CN117005020A - A process to improve the early crystallization rate of shoulder expansion and equal diameter of large-sized single crystals - Google Patents
A process to improve the early crystallization rate of shoulder expansion and equal diameter of large-sized single crystals Download PDFInfo
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- CN117005020A CN117005020A CN202210467171.XA CN202210467171A CN117005020A CN 117005020 A CN117005020 A CN 117005020A CN 202210467171 A CN202210467171 A CN 202210467171A CN 117005020 A CN117005020 A CN 117005020A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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Abstract
本发明提供一种提高大尺寸单晶扩肩及等径前期成晶率的工艺,包括:第一扩肩阶段和第二扩肩阶段,第一扩肩阶段中,将埚位从第一位置调整至第二位置处,随后使用第一拉速拉制第一段肩,并在拉制过程中降低温度;第二扩肩阶段中,埚位保持不变,将第一拉速改变至第二拉速,使用第二拉速继续在第一段肩的底部拉制第二段肩,并在拉制过程中继续降低温度,扩肩完成。本发明的有益效果是将现有技术中的只有一段肩分为两段肩进行拉制,增大整个扩肩部分的表面积,从而从物理角度加快了散热速度,增加单晶的散热能力,使单晶生长中的界面翻转过程从等径阶段加快至扩肩阶段中,在扩肩阶段使其完成界面翻转。
The invention provides a process for improving large-size single crystal shoulder expansion and equal-diameter pre-crystallization rate, which includes: a first shoulder expansion stage and a second shoulder expansion stage. In the first shoulder expansion stage, the crucible is moved from the first position to the first shoulder expansion stage. Adjust to the second position, and then use the first drawing speed to draw the first shoulder, and reduce the temperature during the drawing process; in the second shoulder expansion stage, the crucible position remains unchanged, and the first drawing speed is changed to the second shoulder. Second drawing speed, use the second drawing speed to continue drawing the second shoulder section at the bottom of the first shoulder section, and continue to reduce the temperature during the drawing process to complete the shoulder expansion. The beneficial effect of the present invention is that the only one shoulder in the prior art is divided into two shoulders for drawing, thereby increasing the surface area of the entire expanded shoulder part, thereby speeding up the heat dissipation speed from a physical point of view, increasing the heat dissipation capacity of the single crystal, and making the The interface flipping process in single crystal growth is accelerated from the equal diameter stage to the shoulder expansion stage, and the interface flip is completed in the shoulder expansion stage.
Description
技术领域Technical field
本发明属于光伏半导体工艺技术领域,尤其是涉及一种提高大尺寸单晶扩肩及等径前期成晶率的工艺。The invention belongs to the field of photovoltaic semiconductor process technology, and in particular relates to a process for improving the shoulder expansion and equal diameter pre-crystallization rates of large-size single crystals.
背景技术Background technique
在直拉法单晶硅生长的过程中,扩肩(又称放肩)是整个拉晶流程的关键步骤之一,扩肩主要目的是通过降低熔体温度,结合晶体提升拉速,将晶体由籽晶直径放大至保持直径。扩肩工艺不合理将直接导致扩肩断苞或等径前期断苞。In the process of growing single crystal silicon by Czochralski method, shoulder expansion (also called shoulder release) is one of the key steps in the entire crystal pulling process. The main purpose of shoulder expansion is to increase the pulling speed by lowering the melt temperature and combining the crystal with the crystal. Enlarge from seed diameter to maintaining diameter. Unreasonable shoulder expansion technology will directly lead to shoulder expansion and bract breakage or early equal diameter bract breakage.
在大尺寸单晶生长过程中,由于单晶直径大,整体散热能力较常规M2单晶偏弱,出炉单晶生长界面为凸向液面或马鞍状,导致大尺寸单晶扩肩断苞,等径前期断苞比例高。During the growth process of large-sized single crystals, due to the large diameter of the single crystal, the overall heat dissipation capacity is weaker than that of conventional M2 single crystals. The growth interface of the single crystal is convex to the liquid surface or saddle-shaped, resulting in the shoulder expansion and bud breakage of the large-sized single crystal. The proportion of broken bracts is high in the early stage of equal diameter.
发明内容Contents of the invention
本发明要解决的问题是提供一种提高大尺寸单晶扩肩及等径前期成晶率的工艺,有效的解决大尺寸单晶生长过程中,由于单晶直径大,整体散热能力较常规M2单晶偏弱,出炉单晶生长界面为凸向液面或马鞍状,导致大尺寸单晶扩肩断苞,等径前期断苞比例高的问题。The problem to be solved by the present invention is to provide a process for improving the early crystallization rate of shoulder expansion and equal diameter of large-sized single crystals, and effectively solve the problem that during the growth process of large-sized single crystals, due to the large diameter of the single crystals, the overall heat dissipation capacity is higher than that of conventional M2 The single crystal is weak, and the growth interface of the single crystal is convex to the liquid surface or saddle-shaped, which leads to the problem of shoulder expansion and breakage of large-sized single crystals, and a high proportion of breakage in the early stage of equal diameter.
为解决上述技术问题,本发明采用的技术方案是:一种提高大尺寸单晶扩肩及等径前期成晶率的工艺,包括:In order to solve the above technical problems, the technical solution adopted by the present invention is: a process for improving the shoulder expansion and equal diameter pre-crystallization rate of large-sized single crystals, including:
稳温阶段,在稳温过程中将埚位调整至第一位置处;In the temperature stabilization stage, the crucible position is adjusted to the first position during the temperature stabilization process;
扩肩阶段,其包括第一扩肩阶段和第二扩肩阶段,其中,The shoulder expansion stage includes the first shoulder expansion stage and the second shoulder expansion stage, wherein,
所述第一扩肩阶段中,将所述埚位从所述第一位置调整至第二位置处,随后使用第一拉速拉制第一段肩,并在拉制过程中降低温度;In the first shoulder expansion stage, the crucible position is adjusted from the first position to the second position, and then the first shoulder section is drawn using the first drawing speed, and the temperature is lowered during the drawing process;
所述第二扩肩阶段中,所述埚位保持不变,将所述第一拉速改变至第二拉速,使用所述第二拉速继续在所述第一段肩的底部拉制第二段肩,并在拉制过程中继续降低温度,扩肩完成。In the second shoulder expansion stage, the crucible position remains unchanged, the first pulling speed is changed to the second pulling speed, and the second pulling speed is used to continue drawing at the bottom of the first shoulder section. The second shoulder section continues to lower the temperature during the drawing process, and the shoulder expansion is completed.
优选地,所述第一位置为坩埚内的液面距导流筒20-30mm处。Preferably, the first position is a position where the liquid level in the crucible is 20-30 mm away from the guide tube.
优选地,所述第二位置为坩埚内的液面距导流筒15-25mm处。Preferably, the second position is a position where the liquid level in the crucible is 15-25 mm away from the guide tube.
优选地,所述第一拉速范围为50-65mm/h。Preferably, the first pulling speed range is 50-65mm/h.
优选地,所述第二拉速高于所述第一拉速,其范围为70-90mm/h。Preferably, the second pulling speed is higher than the first pulling speed, and is in the range of 70-90mm/h.
优选地,所述第一扩肩阶段中,降低加热器的功率,从而在拉制过程中进行降温,其中,第一功率的降幅范围为7-17kw。Preferably, in the first shoulder expansion stage, the power of the heater is reduced to reduce the temperature during the drawing process, wherein the reduction range of the first power is 7-17kw.
优选地,所述第二扩肩范围中,继续降低加热器的功率,从而进行降温,其中,第二功率的降幅范围为3-8kw。Preferably, in the second shoulder expansion range, the power of the heater is continued to be reduced to perform temperature cooling, wherein the reduction range of the second power is 3-8 kw.
优选地,所述第一段肩的高度为H1,所述第二段肩的高度为H2,其中,所述H1:H2的比例范围为1:1-2:1。Preferably, the height of the first shoulder section is H1, and the height of the second shoulder section is H2, wherein the ratio range of H1:H2 is 1:1-2:1.
采用上述技术方案,将现有技术中的只有一段肩分为两段肩进行拉制,使得两段肩的外表面形成一定角度,增大整个扩肩部分的表面积,从而从物理角度加快了散热速度,增加单晶的散热能力,使单晶生长中的界面翻转过程从等径阶段加快至扩肩阶段中,在扩肩阶段使其完成界面翻转,即单晶的生长界面由凸向液面翻转至凹向液面。Using the above technical solution, the only one shoulder in the prior art is divided into two shoulders for drawing, so that the outer surfaces of the two shoulder sections form a certain angle, increasing the surface area of the entire shoulder expansion part, thereby speeding up heat dissipation from a physical perspective speed, increasing the heat dissipation capacity of the single crystal, accelerating the interface flipping process in the growth of the single crystal from the equal diameter stage to the shoulder expansion stage. In the shoulder expansion stage, it completes the interface flip, that is, the growth interface of the single crystal changes from convex to the liquid surface. Turn over to the concave surface.
采用上述技术方案,通过改变埚位的位置、分段拉制的速度以及降温的功率来确保二段肩的形成,尽可能的避免马鞍状单晶界面的形成,加快单晶生长界面的翻转速度,从而提高大尺寸单晶扩肩及等径前期成晶率,同时能够提高产量。Using the above technical solution, by changing the position of the crucible, the speed of segmented drawing and the power of cooling to ensure the formation of the second shoulder, avoid the formation of a saddle-shaped single crystal interface as much as possible, and speed up the flipping speed of the single crystal growth interface. , thereby improving the early-stage crystallization rate of shoulder expansion and equal diameter of large-size single crystals, and at the same time increasing the output.
附图说明Description of the drawings
图1是本发明实施例一种提高大尺寸单晶扩肩及等径前期成晶率的工艺中扩肩单晶生长界面模拟图Figure 1 is a simulation diagram of the growth interface of a shoulder-expanded single crystal in a process for improving the shoulder-expanding and equal-diameter pre-crystallization rates of large-sized single crystals according to an embodiment of the present invention.
图2是本发明现有技术中单晶生长界面模拟图Figure 2 is a simulation diagram of the single crystal growth interface in the prior art of the present invention.
图中:In the picture:
1、第一段肩2、第二段肩1. The first shoulder section 2. The second shoulder section
具体实施方式Detailed ways
下面结合实施例和附图对本发明作进一步说明:The present invention will be further described below in conjunction with the examples and drawings:
在本发明实施例的描述中,需要理解的是,术语“顶部”、“底部”等指示的方位或位置关系为基于附图所示的方位或位置关系,仅是为了便于描述本发明和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本发明的限制。对于本领域的普通技术人员而言,可以通过具体情况理解上述术语在本发明中的具体含义。In the description of the embodiments of the present invention, it should be understood that the orientation or positional relationship indicated by the terms "top", "bottom", etc. is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the present invention and simplifying it. The description does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operate in a specific orientation, and therefore is not to be construed as a limitation of the invention. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood through specific situations.
一种提高大尺寸单晶扩肩及等径前期成晶率的工艺,包括:A process to improve the early-stage crystallization rate of shoulder expansion and equal diameter of large-size single crystals, including:
S1:稳温阶段,在稳温过程中将埚位调整至第一位置处;S1: Temperature stabilization stage, during the temperature stabilization process, adjust the crucible position to the first position;
埚位即坩埚位位置,在本发明中代表坩埚内的熔融的原料液面距导流筒底部一定距离的位置处,第一位置为坩埚内的液面距导流筒底部20-30mm处,优选为坩埚内的液面距导流筒底部22-28mm处,更优选的为坩埚内的液面距导流筒底部为24mm、25mm、26mm处;The crucible position is the crucible position. In the present invention, it represents the position where the molten raw material liquid level in the crucible is at a certain distance from the bottom of the guide tube. The first position is the position where the liquid level in the crucible is 20-30mm away from the bottom of the guide tube. Preferably, the liquid level in the crucible is 22-28mm from the bottom of the guide tube, and more preferably, the liquid level in the crucible is 24mm, 25mm, or 26mm from the bottom of the guide tube;
相比现有技术中稳温阶段的埚位,降低了5-15mm,能够改变成晶区域,还能够改变肩部形状,同时加快单晶生长界面翻转,使其在扩肩阶段使其完成界面翻转,提高单晶的成晶率;Compared with the existing technology, the crucible position in the temperature stabilization stage is lowered by 5-15mm, which can change the crystallization area and the shape of the shoulder. At the same time, it accelerates the flipping of the single crystal growth interface so that it can complete the interface during the shoulder expansion stage. Flip to improve the crystallization rate of single crystals;
调整埚位至第一位置处后,在此处位置保持不动,直至结束稳温阶段,进入下一扩肩阶段。After adjusting the crucible position to the first position, it remains stationary until the temperature stabilization phase is completed and the next shoulder expansion phase is entered.
S2:扩肩阶段,其包括第一扩肩阶段和第二扩肩阶段,需要说明的是,晶体拉速越低或纵向温度梯度越小,单晶生长界面凸向液面程度越大;晶体拉速越高或纵向温度梯度越大,单晶生长界面凹向液面程度越大,其中,S2: Shoulder expansion stage, which includes the first shoulder expansion stage and the second shoulder expansion stage. It should be noted that the lower the crystal pulling speed or the smaller the longitudinal temperature gradient, the greater the degree of the single crystal growth interface convex to the liquid surface; the crystal The higher the pulling speed or the greater the longitudinal temperature gradient, the greater the concaveness of the single crystal growth interface toward the liquid surface, where,
S21:第一扩肩阶段中,将埚位从所述第一位置调整至第二位置处,随后使用第一拉速拉制第一段肩1,并在拉制过程中降低温度;S21: In the first shoulder expansion stage, adjust the crucible position from the first position to the second position, and then use the first drawing speed to draw the first shoulder section 1, and reduce the temperature during the drawing process;
埚位与S1中的含义一致,埚位的第二位置为坩埚内的液面距导流筒底部15-25mm处,优选为坩埚内的液面距导流筒底部17-23mm处,更优选的为坩埚内的液面距导流筒底部的18mm、19mm、20mm、21mm、22mm处;The meaning of the crucible position is consistent with that in S1. The second position of the crucible position is 15-25mm from the liquid level in the crucible to the bottom of the flow guide tube, preferably 17-23mm from the bottom of the flow guide tube to the liquid level in the crucible, more preferably are 18mm, 19mm, 20mm, 21mm, and 22mm from the liquid level in the crucible to the bottom of the guide tube;
当坩埚位置从第一位置移动至第二位置处时,开始拉制单晶,使用第一拉速拉制第一段肩1,其中,第一拉速范围为50-65mm/h,优选范围为55-60mm/h,更优选的,第一拉速为56mm/h、57mm/h、58mm/h、59mm/h;When the crucible position moves from the first position to the second position, start pulling the single crystal, and use the first pulling speed to pull the first shoulder 1, where the first pulling speed range is 50-65mm/h, and the preferred range is is 55-60mm/h, more preferably, the first pulling speed is 56mm/h, 57mm/h, 58mm/h, 59mm/h;
相较现有技术中,第一扩肩阶段中的拉速变化较小,基本不变,正常拉制第一段肩1;Compared with the existing technology, the drawing speed in the first shoulder expansion stage changes slightly and is basically unchanged, and the first shoulder 1 is drawn normally;
在第一扩肩阶段中需要降低拉晶温度,本发明中采用的降温方法为降低加热器的功率,从而在拉制过程中进行降温,其中,In the first shoulder expansion stage, the crystal pulling temperature needs to be lowered. The cooling method used in the present invention is to reduce the power of the heater to cool down during the drawing process, where,
第一功率的降幅范围为7-17kw,优选为10-15kw,更优选为11kw、12kw、13kw、14kw;相较于现有技术,功率的降幅提高了2-5kw,即降低了更多的加热器功率,使得单晶炉内温度更低;The first power reduction range is 7-17kw, preferably 10-15kw, more preferably 11kw, 12kw, 13kw, 14kw; compared with the existing technology, the power reduction range is increased by 2-5kw, that is, more power is reduced The heater power makes the temperature in the single crystal furnace lower;
拉制第一段肩1的肩长至H1时,第一扩肩阶段结束;When the shoulder length of the first section of shoulder 1 is drawn to H1, the first shoulder expansion stage ends;
肩长即为肩部的高度,在本发明中代表肩的顶部至底部的最短距离,即垂直距离,一般的,H1为总体肩长的二分之一到三分之一之间,优选为总体肩长的35-45%,更优选的,为总体肩长的40%;The shoulder length is the height of the shoulder. In the present invention, it represents the shortest distance from the top to the bottom of the shoulder, that is, the vertical distance. Generally, H1 is between one-half and one-third of the overall shoulder length, preferably 35-45% of the overall shoulder length, more preferably 40% of the overall shoulder length;
S22:第二扩肩阶段中,埚位保持不变,将第一拉速改变至第二拉速,使用第二拉速继续在第一段肩的底部拉制第二段肩2,并在拉制过程中继续降低温度,扩肩完成;S22: In the second shoulder expansion stage, the crucible position remains unchanged, change the first pulling speed to the second pulling speed, use the second pulling speed to continue drawing the second shoulder 2 at the bottom of the first shoulder, and During the drawing process, the temperature continues to be lowered and the shoulder expansion is completed;
埚位与S1中的含义一致,在第二扩肩阶段中保持埚位的第二位置不变,与步骤S21一致,坩埚内的液面距导流筒底部15-25mm处,优选为坩埚内的液面距导流筒底部17-23mm处,更优选的为坩埚内的液面距导流筒底部的18mm、19mm、20mm、21mm、22mm处;The meaning of the crucible position is consistent with S1. In the second shoulder expansion stage, the second position of the crucible position is kept unchanged, consistent with step S21. The liquid level in the crucible is 15-25mm from the bottom of the guide tube, preferably inside the crucible. The liquid level in the crucible is 17-23mm from the bottom of the guide tube, and more preferably, the liquid level in the crucible is 18mm, 19mm, 20mm, 21mm, or 22mm from the bottom of the guide tube;
在第一段肩1的底部继续拉制第二段肩2,使用第二拉速拉制第二段肩2,其中,第二拉速高于第一拉速,其范围为70-90mm/h,优选范围为75-85mm/h,更优选的为78mm/h、79mm/h、80mm/h、81mm/h、82mm/h、83mm/h;Continue to draw the second shoulder 2 at the bottom of the first shoulder 1, and use the second drawing speed to draw the second shoulder 2. The second drawing speed is higher than the first drawing speed, and its range is 70-90mm/ h, the preferred range is 75-85mm/h, more preferably 78mm/h, 79mm/h, 80mm/h, 81mm/h, 82mm/h, 83mm/h;
相较现有技术,第二拉速提高了0-40mm/h,在第二扩肩过程中加快拉速能够改变肩部形状,如图1和图2所示,使第一段肩1与第二段肩2之间形成一个夹角,该夹角的角度一般为150-180°(不包括180°),并且在第二段肩2内能够加快界面翻转,将单晶的生长界面翻转过来,由凸向液面转变为凹向液面,从而提高单晶的成晶率;Compared with the existing technology, the second pulling speed is increased by 0-40mm/h. Accelerating the pulling speed during the second shoulder expansion process can change the shape of the shoulder, as shown in Figures 1 and 2, making the first section shoulder 1 and An included angle is formed between the second shoulders 2. The angle of the included angle is generally 150-180° (excluding 180°), and the interface flipping in the second shoulder 2 can be accelerated and the growth interface of the single crystal can be flipped. Over, the liquid surface changes from convex to concave, thereby increasing the crystallization rate of single crystals;
在第二扩肩阶段中需要降低拉晶温度,本发明中采用的降温方法为降低加热器的功率,从而在拉制过程中进行降温,其中,In the second shoulder expansion stage, the crystal pulling temperature needs to be lowered. The cooling method used in the present invention is to reduce the power of the heater to cool down during the drawing process, where,
继续降低第一扩肩阶段中降低功率后的加热器的功率,从而进行再次降温,其中,第二功率的降幅范围为3-8kw,优选为4-7kw,更优选的为5kw、6kw、7kw;Continue to reduce the power of the heater after reducing the power in the first shoulder expansion stage, so as to cool down again, wherein the reduction range of the second power is 3-8kw, preferably 4-7kw, and more preferably 5kw, 6kw, 7kw ;
相较现有技术的功率降幅,本工艺中的功率降幅降低了2-5kw,即相对适当升高一定的单晶炉内温度,目的也是为了配合升高的第二拉速对单晶进行拉制,加速单晶生长界面的翻转;Compared with the power reduction of the existing technology, the power reduction in this process is reduced by 2-5kw, that is, the temperature in the single crystal furnace is relatively appropriately increased to a certain extent, and the purpose is also to cooperate with the increased second pulling speed to pull the single crystal. system, accelerating the flipping of the single crystal growth interface;
拉制第二段肩2的肩长为H2时,扩肩步骤结束;When the shoulder length of the second section of shoulder 2 is drawn to H2, the shoulder expansion step ends;
肩长即为肩部的高度,在本发明中代表肩的顶部至底部的最短距离,即垂直距离,一般的,H1:H2的比例范围为1:1-2:1,H2为总体肩长的二分之一到三分之二之间,优选为总体肩长的55-65%,更优选的,为总体肩长的60%。Shoulder length is the height of the shoulder. In the present invention, it represents the shortest distance from the top to the bottom of the shoulder, that is, the vertical distance. Generally, the ratio range of H1:H2 is 1:1-2:1, and H2 is the overall shoulder length. Between one-half and two-thirds of the overall shoulder length, preferably 55-65% of the overall shoulder length, and more preferably 60% of the overall shoulder length.
由于将扩肩阶段中的整体肩型改变为二段肩,即加大了整体肩部的外表面积,从物理角度直接增加了单晶的散热能力,并且使单晶的生长界面翻转过程提前至扩肩过程中,减少扩断或断苞次数,减少产量损失,即提高了大尺寸单晶扩肩及等径前期成晶率,提高产量。Since the overall shoulder shape in the shoulder expansion stage is changed to a two-section shoulder, the outer surface area of the overall shoulder is increased, which directly increases the heat dissipation capacity of the single crystal from a physical point of view, and advances the growth interface flipping process of the single crystal. During the shoulder expansion process, the number of expansion or bud breakage is reduced, and the yield loss is reduced, which means that the large-size single crystal shoulder expansion and equal diameter pre-crystallization rate are increased, and the output is increased.
下面列举几个实施例:Here are a few examples:
实施例1Example 1
S1:稳温阶段,在稳温过程中将埚位调整至第一位置处;S1: Temperature stabilization stage, during the temperature stabilization process, adjust the crucible position to the first position;
埚位即坩埚位位置,在本发明中代表坩埚内的熔融的原料液面距导流筒底部一定距离的位置处,第一位置为坩埚内的液面距导流筒底部20mm处;The crucible position is the crucible position. In the present invention, it represents the position where the molten raw material liquid level in the crucible is at a certain distance from the bottom of the flow guide tube. The first position is the position where the liquid level in the crucible is 20mm away from the bottom of the flow guide tube;
相比现有技术中稳温阶段的埚位,降低了一定距离,能够改变成晶区域,还能够改变肩部形状,同时加快单晶生长界面翻转,使其在扩肩阶段使其完成界面翻转,提高单晶的成晶率;Compared with the crucible position in the temperature stabilization stage in the existing technology, the distance is reduced by a certain distance, which can change the crystallization area and the shape of the shoulder. At the same time, it speeds up the interface flip of single crystal growth so that it can complete the interface flip in the shoulder expansion stage. , improve the crystallization rate of single crystal;
调整埚位至第一位置处后,在此处位置保持不动,直至结束稳温阶段,进入下一扩肩阶段。After adjusting the crucible position to the first position, it remains stationary until the temperature stabilization phase is completed and the next shoulder expansion phase is entered.
S2:扩肩阶段,其包括第一扩肩阶段和第二扩肩阶段,需要说明的是,晶体拉速越低或纵向温度梯度越小,单晶生长界面凸向液面程度越大;晶体拉速越高或纵向温度梯度越大,单晶生长界面凹向液面程度越大,其中,S2: Shoulder expansion stage, which includes the first shoulder expansion stage and the second shoulder expansion stage. It should be noted that the lower the crystal pulling speed or the smaller the longitudinal temperature gradient, the greater the degree of the single crystal growth interface convex to the liquid surface; the crystal The higher the pulling speed or the greater the longitudinal temperature gradient, the greater the concaveness of the single crystal growth interface toward the liquid surface, where,
S21:第一扩肩阶段中,将埚位从所述第一位置调整至第二位置处,随后使用第一拉速拉制第一段肩1,并在拉制过程中降低温度;S21: In the first shoulder expansion stage, adjust the crucible position from the first position to the second position, and then use the first drawing speed to draw the first shoulder section 1, and reduce the temperature during the drawing process;
埚位与S1中的含义一致,埚位的第二位置为坩埚内的液面距导流筒底部15mm处;The meaning of the crucible position is consistent with that in S1. The second position of the crucible position is 15mm from the liquid level in the crucible to the bottom of the guide tube;
当坩埚位置从第一位置移动至第二位置处时,开始拉制单晶,使用第一拉速拉制第一段肩1,其中,第一拉速为50mm/h;When the crucible moves from the first position to the second position, start pulling the single crystal, and use the first pulling speed to pull the first section 1, where the first pulling speed is 50mm/h;
在第一扩肩阶段中需要降低拉晶温度,本发明中采用的降温方法为降低加热器的功率,从而在拉制过程中进行降温,其中,In the first shoulder expansion stage, the crystal pulling temperature needs to be lowered. The cooling method used in the present invention is to reduce the power of the heater to cool down during the drawing process, where,
第一功率的降幅为7kw;The first power reduction is 7kw;
拉制第一段肩1的肩长至H1时,第一扩肩阶段结束;When the shoulder length of the first section of shoulder 1 is drawn to H1, the first shoulder expansion stage ends;
肩长即为肩部的高度,在本发明中代表肩的顶部至底部的最短距离,即垂直距离,本实施例中,H1为总体肩长的三分之一;The shoulder length is the height of the shoulder. In the present invention, it represents the shortest distance from the top to the bottom of the shoulder, that is, the vertical distance. In this embodiment, H1 is one-third of the overall shoulder length;
S22:第二扩肩阶段中,埚位保持不变,将第一拉速改变至第二拉速,使用第二拉速继续在第一段肩的底部拉制第二段肩2,并在拉制过程中继续降低温度,扩肩完成;S22: In the second shoulder expansion stage, the crucible position remains unchanged, change the first pulling speed to the second pulling speed, use the second pulling speed to continue drawing the second shoulder 2 at the bottom of the first shoulder, and During the drawing process, the temperature continues to be lowered and the shoulder expansion is completed;
埚位与S1中的含义一致,在第二扩肩阶段中保持埚位的第二位置不变,与步骤S21一致,坩埚内的液面距导流筒底部15mm处;The meaning of the crucible position is consistent with that in S1. In the second shoulder expansion stage, the second position of the crucible position remains unchanged, which is consistent with step S21. The liquid level in the crucible is 15mm from the bottom of the guide tube;
在第一段肩1的底部继续拉制第二段肩2,使用第二拉速拉制第二段肩2,其中,第二拉速高于第一拉速,为70mm/h;Continue to draw the second shoulder 2 at the bottom of the first shoulder 1, and use the second drawing speed to draw the second shoulder 2, where the second drawing speed is higher than the first drawing speed and is 70mm/h;
相较现有技术,在第二扩肩过程中加快拉速能够改变肩部形状,使第一段肩1与第二段肩2之间形成一个夹角,该夹角的角度一般为150-180°(不包括180°),并且在第二段肩2内能够加快界面翻转,将单晶的生长界面翻转过来,由凸向液面转变为凹向液面,从而提高单晶的成晶率;Compared with the existing technology, increasing the pulling speed during the second shoulder expansion process can change the shape of the shoulder, so that an included angle is formed between the first shoulder 1 and the second shoulder 2. The included angle is generally 150- 180° (excluding 180°), and can accelerate the interface flip in the second shoulder 2, flip the growth interface of the single crystal over, and change it from convex to the liquid surface to concave to the liquid surface, thereby improving the crystallization of the single crystal. Rate;
在第二扩肩阶段中需要降低拉晶温度,本发明中采用的降温方法为降低加热器的功率,从而在拉制过程中进行降温,其中,In the second shoulder expansion stage, the crystal pulling temperature needs to be lowered. The cooling method used in the present invention is to reduce the power of the heater to cool down during the drawing process, where,
继续降低第一扩肩阶段中降低功率后的加热器的功率,从而进行再次降温,其中,第二功率的降幅为8kw;Continue to reduce the power of the heater after reducing the power in the first shoulder expansion stage, so as to cool down again, in which the second power reduction is 8kw;
相较现有技术的功率降幅,相对适当升高一定的单晶炉内温度,目的也是为了配合升高的第二拉速对单晶进行拉制,加速单晶生长界面的翻转;Compared with the power reduction of the existing technology, the temperature in the single crystal furnace is relatively appropriately increased to a certain extent. The purpose is also to pull the single crystal with the increased second pulling speed and accelerate the flipping of the single crystal growth interface;
拉制第二段肩2的肩长为H2时,扩肩步骤结束;When the shoulder length of the second section of shoulder 2 is drawn to H2, the shoulder expansion step ends;
肩长即为肩部的高度,在本发明中代表肩的顶部至底部的最短距离,即垂直距离,H2为总体肩长的三分之二。The shoulder length is the height of the shoulder. In the present invention, it represents the shortest distance from the top to the bottom of the shoulder, that is, the vertical distance. H2 is two-thirds of the overall shoulder length.
实施例2Example 2
S1:稳温阶段,在稳温过程中将埚位调整至第一位置处;S1: Temperature stabilization stage, during the temperature stabilization process, adjust the crucible position to the first position;
埚位即坩埚位位置,在本发明中代表坩埚内的熔融的原料液面距导流筒底部一定距离的位置处,第一位置为坩埚内的液面距导流筒底部30mm处,The crucible position is the crucible position. In the present invention, it represents the position where the molten raw material liquid level in the crucible is at a certain distance from the bottom of the flow guide tube. The first position is the position where the liquid level in the crucible is 30mm away from the bottom of the flow guide tube.
相比现有技术中稳温阶段的埚位,降低了一定距离,能够改变成晶区域,还能够改变肩部形状,同时加快单晶生长界面翻转,使其在扩肩阶段使其完成界面翻转,提高单晶的成晶率;Compared with the crucible position in the temperature stabilization stage in the existing technology, the distance is reduced by a certain distance, which can change the crystallization area and the shape of the shoulder. At the same time, it speeds up the interface flip of single crystal growth so that it can complete the interface flip in the shoulder expansion stage. , improve the crystallization rate of single crystal;
调整埚位至第一位置处后,在此处位置保持不动,直至结束稳温阶段,进入下一扩肩阶段。After adjusting the crucible position to the first position, it remains stationary until the temperature stabilization phase is completed and the next shoulder expansion phase is entered.
S2:扩肩阶段,其包括第一扩肩阶段和第二扩肩阶段,需要说明的是,晶体拉速越低或纵向温度梯度越小,单晶生长界面凸向液面程度越大;晶体拉速越高或纵向温度梯度越大,单晶生长界面凹向液面程度越大,其中,S2: Shoulder expansion stage, which includes the first shoulder expansion stage and the second shoulder expansion stage. It should be noted that the lower the crystal pulling speed or the smaller the longitudinal temperature gradient, the greater the degree of the single crystal growth interface convex to the liquid surface; the crystal The higher the pulling speed or the greater the longitudinal temperature gradient, the greater the concaveness of the single crystal growth interface toward the liquid surface, where,
S21:第一扩肩阶段中,将埚位从所述第一位置调整至第二位置处,随后使用第一拉速拉制第一段肩1,并在拉制过程中降低温度;S21: In the first shoulder expansion stage, adjust the crucible position from the first position to the second position, and then use the first drawing speed to draw the first shoulder section 1, and reduce the temperature during the drawing process;
埚位与S1中的含义一致,埚位的第二位置为坩埚内的液面距导流筒底部25mm处;The meaning of the crucible position is consistent with that in S1. The second position of the crucible position is 25mm from the liquid level in the crucible to the bottom of the guide tube;
当坩埚位置从第一位置移动至第二位置处时,开始拉制单晶,使用第一拉速拉制第一段肩1,其中,第一拉速为65mm/h;When the crucible position moves from the first position to the second position, start pulling the single crystal, and use the first pulling speed to pull the first section 1, where the first pulling speed is 65mm/h;
在第一扩肩阶段中需要降低拉晶温度,本发明中采用的降温方法为降低加热器的功率,从而在拉制过程中进行降温,其中,In the first shoulder expansion stage, the crystal pulling temperature needs to be lowered. The cooling method used in the present invention is to reduce the power of the heater to cool down during the drawing process, where,
第一功率的降幅为17kw;相较于现有技术,降低了更多的加热器功率,使得单晶炉内温度更低;The first power reduction is 17kw; compared with the existing technology, more heater power is reduced, resulting in a lower temperature in the single crystal furnace;
拉制第一段肩1的肩长至H1时,第一扩肩阶段结束;When the shoulder length of the first section of shoulder 1 is drawn to H1, the first shoulder expansion stage ends;
肩长即为肩部的高度,在本发明中代表肩的顶部至底部的最短距离,即垂直距离,H1为总体肩长的二分之一;The shoulder length is the height of the shoulder. In the present invention, it represents the shortest distance from the top to the bottom of the shoulder, that is, the vertical distance. H1 is one-half of the overall shoulder length;
S22:第二扩肩阶段中,埚位保持不变,将第一拉速改变至第二拉速,使用第二拉速继续在第一段肩的底部拉制第二段肩2,并在拉制过程中继续降低温度,扩肩完成;S22: In the second shoulder expansion stage, the crucible position remains unchanged, change the first pulling speed to the second pulling speed, use the second pulling speed to continue drawing the second shoulder 2 at the bottom of the first shoulder, and During the drawing process, the temperature continues to be lowered and the shoulder expansion is completed;
埚位与S1中的含义一致,在第二扩肩阶段中保持埚位的第二位置不变,与步骤S21一致,坩埚内的液面距导流筒底部25mm处;The meaning of the crucible position is consistent with that in S1. In the second shoulder expansion stage, the second position of the crucible position remains unchanged, which is consistent with step S21. The liquid level in the crucible is 25mm from the bottom of the guide tube;
在第一段肩1的底部继续拉制第二段肩2,使用第二拉速拉制第二段肩2,其中,第二拉速高于第一拉速,为90mm/h;Continue to draw the second shoulder 2 at the bottom of the first shoulder 1, and use the second drawing speed to draw the second shoulder 2, where the second drawing speed is higher than the first drawing speed and is 90mm/h;
相较现有技术,在第二扩肩过程中加快拉速能够改变肩部形状,使第一段肩1与第二段肩2之间形成一个夹角,该夹角的角度一般为150-180°(不包括180°),并且在第二段肩2内能够加快界面翻转,将单晶的生长界面翻转过来,由凸向液面转变为凹向液面,从而提高单晶的成晶率;Compared with the existing technology, increasing the pulling speed during the second shoulder expansion process can change the shape of the shoulder, so that an included angle is formed between the first shoulder 1 and the second shoulder 2. The included angle is generally 150- 180° (excluding 180°), and can accelerate the interface flip in the second shoulder 2, flip the growth interface of the single crystal over, and change it from convex to the liquid surface to concave to the liquid surface, thereby improving the crystallization of the single crystal. Rate;
在第二扩肩阶段中需要降低拉晶温度,本发明中采用的降温方法为降低加热器的功率,从而在拉制过程中进行降温,其中,In the second shoulder expansion stage, the crystal pulling temperature needs to be lowered. The cooling method used in the present invention is to reduce the power of the heater to cool down during the drawing process, where,
继续降低第一扩肩阶段中降低功率后的加热器的功率,从而进行再次降温,其中,第二功率的降幅为3kw;Continue to reduce the power of the heater after reducing the power in the first shoulder expansion stage, so as to cool down again, in which the second power reduction is 3kw;
相较现有技术的功率降幅,相对适当升高一定的单晶炉内温度,目的也是为了配合升高的第二拉速对单晶进行拉制,加速单晶生长界面的翻转;Compared with the power reduction of the existing technology, the temperature in the single crystal furnace is relatively appropriately increased to a certain extent. The purpose is also to pull the single crystal with the increased second pulling speed and accelerate the flipping of the single crystal growth interface;
拉制第二段肩2的肩长为H2时,扩肩步骤结束;When the shoulder length of the second section of shoulder 2 is drawn to H2, the shoulder expansion step ends;
肩长即为肩部的高度,在本发明中代表肩的顶部至底部的最短距离,即垂直距离,H2为总体肩长的二分之一。The shoulder length is the height of the shoulder. In the present invention, it represents the shortest distance from the top to the bottom of the shoulder, that is, the vertical distance. H2 is one-half of the overall shoulder length.
实施例3Example 3
S1:稳温阶段,在稳温过程中将埚位调整至第一位置处;S1: Temperature stabilization stage, during the temperature stabilization process, adjust the crucible position to the first position;
埚位即坩埚位位置,在本发明中代表坩埚内的熔融的原料液面距导流筒底部一定距离的位置处,第一位置为坩埚内的液面距导流筒底部20-30mm处,优选为坩埚内的液面距导流筒底部24mm处;The crucible position is the crucible position. In the present invention, it represents the position where the molten raw material liquid level in the crucible is at a certain distance from the bottom of the guide tube. The first position is the position where the liquid level in the crucible is 20-30mm away from the bottom of the guide tube. Preferably, the liquid level in the crucible is 24mm from the bottom of the guide tube;
相比现有技术中稳温阶段的埚位,能够改变成晶区域,还能够改变肩部形状,同时加快单晶生长界面翻转,使其在扩肩阶段使其完成界面翻转,提高单晶的成晶率;Compared with the crucible position in the temperature stabilizing stage in the existing technology, it can change the crystallization area and the shoulder shape, and at the same time accelerate the interface flip of the single crystal growth, so that it can complete the interface flip during the shoulder expansion stage, improving the single crystal's Crystallization rate;
调整埚位至第一位置处后,在此处位置保持不动,直至结束稳温阶段,进入下一扩肩阶段。After adjusting the crucible position to the first position, it remains stationary until the temperature stabilization phase is completed and the next shoulder expansion phase is entered.
S2:扩肩阶段,其包括第一扩肩阶段和第二扩肩阶段,需要说明的是,晶体拉速越低或纵向温度梯度越小,单晶生长界面凸向液面程度越大;晶体拉速越高或纵向温度梯度越大,单晶生长界面凹向液面程度越大,其中,S2: Shoulder expansion stage, which includes the first shoulder expansion stage and the second shoulder expansion stage. It should be noted that the lower the crystal pulling speed or the smaller the longitudinal temperature gradient, the greater the degree of the single crystal growth interface convex to the liquid surface; the crystal The higher the pulling speed or the greater the longitudinal temperature gradient, the greater the concaveness of the single crystal growth interface toward the liquid surface, where,
S21:第一扩肩阶段中,将埚位从所述第一位置调整至第二位置处,随后使用第一拉速拉制第一段肩1,并在拉制过程中降低温度;S21: In the first shoulder expansion stage, adjust the crucible position from the first position to the second position, and then use the first drawing speed to draw the first shoulder section 1, and reduce the temperature during the drawing process;
埚位与S1中的含义一致,埚位的第二位置为坩埚内的液面距导流筒底部15-25mm处,优选为坩埚内的液面距导流筒底部20mm处;The meaning of the crucible position is consistent with that in S1. The second position of the crucible position is where the liquid level in the crucible is 15-25mm from the bottom of the flow guide tube, preferably 20mm between the liquid level in the crucible and the bottom of the flow guide tube;
当坩埚位置从第一位置移动至第二位置处时,开始拉制单晶,使用第一拉速拉制第一段肩1,其中,第一拉速为60mm/h;When the crucible moves from the first position to the second position, start pulling the single crystal, and use the first pulling speed to pull the first section 1, where the first pulling speed is 60mm/h;
相较现有技术中,第一扩肩阶段中的拉速变化较小,基本不变,正常拉制第一段肩1;Compared with the existing technology, the drawing speed in the first shoulder expansion stage changes slightly and is basically unchanged, and the first shoulder 1 is drawn normally;
在第一扩肩阶段中需要降低拉晶温度,本发明中采用的降温方法为降低加热器的功率,从而在拉制过程中进行降温,其中,In the first shoulder expansion stage, the crystal pulling temperature needs to be lowered. The cooling method used in the present invention is to reduce the power of the heater to cool down during the drawing process, where,
第一功率的降幅为12kw;相较于现有技术,降低了更多的加热器功率,使得单晶炉内温度更低;The first power reduction is 12kw; compared with the existing technology, more heater power is reduced, resulting in a lower temperature in the single crystal furnace;
拉制第一段肩1的肩长至H1时,第一扩肩阶段结束;When the shoulder length of the first section of shoulder 1 is drawn to H1, the first shoulder expansion stage ends;
肩长即为肩部的高度,在本发明中代表肩的顶部至底部的最短距离,即垂直距离,一般的,H1为为总体肩长的40%;The shoulder length is the height of the shoulder. In the present invention, it represents the shortest distance from the top to the bottom of the shoulder, that is, the vertical distance. Generally, H1 is 40% of the overall shoulder length;
S22:第二扩肩阶段中,埚位保持不变,将第一拉速改变至第二拉速,使用第二拉速继续在第一段肩的底部拉制第二段肩2,并在拉制过程中继续降低温度,扩肩完成;S22: In the second shoulder expansion stage, the crucible position remains unchanged, change the first pulling speed to the second pulling speed, use the second pulling speed to continue drawing the second shoulder 2 at the bottom of the first shoulder, and During the drawing process, the temperature continues to be lowered and the shoulder expansion is completed;
埚位与S1中的含义一致,在第二扩肩阶段中保持埚位的第二位置不变,与步骤S21一致,坩埚内的液面距导流筒底部20mm处;The crucible position has the same meaning as in S1. In the second shoulder expansion stage, the second position of the crucible position remains unchanged, consistent with step S21. The liquid level in the crucible is 20mm from the bottom of the guide tube;
在第一段肩1的底部继续拉制第二段肩2,使用第二拉速拉制第二段肩2,其中,第二拉速高于第一拉速,其为80mm/h;Continue to draw the second shoulder 2 at the bottom of the first shoulder 1, and draw the second shoulder 2 using a second drawing speed, where the second drawing speed is higher than the first drawing speed, which is 80mm/h;
相较现有技术,在第二扩肩过程中加快拉速能够改变肩部形状,使第一段肩1与第二段肩2之间形成一个夹角,该夹角的角度一般为150-180°(不包括180°),并且在第二段肩2内能够加快界面翻转,将单晶的生长界面翻转过来,由凸向液面转变为凹向液面,从而提高单晶的成晶率;Compared with the existing technology, increasing the pulling speed during the second shoulder expansion process can change the shape of the shoulder, so that an included angle is formed between the first shoulder 1 and the second shoulder 2. The included angle is generally 150- 180° (excluding 180°), and can accelerate the interface flip in the second shoulder 2, flip the growth interface of the single crystal over, and change it from convex to the liquid surface to concave to the liquid surface, thereby improving the crystallization of the single crystal. Rate;
在第二扩肩阶段中需要降低拉晶温度,本发明中采用的降温方法为降低加热器的功率,从而在拉制过程中进行降温,其中,In the second shoulder expansion stage, the crystal pulling temperature needs to be lowered. The cooling method used in the present invention is to reduce the power of the heater to cool down during the drawing process, where,
继续降低第一扩肩阶段中降低功率后的加热器的功率,从而进行再次降温,其中,第二功率的降幅为5kw;Continue to reduce the power of the heater after reducing the power in the first shoulder expansion stage, so as to cool down again, in which the second power reduction is 5kw;
相较现有技术的功率降幅,相对适当升高一定的单晶炉内温度,目的也是为了配合升高的第二拉速对单晶进行拉制,加速单晶生长界面的翻转;Compared with the power reduction of the existing technology, the temperature in the single crystal furnace is relatively appropriately increased to a certain extent. The purpose is also to pull the single crystal with the increased second pulling speed and accelerate the flipping of the single crystal growth interface;
拉制第二段肩2的肩长为H2时,扩肩步骤结束;When the shoulder length of the second section of shoulder 2 is drawn to H2, the shoulder expansion step ends;
肩长即为肩部的高度,在本发明中代表肩的顶部至底部的最短距离,即垂直距离,H2为总体肩长的60%。The shoulder length is the height of the shoulder. In the present invention, it represents the shortest distance from the top to the bottom of the shoulder, that is, the vertical distance. H2 is 60% of the overall shoulder length.
以上对本发明的实施例进行了详细说明,但所述内容仅为本发明的较佳实施例,不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的均等变化与改进等,均应仍归属于本发明的专利涵盖范围之内。The embodiments of the present invention have been described in detail above, but the contents are only preferred embodiments of the present invention and cannot be considered to limit the implementation scope of the present invention. All equivalent changes and improvements made within the scope of the present invention shall still fall within the scope of the patent of the present invention.
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| PCT/CN2023/088513 WO2023207641A1 (en) | 2022-04-29 | 2023-04-14 | Process for increasing crystallization rates in shoulder expansion and isodiametric early stage of large-size single crystal |
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| CN118007229A (en) * | 2024-03-26 | 2024-05-10 | 宁夏中欣晶圆半导体科技有限公司 | Crystal pulling method for heavily doped single crystal seeding and shoulder removal |
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| JP2009292659A (en) * | 2008-06-03 | 2009-12-17 | Sumco Corp | Method for forming shoulder in growing silicon single crystal |
| CN107858751A (en) * | 2016-09-22 | 2018-03-30 | 宁夏隆基硅材料有限公司 | A kind of crystal pulling method for improving pulling of crystals method crystal forming rate |
| CN109112625A (en) * | 2018-09-28 | 2019-01-01 | 宁晋晶兴电子材料有限公司 | A kind of monocrystalline silicon speed change shouldering technique |
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| CN118007229A (en) * | 2024-03-26 | 2024-05-10 | 宁夏中欣晶圆半导体科技有限公司 | Crystal pulling method for heavily doped single crystal seeding and shoulder removal |
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