Liquid level anti-shake quartz crucible and preparation method and application thereof
By forming a quartz sand belt on the inner wall of the quartz crucible, the liquid level shaking problem caused by the escape of silicon monoxide gas in the crystal drawing process of the traditional quartz crucible is solved, and the whole rod rate of the single crystal silicon rod is improved and the defect rate is reduced.
Patent Information
- Application Number
- CN202510796603.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-16
- Publication Date
- 2025-07-18
- Estimated Expiration
- 2045-06-16
AI Technical Summary
During the crystal drawing process, traditional quartz crucibles cause silicon liquid surface to shake due to the escape of silicon monoxide gas, which increases the risk of crystal rod dislocation.
Quartz sand belt is formed on the circumferential inner wall of the quartz crucible, and small gaps are formed through arc melting and sandblasting. The position of the quartz sand belt is controlled to overflow silicon monoxide gas and reduce liquid surface shaking.
It effectively reduces gas overflow on the silicon liquid surface, improves the whole rod rate of the single crystal silicon rod during crystal drawing, and reduces the defect rate of the crystal rod.
Smart Images

Figure SMS_1 
Figure SMS_2
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of quartz crucibles, and more particularly, to a liquid surface anti-vibration quartz crucible and its preparation method and application. Background Art
[0002] The inner surface of a traditional quartz crucible is not treated in any way except for etching and cold coating processes to ensure the cleanliness of the inner surface of the crucible. During the crystal pulling production process, silicon liquid reacts with the quartz crucible (SiO2) to generate silicon monoxide gas. During the process of the gas escaping from the silicon liquid surface, it will cause the shaking of the silicon liquid surface, and this shaking often leads to the generation of crystal rod dislocations. Therefore, in order to reduce the risk of liquid surface shaking during crystal pulling, it is very necessary to perform anti-vibration treatment on the inner surface of the quartz crucible.
[0003] In view of this, the present invention is specifically proposed. Summary of the Invention
[0004] The purpose of the present invention is to provide a liquid surface anti-vibration quartz crucible and its preparation method and application to solve or improve the above technical problems.
[0005] The present invention can be implemented as follows: In a first aspect, the present invention provides a preparation method of a liquid surface anti-vibration quartz crucible, including the following steps: arc melting the quartz crucible body formed in a mold, and performing sandblasting treatment on the straight wall position of the rotating quartz crucible body to form a quartz sand belt on the circumferential inner wall of the quartz crucible body, and then cooling and demolding; The upper surface of the quartz sand belt is located above the preset crystal pulling liquid level line, and the lower surface of the quartz sand belt is located below the preset crystal pulling liquid level line.
[0006] In an alternative embodiment, the forming of the quartz crucible body includes: pouring high-purity quartz sand into a rotating mold for laying and forming; Wherein, the rotation speed of the mold is 50 r / min to 120 r / min.
[0007] In an alternative embodiment, the inner diameter of the mold is 18 inches to 40 inches.
[0008] In an alternative embodiment, the current of the arc melting is 1000 A to 5000 A.
[0009] In an alternative embodiment, the sandblasting treatment is performed 15 min to 40 min after the arc melting.
[0010] In an alternative embodiment, the sandblasting treatment includes at least one of the following features: Feature 1: The purity of the quartz sand used for the sandblasting treatment is not less than 99.9999%; Feature 2: The particle size of the quartz sand used for sandblasting is 300 μm to 500 μm; Feature 3: During the sandblasting process, the rotation speed of the quartz crucible body is 50 r / min to 120 r / min; Feature 4: The sandblasting time is 30 s to 100 s; Feature 5: The distance between the nozzle of the sandblasting and the upper port of the mold is 50 mm to 200 mm; Feature 6: The distance between the nozzle of the sandblasting and the inner wall of the quartz crucible body is 30 mm to 50 mm.
[0011] In an alternative embodiment, post-treatment is further included after demolding; the post-treatment includes edge cutting, pickling and etching, rinsing, and drying.
[0012] In a second aspect, the present invention provides a liquid surface anti-vibration quartz crucible, which is prepared by the preparation method of any one of the foregoing embodiments.
[0013] In an alternative embodiment, the liquid surface anti-vibration quartz crucible has at least one of the following features: Feature 7: The width of the quartz sand belt is 30 mm to 110 mm; Feature 8: The thickness of the quartz sand belt is 1 mm to 1.5 mm; Feature 9: The roughness of the quartz sand belt is 7 μm to 23 μm; Feature 10: The porosity of the quartz sand belt is 30% to 60%; Feature 11: The pore diameter of the pores in the quartz sand belt is 43 μm to 104 μm.
[0014] In a third aspect, the present invention provides an application of the liquid surface anti-vibration quartz crucible as described in the foregoing embodiment in the preparation of a single crystal rod.
[0015] In a fourth aspect, the present invention provides a single crystal rod, which is prepared from the liquid surface anti-vibration quartz crucible of the foregoing embodiment.
[0016] The beneficial effects of the present invention include: The preparation method of the liquid surface anti-vibration quartz crucible provided by the present invention is simple and easy to operate. The circumferential inner wall of the straight wall area of the prepared liquid surface anti-vibration quartz crucible is formed with a quartz sand belt, and the quartz sand belt has fine voids, which can enable the silicon monoxide gas generated during the crystal pulling process to overflow from these fine voids, reduce the gas overflowing from the silicon liquid surface, thereby improving or avoiding the liquid surface jitter caused by the gas overflowing from the silicon liquid surface, and further being beneficial to improving the whole rod rate of the single crystal rod during the crystal pulling process. Specific Embodiments
[0017] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. For those not specified in the embodiments, they are carried out according to conventional conditions or conditions recommended by the manufacturer. For reagents or instruments not indicated with the manufacturer, they are all conventional products that can be obtained through commercial purchase.
[0018] The following specifically describes the liquid surface anti-vibration quartz crucible provided by the present invention, its preparation method, and applications.
[0019] The present invention provides a method for preparing a liquid surface anti-vibration quartz crucible, which includes the following steps: arc melting the quartz crucible body formed in the mold, and performing sandblasting on the straight wall position of the rotating quartz crucible body to form a quartz sand belt on the circumferential inner wall of the quartz crucible body, and then cooling and demolding; The upper surface of the quartz sand belt is above the preset crystal pulling liquid level line, and the lower surface of the quartz sand belt is below the preset crystal pulling liquid level line.
[0020] During the high-temperature melting process of the quartz crucible body, by spraying the quartz sand used to form the quartz sand belt onto the rotating and molten straight wall of the quartz crucible body at specific positions, the quartz sand particles used to form the quartz sand belt can adhere to and melt on the inner surface of the quartz crucible body, thereby forming a quartz sand belt with quartz particles and having many fine voids. In addition, spraying the quartz sand used to form the quartz sand belt during the high-temperature melting process of the quartz crucible body is a one-time molding, which will not change the composition and the number of bubbles in the transparent layer of the quartz crucible body, and there is no hard contact, so it will not damage the quartz crucible.
[0021] Herein, the "crystal pulling liquid level line" specifically refers to the liquid level line corresponding to the silicon liquid surface during the crystal pulling process. The present invention creatively forms a quartz sand belt with a certain width on the circumferential inner wall of the straight wall area of the quartz crucible body, and this width can make the preset crystal pulling liquid level line within the width range of this quartz sand belt. Through the setting of this quartz sand belt, during the crystal pulling production process, at least part of the silicon monoxide gas generated by the reaction of the silicon liquid with SiO2 in the quartz crucible can overflow from the fine voids in the quartz sand belt at the edge of the silicon liquid, reducing the gas overflowing from the silicon liquid surface, thereby improving or avoiding the liquid surface shaking situation caused by the gas overflowing from the silicon liquid surface, and further being beneficial to improving the whole rod rate of the single crystal rod during the crystal pulling process.
[0022] In some alternative embodiments, the forming of the quartz crucible body includes: pouring high-purity quartz sand into a rotating mold for laying and forming.
[0023] Among them, the purity of the high-purity quartz sand is preferably not less than 99.9999%, and can be specifically set according to the requirements of each layer of the quartz crucible body.
[0024] The rotational speed of the mold can be 50 r / min to 120 r / min, such as 50 r / min, 60 r / min, 70 r / min, 80 r / min, 90 r / min, 100 r / min, 110 r / min or 120 r / min, etc., or other values within the range of 50 r / min to 120 r / min.
[0025] In some alternative embodiments, the inner diameter of the mold can be 18 inches to 40 inches, such as 18 inches, 20 inches, 24 inches, 30 inches, 36 inches or 40 inches, etc., and can be specifically set according to actual needs.
[0026] The layer structure of the quartz crucible body in the present invention can be understood as the layer structure of the quartz crucible in the prior art. For example, in some alternative embodiments, the quartz crucible body can include a bubble layer and a transparent layer; in some other alternative embodiments, the quartz crucible body can also be provided with some auxiliary layers or protective layers according to needs, such as a silicon carbide protective layer, etc. In other words, the improvement of the present invention compared with the quartz crucible in the prior art lies in the newly provided quartz sand belt on the circumferential inner wall of the straight wall region.
[0027] In some alternative embodiments, the current of the arc melting can be 1000 A to 5000 A, such as 1000 A, 1500 A, 2000 A, 2500 A, 3000 A, 3500 A, 4000 A, 4500 A or 5000 A, etc., or other values within the range of 1000 A to 5000 A.
[0028] If the current of the arc melting is less than 1000 A, it is likely to cause the outer diameter size of the crucible to be too small, and the synthetic quartz sand is not easily adhered to the inner surface of the crucible; if the current of the arc melting is greater than 5000 A, it is likely to cause the outer diameter size of the crucible to be too large.
[0029] In some alternative embodiments, the sandblasting treatment is carried out after 15 min to 40 min (such as 15 min, 20 min, 25 min, 30 min, 35 min or 40 min, etc.) of arc melting.
[0030] If the sandblasting treatment is carried out within 15 min of arc melting, the size of the liquid surface anti-vibration quartz crucible prepared will be too small; if the sandblasting treatment is carried out after 40 min of arc melting, the size of the liquid surface anti-vibration quartz crucible prepared will be too large.
[0031] In the present invention, the sandblasting treatment is to spray quartz sand circumferentially on the straight wall of the quartz crucible body, and the purity of the quartz sand is not less than 99.9999%. The particle size of the quartz sand is 300 μm to 500 μm, such as 300 μm, 350 μm, 400 μm, 450 μm or 500 μm, etc., or other values within the range of 300 μm to 500 μm.
[0032] If the particle size of the quartz sand used to form the quartz sand belt is less than 300 μm, it will result in too low porosity and too small pore diameter; if the particle size of the quartz sand used to form the quartz sand belt is greater than 500 μm, it will cause the quartz sand to be not easily adhered to the inner surface of the crucible, and the porosity is too high and the pore diameter is too large.
[0033] In some alternative embodiments, during the sandblasting treatment, the rotation speed of the quartz crucible body can be 50 r / min to 120 r / min, such as 50 r / min, 60 r / min, 70 r / min, 80 r / min, 90 r / min, 100 r / min, 110 r / min or 120 r / min, etc., or other values within the range of 50 r / min to 120 r / min. If the rotation speed of the quartz crucible body is too slow during the sandblasting treatment, it will be difficult to hang the sand on the mold and the crucible is difficult to be formed; if the rotation speed of the quartz crucible body is too fast during the sandblasting treatment, it will cause the quartz sand to be thrown out of the mold and the crucible is difficult to be formed.
[0034] In some alternative embodiments, the sandblasting treatment time can be 30 s to 100 s, such as 30 s, 40 s, 50 s, 60 s, 70 s, 80 s, 90 s or 100 s, etc., or other values within the range of 30 s to 100 s. By controlling the sandblasting treatment time within 30 s to 100 s, the thickness of the quartz sand belt can be within the range of 1 mm to 1.5 mm. If the sandblasting treatment time is shorter than 30 s, the thickness of the quartz sand belt will be too thin and it is difficult to effectively play the role of overflowing the silicon monoxide gas; if the sandblasting treatment time is longer than 100 s, the thickness of the quartz sand belt will be too thick, and it may cause some quartz sand in the quartz sand belt to fall off during the later use process.
[0035] In some alternative embodiments, the distance between the nozzle of the sandblasting treatment and the upper port of the mold can be 50 mm to 200 mm, such as 50 mm, 80 mm, 100 mm, 120 mm, 150 mm, 180 mm or 200 mm, etc., or other values within the range of 50 mm to 200 mm. The control of this distance can make the quartz sand belt in a better position within the height range of the liquid surface anti-vibration quartz crucible, and further meet the requirement that the upper surface of the quartz sand belt is above the preset crystal pulling liquid level line and the lower surface of the quartz sand belt is below the preset crystal pulling liquid level line.
[0036] In some alternative embodiments, the distance between the nozzle of the sandblasting treatment and the inner wall of the quartz crucible body can be 30 mm to 50 mm, such as 30 mm, 35 mm, 40 mm, 45 mm or 50 mm, etc., or other values within the range of 30 mm to 50 mm. The control of this distance mainly affects the width of the quartz sand belt. If this distance is too short, on the one hand, it is easy to make the width of the quartz sand belt too narrow, making it difficult to effectively play the role of overflowing silicon monoxide gas. On the other hand, it is also easy to cause damage to the inner wall of the quartz crucible body during the sandblasting process. If this distance is too long, on the one hand, it is easy to make the width of the quartz sand belt too wide, which is not conducive to crystal pulling. On the other hand, it is also easy to make the quartz sand spray to other positions and areas of the quartz crucible body, which instead affects the crystal pulling effect.
[0037] Further, after demolding, a post-treatment process may also be included. Exemplarily, the post-treatment may exemplary but non-limitingly include edge cutting, pickling etching, rinsing and drying, etc.
[0038] The specific methods related to the post-treatment above can refer to the relevant prior arts and will not be elaborated and limited too much here.
[0039] Correspondingly, the present invention also provides a liquid surface anti-vibration quartz crucible, which is prepared by the above preparation method.
[0040] In some preferred embodiments, the central position of the quartz sand belt is within the range of -10 mm to +10 mm of the preset crystal pulling liquid level line, and a better anti-vibration effect can be obtained.
[0041] In some alternative embodiments, the width of the quartz sand belt can be 30 mm to 110 mm, such as 30 mm, 40 mm, 50 mm, 60 mm, 70 mm, 80 mm, 90 mm, 100 mm or 110 mm, etc., or other values within the range of 30 mm to 110 mm. If the width of the quartz sand belt is too narrow, it is difficult to effectively play the role of overflowing silicon monoxide gas. If the width of the quartz sand belt is too wide, it is not conducive to crystal pulling.
[0042] In some alternative embodiments, the thickness of the quartz sand belt can be 1 mm to 1.5 mm, such as 1 mm, 1.1 mm, 1.2 mm, 1.3 mm, 1.4 mm or 1.5 mm, etc., or other values within the range of 1 mm to 1.5 mm. If the thickness of the quartz sand belt is too thin, it is difficult to effectively play the role of overflowing silicon monoxide gas. If the thickness of the quartz sand belt is too thick, it may cause the quartz sand belt to fall off during the later use process.
[0043] In some alternative embodiments, the roughness of the quartz sand belt can be 7 μm to 23 μm, such as 7 μm, 10 μm, 15 μm, 20 μm, or 23 μm, etc., or other values within the range of 7 μm to 23 μm. Preferably, the roughness of the quartz sand belt can be 12 μm to 23 μm. The above roughness is beneficial to increasing the frictional force on the crucible wall and weakening the up-and-down fluctuation of the liquid surface.
[0044] In some alternative embodiments, the porosity of the quartz sand belt is 30% to 60%.
[0045] In some alternative embodiments, the pore diameter of the pores in the quartz sand belt is 43 μm to 104 μm.
[0046] In addition, the present invention also provides an application of the above liquid surface anti-vibration quartz crucible in the preparation of single crystal silicon rods, which can improve the whole rod rate of the single crystal silicon rods.
[0047] Correspondingly, the present invention also provides a single crystal silicon rod, which is prepared from the above liquid surface anti-vibration quartz crucible. This single crystal silicon rod has a relatively high whole rod rate.
[0048] The features and properties of the present invention will be further described in detail below in conjunction with examples.
[0049] Example 1 This example provides a liquid surface anti-vibration quartz crucible, and its preparation method is as follows: S1: Prepare the quartz crucible body.
[0050] Pour high-purity quartz sand into a rotating mold and lay and form it under vacuum conditions. The quartz crucible body is composed of a transparent layer and a bubble layer from the inside to the outside (the total thickness of the transparent layer and the bubble layer is 60 mm, and the vacuum time is 8 min). The purity of the quartz sand for preparing the transparent layer is 99.9999%, and the particle size is 300 μm; the purity of the quartz sand for preparing the bubble layer is 99.9999%, and the particle size is 300 μm. The rotation speed of the mold is 100 r / min. The inner diameter of the mold is 32 inches.
[0051] S2: Perform arc melting on the quartz crucible body.
[0052] Among them, the current of the arc melting is 3000 A.
[0053] S3: Perform sandblasting treatment on the straight wall position of the rotating quartz crucible body.
[0054] Among them, the sandblasting treatment is carried out 30 minutes after the arc melting, and the rotation speed of the quartz crucible body is 100 r / min. The purity of the quartz sand used for the sandblasting treatment is 99.9999%, and the particle size is 300 μm to 500 μm. The distance between the nozzle of the sandblasting treatment and the upper port of the mold is 100 mm, the distance between the nozzle and the inner wall of the quartz crucible body is 40 mm, and the time of the sandblasting treatment is 50 s.
[0055] S4: Cooling and demolding.
[0056] After the sandblasting treatment is completed, demolding is carried out after maintaining the upright rotation state for 10 minutes.
[0057] S5: Post-treatment.
[0058] After demolding, edge cutting, pickling etching, rinsing and drying are carried out.
[0059] Example 2 This example provides a liquid surface anti-vibration quartz crucible, and its preparation method is as follows: S1: Prepare the quartz crucible body.
[0060] Pour high-purity quartz sand into the rotating mold and carry out laying and forming under vacuum conditions. The quartz crucible body consists of a transparent layer and a bubble layer from the inside to the outside (the total thickness of the transparent layer and the bubble layer is 60 mm, and the vacuum time is 8 minutes). The purity of the quartz sand for preparing the transparent layer is 99.9999%, and the particle size is 300 μm; the purity of the quartz sand for preparing the bubble layer is 99.9999%, and the particle size is 300 μm. The rotation speed of the mold is 50 r / min. The inner diameter of the mold is 18 inches.
[0061] S2: Carry out arc melting on the quartz crucible body.
[0062] Among them, the current of the arc melting is 1000 A.
[0063] S3: Carry out sandblasting treatment on the straight wall position of the rotating quartz crucible body.
[0064] Among them, the sandblasting treatment is carried out 15 minutes after the arc melting, and the rotation speed of the quartz crucible body is 50 r / min. The purity of the quartz sand used for the sandblasting treatment is 99.9999%, and the particle size is 300 μm to 500 μm. The distance between the nozzle of the sandblasting treatment and the upper port of the mold is 50 mm, the distance between the nozzle and the inner wall of the quartz crucible body is 30 mm, and the time of the sandblasting treatment is 30 s.
[0065] S4: Cooling and demolding.
[0066] After the sandblasting treatment is completed, demolding is carried out after maintaining the upright rotation state for 5 minutes.
[0067] S5: Post-treatment.
[0068] After demolding, perform edge cutting, pickling etching, rinsing, and drying.
[0069] Example 3 This example provides a liquid surface anti-vibration quartz crucible, and its preparation method is as follows: S1: Prepare the quartz crucible body.
[0070] Pour high-purity quartz sand into a rotating mold and lay and form it under vacuum conditions. The quartz crucible body consists of a transparent layer and a bubble layer from the inside to the outside (the total thickness of the transparent layer and the bubble layer is 60 mm, and the vacuum time is 8 min). The purity of the quartz sand for preparing the transparent layer is 99.9999%, and the particle size is 300 μm; the purity of the quartz sand for preparing the bubble layer is 99.9999%, and the particle size is 300 μm. The rotation speed of the mold is 120 r / min. The inner diameter of the mold is 40 inches.
[0071] S2: Perform arc melting on the quartz crucible body.
[0072] Among them, the current of arc melting is 5000 A.
[0073] S3: Perform sandblasting treatment on the straight wall position of the rotating quartz crucible body.
[0074] Among them, the sandblasting treatment is carried out 40 min after arc melting, and the rotation speed of the quartz crucible body is 120 r / min. The purity of the quartz sand used for sandblasting treatment is 99.9999%, and the particle size is 300 μm - 500 μm. The distance between the nozzle of the sandblasting treatment and the upper port of the mold is 200 mm, the distance between the nozzle and the inner wall of the quartz crucible body is 50 mm, and the time of sandblasting treatment is 100 s.
[0075] S4: Cooling and demolding.
[0076] After the sandblasting treatment is completed, keep it in an upright rotating state for 10 min and then demold.
[0077] S5: Post-treatment.
[0078] After demolding, perform edge cutting, pickling etching, rinsing, and drying.
[0079] Comparative Example 1 The difference between this comparative example and Example 1 is that the sandblasting treatment in S3 is not carried out.
[0080] That is, the obtained quartz crucible in this comparative example does not have a quartz sand belt.
[0081] Comparative Example 2 The difference between this comparative example and Example 1 lies in that: the sandblasting treatment in S3 was not carried out, and the quartz sand at the position of the transparent layer of the quartz crucible body corresponding to the quartz sand belt was replaced with the quartz sand used to form the quartz sand belt.
[0082] Comparative Example 3 The difference between this comparative example and Example 1 lies in that: the particle size of the quartz sand used for the sandblasting treatment is 100 μm to 200 μm.
[0083] Comparative Example 4 The difference between this comparative example and Example 1 lies in that: the particle size of the quartz sand used for the sandblasting treatment is 600 μm to 700 μm.
[0084] Comparative Example 5 The difference between this comparative example and Example 1 lies in that: the time of the sandblasting treatment is 20 s.
[0085] Comparative Example 6 The difference between this comparative example and Example 1 lies in that: the time of the sandblasting treatment is 120 s.
[0086] Comparative Example 7 The difference between this comparative example and Example 1 lies in that: the distance between the nozzle of the sandblasting treatment and the upper port of the mold is 20 mm.
[0087] Comparative Example 8 The difference between this comparative example and Example 1 lies in that: the distance between the nozzle of the sandblasting treatment and the upper port of the mold is 250 mm.
[0088] Comparative Example 9 The difference between this comparative example and Example 1 lies in that: the distance between the nozzle of the sandblasting treatment and the inner wall of the quartz crucible body is 20 mm.
[0089] Comparative Example 10 The difference between this comparative example and Example 1 lies in that: the distance between the nozzle of the sandblasting treatment and the inner wall of the quartz crucible body is 60 mm.
[0090] Test Example (1) The width, thickness, roughness, porosity, and pore diameter of the quartz sand belts of the quartz crucibles prepared in Examples 1 to 3 and Comparative Examples 3 to 6 were statistically analyzed, and the results are shown in Table 1.
[0091] Among them, the roughness was tested with reference to "GB / T 3505", the porosity was tested with reference to "GB / T 5163-2013", and the pore diameter was measured by the mercury intrusion method.
[0092] Table 1 Statistical Results
[0093] (2)The single-crystal silicon rods were prepared by using the quartz crucibles provided in Examples 1 to 3 and Comparative Examples 1 to 10 according to the same crystal pulling method. Specifically, the crystal pulling process and conditions included: seed crystal introduction, shoulder release, shoulder turning, equal diameter, and tailing. The liquid surface jitter during the crystal pulling process and the whole rod rate of the single-crystal silicon rods obtained by crystal pulling preparation were compared, and the results are shown in Table 2. Among them, the liquid surface jitter was judged by whether the jitter could be seen visually, and the whole rod rate was calculated as the percentage of the single-crystal silicon rods with broken rods in the total amount of the measured single-crystal silicon rods.
[0094] Table 2 Comparison Results
[0095] As can be seen from Table 2, the liquid surface anti-vibration quartz crucibles provided in Examples 1 to 3 of the present invention can effectively avoid the jitter of the silicon liquid surface during the crystal pulling process, and at the same time, a high whole rod rate of the single-crystal silicon rods can be obtained.
[0096] Regarding the above Comparative Example 4, the particle size of the quartz sand used to form the quartz sand belt was too large, resulting in too high a porosity and too large a pore diameter, causing part of the quartz sand belt to fall off during the later use process, and thus resulting in a lower whole rod rate.
[0097] Regarding the above Comparative Example 6, the sandblasting time was too long, making the thickness of the quartz sand belt too thick, resulting in part of the quartz sand in the quartz sand belt falling off during the later use process, resulting in a lower whole rod rate.
[0098] Regarding the above Comparative Example 10, the distance between the nozzle of the sandblasting treatment and the inner wall of the quartz crucible body was too long, resulting in too wide a width of the quartz sand belt, which was not conducive to crystal pulling. On the other hand, it was also easy to spray the quartz sand to other positions and areas of the quartz crucible body, resulting in a decrease in the whole rod rate.
[0099] In summary, the preparation method of the liquid surface anti-vibration quartz crucible provided by the present invention is simple and easy to operate. The circumferential inner wall of the prepared liquid surface anti-vibration quartz crucible is formed with a quartz sand belt, and the quartz sand belt has fine voids, which can allow the silicon monoxide gas generated during the crystal pulling process to overflow from these fine voids, reducing the gas overflowing from the silicon liquid surface, thereby improving or avoiding the liquid surface jitter caused by the gas overflowing from the silicon liquid surface, and further being beneficial to improving the whole rod rate of the single-crystal silicon rods during the crystal pulling process and reducing the defect rate of the single-crystal silicon rods.
[0100] The above are only the preferred embodiments of the present invention and are not used to limit the present invention. For those skilled in the art, the present invention can have various changes and modifications. Any modifications, equivalent replacements, improvements, 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 preparation method of a liquid surface anti-vibration quartz crucible, characterized in that, It includes the following steps: Arc melt the quartz crucible body formed in the mold, and conduct sandblasting treatment on the straight wall position of the rotating quartz crucible body to form a quartz sand belt on the circumferential inner wall of the quartz crucible body, and then cool and demold; The upper surface of the quartz sand belt is above the preset crystal pulling liquid level line, and the lower surface of the quartz sand belt is below the preset crystal pulling liquid level line.
2. The preparation method according to claim 1, characterized in that, The forming of the quartz crucible body includes: pouring high-purity quartz sand into a rotating mold for laying and forming; Among them, the rotation speed of the mold is 50 r / min to 120 r / min.
3. The preparation method according to claim 1, characterized in that, The current of arc melting is 1000 A to 5000 A.
4. The preparation method according to claim 1, characterized in that, The sandblasting treatment is carried out 15 min to 40 min after arc melting.
5. The preparation method according to claim 1, wherein The sandblasting treatment includes at least one of the following features: Feature 1: The purity of the quartz sand used in the sandblasting treatment is not less than 99.9999%; Feature 2: The particle size of the quartz sand used in the sandblasting treatment is 300 μm to 500 μm; Feature 3: During the sandblasting treatment, the rotation speed of the quartz crucible body is 50 r / min to 120 r / min; Feature 4: The time of the sandblasting treatment is 30 s to 100 s; Feature 5: The distance between the nozzle of the sandblasting treatment and the upper port of the mold is 50 mm to 200 mm; Feature 6: The distance between the nozzle of the sandblasting treatment and the inner wall of the quartz crucible body is 30 mm to 50 mm.
6. The preparation method according to any one of claims 1 to 5, characterized in that, After demolding, it also includes post-treatment; the post-treatment includes edge cutting, pickling and etching, rinsing and drying.
7. A liquid surface anti-vibration quartz crucible, characterized in that, The liquid level anti-vibration quartz crucible is prepared by the preparation method according to any one of claims 1 to 6.
8. The liquid surface anti-vibration quartz crucible according to claim 7, wherein The liquid level anti-vibration quartz crucible has at least one of the following features: Feature 7: The width of the quartz sand belt is 30 mm to 110 mm; Feature 8: The thickness of the quartz sand belt is 1 mm to 1.5 mm; Feature 9: The roughness of the quartz sand belt is 7 μm to 23 μm; Feature 10: The porosity of the quartz sand belt is 30% to 60%; Feature 11: The pore diameter of the pores in the quartz sand belt is 43 μm to 104 μm.
9. Use of a liquid level anti-vibration quartz crucible according to claim 7 or 8 in the preparation of a single crystal silicon rod.
10. A single crystal silicon rod, characterized in that, The single crystal silicon rod is prepared from the liquid level anti-vibration quartz crucible according to claim 7 or 8.
Citation Information
Patent Citations
Process for producing arc quartz crucible by vacuum plus coating, equipment, product thereof
CN101570391A
Quartz crucible production process
CN104445886A
Semiconductor-level quartz crucible and production method thereof
CN109111102A
Quartz crucible and preparation method thereof
CN116730596A
Quartz crucible preparation process, quartz crucible and crystal pulling method
CN118164666A