CN112859554A - Vanadium oxide corrosion-inhibition fluorine-containing stripping liquid, preparation method and application thereof - Google Patents

Vanadium oxide corrosion-inhibition fluorine-containing stripping liquid, preparation method and application thereof Download PDF

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CN112859554A
CN112859554A CN202110156148.4A CN202110156148A CN112859554A CN 112859554 A CN112859554 A CN 112859554A CN 202110156148 A CN202110156148 A CN 202110156148A CN 112859554 A CN112859554 A CN 112859554A
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organic solvent
mass fraction
ether
fluoride
aminobutan
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CN112859554B (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

Abstract

The invention discloses a vanadium oxide corrosion-inhibition fluorine-containing stripping liquid, and a preparation method and application thereof. The preparation method of the vanadium oxide corrosion-inhibition fluorine-containing stripping solution comprises the following steps of mixing raw materials, wherein the raw materials comprise the following components: fluoride, alkanolamine, corrosion inhibitor, complexing agent, linear-chain 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 Tetronic 908. The vanadium oxide corrosion-inhibition fluorine-containing stripping solution can effectively remove the material to be stripped, and has low corrosion to photoresist materials such as VOX/PI/Ni and the like.

Description

Vanadium oxide corrosion-inhibition fluorine-containing stripping liquid, preparation method and application thereof
Technical Field
The invention relates to a vanadium oxide corrosion-inhibition fluorine-containing stripping liquid, a preparation method and application thereof.
Background
In the field of infrared sensing chips, chip preparation mainly depends on MEMS (micro-electromechanical systems) technology. At present, the process is advanced and defended, the domestic technology is not behind the foreign technology, and the process is almost synchronously developed. Due to the newer technology, the development of materials and equipment related to the chip preparation is also synchronously followed up, and no mature foreign technology can be learned.
In the MEMS process, a chip needs to be stripped and cleaned by using a photoresist stripping solution. Photoresists involved in MEMS processes include G-line/I-line and DUV photoresists, among others. Therefore, when a photoresist is stripped and cleaned by using a photoresist stripping solution, in addition to effective removal of photoresist residues, strict protection (i.e., low corrosion to the photoresist) is required particularly for materials such as VOX/PI/Ni in the photoresist, which puts higher demands on the photoresist cleaning solution.
Therefore, there is a need in the art to develop a stripper that can effectively remove photoresist residues and has low corrosion to photoresist materials (such as VOX/PI/Ni materials).
Disclosure of Invention
The invention provides a vanadium oxide corrosion-inhibition fluorine-containing stripping liquid, and a preparation method and application thereof. The vanadium oxide corrosion-inhibition fluorine-containing stripping solution can effectively remove materials to be stripped, and has low corrosivity on photoresist materials, such as VOX/PI/Ni materials and the like.
The present invention mainly solves the above problems with the following technical means.
The invention provides a vanadium oxide corrosion-inhibition fluorine-containing stripping liquid which comprises the following raw materials in parts 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 Tetronic 908.
In some embodiments, the mass fraction of fluoride may be 2.0% to 10.00%. In some preferred embodiments, the mass fraction of fluoride may be 2.0% to 6.0%. In some more preferred embodiments, the mass fraction of fluoride may be 5.3%.
Specifically, 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 mass fraction of the alkanolamine may be from 18.0% to 35.0. In some preferred embodiments, the mass fraction of the alkanolamine may be from 20.0% to 29.0%. In some more preferred embodiments, the mass fraction of alkanolamine may be 25.4%.
Specifically, in some embodiments, the mass fraction of the alkanolamine may be 18%, 20.0%, 25.0%, 25.4%, 29.0%, 30.0%, 35.0%, or 40%.
In some embodiments, the mass fraction of the corrosion inhibitor may be 1.2% to 4.3%. In some preferred embodiments, the mass fraction of the corrosion inhibitor may be 1.8% to 3.5%. In some more preferred embodiments, the mass fraction of the corrosion inhibitor may be 2.2%.
Specifically, in some embodiments, the mass fraction of the corrosion inhibitor may be 0.50%, 1.20%, 1.80%, 2.00%, 2.20%, 3.50%, 4.30%, or 5.00%.
In some embodiments, the mass fraction of the complexing agent may be 0.80% to 4.5%. In some preferred embodiments, the mass fraction of the complexing agent may be 1.10% to 3.6%. In some more preferred embodiments, the mass fraction of the complexing agent may be 1.50%.
Specifically, in some embodiments, the mass fraction of the complexing agent may be 0.50%, 0.80%, 1.10%, 1.30%, 1.50%, 3.60%, 4.50%, or 5.00%.
In some embodiments, the mass fraction of the linear amide organic solvent may be 13% to 18%. In some preferred embodiments, the mass fraction of the linear amide organic solvent may be 15% to 18%. In some more preferred embodiments, the mass fraction of the linear amide-based organic solvent may be 17.8%.
Specifically, in some embodiments, the mass fraction of the linear amide organic solvent may be 10%, 13%, 15%, 16%, 17.8%, 18%, or 20%.
In some embodiments, the mass fraction of the sulfones and/or sulfoxide organic solvent may be 6.70% to 15%. In some preferred embodiments, the mass fraction of the sulfones and/or sulfoxide organic solvent may be 7.50% to 12.4%. In some more preferred embodiments, the mass fraction of the sulfones and/or sulfoxide organic solvent may be 12.4%.
Specifically, in some embodiments, the mass fraction of the sulfones and/or sulfoxide 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% to 9.6%. In some preferred embodiments, the mass fraction of the alcohol ether organic solvent may be 7.50% to 8.2%. In some more preferred embodiments, the mass fraction of the alcohol ether-based organic solvent may be 7.8%.
Specifically, in some embodiments, the mass fraction of the alcohol ether-based 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-based organic solvent may be 6.70% to 10%. In some preferred embodiments, the mass fraction of the alkanone-based organic solvent may be 7.50% to 9.1%. In some more preferred embodiments, the mass fraction of the alkanone-based organic solvent may be 9.1%.
Specifically, in some embodiments, the mass fraction of the alkanone-based organic solvent may be 5%, 6.70%, 7.50%, 8.20%, 9.1%, or 10%.
In some embodiments, the PO-EO-vinyl diamine copolymer may be 0.56% to 1.5%. In some preferred embodiments, the PO-EO-vinyl diamine copolymer may be 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 one or more of hydrogen fluoride and salts formed by the hydrogen fluoride and alkali; preferably one or more of ammonium bifluoride, ammonium fluoride, hydrogen fluoride, tetramethylammonium fluoride, tetraethylammonium fluoride, tetrapropylammonium fluoride, tetrabutylammonium fluoride, benzyltrimethylammonium 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 conventional 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-ethylisopropanolamine, N-propylisopropanolamine, 2-aminopropan-1-ol, N-methyl-2-aminopropan-1-ol, N-ethyl-2-aminopropan-1-ol, 1-aminopropan-3-ol, N-methyl-2-aminopropan-1-ol, N-ethylethanolamine, N-propylethanolamine, N-butylethanolamine, diethanolamine, triethanolamine, N-, N-ethyl-1-aminopropan-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-3-aminobutan-1-ol, N-ethyl-3-aminobutan-1-ol, 1-aminobutan-4-ol, 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-methylpentane-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, methyl-1-aminopropane-2-ol, methyl-1-aminopropane-1, 3-diol, methyl-1-aminopropane-2-ol, methyl-1, One or more of 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 a plurality, the plurality is preferably two, for example, N-ethyl isopropanolamine and tris (hydroxymethyl) aminomethane. When the alkanolamine is two, the mass ratio of the two may be 0.5 to 2.0, for example, 1: 1. For example, the mass ratio of N-ethyl isopropanolamine to tris (hydroxymethyl) aminomethane can be 0.5 to 2.0, e.g., 1: 1.
The corrosion inhibitor can be a conventional corrosion inhibitor in the field, preferably one or more of 1-thioglycerol, 2-mercaptopropionic acid, benzotriazole, catechol, gallic acid and pyrogallol, and 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 can be 0.5 to 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, ethylene diamine 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 may be 0.5 to 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-ethylhexyloxy) -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-ethylhexyloxy) -N, N-dimethylpropionamide and 3-butoxy-N, N-dimethylpropionamide; further preferred is N-methylformamide.
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 can be (0.5-2.0) to (0.5-2.0): (0.5-2.0), for example, 1: 1.
The sulfone organic solvent can be a conventional sulfone organic solvent in the field; preferably one or more of methyl sulfone, 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, methyl ethyl sulfoxide, diphenyl sulfoxide, thionyl chloride and benzyl benzene sulfoxide.
When the sulfone organic solvent and the sulfoxide organic solvent are mixed, the mass ratio of the sulfone organic solvent to the sulfoxide organic solvent can be 0.5-2.0, 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 preferably ethylene glycol monomethyl ether.
When the alcohol ether organic solvent is plural, the plural is preferably two, for example, ethylene glycol monomethyl ether and dipropylene glycol monobutyl ether. When the alcohol ether 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 can be from 0.5 to 2.0, e.g., 1: 1.
The organic solvent of the alkanones can be the organic solvent of the alkanones which is conventional in the field; preferably, the organic solvent is an imidazolidinone and/or a pyrrolidinone, and more preferably, an imidazolidinone organic solvent. The organic solvent of the imidazolidinone type is preferably 2-imidazolidinone and/or 1, 3-dimethyl-2-imidazolidinone, and more preferably 2-imidazolidinone. The pyrrolidone organic solvent is preferably one or more of N-ethyl pyrrolidone, N-methyl pyrrolidone and N-cyclohexyl pyrrolidone.
When the organic solvent of the alkyl ketone is a mixture of an organic solvent of the imidazolidinone type and an organic solvent of the pyrrolidone type, the mass ratio of the organic solvent of the imidazolidinone type to the organic solvent of the pyrrolidone type may be 0.5 to 2.0, for example, 1: 1. For example, the mass ratio of 2-imidazolidinone to N-ethylpyrrolidone may be from 0.5 to 2.0, e.g., 1: 1.
The PO-EO-vinyl diamine copolymer is preferably Tetronic 908.
In some preferred embodiments of the present invention, the raw material components of the vanadium oxide corrosion-inhibition fluorine-containing stripping liquid 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, and the sum of the mass fractions 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: and mixing the raw materials. The mixing is preferably carried out by adding the solid components in the raw material components into the liquid components and uniformly stirring. The temperature of the mixing is room temperature. After the mixing, preferably, the method further comprises the operations of shaking and filtering. The purpose of shaking is to fully mix the raw material components, and the shaking speed and the shaking time are not limited. Filtration was performed to remove insoluble matter.
The invention also provides application of the vanadium oxide corrosion-inhibition fluorine-containing stripping liquid in stripping and cleaning of a material to be stripped in a semiconductor device. The semiconductor device is preferably one or more of a logic chip, a memory chip, a micro-electro-mechanical chip (i.e., a MEMS chip), an optoelectronic chip, and a power chip (e.g., an IGBT, etc.). The material to be peeled is preferably: one or more of positive tone photoresist, photoresist residue, hardened cross-linked photoresist, and polymer. The photoresist residue can be the residue of the photoresist after dry etching and/or dry photoresist stripping. The hardened crosslinking photoresistor can be a reaction product of the photoresistor and plasma or oxygen and other gases after dry etching and/or dry photoresist removing processes. The polymer can be a reaction product of light, a dielectric layer, a metal layer and the like on a wafer under the action of plasma in a dry etching and/or dry photoresist removing process. The material to be stripped can be specifically: positive photoresists RZJ-5701 from suzhou reihong corporation; AZ MIR 701 from AZ Corp. Said application preferably comprises the following steps: and (3) contacting the material to be stripped with stripping liquid. The contacting is preferably by a dipping method.
The temperature of the contact is preferably 55 to 85 deg.C, more preferably 60 to 75 deg.C.
The contact time is preferably 10 to 65min, more preferably 30 to 60 min.
The room temperature in the present invention means 10 to 30 ℃.
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, wherein the PO-EO-vinyl diamine copolymer selected from the group consisting of Tetronic908, Tetronic 904, Tetronic 901 is available from Shanghai Tai jin International trade company, Inc.
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.
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 operation temperature is not limited, and all the operations are carried out at room temperature.
Embodiment of preparation method of vanadium oxide corrosion-inhibition fluorine-containing stripping liquid
The raw material components of table 1 were mixed uniformly in 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 uniformly. The mixing is generally to add the solid components in the raw material components into the liquid components and stir the mixture evenly. The temperature of the mixing is room temperature. After the mixing, the operation of shaking and filtering is further included. The purpose of shaking is to fully mix the raw material components, and the shaking speed and the shaking time are not limited. Filtration was performed to remove insoluble matter.
Table 1 component kinds in examples
Figure BDA0002933556350000081
Figure BDA0002933556350000091
Figure BDA0002933556350000101
Figure BDA0002933556350000111
Table 2 mass fraction of each raw material component (%)
Figure BDA0002933556350000112
Figure BDA0002933556350000121
Figure BDA0002933556350000131
Wherein, comparative example 1 is to examine the mass fraction boundary value of the fluoride;
comparative example 2 was to investigate the mass fraction boundary value of the alkanolamine;
comparative example 3 was conducted to examine the mass fraction boundary value of the PO-EO-vinyl diamine copolymer;
comparative examples 4 to 19 are for the purpose of examining the kind of PO-EO-vinyl diamine copolymer.
Second, effect embodiment
1. Sheet metal corrosion testing
Titanium (Ti) sheets, aluminum sheets (Al sheets) and nickel sheets deposited with certain thicknesses are soaked in stripping liquid (60 ℃ for 30 minutes) for corrosion treatment, and then are rinsed by pure water. The change of the resistivity before and after the corrosion was measured by a four-point probe instrument to calculate the corrosion rate.
2. Dielectric layer corrosion testing
The silicon oxide wafer, the silicon nitride wafer, the vanadium oxide wafer and the polyimide wafer with certain thicknesses are soaked in stripping liquid (60 ℃ for 30 minutes) for corrosion treatment, and then are rinsed by pure water. And measuring the thickness change of the dielectric layer before and after corrosion by using a film thickness meter.
3. Photoresist residue cleaning effect test
The display main wafer containing this material to be peeled was immersed in a cleaning solution (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 grade A is that the cleaning rate reaches 100 percent; the B level is 50 to 99.9 percent of the cleaning; the grade C is 20 to 49.9 percent of the washing; grade D was only washed off 19.9% or less.
4. Cleaning effect test of hardened cross-linked photoresist
The display main wafer containing this material to be peeled was immersed in a cleaning solution (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 grade A is that the cleaning rate reaches 100 percent; the B level is 50 to 99.9 percent of the cleaning; the grade C is 20 to 49.9 percent of the washing; grade D is a grade of washing off only 19.9% or less
5. Polymer cleaning Effect test
The display main wafer containing this material to be peeled was immersed in a cleaning solution (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 grade A is that the cleaning rate reaches 100 percent; the B level is 50 to 99.9 percent of the cleaning; the grade C is 20 to 49.9 percent of the washing; grade D was only washed off 19.9% or less.
Table 3 effects of examples results
Figure BDA0002933556350000141
Figure BDA0002933556350000151
According to the embodiment 1 and the comparative example 1, the vanadium oxide corrosion-inhibition fluorine-containing stripping solution provided by the invention uses 0.05-15% of fluoride by mass fraction, can effectively improve the cleaning effect, and effectively reduces the corrosion rate of VOX and PI.
According to the example 1 and the comparative example 2, the vanadium oxide corrosion-inhibition fluorine-containing stripping liquid provided by the invention can effectively reduce the corrosion rate of Al, Ti, VOX, PI, Ni, SiO2 and SiN by using 18-40% of alkanolamine.
According to the example 1 and the comparative example 3, the vanadium oxide corrosion-inhibition fluorine-containing stripping solution 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, SiO2 and SiN can be effectively reduced.
According to the embodiment 1 and the comparative examples 4 to 19, it can be found that the vanadium oxide corrosion inhibition fluorine-containing stripping solution provided by the invention adopts one or more of Tetronic 901, Tetronic 904 and Tetronic908 as PO-EO-vinyl diamine copolymer, so that the cleaning effect can be effectively improved, or the corrosion rate of Al, Ti, VOX, PI, Ni, SiO2 and SiN can be effectively reduced.
In summary, according to table 3, the vanadium oxide corrosion-inhibiting fluorine-containing stripping solution provided by the present invention has lower corrosion to various materials and has stronger removal effects on photo resist residues, hardened cross-linked photo resists 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 solution is characterized by mixing raw materials of the vanadium oxide corrosion inhibition fluorine-containing stripping solution, 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 Tetronic 908.
2. The method according to claim 1, wherein the reaction mixture,
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 mass fraction of the alkanolamine is 18.0-35.0;
and/or, the PO-EO-vinyl diamine copolymer is 0.56% to 1.5%;
and/or the mass fraction of the corrosion inhibitor is 1.2-4.3%;
and/or the mass fraction of the linear-chain 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 organic alkane ketone solvent is 6.70-10%.
3. The method according to claim 2,
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 mass fraction of the alkanolamine is 20.0% -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-chain 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 organic alkane ketone solvent is 7.50-9.1%.
4. The method according to claim 3,
the mass fraction of the fluoride is 5.3%;
and/or the mass fraction of the complexing agent is 1.50%;
and/or the mass fraction of alkanolamine is 25.4%;
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-chain amide 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 organic alkane ketone solvent is 9.1 percent.
5. The method according to claim 1, wherein the reaction mixture,
the fluoride is selected from one or more of hydrogen fluoride and a salt formed by the hydrogen fluoride and alkali;
and/or the alkanolamines are 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-aminopropan-1-ol, N-methyl-2-aminopropan-1-ol, N-ethyl-2-aminopropan-1-ol, 1-aminopropan-3-ol, N-methyl-1-aminopropan-3-ol, N-ethylethanolamine, N-, N-ethyl-1-aminopropan-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-3-aminobutan-1-ol, N-ethyl-3-aminobutan-1-ol, 1-aminobutan-4-ol, 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-methylpentane-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, methyl-1-aminopropane-2-ol, methyl-1-aminopropane-1, 3-diol, methyl-1-aminopropane-2-ol, methyl-1, One or more of 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-ethylhexyloxy) -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 benzene 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 organic solvent of the ketonic is an organic solvent of imidazolone and/or pyrrolidone.
6. The method according to claim 5,
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-aminooctan-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-chain amide organic solvent is one or more of N-methylformamide, N-ethylformamide, N-diethylformamide, N-methylacetamide, 3- (2-ethylhexyloxy) -N, N-dimethylpropionamide and 3-butoxy-N, N-dimethylpropionamide;
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,
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-chain amide organic solvent is N-methylformamide;
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-imidazolidinone;
and/or the PO-EO-vinyl diamine copolymer is Tetronic 908.
8. The production method according to any one of claims 1 to 7,
the mixing is to add the solid components in the raw materials into the liquid components and stir the mixture evenly.
9. The method of any one of claims 1-7, wherein the temperature of mixing is room temperature.
10. The method of any one of claims 1-7, wherein the mixing further comprises shaking and filtering.
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CN110262199A (en) * 2019-07-25 2019-09-20 上海新阳半导体材料股份有限公司 A kind of negtive photoresist stripper, preparation method and application

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WO2009146606A1 (en) * 2008-06-06 2009-12-10 安集微电子科技(上海)有限公司 Cleaning solution for removing residues from plasma etching
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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