CN112280623B - Water-based neutral cleaning solution for semiconductor manufacturing base station - Google Patents
Water-based neutral cleaning solution for semiconductor manufacturing base station Download PDFInfo
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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
- C11D1/825—Mixtures of compounds all of which are non-ionic
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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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2041—Dihydric alcohols
- C11D3/2044—Dihydric alcohols linear
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- 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
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- C11D3/20—Organic compounds containing oxygen
- C11D3/2068—Ethers
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- 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
- C11D3/2093—Esters; Carbonates
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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
- 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
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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
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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
- C11D1/662—Carbohydrates or derivatives
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Abstract
The invention belongs to the technical field of preparation of cleaning materials for a semiconductor process, and particularly relates to a water-based neutral cleaning solution for a semiconductor manufacturing base station. The cleaning solution comprises the following raw materials in percentage by mass and the following amount of the raw materials in percentage by mass, wherein the sum of the mass percentages is 100 percent: 5-15% of dihydric alcohol or glycol ether, 10-25% of pyrrolidone solvent, 1-5% of a brizer surfactant, 10-20% of an alkyl glycoside derivative surfactant, 0.5-1% of a corrosion inhibitor and the balance of water. The water-based neutral cleaning solution provided by the invention has excellent cleaning capability aiming at the photoresist mainly composed of the linear phenolic resin in the photoetching process and the matched wet electronic chemical residues thereof, has no corrosiveness on base station materials, and is simple in cleaning process, non-toxic and free of residues.
Description
Technical Field
The invention belongs to the technical field of preparation of cleaning materials for a semiconductor process, and particularly relates to a water-based neutral cleaning solution for a semiconductor manufacturing base station, which is suitable for cleaning the surface of substrate equipment in the manufacturing and packaging processes of semiconductor wafers and the production and manufacturing photoetching processes of OLEDs (organic light emitting diodes), TFTs (thin film transistors) and the like.
Background
In the photolithography process for manufacturing and packaging semiconductor wafers and for manufacturing mini-LEDs, OLEDs, TFT-LCDs, etc., several to tens of repeated photolithography processes are performed to obtain a specific pattern, so that a large amount of photoresist mainly composed of novolac resin and its associated wet electronic chemicals are used, and the photoresist and its associated wet electronic chemicals remain on the surface of the device substrate in the whole processes of coating, prebaking, exposure, development, postbaking, stripping, etc. The accumulation of residual impurities can cause the blockage of the spray head, the falling of the impurities can also influence the product and the subsequent process, and meanwhile, the long-time contact between the impurities and the base station can cause the corrosion of the base material and also bring potential safety hazards to operators.
The existing base station cleaning solution is generally diluted by developing solution or other alkaline cleaning agents for regular maintenance and maintenance, but the method usually needs to be stopped for cleaning, seriously influences the productivity and has limited cleaning effect on parts which are easy to accumulate and block; in addition, if the cleaning agent is not clean, the base station is also corroded, and the generated waste water needs more treatment procedures and is higher in cost. Therefore, it is necessary to provide a simple, effective and non-corrosive cleaning solution for a base.
Disclosure of Invention
The invention aims to provide a water-based neutral cleaning solution which has excellent cleaning capability on a semiconductor manufacturing base station, has no corrosivity on base station materials, and has simple cleaning process, no toxicity and no residue.
In order to achieve the purpose, the invention adopts the following technical scheme:
the water-based neutral cleaning solution for the semiconductor manufacturing base station comprises the following raw materials in percentage by mass, wherein the total mass percentage of the raw materials is 100 percent: 5-15% of dihydric alcohol or glycol ether, 10-25% of pyrrolidone solvent, 1-5% of a brizer surfactant, 10-20% of an alkyl glycoside derivative surfactant, 0.5-1% of a corrosion inhibitor and the balance of water.
Specifically, in the water-based neutral cleaning solution, the dihydric alcohol is any 1 or 2 of ethylene glycol, diethylene glycol and propylene glycol; the glycol ether is any 1 or 2 of ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol monomethyl ether acetate, ethylene glycol ethyl ether acetate, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monopropyl ether, diethylene glycol monobutyl ether, diethylene glycol monomethyl ether acetate, diethylene glycol monoethyl ether acetate, diethylene glycol monopropyl ether acetate, diethylene glycol monobutyl ether acetate, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monobutyl ether, propylene glycol methyl ether acetate and propylene glycol ethyl ether acetate.
The pyrrolidone solvent is any 1 or 2 of N-methyl pyrrolidone, N-ethyl pyrrolidone, N-propyl pyrrolidone, N-hydroxymethyl pyrrolidone and N-hydroxyethyl pyrrolidone, and N-methyl pyrrolidone and N-ethyl pyrrolidone are preferred in consideration of price and the wide range of raw materials.
The Brij surfactant is any 1 or 2 of Brij 30, Brij35, Brij52, Brij 56, Brij58 and Brij 72. The brij surfactant has excellent water solubility and solubilization effect, is non-toxic and environment-friendly, and is preferably brij35 and brij 58.
The alkyl glycoside derivative surfactant is specifically an alkyl glycoside citrate ester surfactant, and the chemical structural formula of the alkyl glycoside derivative surfactant is as follows:
wherein, R is alkyl with 10, 12, 14 and 16 carbon atoms in a long carbon chain, and n is 1 or 2. The surfactant has excellent cleaning capacity, and has strong cleaning effect on pollutants with strong adsorption capacity after being compounded with the benzyl cleaning agent in a proper proportion.
The corrosion inhibitor is alkyl gallate corrosion inhibitor, specifically 1 or 2 of dodecyl gallate and hexadecyl gallate.
The water is preferably deionized water filtered through an ion exchange resin, and has a resistivity of not less than 18M omega at 25 ℃ and a total metal ion concentration of not more than 500 ug/L.
The preparation method of the water-based neutral cleaning solution comprises the steps of uniformly mixing the raw materials, and filtering the mixture at room temperature through a 0.5-micrometer filter element.
The water-based neutral cleaning solution needs to be diluted by 5-20 times when in use, and is selected according to the product process.
The invention has the following advantages: the water-based neutral cleaning method can effectively remove the residues of the photoresist and the matched wet electronic chemicals on the substrate equipment, which are used in the photoetching process of manufacturing and packaging semiconductor wafers and producing and manufacturing mini-LEDs, OLEDs, TFT-LCDs and the like, and has the advantages of simple cleaning process, excellent cleaning effect, no corrosion to base station materials, environmental friendliness, safety and no toxicity.
Drawings
FIG. 1 is an infrared spectrum of the alkyl glycoside citrate ester prepared in the example (C12).
Detailed Description
The water-based neutral cleaning solution for the semiconductor manufacturing base station comprises the following raw materials in percentage by mass, wherein the total mass percentage of the raw materials is 100 percent: 5-15% of dihydric alcohol or glycol ether, 10-25% of pyrrolidone solvent, 1-5% of a brizer surfactant, 10-20% of an alkyl glycoside derivative surfactant, 0.5-1% of a corrosion inhibitor and the balance of water.
Specifically, in the water-based neutral cleaning solution, the dihydric alcohol is any 1 or 2 of ethylene glycol, diethylene glycol and propylene glycol; the glycol ether is any 1 or 2 of ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol monomethyl ether acetate, ethylene glycol ethyl ether acetate, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monopropyl ether, diethylene glycol monobutyl ether, diethylene glycol monomethyl ether acetate, diethylene glycol monoethyl ether acetate, diethylene glycol monopropyl ether acetate, diethylene glycol monobutyl ether acetate, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monobutyl ether, propylene glycol methyl ether acetate and propylene glycol ethyl ether acetate.
The pyrrolidone solvent is any 1 or 2 of N-methyl pyrrolidone, N-ethyl pyrrolidone, N-propyl pyrrolidone, N-hydroxymethyl pyrrolidone and N-hydroxyethyl pyrrolidone, and N-methyl pyrrolidone and N-ethyl pyrrolidone are preferred in consideration of price and the wide range of raw materials.
The Brij surfactant is any 1 or 2 of Brij 30, Brij35, Brij52, Brij 56, Brij58 and Brij 72. The brij surfactant has excellent water solubility and solubilization effect, is non-toxic and environment-friendly, and is preferably brij35 and brij 58.
The alkyl glycoside derivative surfactant is specifically an alkyl glycoside citrate ester surfactant, and the chemical structural formula of the alkyl glycoside derivative surfactant is as follows:
wherein, R is alkyl with 10, 12, 14 and 16 carbon atoms in a long carbon chain, and n is 1 or 2. The surfactant has excellent cleaning capacity, and has strong cleaning effect on pollutants with strong adsorption capacity after being compounded with the benzyl cleaning agent in a proper proportion.
The corrosion inhibitor is alkyl gallate corrosion inhibitor, specifically 1 or 2 of dodecyl gallate and hexadecyl gallate.
The water is preferably deionized water filtered through an ion exchange resin, and has a resistivity of not less than 18M omega at 25 ℃ and a total metal ion concentration of not more than 500 ug/L.
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto. The experimental methods used in the examples are all conventional methods unless otherwise specified. The materials, reagents and the like used in the examples are commercially available unless otherwise specified.
Examples
At room temperature, adding dihydric alcohol or dihydric alcohol ether, a pyrrolidone solvent, a benzyl Zener surfactant, an alkyl glycoside derivative surfactant, a corrosion inhibitor and deionized water in sequence according to the formula shown in the table 1, stirring until the mixture is uniformly clear, and filtering through a filter element with the diameter of 0.5 mu m to obtain the water-based neutral cleaning solution.
TABLE 1 raw materials and their proportions for preparing water-based neutral detergent
The synthetic route of the alkyl glycoside citrate (C12) is as follows:
wherein R is an alkyl group having a carbon chain length of 12 carbons; n is 2.
The preparation method comprises the following specific steps: 3L of C with a concentration of 50%12Adding the alkyl glycoside aqueous solution into a reaction kettle, stirring for 2min under the conditions of vacuum degree of 5000Pa and stirring speed of 30r/min, then adding 122g of citric acid in portions, increasing the rotating speed according to 200r/min, controlling the adding time to be about 30min, adjusting the rotating speed to 10000r/min after the citric acid is added, starting a water bath heater of a reaction kettle, controlling the reaction temperature to be 42 ℃, adding a composite catalyst (formed by compounding hydrogen peroxide, ethylene diamine tetraacetic acid and acetic anhydride according to the mass ratio of 2:13: 5) with the mass ratio of 10:1 to the alkyl glucoside into the reaction kettle, reacting for 40min to obtain a mixed solution of alkyl glucoside citrate and alkyl glucoside, sampling and detecting the content of the citric acid in the obtained mixed solution to be not higher than 0.5%, and (3) immediately reaching the reaction end point, extracting with ethyl acetate, drying, and performing rotary evaporation to remove the ethyl acetate to obtain the alkyl glycoside citrate (C12).
Visible from the infrared spectrogram: it is at 1725cm-1V of carboxylate carbonyl as a nearby peakC═OAt 1202.91-1202.81 cm-1The peak of (A) is the voas of the carboxylic esterC—O—CThe presence of the ester structure-COOC in the product is indicated; 1403.99-1402.80 cm-1The peak of (A) is ν in carboxylic acidC—O，1597.10 cm-1 Peak of (A) is carboxylate-CO2 —The antisymmetric stretching vibration absorption peak of (1). At 3329.01 cm-1The peak of (a) is ν of glycosideOH，2938.38、2879.23 cm-1The double peaks of (A) and (B) are methyl and methylene stretching vibration peaks of 1082.48 cm-1And 1037.41 cm-1The absorption band of (A) is a stretching vibration peak of the saturated ether bond C-O-C, and it was confirmed that the obtained product was the alkyl glycoside citrate (C12).
The above-mentioned preparation steps are usedC of (A)12Replacement of alkyl glycoside by C10Alkyl glycoside, C14Alkyl glycoside, C16Alkyl glycoside, corresponding alkyl glycoside citrate (C10), alkyl glycoside citrate (C14), alkyl glycoside citrate (C16) can be prepared.
In addition, comparative examples 1 to 8 were prepared according to the formulation shown in Table 2, and the preparation method was the same as above, to compare the cleaning effects of different cleaning solutions.
TABLE 2 raw materials and their ratios for preparing water-based neutral cleaning agent for comparison
Performance measurement of Water-based neutral cleaning solution
1. Determination of flushing Effect
And (3) coating the photoresist on a silicon wafer with the diameter of 3cm and the thickness of about 10 microns, putting the silicon wafer into a 110 ℃ oven for baking for 10 minutes, and standing the silicon wafer to room temperature. Diluting the water-based neutral cleaning solution to 10% with deionized water, placing into spraying equipment at a concentration of 2kg/cm2Spraying the silicon wafer coated with the photoresist for 120s, then cleaning the silicon wafer with deionized water for 30s, and observing the cleanliness of the surface of the silicon wafer under the condition of 50 times of an electron microscope. The criteria are as follows:
it: the surface is smooth and clean, and photoresist and the like are remained;
o: the surface is basically clean, and a small amount of photoresist remains at individual places;
x: the surface photoresist had a significant residue.
2. Measurement of scrubbing Effect
Coating the photoresist on a 304 stainless steel sheet with the thickness of about 30-50 microns, baking in an oven at 110 ℃ for 10 minutes, and standing to room temperature. Diluting the water-based neutral cleaning solution to 20% by using deionized water, scrubbing by dipping the dust-free cloth in the water-based neutral cleaning solution, and then cleaning by using the deionized water. The cleanliness of the surface of the stainless steel sheet was observed under an electron microscope at 50 times. The criteria are as follows:
it: the photoresist has strong solubility and is easy to clean;
o: the photoresist has a cleaning effect, and can be removed only by repeated scrubbing;
x: the photoresist is difficult to clean and difficult to remove after repeated scrubbing.
3. Solution stability test
The prepared water-based neutral cleaning solution is placed in a constant temperature box, and the stability of the cleaning solution at 5-45 ℃ is tested. The criteria are as follows:
it: the cleaning agent composition is uniform and stable;
o: clouding of the cleaner composition;
x: the cleaning composition had delamination.
4. And (5) testing the corrosion of the metal.
The prepared water-based neutral cleaning solution is placed in a 250mL beaker, diluted to 5% and 20% respectively by deionized water, 3 aluminum metal test pieces are immersed in the water-based neutral cleaning solution, the cleaning agent is heated to 40 ℃, and the temperature is kept for 30 min. Removing the metal sample, washing with deionized water and drying. Performing a salt spray test for 19h according to GB/T10125-2012, observing the corrosion condition of the surface of the aluminum metal test piece by a microscope of 40 times after drying, wherein the judgment standards are as follows:
it: the surface has no obvious change and no corrosion;
o: the surface has uniform color change or slight light loss;
x: the surface has non-uniform discoloration, light loss and local corrosion spots.
The results are shown in Table 3.
TABLE 3 Performance evaluation results for different water-based neutral cleaning solutions
From the results, the water-based neutral cleaning agent composition with excellent cleaning effect and stable performance can be obtained only by compounding the alkyl glycoside citrate surfactant and the benzyl Zea surfactant at a certain ratio, and the cleaning agent prepared by compounding the alkyl glycoside citrate surfactant and the benzyl Zea surfactant at other ratios or with other surfactants is difficult to meet the requirements of the cleaning process.
The above description is only for the preferred embodiment of the present invention, and it should be understood by those skilled in the art that the present invention is not limited by the claims, and all equivalent changes and modifications made by the present invention in the specification and other related fields can be directly or indirectly applied to the present invention, and the same shall be included in the scope of the present invention.
Claims (4)
1. A water-based neutral cleaning solution for a semiconductor manufacturing base station is characterized in that: the cleaning solution comprises the following raw materials in percentage by mass and the usage thereof is 100 percent: 5-15% of dihydric alcohol or glycol ether, 10-25% of pyrrolidone solvent, 1-5% of a brizer surfactant, 10-20% of an alkyl glycoside derivative surfactant, 0.5-1% of a corrosion inhibitor and the balance of water;
the alkyl glycoside derivative surfactant is specifically an alkyl glycoside citrate ester surfactant, and the chemical structural formula of the alkyl glycoside derivative surfactant is as follows:
wherein R is alkyl with 10, 12, 14 and 16 carbon atoms in a long carbon chain, and n is 1 or 2;
the corrosion inhibitor is alkyl gallate corrosion inhibitor, specifically 1 or 2 of dodecyl gallate and hexadecyl gallate.
2. The water-based neutral cleaning solution as claimed in claim 1, wherein: the dihydric alcohol is any 1 or 2 of ethylene glycol, diethylene glycol and propylene glycol;
the glycol ether is any 1 or 2 of ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monopropyl ether, diethylene glycol monobutyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether and propylene glycol monobutyl ether.
3. The water-based neutral cleaning solution as claimed in claim 1, wherein: the pyrrolidone solvent is any 1 or 2 of N-methyl pyrrolidone, N-ethyl pyrrolidone, N-propyl pyrrolidone, N-hydroxymethyl pyrrolidone and N-hydroxyethyl pyrrolidone.
4. The water-based neutral cleaning solution as claimed in claim 1, wherein: the Brij surfactant is any 1 or 2 of Brij 30, Brij35, Brij52, Brij 56, Brij58 and Brij 72.
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| US9421236B2 (en) * | 2010-12-17 | 2016-08-23 | Johnson & Johnson Consumer Inc. | Compositions comprising Lilium siberia extracts and uses thereof |
| CN102872753B (en) * | 2012-10-30 | 2014-06-18 | 大庆浩拓化工有限公司 | Surfactant composition and preparation method thereof |
| CN105695126B (en) * | 2016-04-19 | 2018-09-18 | 福州大学 | A kind of environment-friendly type water based cleaning agent for printed wiring board |
| CN110331049B (en) * | 2019-06-24 | 2021-02-12 | 上海发凯化工有限公司 | Surfactant composition containing alkyl glycoside and preparation method thereof |
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| CN105695159A (en) * | 2016-03-25 | 2016-06-22 | 中国日用化学工业研究院 | Solvent-free high-enriched tableware scouring agent and preparation method thereof |
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