Method for improving cleanliness of high-purity quartz product

Abstract

The invention discloses a method for improving the cleanliness of a high-purity quartz product, and belongs to the technical field of quartz product production. The method comprises the following steps: soaking a to-be-treated high-purity quartz product in a cleaning solution for the first time, then soaking the to-be-treated high-purity quartz product in an acid solution for the second time, and cleaning the to-be-treated high-purity quartz product with water; the cleaning solution is composed of OP-10, AEO-3 and water according to the volume ratio of (2-8): (2-8): 100. The method is easy to operate, high in efficiency, small in water consumption and low in cost, dead corners of products in different shapes can be cleaned, and product scrapping caused by product scratching in the cleaning process can be avoided. Furthermore, the cleaned product can be used after being dried.

Description

Technical Field

[0001] The invention relates to the technical field of quartz product production, and in particular to a method for improving the cleanliness of high-purity quartz products. Background Art

[0002] Quartz material is a high-quality, highly reliable and highly stable material. Quartz products are widely used in electronics, optics, semiconductors and other fields. In the semiconductor industry, quartz products are widely used, and high-purity quartz products are important consumables in wafer production. Quartz parts such as crucibles and crystal boats used to produce silicon single crystals must use high-purity quartz products (purity not less than 99.999%). The cleanliness of quartz products directly affects the processing of semiconductors. Therefore, quartz products need to be cleaned before use and reach a certain cleanliness level to ensure that they meet the requirements of semiconductor processing.

[0003] At present, the cleaning steps in the production process of high-purity quartz products include: placing the quartz products on the shower table, spraying alcohol on the surface of the sample, wiping the surface with a dust-free cloth and then rinsing; then soaking the sponge with laundry detergent or detergent solution, wiping the quartz products evenly and then rinsing with pure water (for degreasing and cleaning of long tubular products, different coarse and fine cleaning jigs are required. Because the other parts of the jig except the sponge are relatively hard, do not use too much force during the cleaning process to avoid damaging the product).

[0004] The above method not only consumes a large amount of water and has low efficiency, but also easily scratches the product during manual wiping, causing the product to be scrapped. In addition, for some products with strange shapes, their dead corners cannot be thoroughly cleaned, resulting in product devitrification during subsequent processing.

[0005] In view of this, the present invention is proposed. Summary of the invention

[0006] The object of the present invention is to provide a method for improving the cleanliness of high-purity quartz products to solve or improve the above technical problems.

[0007] The present invention can be implemented like this:

[0008] In a first aspect, the present invention provides a method for improving the cleanliness of a high-purity quartz product, comprising the following steps: soaking the high-purity quartz product to be cleaned in a cleaning solution for a first time, then soaking it in an acid solution for a second time, and then washing it with water;

[0009] The cleaning solution is composed of OP-10, AEO-3 and water in a volume ratio of (2-8):(2-8):100.

[0010] In an optional embodiment, the cleaning solution consists of OP-10, AEO-3 and water in a volume ratio of (4-8):(2-4):100.

[0011] In an optional embodiment, the temperature of the first soaking is 28° C. to 35° C., and the time of the first soaking is 4 min to 10 min.

[0012] In an optional embodiment, the temperature of the second soaking is 20° C. to 40° C., and the time of the second soaking is 1 min to 30 min.

[0013] In an optional embodiment, the acid solution used for the second immersion is hydrofluoric acid with a concentration of 4.5% to 5%.

[0014] In an optional embodiment, cleaning with water includes: first performing overflow cleaning in a pure water overflow tank, and then rinsing with pure water.

[0015] In an optional embodiment, the overflow cleaning time is 1 min to 5 min.

[0016] In an optional embodiment, the method further comprises: drying the product obtained by washing with water.

[0017] In an optional embodiment, drying is performed by air gun drying.

[0018] In an optional embodiment, the gas used for air gun drying is helium with a purity of not less than 99.999%.

[0019] The beneficial effects of the present invention include:

[0020] The present invention creatively proposes a method for improving the cleanliness of high-purity quartz products, wherein OP-10, AEO-3 and water are compounded in a specific volume ratio and used as a cleaning liquid, which can effectively play a degreasing role, so that there is basically no residual lipid impurities on the surface of the high-purity quartz products. The high-purity quartz products to be treated are first immersed in the above-mentioned cleaning liquid, then immersed in an acid solution for a second time, and then washed with water. The method is simple to operate, high in efficiency, uses less water, and has low cost. It can not only clean the dead corners of products with strange shapes, but also avoid scratching the products during the cleaning process, resulting in product scrapping. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments are briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without creative work.

[0022] Figure 1 This is a surface result diagram of the high-purity quartz product after high-temperature treatment in Comparative Example 1;

[0023] Figure 2 This is a diagram of the surface results of the high-purity quartz product after high-temperature treatment after treatment in Example 1. DETAILED DESCRIPTION

[0024] In order to make the purpose, technical scheme and advantages of the embodiments of the present invention clearer, the technical scheme in the embodiments of the present invention will be described clearly and completely below. If the specific conditions are not specified in the embodiments, they are carried out according to conventional conditions or conditions recommended by the manufacturer. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be purchased commercially.

[0025] The method for improving the cleanliness of high-purity quartz products provided by the present invention is specifically described below.

[0026] The invention provides a method for improving the cleanliness of high-purity quartz products, which comprises the following steps: soaking the high-purity quartz products to be cleaned in a cleaning solution for the first time, then soaking them in an acid solution for the second time, and then cleaning them with water.

[0027] In the present invention, the cleaning solution is composed of OP-10, AEO-3 and water in a volume ratio of (2-8):(2-8):100.

[0028] In some embodiments, the volume ratio of OP-10, AEO-3, and water may be 2:2:100, 2:3:100, 2:4:100, 2:5:100, 2:6:100, 2:7:100, 2:8:100, 3:2:100, 3:3:100, 3:4:100, 3:5:100, 3:6:100, 3:7:100, 3:8:100, 4:2:100, 4:3:100, 4:4:100, 4:5:100, 4:6:100, 4:7:100, 4:8:100, 5:2:100, 5:3:100, 5:4:100, 5:5:100. :100, 5:6:100, 5:7:100, 5:8:100, 6:2:100, 6:3:100, 6:4:100, 6:5:100, 6:6:100, 6:7:100, 6:8:100, 7:2:100, 7:3:100, 7:4:100, 7:5:100, 7:6:100, 7:7:100, 7:8:100, 8:2:100, 8:3:100, 8:4:100, 8:5:100, 8:6:100, 8:7:100 or 8:8:100, etc., and can also be other values ​​in the range of (2-8):(2-8):100.

[0029] In some preferred embodiments, the volume of OP-10 in the cleaning solution is not less than the volume of AEO-3. Under this condition, the cleaning effect is better than when the volume of AEO-3 is higher than that of OP-10. In some typical embodiments, the cleaning solution is composed of OP-10, AEO-3 and water in a volume ratio of (4-8):(2-4):100.

[0030] In the above cleaning solution, OP-10 can play the role of emulsification, wetting, diffusion and cleaning; AEO-3 can play the role of solubilization and defoaming. By compounding OP-10 and AEO-3 according to the above specific volume ratio, it can effectively play the role of degreasing, so that there is basically no residual lipid impurities on the surface of high-purity quartz products.

[0031] It should be noted that in the above cleaning solution, if the volume ratio of OP-10 to water is lower than 4:100, it is not conducive to degreasing, the immersion time will be prolonged, and incomplete degreasing may occur; if the volume ratio of OP-10 to water is higher than 8:100, it is not conducive to pure water rinsing, the amount of pure water rinsing water will increase, and incomplete rinsing may occur. If the volume ratio of AEO-3 to water is lower than 4:100, it is not conducive to degreasing, and incomplete degreasing may occur; if the volume ratio of AEO-3 to water is higher than 8:100, it is not conducive to pure water rinsing, the amount of pure water rinsing water will increase, and incomplete rinsing may occur.

[0032] In some optional embodiments, the temperature of the first immersion can be 28°C to 35°C, such as 28°C, 29°C, 30°C, 31°C, 32°C, 33°C, 34°C or 35°C, or other values ​​within the range of 28°C to 35°C.

[0033] The first immersion time may be 4 min to 10 min, such as 4 min, 5 min, 6 min, 7 min, 8 min, 9 min or 10 min, or may be other values ​​within the range of 4 min to 10 min.

[0034] If the temperature of the first immersion is too low or the time is too short, the lipid impurities on the surface of the quartz product cannot be effectively removed; if the temperature of the first immersion is too high or the time is too long, the stability of OP-10 will deteriorate, affecting the degreasing effect.

[0035] In some typical implementations, the temperature of the first soaking is 30° C., and the time of the first soaking is 4 minutes.

[0036] In some typical embodiments, the first immersion process is performed under ultrasonic conditions.

[0037] In some optional embodiments, the temperature of the second immersion can be 20°C to 40°C, such as 20°C, 25°C, 30°C, 35°C or 40°C, etc., or other values ​​within the range of 20°C to 40°C.

[0038] The second immersion time can be 1 min to 30 min, such as 1 min, 2 min, 5 min, 10 min, 15 min, 20 min, 25 min or 30 min, or other values ​​within the range of 1 min to 30 min.

[0039] If the temperature of the second immersion is too low or the time is too short, impurities other than lipids on the surface of the quartz product cannot be effectively removed; if the temperature of the second immersion is too high or the time is too long, it will cause excessive etching and damage the surface of the quartz product; and if the temperature of the second immersion is too high, the reaction speed will be too fast, resulting in a surface spike effect, causing the surface of the quartz product to be uneven.

[0040] In some typical implementations, the temperature of the second soaking is 30° C., and the time of the second soaking is 5 minutes.

[0041] In some optional embodiments, the acid solution used for the second immersion may be hydrofluoric acid with a concentration of 4.5% to 5% (eg, 4.5%, 4.6%, 4.7%, 4.8%, 4.9% or 5%).

[0042] The second immersion can fully etch the surface of the quartz product to remove impurities other than lipids.

[0043] In some optional embodiments, water cleaning can be performed by directly rinsing with pure water, but this method requires a large amount of water to clean the surface of the quartz product with heterogeneity or dead corners, which easily causes water waste and increases costs.

[0044] In some preferred embodiments, washing with water includes: firstly performing overflow washing in a pure water overflow tank, and then rinsing with pure water.

[0045] The overflow cleaning time may be 1 min to 5 min, such as 1 min, 2 min, 3 min, 4 min or 5 min, etc., or may be other values ​​within the range of 1 min to 5 min.

[0046] By first performing overflow cleaning in the overflow tank, the hydrofluoric acid remaining on the surface of the quartz product can be basically removed, especially for quartz products with heterogeneity or dead corners. This step can effectively remove the hydrofluoric acid in the dead corners under the condition of using less water. After overflow cleaning, rinse with pure water to remove the weak acid that may remain after overflow cleaning under the condition of using less water.

[0047] Furthermore, the product obtained by washing with water is dried.

[0048] In some optional embodiments, the drying is performed by air gun drying, and the gas used for air gun drying is helium with a purity of not less than 99.999%.

[0049] By adopting the above-mentioned air gun drying method for drying, it can have the advantages of being convenient, fast and applicable to a wide range of products compared with other drying methods (such as drying methods).

[0050] In some specific implementations, the cleanliness of high-purity quartz products can be improved by referring to the following steps:

[0051] Step S1: Pour 100L of pure water, 4L-8L of OP-10 and 4L-8L of AEO-3 as cleaning liquid into the degreasing tank and stir evenly, place the high-purity quartz product to be treated in the above degreasing tank and completely immerse it in the cleaning liquid at a temperature of 28°C to 35°C, and take it out after ultrasonic immersion for 4min to 10min;

[0052] Step S2: placing the high-purity quartz product obtained in step S1 in an acid tank containing hydrofluoric acid at a concentration of 4.5% to 5% and a temperature of 20° C. to 40° C., soaking for 1 to 30 minutes and then taking it out;

[0053] S3: placing the high-purity quartz product taken out in step S2 in a pure water overflow tank for overflow cleaning for 1 min to 5 min;

[0054] Step S4: taking out the high-purity quartz product after overflow cleaning from the pure water overflow tank, placing it on a shower table and washing it with pure water;

[0055] Step S5: Dry the high-purity quartz product after washing with pure water using an air gun, wherein the gas used for the air gun drying is helium with a purity of not less than 99.999%.

[0056] The features and performance of the present invention are further described in detail below in conjunction with the embodiments.

[0057] Example 1

[0058] This embodiment provides a method for improving the cleanliness of a high-purity quartz product, comprising the following steps:

[0059] Step S1: Pour 100L of pure water, 4L of OP-10 and 4L of AEO-3 as cleaning liquid into the degreasing tank and stir evenly, place the high-purity quartz product to be treated in the above degreasing tank and immerse it completely in the cleaning liquid at a temperature of 30°C, and take it out after ultrasonic immersion for 4 minutes;

[0060] Step S2: placing the high-purity quartz product obtained in step S1 in an acid tank containing 5% hydrofluoric acid at a temperature of 30° C., soaking for 5 minutes and then taking it out;

[0061] S3: placing the high-purity quartz product taken out in step S2 in a pure water overflow tank for overflow cleaning for 3 minutes;

[0062] Step S4: taking out the high-purity quartz product after overflow cleaning from the pure water overflow tank, placing it on a shower table and washing it with pure water;

[0063] Step S5: Dry the high-purity quartz product after washing with pure water using an air gun, wherein the gas used for the air gun drying is helium with a purity of not less than 99.999%.

[0064] Example 2

[0065] The difference between this embodiment and embodiment 1 is that the cleaning liquid consists of OP-10, AEO-3 and water in a volume ratio of 2:2:100.

[0066] Example 3

[0067] The difference between this embodiment and embodiment 1 is that the cleaning liquid consists of OP-10, AEO-3 and water in a volume ratio of 8:8:100.

[0068] Example 4

[0069] The difference between this embodiment and embodiment 1 is that the cleaning liquid consists of OP-10, AEO-3 and water in a volume ratio of 4:2:100.

[0070] Example 5

[0071] The difference between this embodiment and embodiment 1 is that the cleaning liquid consists of OP-10, AEO-3 and water in a volume ratio of 6:4:100.

[0072] Example 6

[0073] The difference between this embodiment and embodiment 1 is that the cleaning liquid consists of OP-10, AEO-3 and water in a volume ratio of 8:2:100.

[0074] Example 7

[0075] The difference between this embodiment and embodiment 1 is that the cleaning liquid consists of OP-10, AEO-3 and water in a volume ratio of 4:8:100.

[0076] Example 8

[0077] This embodiment provides a method for improving the cleanliness of a high-purity quartz product, comprising the following steps:

[0078] Step S1: Pour the cleaning solution (same as in Example 1) into the degreasing tank and stir evenly, place the high-purity quartz product to be treated in the degreasing tank and completely immerse it in the cleaning solution at a temperature of 28°C, and take it out after ultrasonic immersion for 10 minutes;

[0079] Step S2: placing the high-purity quartz product obtained in step S1 in an acid tank containing hydrofluoric acid with a concentration of 4.5% and a temperature of 20° C., soaking for 30 minutes and then taking it out;

[0080] S3: placing the high-purity quartz product taken out in step S2 in a pure water overflow tank for overflow cleaning for 1 minute;

[0081] Step S4: taking out the high-purity quartz product after overflow cleaning from the pure water overflow tank, placing it on a shower table and washing it with pure water;

[0082] Step S5: Dry the high-purity quartz product after washing with pure water using an air gun, wherein the gas used for the air gun drying is helium with a purity of not less than 99.999%.

[0083] Example 9

[0084] This embodiment provides a method for improving the cleanliness of a high-purity quartz product, comprising the following steps:

[0085] Step S1: Pour the cleaning solution (same as in Example 1) into the degreasing tank and stir evenly, place the high-purity quartz product to be treated in the degreasing tank and completely immerse it in the cleaning solution at a temperature of 35°C, and take it out after ultrasonic immersion for 6 minutes;

[0086] Step S2: placing the high-purity quartz product obtained in step S1 in an acid tank containing 5% hydrofluoric acid at a temperature of 40° C., soaking for 1 minute and then taking it out;

[0087] S3: placing the high-purity quartz product taken out in step S2 in a pure water overflow tank for overflow cleaning for 5 minutes;

[0088] Step S4: taking out the high-purity quartz product after overflow cleaning from the pure water overflow tank, placing it on a shower table and washing it with pure water;

[0089] Step S5: Dry the high-purity quartz product after washing with pure water using an air gun, wherein the gas used for the air gun drying is helium with a purity of not less than 99.999%.

[0090] Example 10

[0091] The difference between this embodiment and embodiment 1 is that step S3 is not performed, and the high-purity quartz product taken out in step S2 is directly performed in step S4.

[0092] Comparative Example 1

[0093] This comparative example provides a method for improving the cleanliness of a quartz product, comprising the following steps:

[0094] Step S1: Place the quartz product to be treated on the shower table, spray alcohol on the surface of the sample, wipe the surface with a dust-free cloth, and then rinse;

[0095] Step S2: Soak a sponge with washing powder or detergent solution, evenly wipe the quartz product rinsed in step S1 for 5 minutes, and then rinse with pure water;

[0096] Step S3: Place the quartz product rinsed and cleaned in step S2 into an acid tank containing 5% hydrofluoric acid at a temperature of 30° C., soak for 5 minutes, and then take it out;

[0097] Step S4: placing the high-purity quartz product taken out in step S3 in a pure water overflow tank for overflow cleaning for 3 minutes;

[0098] Step S5: taking out the high-purity quartz product after overflow cleaning from the pure water overflow tank, placing it on a shower table and washing it with pure water;

[0099] Step S6: Dry the high-purity quartz product after washing with pure water using an air gun, wherein the gas used for the air gun drying is helium with a purity of not less than 99.999%.

[0100] Comparative Example 2

[0101] The difference between this comparative example and Example 1 is that OP-7 is used in an equal amount to replace OP-10.

[0102] Comparative Example 3

[0103] The difference between this comparative example and Example 1 is that AEO-7 is used in an equal amount to replace AEO-3.

[0104] Test example

[0105] Taking Examples 1 to 3, Examples 8 to 10 and Comparative Examples 1 to 3 as examples, the corresponding water cost, yield, cleaning efficiency and degreasing conditions are compared, and the results are shown in Table 1. Figure 1 and Figure 2 The degreasing condition is characterized by subjecting the treated high-purity quartz product to a high-temperature treatment (temperature of 2300°C, time of 0.1h) and observing the pitting and devitrification points on the surface of the product after the high-temperature treatment.

[0106] Table 1 Comparison results

[0107]

[0108] Take Example 1 and Comparative Example 1 as examples for analysis:

[0109] ①, the water cost for degreasing and washing the quartz products provided in Comparative Example 1 is 1.53 yuan / piece, and the water cost for degreasing and washing the quartz products provided in Example 1 is 1.33 yuan / piece. The water cost for a single quartz product in Example 1 is 0.2 yuan lower than that in Comparative Example 1;

[0110] ②, the quartz product degreasing and cleaning link provided in Comparative Example 1 had scratches on the product, and the yield rate was 97%, while the quartz product degreasing and cleaning link provided in Example 1 had a yield rate of 100%, and no product was scratched or scrapped;

[0111] ③. The cleaning efficiency of the quartz product degreasing and cleaning link provided in Comparative Example 1 is 30 minutes / piece, and the cleaning efficiency of the quartz product degreasing and cleaning link provided in Example 1 is 26 minutes / piece, and multiple products can be degreased at one time;

[0112] ④. Combination Figure 1 After high temperature treatment, a large number of pitting and devitrification points appeared on the surface of the high-purity quartz product treated in Comparative Example 1, indicating that the method of Comparative Example 1 did not achieve the effect of complete degreasing; combined with Figure 2 After high-temperature treatment, the surface of the high-purity quartz product treated in Example 1 is bright and has no devitrification points, indicating that the quartz product degreasing and cleaning method provided in Example 1 can achieve complete degreasing of the product surface.

[0113] Furthermore, it can be seen from the comparison between Example 1 and Comparative Examples 2 to 3 that when the components in the cleaning solution are changed, the water cost, yield, cleaning efficiency and degreasing conditions will change.

[0114] In summary, the method for improving the cleanliness of high-purity quartz products provided by the present invention is simple to operate, highly efficient, uses less water, and has a low cost. It can not only clean the dead corners of products with strange shapes, but also avoid scratching the products during the cleaning process, resulting in the scrapping of the products.

[0115] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for improving the cleanliness of high-purity quartz products, characterized in that: The following steps are involved: The high-purity quartz product to be cleaned is immersed in the cleaning solution for the first time, then immersed in the acid solution for the second time, and then cleaned with water; The cleaning solution is composed of OP-10, AEO-3 and water in a volume ratio of (2-8):(2-8):

100.

2. The method according to claim 1, characterized in that The cleaning solution is composed of OP-10, AEO-3 and water in a volume ratio of (4-8):(2-4):

100.

3. The method according to claim 1, characterized in that The temperature of the first soaking is 28°C to 35°C, and the time of the first soaking is 4min to 10min.

4. The method according to claim 1, characterized in that: The temperature of the second soaking is 20°C to 40°C, and the time of the second soaking is 1min to 30min.

5. The method according to claim 4, characterized in that The acid solution used for the second immersion is hydrofluoric acid with a concentration of 4.5% to 5%.

6. The method according to claim 1, characterized in that Cleaning with water includes: firstly performing overflow cleaning in a pure water overflow tank, and then rinsing with pure water.

7. The method according to claim 6, characterized in that The overflow cleaning time is 1min to 5min.

8. The method according to claim 1, characterized in that Also includes: The product obtained by washing with water is dried.

9. The method according to claim 8, characterized in that Drying is carried out by air gun drying.

10. The method according to claim 9, characterized in that The gas used for air gun drying is helium with a purity of not less than 99.999%.

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