CN114317128A - High-purity water-soluble silicon wafer cleaning agent and preparation method thereof - Google Patents
High-purity water-soluble silicon wafer cleaning agent and preparation method thereof Download PDFInfo
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- CN114317128A CN114317128A CN202111620195.6A CN202111620195A CN114317128A CN 114317128 A CN114317128 A CN 114317128A CN 202111620195 A CN202111620195 A CN 202111620195A CN 114317128 A CN114317128 A CN 114317128A
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Abstract
The invention relates to a high-purity water-soluble silicon wafer cleaning agent and a preparation method thereof, wherein the cleaning agent comprises the following components in percentage by weight: 5-10% of surfactant, 5-15% of polymer builder, 1-5% of cosolvent, 25-40% of reinforcing agent and 35-50% of high-purity water. Compared with the prior art, the primer disclosed by the invention is low in VOC content, a paint film is quick to dry, good in toughness, good in early water resistance and excellent in corrosion resistance, and in addition, the cleaning agent disclosed by the invention is mainly used for cleaning and wiping the polished silicon wafer, and is mainly used for removing lubricants, dust and other dirt on the surface of the silicon wafer in the processing process. Is a non-toxic, harmless, safe and pollution-free cleaning agent.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a high-purity water-soluble silicon wafer cleaning agent and a preparation method thereof, which are mainly used for cleaning and wiping polished silicon wafers and mainly remove lubricants, dust and other dirt on the surfaces of the silicon wafers in the processing process. Is a non-toxic, harmless, safe and pollution-free cleaning agent.
Background
The base materials of the solar cell panel and various electronic product chips are monocrystalline silicon wafers which are formed by cutting monocrystalline silicon, polishing treatment is needed after cutting, substances such as lubricants and the like are needed in the polishing process, the components of the substances include organic substances and inorganic substances, and cleaning treatment is needed after polishing in order to ensure that the cleanliness of the silicon wafers meets the subsequent processing requirement. In the cleaning process, the conductivity and the size of residual particles of the cleaned residual substance are strictly required, and in order to ensure the standard, the formula of the cleaning agent is required to meet the requirement that the conductivity and the granularity of insoluble substances are within the processing quality index of the silicon wafer. Meanwhile, along with the stricter and stricter environmental protection requirements, the traditional silicon wafer cleaning agent has the defects of large usage amount, high COD content, large wastewater discharge amount, high treatment difficulty, even toxic and harmful substances and the like.
Patent application CN201010566271.5 discloses a silicon wafer cleaning agent, which contains a surfactant, a cosolvent, a metal complex, a suspending agent, a silicon wafer corrosive agent and water, wherein the surfactant contains a water-soluble fluorine-containing nonionic surfactant and an alcohol ether surfactant, and the weight ratio of the water-soluble fluorine-containing nonionic surfactant to the alcohol ether surfactant is 1: 10 to 1: 40. The silicon wafer cleaning agent disclosed by the invention can not cause serious corrosion on the surface of a silicon wafer, and has an excellent cleaning effect. The patent product has low yield in the process of cleaning the silicon wafer applied to high-end chip manufacturing, and the main reason is probably that the silicon wafer surface is seriously corroded due to the silicon wafer corrosive agent in the components, and meanwhile, the cleaning effect on the heavier oil stains on the silicon wafer surface is not good.
Patent application CN202111008614.0 discloses a cleaning agent composition after silicon wafer processing, which comprises the following components in percentage by weight: 10-15% of surfactant, 5-10% of penetrant, 0.01-0.3% of organic polymeric flocculant, 0.2-2% of alkali and the balance of deionized water. The cleaning liquid composition provided by the invention is used for cleaning the processed silicon wafer. Because a large amount of polar groups in a molecular chain of the high molecular weight organic flocculant can adsorb nano solid particles suspended on the surface of a workpiece or in water, bridging among the particles forms large flocculates, so that the nano particles are promoted to be agglomerated into large particles, stripping of the nano particles on the surface of the workpiece and sedimentation of the particles in suspension are accelerated, the purpose of quickly and efficiently removing residual particle pollutants on the surface of a silicon wafer is realized, and a good cleaning effect is achieved. The alkaline component of the product has certain corrosivity on the silicon wafer, so that pits are generated on the surface of the silicon wafer, the defect that the quality of the silicon wafer, particularly a high-end silicon wafer, is fatal is caused, and the yield in the later processing process is possibly reduced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a non-toxic, harmless and pollution-free high-purity water-soluble silicon wafer cleaning agent and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme: the high-purity water-soluble silicon wafer cleaning agent is characterized by comprising the following components in percentage by weight: 5-10% of surfactant, 5-15% of polymer builder, 1-5% of cosolvent, 25-40% of reinforcing agent and 35-50% of high-purity water.
Further, the surfactant is one or a mixture of more of linear alkyl benzene sulfonic acid sodium (LAS), fatty alcohol polyoxyethylene ether sodium sulfate (AES), fatty alcohol polyoxyethylene ether ammonium sulfate (AESA), sodium lauryl sulfate (SDS), lauroyl glutamic acid, nonylphenol polyoxyethylene ether (TX-10), peregal O, stearic acid monoglyceride, lignosulfonate, heavy alkylbenzene sulfonate, alkylsulfonate (petroleum sulfonate), dispersing agent NNO, dispersing agent MF, alkyl polyether (PO-EO copolymer) and fatty alcohol polyoxyethylene ether (AEO-3).
Further, the surfactant is fatty alcohol polyoxyethylene ether ammonium sulfate (AESA).
Further, the polymer builder is one or a mixture of acrylic acid copolymer, acrylamide polymer, carboxymethyl cellulose and vinyl alcohol polymer.
Further, the polymer builder is an acrylic acid copolymer.
Furthermore, the reinforcing agent is a formaldehyde water solution with the mass concentration of 20-40%, and preferably a formaldehyde water solution with the mass concentration of 35%.
Further, the high-purity water is high-purity water with the conductivity of more than or equal to 1M.
The invention also provides a preparation method of the high-purity water-soluble silicon wafer cleaning agent, which comprises the following steps: heating the surfactant, the polymer builder and the cosolvent to 40-60 ℃ for complete dissolution and mixing, then adding high-purity water, stirring fully, performing ion exchange, adding the reinforcing agent, and filtering to obtain a finished product, wherein indexes such as density, pH, viscosity and metal impurities of the finished product are in control index ranges.
Cation exchange resin is adopted in the ion exchange operation;
the aperture of the filtering membrane used for filtering is 0.2-1.0 μm.
The obtained product has the quality indexes of 1.0-1.1 g/ml density, 2.5-6.5 pH and 2.0-60 cm viscosity2S, potassium ion content is less than or equal to 1 multiplied by 10-4Percent, sodium ion content is less than or equal to 1 multiplied by 10-4Percent, calcium ion content less than or equal to 1 multiplied by 10-4Percent, copper ion content less than or equal to 1 multiplied by 10-5Percent, lead ion content less than or equal to 1 multiplied by 10-5Percent, iron ion content less than or equal to 1 multiplied by 10-5Percent, magnesium ion content is less than or equal to 1 multiplied by 10-4％。
Compared with the prior art, the invention has the following beneficial effects:
1. the cleaning agent is mainly used for cleaning and wiping the polished silicon wafer, and mainly removes lubricants, dust and other dirt adhered to the surface of the silicon wafer in the processing process. The substances adopted by the formula are all water-soluble substances which are non-dangerous chemicals; the usage amount of the cleaning agent for cleaning the polished silicon wafer is about 40-50% of that of the existing cleaning agent, so that the discharge amount of three wastes is reduced; the components used by the cleaning agent are all commercially available nontoxic substances, the safety is guaranteed, and the cleaning agent is nontoxic, harmless, safe and pollution-free.
2. The surface active agent in the formula is adopted to reduce the surface tension of water or the oil-water interfacial tension by absorbing on a gas-liquid, liquid-liquid or solid-liquid two-phase interface, thereby achieving the effect of washing the oil stain on the surface of the silicon wafer. The polymer builder adsorbs redundant metal ions in the silicon wafer cleaning process through dotted groups on a polymer mechanism, and simultaneously, the polymer builder has the functions of aggregating and removing precipitates for cleaned substances, the cosolvent mainly has the functions of supplementing a surfactant and the polymer builder in the cleaning process, improving the silicon wafer cleaning effect and protecting the silicon wafer surface, the reinforcing agent is mainly used for protecting the silicon wafer surface and preventing corrosion, high-purity water is used as a solvent of the components to play the roles of dissolving, diluting, washing and the like, and the high-purity water has certain requirements for ensuring the silicon wafer cleaning effect and water conductivity and is mainly supported by high-purity water guarantee.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1:
starting stirring, respectively pumping 140kg of fatty alcohol-polyoxyethylene ether ammonium sulfate (AESA), 160kg of acrylic copolymer and 60kg of PEG-400 into a 2000L stainless steel reaction kettle by using a vacuum pump, opening a steam valve, heating to 40-60 ℃, stopping heating after the pumped raw materials are completely melted, then adding 700kg of conductive water with the resistivity of 1M, fully stirring, carrying out ion exchange, and storing the liquid after the ion exchange into a 2000L plastic storage tank. Sampling and analyzing. The indexes of the finished product such as density, PH, viscosity, metal impurities and the like are all within the control index range, 500kg of 35% formaldehyde is added after the analysis is qualified, then a 0.5 mu m filtering membrane is used for filtering, the finished product is sampled again for analysis, and the finished product is filled in a 25 kg/barrel.
Example 2:
starting stirring, respectively pumping 80kg of fatty alcohol-polyoxyethylene ether sodium sulfate, 120kg of acrylamide polymer and 30kg of PEG-600 into a 2000L stainless steel reaction kettle by using a vacuum pump, opening a steam valve, heating to 40-60 ℃, stopping heating after the pumped raw materials are completely melted, then adding 470kg of conductive water with the resistivity of 1.5M, fully stirring, carrying out ion exchange, and storing the liquid after the ion exchange into a 2000L plastic storage tank. Sampling and analyzing. The indexes of the finished product such as density, PH, viscosity, metal impurities and the like are all within the control index range, 300kg of 35% formaldehyde is added after the analysis is qualified, then a 0.5 mu m filtering membrane is used for filtering, the finished product is sampled again for analysis, and the finished product is filled in a 25 kg/barrel.
Example 3:
starting stirring, respectively pumping 50kg of nonylphenol polyoxyethylene ether (TX-10), 150kg of vinyl alcohol polymer and 50kg of PEG-200 into a 2000L stainless steel reaction kettle by using a vacuum pump, opening a steam valve, heating to 40-60 ℃, stopping heating after the pumped raw materials are completely melted, then adding 450kg of conductive water with the resistivity of 1.5M, fully stirring, carrying out ion exchange, and storing the liquid after the ion exchange into a 2000L plastic storage tank. Sampling and analyzing. The indexes of the finished product such as density, PH, viscosity, metal impurities and the like are all within the control index range, 300kg of 35% formaldehyde is added after the analysis is qualified, then a 0.5 mu m filtering membrane is used for filtering, the finished product is sampled again for analysis, and the finished product is filled in a 25 kg/barrel.
Example 4:
starting stirring, respectively pumping 100kg of fatty alcohol-polyoxyethylene ether (AEO-3), 100kg of carboxymethyl cellulose and 50kg of PEG-400 into a 2000L stainless steel reaction kettle by using a vacuum pump, opening a steam valve to heat to 40-60 ℃, stopping heating after the pumped raw materials are completely melted, then adding 350kg of electric conduction water with the resistivity of 1.5M, fully stirring, carrying out ion exchange, and storing the liquid after the ion exchange into a 2000L plastic storage tank. Sampling and analyzing. The indexes of the finished product such as density, PH, viscosity, metal impurities and the like are all within the control index range, 400kg of 30% formaldehyde is added after the analysis is qualified, then the filter membrane with the thickness of 0.5 mu m is used for filtering, the finished product is sampled again for analysis, and the finished product is filled in a 25 kg/barrel.
The product obtained in each example was subjected to product analysis and performance testing, and the results were as follows:
as can be seen from the above table: after the cleaning solution prepared by the invention is used for cleaning, the number of solid particle residues on the surface of the silicon wafer is 10 or less, and the requirements of manufacturing chips such as solar energy, semiconductors and the like are met.
Various modifications of the above-described embodiments and concepts will be apparent to those skilled in the art and are intended to be included within the scope of the present invention as defined by the appended claims.
Claims (10)
1. The high-purity water-soluble silicon wafer cleaning agent is characterized by comprising the following components in percentage by weight: 5-10% of surfactant, 5-15% of polymer builder, 1-5% of cosolvent, 25-40% of reinforcing agent and 35-50% of high-purity water.
2. The high-purity water-soluble silicon wafer cleaning agent as claimed in claim 1, wherein the surfactant is one or more of linear alkyl benzene sulfonic acid sodium (LAS), fatty alcohol polyoxyethylene ether sodium sulfate (AES), fatty alcohol polyoxyethylene ether ammonium sulfate (AESA), sodium lauryl sulfate (SDS), lauroyl glutamic acid, nonylphenol polyoxyethylene ether (TX-10), peregal O, stearic acid monoglyceride, lignosulfonate, heavy alkylbenzene sulfonate, alkylsulfonate (petroleum sulfonate), dispersant NNO, dispersant MF, alkyl polyether (PO-EO copolymer), and fatty alcohol polyoxyethylene ether (AEO-3).
3. The high-purity water-soluble silicon wafer cleaning agent as claimed in claim 2, wherein the surfactant is fatty alcohol polyoxyethylene ether ammonium sulfate (AESA).
4. The high-purity water-soluble silicon wafer cleaning agent as claimed in claim 1, wherein the polymer builder is one or more of acrylic acid copolymer, acrylamide polymer, carboxymethyl cellulose, and vinyl alcohol polymer.
5. The high purity water soluble silicon wafer cleaner as claimed in claim 4, wherein said polymer builder is an acrylic acid copolymer.
6. The high-purity water-soluble silicon wafer cleaning agent as claimed in claim 1, wherein the reinforcing agent is a formaldehyde aqueous solution with a mass concentration of 20-40%, preferably 35%.
7. The high-purity water-soluble silicon wafer cleaning agent as claimed in claim 1, wherein the high-purity water is high-purity water having an electrical conductivity of not less than 1M.
8. A method for preparing a high-purity water-soluble silicon wafer cleaning agent as claimed in any one of claims 1 to 7, which comprises the following steps: heating the surfactant, the polymer builder and the cosolvent to 40-60 ℃ for complete dissolution and mixing, then adding high-purity water, stirring fully, carrying out ion exchange, adding the reinforcing agent, and filtering to obtain a finished product.
9. The preparation method of the high-purity water-soluble silicon wafer cleaning agent as claimed in claim 8, wherein,
cation exchange resin is adopted in the ion exchange operation;
the aperture of the filtering membrane used for filtering is 0.2-1.0 μm.
10. The preparation method of the high-purity water-soluble silicon wafer cleaning agent as claimed in claim 8, wherein the quality indexes of the obtained product are that the density is 1.0-1.1 g/ml, the pH is 2.5-6.5, and the viscosity is 2.0-60 cm2S, potassium ion content is less than or equal to 1 multiplied by 10-4Percent, sodium ion content is less than or equal to 1 multiplied by 10-4Percent, calcium ion content less than or equal to 1 multiplied by 10-4Percent, copper ion content less than or equal to 1 multiplied by 10-5Percent, lead ion content less than or equal to 1 multiplied by 10-5Percent, iron ion content less than or equal to 1 multiplied by 10-5Percent, magnesium ion content is less than or equal to 1 multiplied by 10-4％。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335382A (en) * | 2001-07-23 | 2002-02-13 | 山东大学 | Scavenger composition for superlarge scale IC chip and its prepn |
| CN103881837A (en) * | 2012-12-19 | 2014-06-25 | 上海工程技术大学 | Semiconductor industrial cleaning agent and application thereof |
| CN113667546A (en) * | 2021-08-31 | 2021-11-19 | 昆山捷纳电子材料有限公司 | Cleaning agent composition used after silicon wafer processing |
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- 2021-12-28 CN CN202111620195.6A patent/CN114317128A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335382A (en) * | 2001-07-23 | 2002-02-13 | 山东大学 | Scavenger composition for superlarge scale IC chip and its prepn |
| CN103881837A (en) * | 2012-12-19 | 2014-06-25 | 上海工程技术大学 | Semiconductor industrial cleaning agent and application thereof |
| CN113667546A (en) * | 2021-08-31 | 2021-11-19 | 昆山捷纳电子材料有限公司 | Cleaning agent composition used after silicon wafer processing |
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