyl-1-aminobutan-2-ol, 2-aminobutan-1-ol, N-methyl-2-aminobutan-1-ol, N-ethyl-2-aminobutan-1-ol, 3-aminobutan-1-ol, N-methyl-1-aminobutan-3-1-ol, N-methyl-1-aminobutan-3-aminobutan-1-ol, one or more of N-methyl-1-aminobutan-4-ol, N-ethyl-1-aminobutan-4-ol, 1-amino-2-methylpropan-2-ol, 2-amino-2-methylpropan-1-ol, 1-aminopentan-4-ol, 2-amino-4-methylpentan-1-ol, 2-aminohexane-1-ol, 3-aminoheptane-4-ol, 1-aminooctane-2-ol, 5-aminooctane-4-ol, 1-aminopropane-2, 3-diol, 2-aminopropane-1, 3-diol, tris (hydroxymethyl) aminomethane, 1, 2-diaminopropane-3-ol, 1, 3-diaminopropane-2-ol and 2- (2-aminoethoxy) ethanol;
and/or the corrosion inhibitor is one or more of 1-thioglycerol, 2-mercaptopropionic acid, benzotriazole, catechol, gallic acid and pyrogallol;
and/or the complexing agent is one or more of glycolic acid, malonic acid, citric acid, iminodiacetic acid, nitrilotriacetic acid, ethylenediamine tetraacetic acid, salicylic acid, pentamethyldiethylenetriamine, sulfamic acid and sulfosalicylic acid;
and/or the linear amide organic solvent is one or more of N-methylformamide, N-ethylformamide, N-dimethylformamide, N-diethylformamide, acetamide, N-methylacetamide, N-dimethylacetamide, N- (2-hydroxyethyl) acetamide, N-dimethylpropionamide, 3-methoxy-N, N-dimethylpropionamide, 3- (2-ethylhexyl oxy) -N, N-dimethylpropionamide and 3-butoxy-N, N-dimethylpropionamide;
and/or the sulfone organic solvent is one or more of methyl sulfone, sulfolane and dipropyl sulfone;
and/or the sulfoxide organic solvent is one or more of dimethyl sulfoxide, methyl ethyl sulfoxide, diphenyl sulfoxide, thionyl chloride and benzyl sulfoxide;
and/or the alcohol ether organic solvent is one or more of ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monoisopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monoisopropyl ether, diethylene glycol monobutyl ether, triethylene glycol monomethyl ether, triethylene glycol monoethyl ether, triethylene glycol monoisopropyl ether, triethylene glycol monobutyl ether, polyethylene glycol, polypropylene glycol, polyethylene glycol monomethyl ether, polyethylene glycol monobutyl ether, propylene glycol monomethyl ether, dipropylene glycol monomethyl ether, tripropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, dipropylene glycol monopropyl ether and dipropylene glycol monobutyl ether;
and/or the alkanone organic solvent is an imidazolidinone and/or pyrrolidone organic solvent.
6. The method according to claim 5, wherein,
the fluoride is one or more of ammonium bifluoride, ammonium fluoride, hydrogen fluoride, tetramethyl ammonium fluoride, tetraethyl ammonium fluoride, tetrapropyl ammonium fluoride, benzyl trimethyl ammonium fluoride and choline fluoride;
and/or the alkanolamine is one or more of monoethanolamine, diethanolamine, triethanolamine, isopropanolamine, N-methyldiethanolamine, 1-aminobutan-2-ol, N-ethylisopropanolamine, 1-aminooctane-2-ol and tris (hydroxymethyl) aminomethane;
and/or the complexing agent is one or more of glycolic acid, malonic acid, citric acid, iminodiacetic acid, pentamethyldiethylenetriamine, sulfamic acid and sulfosalicylic acid;
and/or the linear amide organic solvent is one or more of N-methyl formamide, N-ethyl formamide, N-diethyl formamide, N-methyl acetamide, 3- (2-ethylhexyl oxy) -N, N-dimethyl propionamide and 3-butoxy-N, N-dimethyl propionamide;
and/or the alcohol ether organic solvent is one or more of ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monoisopropyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, propylene glycol monomethyl ether, tripropylene glycol monomethyl ether and dipropylene glycol monobutyl ether;
and/or the imidazolidinone organic solvent is 2-imidazolidinone and/or 1, 3-dimethyl-2-imidazolidinone;
and/or the pyrrolidone organic solvent is one or more of N-ethyl pyrrolidone, N-methyl pyrrolidone and N-cyclohexyl pyrrolidone.
7. The method according to claim 6, wherein,
the fluoride is ammonium fluoride;
and/or, the alkanolamine is monoethanolamine;
and/or, the corrosion inhibitor is 1-thioglycerol;
and/or the complexing agent is ethanolamine;
and/or the linear amide organic solvent is N-methyl formamide;
and/or, the sulfone and/or sulfoxide organic solvent is sulfolane;
and/or the alcohol ether organic solvent is ethylene glycol monomethyl ether;
and/or, the alkanone organic solvent is 2-imidazolidone;
and/or, the PO-EO-vinyl diamine copolymer is Tetronic908.
8. The process according to any one of claim 1 to 7,
the mixing is to add the solid component in the raw materials into the liquid component and stir the mixture uniformly.
9. The method of any one of claims 1-7, wherein the temperature of the mixing is room temperature.
10. The method of any one of claims 1-7, wherein the mixing is followed by shaking and filtering.
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CN104024394A (en) * 2012-11-21 2014-09-03 戴纳洛伊有限责任公司 Process And Composition For Removing Substances From Substrates
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