CN111117623A - Acidic etching auxiliary agent and preparation method thereof - Google Patents
Acidic etching auxiliary agent and preparation method thereof Download PDFInfo
- Publication number
- CN111117623A CN111117623A CN201911386203.8A CN201911386203A CN111117623A CN 111117623 A CN111117623 A CN 111117623A CN 201911386203 A CN201911386203 A CN 201911386203A CN 111117623 A CN111117623 A CN 111117623A
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- acidic etching
- acid
- auxiliary agent
- aid according
- etching
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
Abstract
The invention provides an acid etching auxiliary agent and a preparation method thereof, wherein the acid-washing etching auxiliary agent comprises the following components in percentage by mass of 100 percent: 2-7% of polyether, 5-20% of surfactant, 0.5-5% of penetrating agent, 0.1-2% of chelating agent, 0.1-2% of pH value stabilizer, 1-10% of defoaming agent and the balance of water. The acid etching auxiliary agent prepared by the invention can reduce the consumption of hydrofluoric acid and nitric acid, and simultaneously improves the etching efficiency to a certain extent, thereby having good application prospect.
Description
Technical Field
The invention relates to the technical field of etching, in particular to an acidic etching auxiliary agent and a preparation method thereof.
Background
With the rapid development of the global solar energy and microelectronic industries, the demand for silicon wafers is rapidly increased, the silicon wafers are indispensable treatment processes for the front-stage processes of the cells at all times, and the process is also the link causing the most pollution to the environment, and how to effectively reduce the concentrations of nitric acid and hydrofluoric acid in the acidic etching solution becomes the most urgent problem in the current photovoltaic industry. Therefore, the development of a high-quality acid etching auxiliary agent becomes one of better solutions, and the high-quality acid etching auxiliary agent can not only reduce the consumption of acid, but also improve the etching efficiency.
The acid etching liquid used at present is a combination of nitric acid and hydrofluoric acid, and the concentration of the nitric acid and the hydrofluoric acid is high due to the requirement of polishing the back surface of the battery piece, but the treatment of the waste water of the nitric acid and the hydrofluoric acid becomes difficult due to the high concentration of the acid, and the production cost is also increased.
Disclosure of Invention
In view of the above, the invention provides an acidic etching auxiliary agent capable of reducing the amount of acid used in an acidic etching solution and improving the efficiency to a small extent, and a preparation method thereof.
The technical scheme of the invention is realized as follows: the invention provides an acidic etching auxiliary agent, which comprises the following components in percentage by mass of 100 percent:
on the basis of the above technical solution, preferably, the polyether is a polyoxyethylene-polyoxypropylene block copolymer.
On the basis of the above technical solution, preferably, the surfactant is an alcohol nonionic surfactant.
On the basis of the technical scheme, preferably, the alcohol nonionic surfactant is sorbitan ester.
More preferably, the penetrating agent is fatty alcohol-polyoxyethylene ether or alkylphenol polyoxyethylene ether.
On the basis of the technical scheme, preferably, the chelating agent is ethylenediamine tetraacetic acid.
On the basis of the technical scheme, preferably, the pH value stabilizer is amine Wanda.
On the basis of the technical scheme, preferably, the defoaming agent is defoaming agent silicone oil.
On the basis of the technical scheme, preferably, the water is deionized water, and the resistance of the deionized water is less than or equal to 1.0M omega.
The scheme also provides a preparation method of the acidic etching auxiliary agent, which comprises the following steps: adding polyether, surfactant, penetrant, chelating agent, defoaming agent and pH value stabilizer into deionized water, and uniformly stirring to obtain the acidic etching auxiliary agent.
Compared with the prior art, the acidic etching auxiliary agent and the preparation method thereof have the following beneficial effects:
(1) the acid etching auxiliary agent can effectively improve the etching efficiency of the acid etching liquid, reduce the concentration of nitric acid and hydrofluoric acid in the acid etching liquid to a certain extent, and simultaneously can keep good etching effect;
(2) the polyether and the surfactant added in the acidic etching auxiliary agent can reduce the surface tension of the etching liquid, so that the differential gas can be quickly separated from the surface of the silicon wafer to ensure that the surface of the silicon wafer is smooth, the additive can be uniformly dispersed on the surface of the silicon wafer by the penetrant, and the defoaming agent can eliminate bubbles generated in the reaction process, so that the bubbles are prevented from being attached to the surface of the silicon wafer and are difficult to clean;
(3) the inventor finds that the auxiliary agent compounded by the formula can not only save the using amount of acid, but also improve the etching efficiency compared with a common additive due to higher reflectivity of a back surface field.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
913g of deionized water is weighed, 20g of polyoxyethylene-polyoxypropylene segmented copolymer, 50g of sorbitan ester, 5g of fatty alcohol-polyoxyethylene ether, 1g of ethylene diamine tetraacetic acid, 1g of amine Wanda and 10g of defoaming agent silicone oil are added into the water, and the mixture is stirred for 5min to obtain the acid etching auxiliary agent.
Example 2
540g of deionized water is weighed, 70g of polyoxyethylene-polyoxypropylene segmented copolymer, 200g of sorbitan ester, 50g of fatty alcohol-polyoxyethylene ether, 20g of ethylene diamine tetraacetic acid, 20g of amine Wanda and 100g of defoaming agent silicone oil are added into the water, and the mixture is stirred for 5min to obtain the acidic etching auxiliary agent.
Example 3
Weighing 820g of deionized water, adding 30g of polyoxyethylene-polyoxypropylene segmented copolymer, 100g of sorbitan ester, 10g of alkylphenol polyoxyethylene, 5g of ethylene diamine tetraacetic acid, 5g of amine Wanda and 30g of defoaming agent silicone oil into the water, and stirring for 5min to obtain the acidic etching auxiliary agent.
Example 4
Weighing 700g of deionized water, adding 50g of polyoxyethylene-polyoxypropylene segmented copolymer, 150g of sorbitan ester, 20g of alkylphenol polyoxyethylene, 10g of ethylene diamine tetraacetic acid, 10g of amine Wanda and 60g of defoaming agent silicone oil into the water, and stirring for 5min to obtain the acidic etching auxiliary agent.
Example 5
660g of deionized water is weighed, 60g of polyoxyethylene-polyoxypropylene segmented copolymer, 130g of sorbitan ester, 30g of alkylphenol polyoxyethylene ether, 15g of ethylene diamine tetraacetic acid, 15g of amine Wanda and 90g of defoaming agent silicone oil are added into the water, and the mixture is stirred for 5min to obtain the acid etching auxiliary agent.
The acidic etching assistant prepared in examples 1 to 5 above was mixed with nitric acid having a concentration of 68% and hydrofluoric acid having a concentration of 49% in a mass ratio of 0.5: 4: 2, compounding to form an acidic etching solution, wherein the etching solution corresponding to the embodiment 1-5 is adopted, and the acid etching solution is prepared by mixing 68% of nitric acid and 49% of hydrofluoric acid according to a mass ratio of 4: 2, and a control group 1 etching solution prepared by compounding 68% of nitric acid and 49% of hydrofluoric acid according to a mass ratio of 4: 2.5 the etching solution of the control group 2, which is formed by compounding, is used for respectively etching the same batch of silicon wafers after texturing, the etching time is 60s, and the corresponding detection is carried out on the silicon wafers after the processing process and the processed silicon wafers, and the data are shown in the following table:
| group of | Appearance of the product | Reflectivity of light | Weight reduction |
| Example 1 | Is normal | 31.2％ | 0.296g |
| Example 2 | Is normal | 30.8％ | 0.301g |
| Example 3 | Is normal | 31.11％ | 0.298g |
| Example 4 | Is normal | 29.89％ | 0.308g |
| Example 5 | Is normal | 30.18％ | 0.287g |
| Control group 1 | Is normal | 30.22％ | 0.286g |
| Control group 2 | Is normal | 30.18％ | 0.288g |
The data show that after the auxiliary agent is used, under the condition of using nitric acid and hydrofluoric acid with lower concentration, the etching effect is equivalent to the efficiency of the conventional etching solution, and the effect is still good, so that the acid etching auxiliary agent can greatly reduce the using amount of acid liquor, and compared with the conventional mixed acid etching solution, the auxiliary agent has the advantages of quicker etching weight reduction and higher etching efficiency.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. An acidic etching assistant is characterized by comprising the following components in percentage by mass of 100%:
2. an acidic etching aid according to claim 1, wherein the polyether is a polyoxyethylene-polyoxypropylene block copolymer.
3. An acidic etching aid according to claim 1, wherein the surfactant is an alcoholic nonionic surfactant.
4. An acidic etching aid according to claim 3, wherein the alcoholic nonionic surfactant is a sorbitan ester.
5. An acidic etching aid according to claim 1, wherein the penetrant is a fatty alcohol-polyoxyethylene ether or an alkylphenol polyoxyethylene ether.
6. An acidic etching aid according to claim 1, wherein the chelating agent is ethylenediaminetetraacetic acid.
7. An acidic etching aid according to claim 1, characterized in that the pH stabilizer is amine Wanda.
8. An acidic etching aid according to claim 1, wherein the defoaming agent is a defoaming agent silicone oil.
9. An acidic etching aid according to claim 1, wherein the water is deionized water and has a resistance of 1.0M Ω or less.
10. A method for preparing an acidic etching aid, comprising: adding polyether, surfactant, penetrant, chelating agent, defoaming agent and pH value stabilizer into deionized water, and uniformly stirring to obtain the acidic etching auxiliary agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911386203.8A CN111117623A (en) | 2019-12-29 | 2019-12-29 | Acidic etching auxiliary agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911386203.8A CN111117623A (en) | 2019-12-29 | 2019-12-29 | Acidic etching auxiliary agent and preparation method thereof |
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| CN111117623A true CN111117623A (en) | 2020-05-08 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112662401A (en) * | 2020-11-25 | 2021-04-16 | 重庆臻宝实业有限公司 | Etching solution for low-resistance silicon product and etching method thereof |
| CN114573931A (en) * | 2022-03-04 | 2022-06-03 | 中国工程物理研究院激光聚变研究中心 | Preparation and application of colloid for repairing damaged pit on surface of optical element |
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Application publication date: 20200508 |