A liquid surface anti-shake quartz crucible and its preparation method and application

By forming a quartz sand belt on the inner wall of the quartz crucible, the problem of silicon liquid level jitter is solved, and the whole rod rate of single crystal silicon rods is improved.

CN120328841BActive Publication Date: 2025-10-03MEIJING MATERIAL (ZHEJIANG) CO LTD
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Patent Information

Application Number
CN202510796603.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-06-16
Publication Date
2025-10-03
Estimated Expiration
2045-06-16

AI Technical Summary

Technical Problem

During the crystal pulling process, the traditional quartz crucible generates silicon monoxide gas due to the reaction between the silicon liquid and the quartz crucible, which causes the silicon liquid level to vibrate and thus causes the crystal rod dislocation problem.

Method used

A quartz sand belt is formed on the straight wall area of ​​the quartz crucible, and a quartz sand belt is formed on the inner wall by arc melting and sandblasting, ensuring that the upper surface of the quartz sand belt is above the crystal pulling liquid level line and the lower surface is below the crystal pulling liquid level line to facilitate the overflow of silicon monoxide gas.

Benefits of technology

The gas overflowing from the silicon liquid surface is reduced, the liquid surface shaking is avoided, and the whole rod rate of the single crystal silicon rod is improved.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses a liquid level anti-shake quartz crucible and its preparation method and application, which belong to the field of quartz crucible technology. The preparation of the liquid level anti-shake quartz crucible includes: arc melting the quartz crucible body formed in the mold, sandblasting the straight wall position of the quartz crucible body in the rotating state to form a quartz sand belt on the circumferential inner wall of the quartz crucible body, followed by cooling and demolding; the upper and lower surfaces of the quartz sand belt are respectively located above and below the preset crystal pulling liquid level line. The above method is simple and easy to operate. The quartz sand belt in the prepared liquid level anti-shake quartz crucible has fine gaps, which can make the silicon monoxide gas generated by the reaction during the crystal pulling process overflow from these fine gaps, reduce the gas overflowing from the silicon liquid surface, thereby improving or avoiding the liquid level shaking caused by the gas overflowing from the silicon liquid surface, and thus helping to improve the whole rod rate of single crystal silicon rods during the crystal pulling process.
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Description

Technical Field

[0001] The present invention relates to the technical field of quartz crucibles, and in particular to a liquid surface anti-shake quartz crucible and a preparation method and application thereof. Background Art

[0002] The inner surface of traditional quartz crucibles is not treated in any way other than etching and cold coating to ensure a clean crucible surface. During the crystal pulling process, silicon liquid reacts with the quartz crucible (SiO2) to produce silicon monoxide gas. As this gas escapes from the silicon liquid surface, it causes the silicon liquid surface to vibrate, which often leads to dislocations in the crystal ingot. Therefore, to reduce the risk of liquid surface vibration during the crystal pulling process, it is necessary to treat the inner surface of the quartz crucible with anti-vibration treatment.

[0003] In view of this, the present invention is proposed. Summary of the Invention

[0004] The object of the present invention is to provide a liquid surface anti-shake quartz crucible and a preparation method and application thereof, so as to solve or improve the above-mentioned technical problems.

[0005] The present invention can be achieved like this:

[0006] In a first aspect, the present invention provides a method for preparing a liquid surface anti-shake quartz crucible, comprising the following steps: arc melting a quartz crucible body formed in a mold, sandblasting the straight wall of the rotating quartz crucible body to form a quartz sand belt on the circumferential inner wall of the quartz crucible body, followed by cooling and demolding;

[0007] 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.

[0008] In an optional embodiment, the forming of the quartz crucible body includes: pouring high-purity quartz sand into a rotating mold for laying and forming;

[0009] Among them, the rotation speed of the mold is 50r / min~120r / min.

[0010] In an alternative embodiment, the inner diameter of the mold is between 18 inches and 40 inches.

[0011] In an optional embodiment, the arc melting current is 1000A~5000A.

[0012] In an optional embodiment, the sandblasting is performed 15 minutes to 40 minutes after the arc melting.

[0013] In an optional embodiment, the sandblasting process includes at least one of the following features:

[0014] Feature 1: The purity of the quartz sand used for sandblasting is not less than 99.9999%;

[0015] Feature 2: The particle size of the quartz sand used for sandblasting is 300μm~500μm;

[0016] Feature 3: During the sandblasting process, the rotation speed of the quartz crucible body is 50r / min~120r / min;

[0017] Feature 4: The sandblasting time is 30s~100s;

[0018] Feature 5: The distance between the sandblasting nozzle and the upper port of the mold is 50mm~200mm;

[0019] Feature 6: The distance between the sandblasting nozzle and the inner wall of the quartz crucible body is 30mm~50mm.

[0020] In an optional embodiment, post-processing is further included after demoulding; the post-processing includes edge cutting, pickling and etching, rinsing and drying.

[0021] In a second aspect, the present invention provides a liquid level anti-shake quartz crucible, which is prepared by the preparation method of any one of the aforementioned embodiments.

[0022] In an optional embodiment, the liquid level anti-shake quartz crucible has at least one of the following features:

[0023] Feature 7: The width of the quartz sand belt is 30mm~110mm;

[0024] Feature 8: The thickness of the quartz sand belt is 1mm~1.5mm;

[0025] Feature 9: The roughness of the quartz sand belt is 7μm~23μm;

[0026] Feature 10: The porosity of the quartz sand belt is 30%~60%;

[0027] Feature 11: The pore size of the quartz sand belt is 43μm~104μm.

[0028] In a third aspect, the present invention provides a use of a liquid level anti-shake quartz crucible according to the aforementioned embodiment in preparing single crystal silicon rods.

[0029] In a fourth aspect, the present invention provides a single crystal silicon rod, which is prepared by the liquid level anti-shake quartz crucible of the aforementioned embodiment.

[0030] The beneficial effects of the present invention include:

[0031] The preparation method of the liquid level anti-shake 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 level anti-shake quartz crucible is formed with a quartz sand belt. The quartz sand belt has fine gaps, which can allow the silicon monoxide gas generated by the reaction during the crystal pulling process to overflow from these fine gaps, reducing the gas overflowing from the silicon liquid surface, thereby improving or avoiding the liquid level shaking caused by the gas overflowing from the silicon liquid surface, and further helping to improve the whole rod rate of single crystal silicon rods during the crystal pulling process. DETAILED DESCRIPTION

[0032] To make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are described clearly and completely below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer are used. Where the manufacturer of the reagents or instruments is not specified, all are conventional products that can be purchased commercially.

[0033] The liquid level anti-shake quartz crucible provided by the present invention and its preparation method and application are described in detail below.

[0034] The present invention provides a method for preparing a liquid surface anti-shake quartz crucible, which comprises the following steps: arc melting a quartz crucible body formed in a mold, sandblasting 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;

[0035] 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.

[0036] During the high-temperature melting process of the quartz crucible body, the quartz sand used to form the quartz abrasive belt is sprayed onto specific locations on the vertical wall of the rotating and molten quartz crucible body. The quartz sand particles adhere to and fuse to the inner surface of the quartz crucible body, forming a quartz abrasive belt with quartz particles and numerous fine voids. Furthermore, the quartz sand injected into the quartz crucible body during the high-temperature melting process is a one-step process, which does not alter the composition of the transparent layer or the number of bubbles in the quartz crucible body. Furthermore, there is no hard contact, and no damage to the quartz crucible.

[0037] The "crystal pulling liquid level line" herein 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 the width can make the preset crystal pulling liquid level line within the width range of the quartz sand belt. Through the setting of the 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 small gaps 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 jitter caused by the gas overflowing from the silicon liquid surface, and further facilitating the improvement of the whole rod rate of the single crystal silicon rod during the crystal pulling process.

[0038] In some optional embodiments, the forming of the quartz crucible body includes: pouring high-purity quartz sand into a rotating mold for laying and forming.

[0039] 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.

[0040] The rotation speed of the mold can be 50 r / min~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, or other values ​​within the range of 50 r / min~120 r / min.

[0041] In some optional 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 set according to actual needs.

[0042] The layer structure of the quartz crucible body in the present invention can be understood as similar to that of quartz crucibles in the prior art. For example, in some optional embodiments, the quartz crucible body can include a bubble layer and a transparent layer. In other optional embodiments, the quartz crucible body can also be provided with auxiliary layers or protective layers as needed, such as a silicon carbide protective layer. In other words, the improvement of the present invention over the prior art quartz crucible lies in the newly provided quartz sand belt on the circumferential inner wall of the straight wall area.

[0043] In some optional embodiments, the arc melting current can be 1000A~5000A, such as 1000A, 1500A, 2000A, 2500A, 3000A, 3500A, 4000A, 4500A or 5000A, or other values ​​within the range of 1000A~5000A.

[0044] If the arc melting current is less than 1000A, the outer diameter of the crucible may be too small, and the synthetic quartz sand may not easily adhere to the inner surface of the crucible. If the arc melting current is greater than 5000A, the outer diameter of the crucible may be too large.

[0045] In some optional embodiments, the sandblasting is performed after arc melting for 15 min to 40 min (such as 15 min, 20 min, 25 min, 30 min, 35 min or 40 min, etc.).

[0046] If sandblasting is performed within 15 minutes of arc melting, the size of the prepared liquid surface anti-shake quartz crucible will be too small; if sandblasting is performed after 40 minutes of arc melting, the size of the prepared liquid surface anti-shake quartz crucible will be too large.

[0047] In the present invention, the sandblasting treatment involves spraying quartz sand circumferentially onto the straight walls of the quartz crucible body. 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, or other values ​​within the range of 300 μm to 500 μm.

[0048] If the particle size of the quartz sand used to form the quartz sand belt is less than 300 μm, the porosity will be too low and the pore size will be too small; if the particle size of the quartz sand used to form the quartz sand belt is greater than 500 μm, the quartz sand will not easily adhere to the inner surface of the crucible, and the porosity will be too high and the pore size will be too large.

[0049] In some optional embodiments, during the sandblasting process, 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, 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 process, it will be difficult for sand to stick to the mold, and the crucible will be difficult to form. If the rotation speed of the quartz crucible body is too fast during the sandblasting process, the quartz sand will be thrown out of the mold, and the crucible will be difficult to form.

[0050] In some optional embodiments, the time of sandblasting can be 30s~100s, such as 30s, 40s, 50s, 60s, 70s, 80s, 90s or 100s, etc., or other values ​​within the range of 30s~100s. By controlling the time of sandblasting to 30s~100s, the thickness of the quartz sand belt can be made within the range of 1mm~1.5mm. If the time of sandblasting is shorter than 30s, the thickness of the quartz sand belt will be too thin, and it will be difficult to effectively achieve the effect of silicon monoxide gas overflowing; if the time of sandblasting is longer than 100s, the thickness of the quartz sand belt will be too thick, and some quartz sand in the quartz sand belt may fall off during later use.

[0051] In some optional embodiments, the distance between the sandblasting nozzle and the upper end 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, or other values ​​within the range of 50 mm to 200 mm. Controlling this distance allows the quartz sand belt to be optimally positioned within the height range of the liquid level anti-shake quartz crucible, thereby meeting the requirements of the upper surface of the quartz sand belt being above the preset crystal pulling liquid level and the lower surface of the quartz sand belt being below the preset crystal pulling liquid level.

[0052] In some optional embodiments, the distance between the sandblasting nozzle 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, or other values ​​within the range of 30 mm to 50 mm. Control of this distance primarily affects the width of the quartz sand belt. If the distance is too short, the width of the quartz sand belt may be too narrow, making it difficult to effectively overflow the silicon monoxide gas. Furthermore, the inner wall of the quartz crucible body may be damaged during the sandblasting process. If the distance is too long, the width of the quartz sand belt may be too wide, which is not conducive to crystal pulling. Furthermore, the quartz sand may be sprayed onto other locations and areas of the quartz crucible body, thereby affecting the crystal pulling effect.

[0053] Furthermore, after demoulding, a post-processing process may be further included. For example, the post-processing may include, but is not limited to, edge cutting, pickling and etching, rinsing and drying.

[0054] The specific methods of the above-mentioned post-processing can be referred to the relevant existing technologies, and will not be elaborated or limited here.

[0055] Correspondingly, the present invention also provides a liquid level anti-shake quartz crucible, which is prepared by the above-mentioned preparation method.

[0056] In some preferred embodiments, the center position of the quartz sand belt is located within the range of -10 mm from the preset crystal pulling liquid level line to +10 mm from the preset crystal pulling liquid level line, which can achieve a better anti-shake effect.

[0057] In some optional 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, or other values ​​within the range. If the width of the quartz sand belt is too narrow, it will be difficult to effectively release the silicon monoxide gas; if the width of the quartz sand belt is too wide, it will be difficult to pull the crystal.

[0058] In some optional embodiments, the thickness of the quartz abrasive 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, or other values ​​within the range of 1 mm to 1.5 mm. If the thickness of the quartz abrasive belt is too thin, it will not be able to effectively release the silicon monoxide gas. If the thickness of the quartz abrasive belt is too thick, it may cause the quartz abrasive belt to fall off during later use.

[0059] In some optional 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, or other values ​​within the range. Preferably, the roughness of the quartz sand belt can be 12 μm to 23 μm. This roughness helps increase friction on the crucible wall and reduce vertical fluctuations of the liquid surface.

[0060] In some optional embodiments, the porosity of the quartz sand belt is 30% to 60%.

[0061] In some optional embodiments, the pores in the quartz sand belt have a pore diameter of 43 μm to 104 μm.

[0062] In addition, the present invention also provides an application of the above-mentioned liquid level anti-shake quartz crucible in the preparation of single crystal silicon rods, which can improve the whole rod rate of single crystal silicon rods.

[0063] Correspondingly, the present invention also provides a single crystal silicon rod prepared from the above-mentioned liquid level anti-shake quartz crucible. The single crystal silicon rod has a high whole rod rate.

[0064] The features and performance of the present invention are further described in detail below with reference to the embodiments.

[0065] Example 1

[0066] This embodiment provides a liquid level anti-shake quartz crucible, and the preparation method thereof is as follows:

[0067] S1: Prepare the quartz crucible body.

[0068] High-purity quartz sand was poured into a rotating mold and laid under vacuum. The quartz crucible body consisted of a transparent layer and a bubble layer, from the inside out. The total thickness of the transparent and bubble layers was 60 mm, and the vacuum time was 8 minutes. The quartz sand used to prepare the transparent layer had a purity of 99.9999% and a particle size of 300 μm; the quartz sand used to prepare the bubble layer had a purity of 99.9999% and a particle size of 300 μm. The mold rotated at a speed of 100 rpm. The mold had an inner diameter of 32 inches.

[0069] S2: Arc melting the quartz crucible body.

[0070] Among them, the arc melting current is 3000A.

[0071] S3: performing sandblasting on the vertical wall of the rotating quartz crucible body.

[0072] The sandblasting process was performed 30 minutes after arc melting, with the quartz crucible rotating at a speed of 100 rpm. The quartz sand used for sandblasting had a purity of 99.9999% and a particle size of 300 μm to 500 μm. The distance between the sandblasting nozzle and the upper port of the mold was 100 mm, and the distance between the nozzle and the inner wall of the quartz crucible was 40 mm. The sandblasting time was 50 seconds.

[0073] S4: Cooling and demoulding.

[0074] After the sandblasting is completed, keep it in an upright rotating state for 10 minutes before demoulding.

[0075] S5: Post-processing.

[0076] After demoulding, the edge material is cut, pickled and etched, rinsed and dried.

[0077] Example 2

[0078] This embodiment provides a liquid level anti-shake quartz crucible, and the preparation method thereof is as follows:

[0079] S1: Prepare the quartz crucible body.

[0080] High-purity quartz sand was poured into a rotating mold and laid under vacuum. The quartz crucible body consisted of a transparent layer and a bubble layer, from the inside out. The total thickness of the transparent and bubble layers was 60 mm, and the vacuum time was 8 minutes. The quartz sand used to prepare the transparent layer had a purity of 99.9999% and a particle size of 300 μm; the quartz sand used to prepare the bubble layer had a purity of 99.9999% and a particle size of 300 μm. The mold rotated at a speed of 50 rpm. The mold had an inner diameter of 18 inches.

[0081] S2: Arc melting the quartz crucible body.

[0082] Among them, the arc melting current is 1000A.

[0083] S3: performing sandblasting on the vertical wall of the rotating quartz crucible body.

[0084] Sandblasting was performed 15 minutes after arc melting, with the quartz crucible rotating at a speed of 50 rpm. The quartz sand used for sandblasting had a purity of 99.9999% and a particle size of 300 μm to 500 μm. The distance between the sandblasting nozzle and the upper port of the mold was 50 mm, and the distance between the nozzle and the inner wall of the quartz crucible was 30 mm. The sandblasting time was 30 seconds.

[0085] S4: Cooling and demoulding.

[0086] After the sandblasting is completed, keep it in an upright rotating state for 5 minutes before demoulding.

[0087] S5: Post-processing.

[0088] After demoulding, the edge material is cut, pickled and etched, rinsed and dried.

[0089] Example 3

[0090] This embodiment provides a liquid level anti-shake quartz crucible, and the preparation method thereof is as follows:

[0091] S1: Prepare the quartz crucible body.

[0092] High-purity quartz sand is poured into a rotating mold and laid under vacuum. The quartz crucible body consists of a transparent layer and a bubble layer, from the inside out. The total thickness of the transparent and bubble layers is 60 mm, and the vacuum time is 8 minutes. The quartz sand used to prepare the transparent layer has a purity of 99.9999% and a particle size of 300 μm; the quartz sand used to prepare the bubble layer has a purity of 99.9999% and a particle size of 300 μm. The mold rotates at a speed of 120 rpm. The mold has an inner diameter of 40 inches.

[0093] S2: Arc melting the quartz crucible body.

[0094] Among them, the arc melting current is 5000A.

[0095] S3: performing sandblasting on the vertical wall of the rotating quartz crucible body.

[0096] The sandblasting process was performed 40 minutes after arc melting, with the quartz crucible rotating at a speed of 120 rpm. The quartz sand used for sandblasting had a purity of 99.9999% and a particle size of 300 μm to 500 μm. The distance between the sandblasting nozzle and the upper port of the mold was 200 mm, and the distance between the nozzle and the inner wall of the quartz crucible was 50 mm. The sandblasting time was 100 seconds.

[0097] S4: Cooling and demoulding.

[0098] After the sandblasting is completed, keep it in an upright rotating state for 10 minutes before demoulding.

[0099] S5: Post-processing.

[0100] After demoulding, the edge material is cut, pickled and etched, rinsed and dried.

[0101] Comparative Example 1

[0102] The difference between this comparative example and Example 1 is that the sandblasting process of S3 is not performed.

[0103] That is, the quartz crucible obtained in this comparative example does not have a quartz sand belt.

[0104] Comparative Example 2

[0105] The difference between this comparative example and Example 1 is that the sandblasting process of S3 is not performed, and the quartz sand at the position of the transparent layer of the quartz crucible body corresponding to the quartz sand belt is replaced with quartz sand used to form the quartz sand belt.

[0106] Comparative Example 3

[0107] The difference between this comparative example and Example 1 is that the particle size of the quartz sand used in the sandblasting treatment is 100 μm to 200 μm.

[0108] Comparative Example 4

[0109] The difference between this comparative example and Example 1 is that the particle size of the quartz sand used in the sandblasting treatment is 600 μm to 700 μm.

[0110] Comparative Example 5

[0111] The difference between this comparative example and Example 1 is that the sandblasting time is 20 s.

[0112] Comparative Example 6

[0113] The difference between this comparative example and Example 1 is that the sandblasting time is 120 s.

[0114] Comparative Example 7

[0115] The difference between this comparative example and Example 1 is that the distance between the sandblasting nozzle and the upper port of the mold is 20 mm.

[0116] Comparative Example 8

[0117] The difference between this comparative example and Example 1 is that the distance between the sandblasting nozzle and the upper port of the mold is 250 mm.

[0118] Comparative Example 9

[0119] The difference between this comparative example and Example 1 is that the distance between the sandblasting nozzle and the inner wall of the quartz crucible body is 20 mm.

[0120] Comparative Example 10

[0121] The difference between this comparative example and Example 1 is that the distance between the sandblasting nozzle and the inner wall of the quartz crucible body is 60 mm.

[0122] Test example

[0123] (1) The width, thickness, roughness, porosity and pore size of the quartz sand belts of the quartz crucibles prepared in Examples 1 to 3 and Comparative Examples 3 to 6 were statistically analyzed. The results are shown in Table 1.

[0124] The roughness is tested according to GB / T 3505, the porosity is tested according to GB / T 5163-2013, and the pore size is measured by mercury intrusion.

[0125] Table 1 Statistical results

[0126]

[0127] (2) Single crystal silicon rods were prepared using the same crystal pulling method using the quartz crucibles provided in Examples 1 to 3 and Comparative Examples 1 to 10. Specifically, the crystal pulling process and conditions included seeding, shoulder placement, shoulder rotation, 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 were compared, and the results are shown in Table 2. The liquid surface jitter was determined by visual observation of the jitter, and the whole rod rate was determined by the percentage of single crystal silicon rods with broken rods in the total number of single crystal silicon rods measured.

[0128] Table 2 Comparison results

[0129]

[0130] As can be seen from Table 2, the liquid level anti-shake quartz crucibles provided in Examples 1 to 3 of the present invention can effectively prevent the shaking of the silicon liquid level during the crystal pulling process, and at the same time can obtain a higher single crystal silicon rod whole rod rate.

[0131] As for the comparative example 4 above, the particle size of the quartz sand used to form the quartz sand belt is too large, resulting in too high a porosity and too large a pore size, which causes part of the quartz sand belt to fall off during later use, thereby resulting in a low whole rod rate.

[0132] In the comparative example 6, the sandblasting time was too long, which resulted in the quartz sand belt being too thick, causing some of the quartz sand in the quartz sand belt to fall off during later use, resulting in a low whole rod rate.

[0133] In the comparative example 10, the distance between the sandblasting nozzle and the inner wall of the quartz crucible body is too long, resulting in the quartz sand belt being too wide, which is not conducive to crystal pulling. On the other hand, it is easy for the quartz sand to be sprayed to other positions and areas of the quartz crucible body, resulting in a decrease in the whole rod rate.

[0134] In summary, the preparation method of the liquid level anti-shake quartz crucible provided by the present invention is simple and easy to operate. The circumferential inner wall of the prepared liquid level anti-shake quartz crucible is formed with a quartz sand belt, and the quartz sand belt has fine gaps, which can allow the silicon monoxide gas produced by the reaction during the crystal pulling process to overflow from these fine gaps, reducing the gas overflowing from the silicon liquid surface, thereby improving or avoiding the liquid level shaking caused by the gas overflowing from the silicon liquid surface, and thus helping to improve the whole rod rate of the single crystal silicon rod during the crystal pulling process and reduce the defect rate of the single crystal silicon rod.

[0135] The foregoing description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations of the present invention are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention are intended to be within the scope of protection of the present invention.

Claims

1. A method for preparing a liquid level anti-shake quartz crucible, characterized in that: The following steps are involved: Arc melting is performed on the quartz crucible body formed in the mold, and sandblasting is performed 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, followed by 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; The sandblasting is performed 15 to 40 minutes after the arc melting, and the arc melting current is 1000A to 5000A. The particle size of the quartz sand used for the sandblasting is 300 μm to 500 μm. During the sandblasting process, the rotation speed of the quartz crucible body is 50 r / min to 120 r / min. The sandblasting time is 30 to 100 seconds. The distance between the sandblasting nozzle and the upper port of the mold is 50 mm to 200 mm. The distance between the sandblasting nozzle and the inner wall of the quartz crucible body is 30 mm to 50 mm. The width of the quartz sand belt is 30 mm to 110 mm; the thickness of the quartz sand belt is 1 mm to 1.5 mm; the roughness of the quartz sand belt is 12 μm to 23 μm; the porosity of the quartz sand belt is 30% to 60%; and the pore diameter of the pores in the quartz sand belt is 43 μm to 104 μm.

2. The preparation method according to claim 1, characterized in that The molding of the quartz crucible body includes: pouring high-purity quartz sand into a rotating mold for laying and molding; Wherein, the rotation speed of the mold is 50r / min~120r / min.

3. The preparation method according to claim 1, characterized in that The purity of the quartz sand used for sandblasting is not less than 99.9999%.

4. The preparation method according to any one of claims 1 to 3, characterized in that After demoulding, post-processing is also included; the post-processing includes edge material cutting, pickling and etching, rinsing and drying.

5. A liquid level anti-shake quartz crucible, characterized in that: The liquid level anti-shake quartz crucible is prepared by the preparation method according to any one of claims 1 to 4.

6. Use of the liquid level anti-shake quartz crucible according to claim 5 in preparing single crystal silicon rods.

7. A single crystal silicon rod, characterized in that: The single crystal silicon rod is prepared from the liquid level anti-shake quartz crucible according to claim 5.

Citation Information

Patent Citations

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