WO2005007941A1 - An apparatus and method for recharge raw material - Google Patents

An apparatus and method for recharge raw material Download PDF

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Publication number
WO2005007941A1
WO2005007941A1 PCT/CN2003/000579 CN0300579W WO2005007941A1 WO 2005007941 A1 WO2005007941 A1 WO 2005007941A1 CN 0300579 W CN0300579 W CN 0300579W WO 2005007941 A1 WO2005007941 A1 WO 2005007941A1
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Prior art keywords
raw material
feeding tube
melt
crucible
growing
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PCT/CN2003/000579
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French (fr)
Chinese (zh)
Inventor
Jianzhong Yuan
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Jianzhong Yuan
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Application filed by Jianzhong Yuan filed Critical Jianzhong Yuan
Priority to CNB038266067A priority Critical patent/CN1327040C/en
Priority to PCT/CN2003/000579 priority patent/WO2005007941A1/en
Priority to AU2003255078A priority patent/AU2003255078A1/en
Publication of WO2005007941A1 publication Critical patent/WO2005007941A1/en

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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/02Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon

Definitions

  • the present invention relates to a device and method for growing crystals, and in particular, to a device and method for growing crystals by repeated feeding. Background technique
  • the most common method for growing crystals is the direct drawing method.
  • the direct drawing method is to add a growth raw material in a melt crucible, melt the growth raw material by resistance heating in a single crystal furnace, and grow a whole crystal rod through a seed crystal.
  • the direct drawing method because a melt crucible is used, and because of the structure of the direct drawing single crystal furnace, most of the crystal rods can only be fed at a time to pull one crystal rod. Only a few companies have adopted re-feeding technology. But they can only use rod-shaped growth materials, or granular growth materials, or small growth materials.
  • the rod-shaped growth raw material is made into a rod-shaped growth raw material, hung by a seed crystal hook, and then put into a melt crucible for melting.
  • Granular growth The raw materials are granules with a diameter of a few millimeters, or small pieces of material are poured into a melt crucible by a device and melted to achieve the purpose of feeding.
  • Repeated feeding can increase the amount of charge in a melt crucible, thereby increasing productivity and reducing Consumables, reduce energy consumption, achieve the goal of increasing production and reducing costs.
  • Repeated feeding can pull several crystal rods in one melt crucible, which further reduces consumables, saves energy, and reduces costs.
  • the present invention can provide multiple feeding and multiple repeated feedings for one melt crucible, and provides a device and method for growing crystals repeatedly.
  • the crystal growing device of the present invention mainly includes: a melt crucible 12 for melting growth raw materials, and the melt crucible 12 is placed in a graphite crucible 11 in a graphite heater 10.
  • the feeding tube which is repeatedly fed into the melt crucible 12, and the bottom port of the feeding tube is covered with a bottom plate made of the same raw material as the growing raw material.
  • a growth tube is added to the melt crucible with a feeding tube.
  • the material is not limited by whether the growing raw material is blocky, or small, or granular.
  • a melt crucible not only can feed more at one time, but also it can be repeatedly fed multiple times. This is of great significance for the production of crystals.
  • the quality of the crystal rods grown is improved by increasing the loading amount at one time.
  • the grown single crystal silicon rod has good resistivity uniformity and high product utilization.
  • feeding with the feeding pipe of the present invention improves the output, reduces the loss, and reduces the cost. Repeatedly adding the growth raw material multiple times, in the same melt crucible, several crystal rods can be drawn.
  • the above-mentioned device and method of the present invention can be applied to a variety of crystals grown by the direct-drawing method.
  • it can be used for crystal growth of silicon, lithium niobate, lithium osmate, sapphire, potassium arsenide and the like.
  • Fig. 1 is a schematic diagram of repeated feeding with the whole rod in the prior art.
  • Fig. 2 is a schematic diagram of repeated feeding with granular or small blocks in the prior art.
  • Figure 3 is a schematic diagram of crystal growth from a melt.
  • Figure 4 is a schematic diagram of the residual melt in the melt crucible after growing a crystal rod.
  • Fig. 5 is a schematic diagram of a device for repeatedly feeding with a feeding tube according to the present invention.
  • FIG. 6 is a schematic diagram of the growth raw material falling into the melt after the bottom plate of the bottom port of the feeding tube is melted.
  • Figure 7 shows the feed tube being lifted upwards, with more growth material falling into the melt.
  • Fig. 8 shows that after all the feeding tubes are raised out of the liquid surface, the growth raw materials in all the feeding tubes are added to the melt crucible.
  • Figure 9 shows that when the growth feedstock is repeatedly added once, there is more melt of the growth feedstock in the melt crucible.
  • FIG. 1 shows a prior art in which a melt crucible 12 is placed in a graphite crucible 11 in a graphite heater 10.
  • a whole rod-shaped growth raw material 101 is repeatedly fed into the melt crucible 12.
  • a part of the growing raw material in the melt crucible 12 becomes a melt 13.
  • FIG. 2 shows that in the prior art, a feeder 201 is used to repeatedly feed granular or small block growth raw material 202 into the melt crucible 12.
  • the granular growth raw material 202 is particles having a diameter of several millimeters.
  • Fig. 3 shows that all the growth raw materials in the melt crucible 12 are melted into a melt, and crystals will be drawn from the melt.
  • Fig. 4 shows that after the growth of a crystal rod is completed, some molten material 13 of the growing material always remains in the melting crucible 12.
  • Fig. 5 is a device for repeated feeding by a feeding tube according to the present invention.
  • the bottom port of the feeding tube 18 is blocked by a bottom plate 19 composed of the same raw material as the growing raw material.
  • the feed pipe 18 is filled with the growth raw material 15.
  • a connector 17 is suspended from the seed crystal hook 16.
  • the bottom plate 19 of the feeding tube 18 has been placed in the growth raw material melt 13 in the melt crucible 12.
  • the feeding tube 18 may be made of the same material as the melt crucible 12, or a high melting point material having a melting point higher than that of the growing material. Such as quartz, ceramic, platinum, iridium and so on.
  • Fig. 6 shows that the bottom plate 19 at the bottom of the feeding tube 18 entering the melt crucible 12 in Fig. 5 has been partially melted.
  • 21 is a part of the baseplate after being plutonized. A part of the growth raw material 20 has fallen from the feeding tube 18 into the melt crucible 12.
  • Figure ⁇ shows that when the bottom plate 19 on the bottom port of the feeding tube 18 is completely melted, more growth raw material 22 flows from the feeding tube 18 into the melt crucible 12 and is melted in the growth raw material melt 13. 18 promotion.
  • FIG. 8 shows that all the growth raw materials 22 are added to the melt crucible 12 after all the feeding tubes 18 are raised out of the liquid surface.
  • FIG. 9 shows that when all the growth raw materials in the feeding tube are added to the melt crucible 12, the empty feeding tube 18 has been raised. After the repeated feeding process is completed, the growth raw materials are all melted, and there are more in the melt crucible 12 Growth raw melt.
  • the method steps of the first furnace charging are:
  • the raw materials to be grown all fall into the melt crucible, and the empty feeding tube is raised. After all the growing materials are melted, the seed crystals of the growing crystals are put in, and the crystals are then drawn.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

An apparatus and method for recharge raw material in the crystal growth. Use a feed tube to recharge raw material in a crucible. Cover the lower end of the tube with a plate. The plate is made of the same raw material as the charge in the crucible. Load the raw material in the tube, and then lower the tube into the melt in crucible. When the plate is melted, the raw material in the tube is droped into the crucible. It can be recharged using the feed tube after pulling a ingot, sequentially multiple ingots can be grown by using one crucible. In this apparatus and methods, there are not limited for the shape and size of the raw material, and increase the quantity of the raw material with one time. This apparatus and method can improve productivity, product quality and yield. Lowering material consumption, energy and cost.

Description

重复加料生长晶体的装置及其方法 技术领域 本发明涉及一种生长晶体的装置及其方法,尤其是涉及一种重复加料生长 晶体的装置及其方法。 背景技术  TECHNICAL FIELD The present invention relates to a device and method for growing crystals, and in particular, to a device and method for growing crystals by repeated feeding. Background technique
1、 生长晶体的方法  1. Method for growing crystals
目前生长晶体最普通的方法是直拉法。如在全球有 95%以上的单晶硅是采 用直拉法 (CZ法) 拉制生产的。 直拉法是在熔料坩锅中添加生长原料, 通过 单晶炉中的电阻加热将生长原料熔化, 并通过籽晶生长出整根晶体棒。  At present, the most common method for growing crystals is the direct drawing method. For example, more than 95% of single crystal silicon is produced by the CZ method in the world. The direct drawing method is to add a growth raw material in a melt crucible, melt the growth raw material by resistance heating in a single crystal furnace, and grow a whole crystal rod through a seed crystal.
2、 目前重复加料的方法  2, the current method of repeated feeding
直拉法中, 由于采用了熔料坩埚, 并且由于直拉单晶炉的结构绝大部分都 只能一次加料拉制一根晶体棒。 只有少数公司采用了重复加料技术。 但他们只 能使用棒状生长原料, 或粒状生长原料, 或小块状生长原料。 棒状生长原料是 将生长原料制成棒状, 通过籽晶挂钩吊挂后, 放入熔料坩埚内熔化。 粒状生长 原料是直径几毫米的颗粒, 或小块状料都是通过装置将其倒入熔料坩埚中并熔 化, 以达到加料目的。  In the direct drawing method, because a melt crucible is used, and because of the structure of the direct drawing single crystal furnace, most of the crystal rods can only be fed at a time to pull one crystal rod. Only a few companies have adopted re-feeding technology. But they can only use rod-shaped growth materials, or granular growth materials, or small growth materials. The rod-shaped growth raw material is made into a rod-shaped growth raw material, hung by a seed crystal hook, and then put into a melt crucible for melting. Granular growth The raw materials are granules with a diameter of a few millimeters, or small pieces of material are poured into a melt crucible by a device and melted to achieve the purpose of feeding.
在先技术中, MEMC电子材料有限公司的约瀚 ·侯德(John Holder)博士, 在 2001年半导体设备与材料国际会议 (SEMICON China)上介绍了粒状料重复 及混合加料方法, 并介绍了美国专利号 5,588,993及 5,919,303中所描述的粒状 混合料重复加料的目的。  In the prior art, Dr. John Holder of MEMC Electronic Materials Co., Ltd. introduced the granular material repetition and mixed feeding method at the 2001 International Conference on Semiconductor Equipment and Materials (SEMICON China), and introduced the United States The purpose of repetitive addition of the granular mixture described in Patent Nos. 5,588,993 and 5,919,303.
上述重复加料的方法都局限于使用棒料, 或粒状料, 或小块状料。 而事实 上, 绝大多数生产使用的是块状原料。 并不是砸小了的小块状料。 因此, 在先 技术就大大局限了重复加料的应用。  The above-mentioned repeated feeding methods are all limited to the use of rods, or granular materials, or small pieces. In fact, the vast majority of production uses lumpy raw materials. Not smashing small pieces. Therefore, the prior art greatly limited the application of repeated feeding.
3、 重复加料的意义  3. The significance of repeated feeding
a、 重复加料可以提高一个熔料坩埚中的装料量, 从而提高生产率、 降低 耗材、 降低能耗, 达到提高产量, 降低成本的目的。 a. Repeated feeding can increase the amount of charge in a melt crucible, thereby increasing productivity and reducing Consumables, reduce energy consumption, achieve the goal of increasing production and reducing costs.
b、 重复加料可在一个熔料坩埚中拉制出数根晶体棒, 这就进一步减少了 耗材、 节约了能源、 降低了成本。  b. Repeated feeding can pull several crystal rods in one melt crucible, which further reduces consumables, saves energy, and reduces costs.
以生长单晶硅为例,据 MEMC公司 m Holder博士介绍: 拉制第一根单 晶硅棒, 由于熔料坩埚中多加了料,可使成本由无重复加料的 100%降为 94%, 拉制第二根单晶硅棒时, 成本是无重复加料时成本的 74%, 而第三根单晶硅棒 更可达到 60%。这对于全球超过 100亿美元的单晶硅产业来说, 无疑具有重大 的经济价值。我们知道,超过 90%的直拉单晶硅是使用块状料作为生长原料的。 因此, 对于单晶硅生产来说, 使用块状料重复加料才能真正达到提高产能, 降 低成本的目的。 此例更显示出重复加料, 尤其是重复加块状料的重大意义。 发明内容  Take the growth of single crystal silicon as an example. According to Dr. M Holder of MEMC, the first single crystal silicon rod is drawn. Because more material is added to the melt crucible, the cost can be reduced from 100% to 94% without repeated feeding. When drawing the second single crystal silicon rod, the cost is 74% of the cost without repeated feeding, and the third single crystal silicon rod can reach 60%. This is undoubtedly of great economic value for the global monocrystalline silicon industry with over US $ 10 billion. We know that more than 90% of straight-pull single crystal silicon uses bulk materials as growth raw materials. Therefore, for the production of single crystal silicon, the repeated use of bulk materials can really increase the production capacity and reduce the cost. This example also shows the significance of repeated feeding, especially for block feeding. Summary of the invention
本发明为了使用不受大小形状限制的块状生长原料,对于一个熔料坩埚能 够多加料和多次重复加料, 提供一种重复加料生长晶体的装置及其方法。  In order to use bulk growth raw materials without restriction on size and shape, the present invention can provide multiple feeding and multiple repeated feedings for one melt crucible, and provides a device and method for growing crystals repeatedly.
本发明的生长晶体的装置主要包含:熔化生长原料的熔料坩埚 12,熔料坩 埚 12置于石墨加热器 10内的石墨坩埚 11里。 向熔料坩埚 12里重复加料的加 料管, 加料管的底部端口用与加入生长原料相同原料构成的底板盖住。  The crystal growing device of the present invention mainly includes: a melt crucible 12 for melting growth raw materials, and the melt crucible 12 is placed in a graphite crucible 11 in a graphite heater 10. The feeding tube which is repeatedly fed into the melt crucible 12, and the bottom port of the feeding tube is covered with a bottom plate made of the same raw material as the growing raw material.
如上所述的本发明装置, 生长晶体重复加入生长原料的具体方法步骤是- In the device of the present invention as described above, the specific method steps of repeatedly adding growing materials to growing crystals are −
1、首先将加料管的底部端口用与加入生长原料相同原料构成的底板盖住;1. First, cover the bottom port of the feeding tube with a bottom plate made of the same raw material as the growing raw material;
2、 将生长原料装入加料管内; 2. Fill the growth material into the feeding tube;
3、 将加料管的顶端吊挂在籽晶挂钩上;  3. Hang the top of the feeding tube on the seed crystal hook;
4、 当熔料坩埚里有熔融的熔液时, 将装有生长原料的加料管底端的底板 放入熔液中;  4. When there is molten melt in the melt crucible, put the bottom plate of the bottom end of the feeding tube containing the growth raw material into the melt;
5、 待底端底板熔化后, 生长原料落入熔料坩埚内, 提升加料管;  5. After the bottom plate is melted, the growth material falls into the melt crucible, and the feeding tube is raised;
6、 当加料管内的生长原料全部落入熔料坩埚内, 提出空的加料管, 生长 原料全部熔化成熔液时, 放入所要生长晶体的晶种, 开始拉制晶体;  6. When all the growth raw materials in the feeding tube fall into the melt crucible, raise the empty feeding tube, and when all the growth raw materials are melted into the melt, put the seed crystals to grow crystals and start pulling the crystals;
7、 一根完整的晶体棒拉制完成提出后, 反复重复上述步骤。 至此, 反复 重复上述步骤, 就能够拉制成多根完整的晶体棒。  7. After drawing a complete crystal rod, repeat the above steps repeatedly. At this point, the above steps can be repeated to draw multiple complete crystal rods.
很显然, 上述本发明的装置及其方法, 用加料管向熔料坩埚里加入生长原 料, 不受生长原料是否块状, 或小块状, 或粒状的形状大小的限制。 对于一个 熔料坩埚, 不仅一次加料多, 而且能够多次重复加料。 这对于生产晶体来说, 是有着重大的意义。 提高一次装料量, 生长出的晶体棒质量好。 如生长的单晶 硅棒的电阻率就均匀性好、 产品利用率高。 总之, 用本发明的加料管加料, 提 高了产量, 降低了损耗, 降低了成本。 多次重复加入生长原料, 在同一个熔料 坩埚中, 可以拉制出数根晶体棒, 这当然, 大大减少了耗材, 节约了能源, 将 成倍地降低成本。 本发明上述的装置及其方法, 能够用于多种用直拉法生长的 晶体上。 如, 可以用于硅、 铌酸锂、 钜酸锂、 蓝宝石、 砷化钾等等晶体的生长 上。 附图说明 Obviously, in the above apparatus and method of the present invention, a growth tube is added to the melt crucible with a feeding tube. The material is not limited by whether the growing raw material is blocky, or small, or granular. For a melt crucible, not only can feed more at one time, but also it can be repeatedly fed multiple times. This is of great significance for the production of crystals. The quality of the crystal rods grown is improved by increasing the loading amount at one time. For example, the grown single crystal silicon rod has good resistivity uniformity and high product utilization. In short, feeding with the feeding pipe of the present invention improves the output, reduces the loss, and reduces the cost. Repeatedly adding the growth raw material multiple times, in the same melt crucible, several crystal rods can be drawn. This, of course, greatly reduces consumables, saves energy, and will double the cost. The above-mentioned device and method of the present invention can be applied to a variety of crystals grown by the direct-drawing method. For example, it can be used for crystal growth of silicon, lithium niobate, lithium osmate, sapphire, potassium arsenide and the like. BRIEF DESCRIPTION OF THE DRAWINGS
图 1是在先技术中, 用整根棒料重复加料的示意图。  Fig. 1 is a schematic diagram of repeated feeding with the whole rod in the prior art.
图 2是在先技术中, 用粒状或小块状料重复加料的示意图。  Fig. 2 is a schematic diagram of repeated feeding with granular or small blocks in the prior art.
图 3是从熔液中生长晶体的示意图。  Figure 3 is a schematic diagram of crystal growth from a melt.
图 4是生长一根晶体棒完成后, 在熔料坩埚中有残余熔液的示意图。  Figure 4 is a schematic diagram of the residual melt in the melt crucible after growing a crystal rod.
图 5是本发明用加料管重复加料的装置示意图。  Fig. 5 is a schematic diagram of a device for repeatedly feeding with a feeding tube according to the present invention.
图 6是加料管底部端口的底板熔化后, 生长原料落入熔液中的示意图。 图 7是向上提升加料管, 有更多的生长原料落入熔液中。  FIG. 6 is a schematic diagram of the growth raw material falling into the melt after the bottom plate of the bottom port of the feeding tube is melted. Figure 7 shows the feed tube being lifted upwards, with more growth material falling into the melt.
图 8是将加料管全部提出液面后,所有加料管中的生长原料均加入到熔料 坩埚中。  Fig. 8 shows that after all the feeding tubes are raised out of the liquid surface, the growth raw materials in all the feeding tubes are added to the melt crucible.
图 9是当生长原料一次重复加料过程完成后,在熔料坩埚中有更多的生长 原料熔液。 具体实施方式  Figure 9 shows that when the growth feedstock is repeatedly added once, there is more melt of the growth feedstock in the melt crucible. detailed description
下面结合附图和具体实施例进一步说明本发明的装置及其方法。  The device and method of the present invention are further described below with reference to the drawings and specific embodiments.
图 1是在先技术中,熔料坩埚 12置于石墨加热器 10内的石墨坩埚 11里。 用一整根的棒状生长原料 101在向熔料坩埚 12内重复加料。熔料坩埚 12内已 熔化部分生长原料成熔液 13。石墨坩埚 11底下,石墨加热器 10之间有加热器 连线 14。 图 2是在先技术中,用一加料器 201将粒状或小块状生长原料 202重复加 料于熔料坩埚 12内。 其中粒状生长原料 202是直径为几毫米的颗粒。 FIG. 1 shows a prior art in which a melt crucible 12 is placed in a graphite crucible 11 in a graphite heater 10. A whole rod-shaped growth raw material 101 is repeatedly fed into the melt crucible 12. A part of the growing raw material in the melt crucible 12 becomes a melt 13. Under the graphite crucible 11, there are heater wires 14 between the graphite heaters 10. FIG. 2 shows that in the prior art, a feeder 201 is used to repeatedly feed granular or small block growth raw material 202 into the melt crucible 12. The granular growth raw material 202 is particles having a diameter of several millimeters.
图 3是熔料坩埚 12内的生长原料全部被熔化成熔液, 将从熔液中拉制晶 体。  Fig. 3 shows that all the growth raw materials in the melt crucible 12 are melted into a melt, and crystals will be drawn from the melt.
图 4是当一根晶体棒生长完成后, 在熔料坩埚 12内总要剩余一些生长原 料的熔液 13。  Fig. 4 shows that after the growth of a crystal rod is completed, some molten material 13 of the growing material always remains in the melting crucible 12.
图 5是本发明用加料管重复加料的装置。  Fig. 5 is a device for repeated feeding by a feeding tube according to the present invention.
加料管 18的底部端口有与加入生长原料相同原料构成的底板 19堵住。加 料管 18内装入生长原料 15。 加料管 18的顶端有连接头 17吊在籽晶挂钩 16 上。 图中, 加料管 18的底部底板 19已经放入熔料坩埚 12里的生长原料熔液 13中。所说的加料管 18可以用与熔料坩埚 12同种材料制成,或者用熔点高于 生长原料的高熔点材料制成。 如石英、 陶瓷、 铂、 铱金等。  The bottom port of the feeding tube 18 is blocked by a bottom plate 19 composed of the same raw material as the growing raw material. The feed pipe 18 is filled with the growth raw material 15. At the top of the feeding tube 18, a connector 17 is suspended from the seed crystal hook 16. In the figure, the bottom plate 19 of the feeding tube 18 has been placed in the growth raw material melt 13 in the melt crucible 12. The feeding tube 18 may be made of the same material as the melt crucible 12, or a high melting point material having a melting point higher than that of the growing material. Such as quartz, ceramic, platinum, iridium and so on.
图 6是当图 5中进入熔料坩埚 12里的加料管 18底部的底板 19已经部分 地被熔化了。图中 21是被瑢化后的部分底板。部分生长原料 20已从加料管 18 中落入熔料坩埚 12里。  Fig. 6 shows that the bottom plate 19 at the bottom of the feeding tube 18 entering the melt crucible 12 in Fig. 5 has been partially melted. In the figure, 21 is a part of the baseplate after being plutonized. A part of the growth raw material 20 has fallen from the feeding tube 18 into the melt crucible 12.
图 Ί是当加料管 18底部端口上的底板 19全部被熔化了,有更多的生长原 料 22从加料管 18里流进熔料坩埚 12里, 熔化于生长原料熔液 13中, 将加料 管 18提升。  Figure Ί shows that when the bottom plate 19 on the bottom port of the feeding tube 18 is completely melted, more growth raw material 22 flows from the feeding tube 18 into the melt crucible 12 and is melted in the growth raw material melt 13. 18 promotion.
图 8是将加料管 18全部提出液面后,所有生长原料 22均加入到熔料坩埚 12中。  FIG. 8 shows that all the growth raw materials 22 are added to the melt crucible 12 after all the feeding tubes 18 are raised out of the liquid surface.
图 9是当全部加料管内的生长原料加入到熔料坩埚 12内, 空的加料管 18 已被提出, 重复加料的过程完成后, 生长原料全部被熔化了, 在熔料坩埚 12 中有更多的生长原料熔液。  FIG. 9 shows that when all the growth raw materials in the feeding tube are added to the melt crucible 12, the empty feeding tube 18 has been raised. After the repeated feeding process is completed, the growth raw materials are all melted, and there are more in the melt crucible 12 Growth raw melt.
对于用本发明的加料管重复加料的具体方法步骤是:  The specific method steps for repeated feeding with the feeding tube of the present invention are:
一、 第一炉加料的方法步骤是:  First, the method steps of the first furnace charging are:
1、 先将加料管底部端口用与加入的生长原料相同原料构成的底板盖住; 1. First cover the bottom port of the feeding tube with a bottom plate made of the same raw material as the growing raw material;
2、 将生长原料装入加料管中; 2. Fill the growth material into the feeding tube;
3、 按常规方法在熔料坩埚中装料并加热熔化;  3. Charge and melt in the melt crucible according to the conventional method;
4、 将加料管的顶端吊挂在籽晶挂钩上, 等熔料坩埚中生长原料熔化后, 将加料管底部端口的底板放入熔化的生长原料熔液中,待底部端口底板熔化脱 落后, 加料管中的生长原料落入熔料坩埚中并熔化, 提升加料管; 4. Hang the top of the feeding tube on the seed crystal hook and wait for the growing material in the melt crucible to melt. Place the bottom plate of the bottom port of the feeding tube into the molten growth raw material melt. After the bottom port bottom plate melts and falls off, the growth raw material in the feeding tube falls into the melt crucible and melts to raise the feeding tube;
5、 待生长原料全部落入熔料坩埚中, 提出空的加料管。 生长原料全部熔 化后, 放入生长晶体的籽晶, 幵始拉制晶体。  5. The raw materials to be grown all fall into the melt crucible, and the empty feeding tube is raised. After all the growing materials are melted, the seed crystals of the growing crystals are put in, and the crystals are then drawn.
二、 超过一根完整晶体棒的重复加料的步骤是- Second, the steps for repeated feeding of more than one complete crystal rod are-
1、 将加料管底部端口用与加入的生长原料相同原料构成的底板盖住;1. Cover the bottom port of the feeding tube with a bottom plate made of the same raw material as the growing raw material;
2、 将生长原料装入加料管中; 2. Fill the growth material into the feeding tube;
3、 当单晶炉中生长的一根完整晶体棒取出后, 将加料管的顶端挂到籽晶 挂钩上;  3. After removing a complete crystal rod grown in the single crystal furnace, hang the top of the feeding tube on the seed crystal hook;
4、 保持熔料坩埚的温度;  4. Maintain the temperature of the melt crucible;
5、 将加料管放入熔化的生长原料熔液中, 待底部端口的底板熔化脱落后, 加料管中的生长原料也落入熔料坩埚中并熔化, 提升加料管;  5. Put the feeding tube into the molten growth raw material melt. After the bottom plate of the bottom port melts and falls off, the growth raw material in the feeding tube also falls into the melt crucible and melts to raise the feeding tube;
6、 当加料管中的生长原料全部落入到熔料坩埚内, 提出空的加料管。 生 长原料全部熔化后, 放入晶体的籽晶, 开始拉制晶体;  6. When all the growth materials in the feeding tube fall into the melt crucible, raise the empty feeding tube. After all the growth raw materials are melted, put the seed crystal into the crystal and start to pull the crystal;
7、 拉制一根完整的晶体棒取出后, 再重复这第二部分的步骤。 反复重复 这第二部分的步骤, 即反复重复加料, 就达到了在一个熔料坩埚里, 拉制出多 根晶体棒的目的。  7. After pulling a complete crystal rod out, repeat the steps in this second part. Repeat the steps in this second part repeatedly, that is, repeatedly repeat the feeding, to achieve the purpose of drawing multiple crystal rods in a melt crucible.

Claims

权利 要 求 Rights request
1、 一种重复加料生长晶体的装置, 主要包含: 熔化生长晶体原料的熔料 坩埚, 熔料坩埚置于石墨加热器内的石墨坩埚里, 其特征在于包含有向熔料坩 埚里加生长原料的加料管,加料管的底部端口是用与加入的生长原料相同原料 构成的底板盖住。 1. A device for repeatedly adding and growing crystals, mainly comprising: a melt crucible for melting and growing crystal raw materials, and the melt crucible being placed in a graphite crucible in a graphite heater, which is characterized by containing a material for adding growth materials to the melt crucible. The feeding tube, the bottom port of the feeding tube is covered with a bottom plate made of the same raw material as the growing raw material.
2、 根据权利要求 1所述的重复加料生长晶体的装置的方法, 其特征在于 具体方法步骤是- 2. The method for repeating the device for growing crystals according to claim 1, characterized in that the specific method steps are-
(1) 首先将加料管的底部端口用与加入生长原料相同原料构成的底板盖 住; (1) First, cover the bottom port of the feeding tube with a bottom plate made of the same raw material as the growing raw material;
(2) 将生长原料装入加料管内;  (2) Fill the growth material into the feeding tube;
(3) 将加料管的顶端吊挂在籽晶挂钩上;  (3) Hang the top of the feeding tube on the seed crystal hook;
(4) 当熔料坩埚里有熔融的熔液时, 将装有生长原料的加料管的底端底板 放入熔液中;  (4) When there is a molten melt in the melt crucible, put the bottom plate of the feeding tube containing the growth raw material into the melt;
(5) 待加料管底端的底板熔化后, 一部分生长原料落入熔料坩埚内, 提升 加料管;  (5) After the bottom plate of the bottom end of the feeding tube is melted, a part of the growth raw material falls into the melting crucible, and the feeding tube is lifted;
(6) 当加料管内的生长原料全部落入熔料坩埚内, 提出空的加料管, 生长 原料全部熔化成熔液时, 放入所要生长晶体的晶种, 开始拉制晶体;  (6) When all the growing materials in the feeding tube fall into the melt crucible, raise the empty feeding tube, and when all the growing materials are melted into the melt, insert the seed crystals of the crystals to be grown and start pulling the crystals;
(7)一根完整的晶体棒拉制完成提出后, 再反复重复上述步骤。  (7) After drawing and pulling out a complete crystal rod, repeat the above steps.
PCT/CN2003/000579 2003-07-18 2003-07-18 An apparatus and method for recharge raw material WO2005007941A1 (en)

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