CN113584584A - Method for producing silicon core rod by casting - Google Patents
Method for producing silicon core rod by casting Download PDFInfo
- Publication number
- CN113584584A CN113584584A CN202110901326.1A CN202110901326A CN113584584A CN 113584584 A CN113584584 A CN 113584584A CN 202110901326 A CN202110901326 A CN 202110901326A CN 113584584 A CN113584584 A CN 113584584A
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- China
- Prior art keywords
- quartz
- quartz tubular
- silicon core
- core rod
- silicon
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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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
-
- 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
- C30B29/02—Elements
- C30B29/06—Silicon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to the field of silicon core production, in particular to a method for producing a silicon core rod by casting, which comprises the following steps: s1: preheating a quartz tubular container; s2: adding molten silicon liquid into a quartz tubular container; s3: cooling the quartz tubular container containing the molten silicon liquid to form a silicon core rod crude product; s4: and removing quartz on the periphery of the silicon core rod, and cleaning to obtain the silicon core rod. The method for producing the silicon core rod has simple process and easy operation. The simultaneous preparation of a plurality of silicon core rods can be realized only by arranging a plurality of quartz tubular containers in the production equipment.
Description
Technical Field
The invention relates to the field of silicon core production, in particular to a method for producing a silicon core rod by casting.
Background
The heat carrier for carrying out reduction reaction deposition (CVD) on polycrystalline silicon in a reduction furnace in the production of the polycrystalline silicon by the Siemens process is taken from an initial molybdenum wire or tantalum tube to a silicon core produced by a zone melting method and then to the current wire-cutting square silicon core.
The invention of Chinese patent CN102995108A discloses a continuous charging silicon single crystal furnace. The crucible comprises a lifting device, a feeding device, a quartz crucible, a graphite crucible and a graphite heater, wherein the quartz crucible is divided into an inner crucible and an outer crucible, the bottoms of the inner crucible and the outer crucible are connected with each other and provided with a communicated hole, and a feeding gap is reserved between the inner crucible and the outer crucible; the lifting device is provided with a weighing sensor and a camera for monitoring the growth of the crystal bar; the feeding device feeds materials through the feeding hopper, and the feeding opening is arranged between the inner crucible and the outer crucible. According to the invention, the quartz crucible is arranged into the inner layer and the outer layer, and the feeding device feeds materials between the inner crucible and the outer crucible, so that the influence on the growth of the crystal bar when the raw materials are fed can be effectively prevented, the integral concentration of the produced crystal is ensured, and the production cost of the crystal bar with specific concentration is reduced.
For example, the chinese patent invention CN111945223A discloses a silicon core furnace capable of continuous production and a using method thereof, the silicon core furnace comprises: a lower furnace body, a silicon core drawing device is arranged in the lower furnace body, and a first clapboard which can be opened and closed is arranged at the upper part of the lower furnace body; the at least two upper furnace bodies are detachably connected with the lower furnace body; and the environment control device is used for carrying out environment control on the lower furnace body and the upper furnace body which is not installed on the lower furnace body. Compared with the prior art that the furnace body is divided into two parts which are fixedly connected, the invention can solve the problem of time cost (the total drawing process of the silicon core furnace needs about 5 hours, wherein the material is heated for about 30 minutes, and the replacement process of the dismounting furnace is about 30 minutes), and can solve the problem of energy cost and resource cost waste (the empty burning of a raw material rod in the silicon core drawing device is reduced, so that the lower half part of the raw material rod is effectively utilized).
In the prior art, a single crystal furnace is used for drawing silicon cores, only one silicon core can be produced at a time, and when a plurality of drum cores are required to be produced simultaneously, the number of the single crystal furnace can be increased, and a large amount of space is required to be occupied. And the overall concentration is easy to be uneven by the drawing method.
Disclosure of Invention
The invention aims to provide a method for casting and producing a silicon core rod aiming at the defects in the production of the existing silicon core rod.
The purpose of the invention is realized by the following technical scheme.
A method for casting a silicon core rod comprises the following steps:
s1: preheating a quartz tubular container;
s2: adding molten silicon liquid into a quartz tubular container;
s3: cooling the quartz tubular container containing the molten silicon liquid to form a silicon core rod crude product;
s4: and removing quartz on the periphery of the silicon core rod, and cleaning to obtain the silicon core rod.
Further, in S1, the quartz tube-shaped container was preheated to 1350-.
Further, in S1, the height of the quartz tubular container is 220-320cm, the inner diameter is 5-10cm, and the wall thickness of the container is 0.5-1 cm.
Further, a graphite heat-insulating sheath is arranged outside the quartz tubular container.
The graphite heat-insulating sheath prevents the silicon liquid from crystallizing too fast due to too fast heat dissipation of the silicon liquid, and simultaneously, because the molten silicon liquid has certain expansion during cooling, the quartz tubular container is prevented from being cracked and falling too early under the protection of the graphite sheath, and the uniformity and the stability of the whole size during cooling and forming of the silicon rod are ensured.
Further, in S3, the cooling is performed to 50 to 100 ℃.
Further, a heating system is arranged around the quartz tubular container, and the height of the heating system is larger than that of the quartz tubular container.
Further, the heating system around the quartz tubular vessel was started before S2 to maintain the ambient temperature around the quartz tubular vessel at 1300-.
Further, the heating system is removed before S3.
Further, the heating system is removed from the bottom to the top of the quartz tubular container, so that the silicon liquid at the bottom of the quartz tubular container and the silicon liquid at the top have time difference in crystallization and solidification processes, and the silicon liquid at the bottom is crystallized and solidified before the silicon liquid at the top.
Further, the heating system is uniformly removed in the bottom-to-top direction of the quartz tubular container.
The uniform removal of the heating system in the bottom-to-top direction of the quartz tubular vessel in the present invention can be achieved by relative movement of the heating system and the quartz tubular vessel in space.
Further, the time for complete removal of the heating system is 25-30 h.
The process for producing the silicon core is carried out in a vacuum environment.
The invention has the advantages that:
1. the invention creatively uses the quartz tubular container as the silicon core rod forming die, after the molten silicon liquid is crystallized and solidified to form the silicon core rod, the quartz is removed through mechanical external force, and the silicon rod can be obtained through cleaning, the process is simple, and the operation is easy. Compared with the silicon rod preparation method by adopting a drawing method, the method disclosed by the invention can realize simultaneous preparation of a plurality of silicon core rods only by arranging a plurality of quartz tubular containers in production equipment.
2. In the preferred scheme of the invention, the graphite heat-insulating sheath is arranged outside the quartz tubular container, so that the condition that the crystallization speed of the silicon liquid is too high due to too high heat dissipation of the silicon liquid can be prevented, and meanwhile, the quartz tubular container is prevented from being cracked and falling off too early under the protection of the graphite sheath because the molten silicon liquid is expanded to a certain extent when being cooled, and the uniformity and the stability of the whole size of the silicon rod during cooling and forming are ensured.
3. In a still further preferred aspect of the present invention, the quartz tubular vessel is further prevented from being damaged when the molten silicon liquid is crystallized by cooling by a heating system around the quartz tubular vessel and uniformly removing the heating system in the bottom-to-top direction of the quartz tubular vessel while cooling.
Detailed Description
Example 1
A method for casting a silicon core rod in a vacuum environment comprises the following steps:
s1: preheating a quartz tubular container to 1350 ℃;
s2: adding the molten silicon liquid into a quartz tubular container with the height of 220cm, the inner diameter of 5cm and the thickness of the container wall of 1 cm;
s3: cooling the quartz tubular container containing the molten silicon liquid to 50-100 ℃ to form a silicon core rod crude product;
s4: and (4) smashing and removing quartz on the periphery of the silicon core rod, and cleaning to obtain the silicon core rod.
Example 2
A method for casting a silicon core rod in a vacuum environment comprises the following steps:
s1: preheating a quartz tubular container to 1380 ℃;
s2: adding the molten silicon liquid into a quartz tubular container with the height of 220cm, the inner diameter of 5cm and the thickness of the container wall of 0.5 cm;
s3: cooling the quartz tubular container containing the molten silicon liquid to 50-100 ℃ to form a silicon core rod crude product;
s4: and (4) smashing and removing quartz on the periphery of the silicon core rod, and cleaning to obtain the silicon core rod.
Example 3
A method for casting a silicon core rod in a vacuum environment comprises the following steps:
s1: preheating a quartz tubular container with a graphite sheath to 1400 ℃;
s2: adding the molten silicon liquid into a quartz tubular container with the height of 220cm, the inner diameter of 10cm and the thickness of the container wall of 1 cm;
s3: cooling the quartz tubular container containing the molten silicon liquid to 50-100 ℃ to form a silicon core rod crude product;
s4: and breaking and removing graphite and quartz at the periphery of the silicon core rod, and cleaning to obtain the silicon core rod.
Example 4
A method for casting a silicon core rod in a vacuum environment comprises the following steps:
s1: arranging a movable annular graphite heating sleeve around the quartz tubular container with the graphite sheath, and starting the heating sleeve to preheat the quartz tubular container to 1400 ℃;
s2: adding the molten silicon liquid into a quartz tubular container with the height of 220cm, the inner diameter of 10cm and the thickness of the container wall of 1 cm;
s3: and uniformly removing the annular graphite heating jacket from the bottom of the quartz tubular container to the top of the quartz tubular container, wherein the time for completely removing is 25-30 h. Cooling the quartz tubular container to 50-100 ℃ to form a silicon core rod crude product;
s4: and breaking and removing graphite and quartz at the periphery of the silicon core rod, and cleaning to obtain the silicon core rod.
In the method of embodiments 1-4 of the invention, one or more quartz tubular containers can be arranged according to the size and the requirement of the vacuum furnace, no special requirements are made on the furnace body, and the vacuum degree required by the conventional silicon core production is ensured.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A method for casting a silicon core rod comprises the following steps:
s1: preheating a quartz tubular container;
s2: adding molten silicon liquid into a quartz tubular container;
s3: cooling the quartz tubular container containing the molten silicon liquid to form a silicon core rod crude product;
s4: and removing quartz on the periphery of the silicon core rod, and cleaning to obtain the silicon core rod.
2. The method as claimed in claim 1, wherein in S1, the quartz tube-shaped container is preheated to 1350-1400 ℃.
3. The method as claimed in claim 1, wherein in S1, the quartz tubular container has a height of 220-330cm, an inner diameter of 5-10cm, and a wall thickness of 0.5-1 cm.
4. The method of claim 1, wherein the quartz tubular vessel is externally jacketed with a graphite thermal jacket.
5. The method of claim 1, wherein a heating system is disposed around the quartz tubular vessel, the heating system having a height greater than a height of the quartz tubular vessel.
6. The method as claimed in claim 5, wherein the heating system around the quartz tubular vessel is activated before S2 to maintain the ambient temperature around the quartz tubular vessel at 1300-1500 ℃.
7. The method of claim 5, wherein the heating system is removed prior to S3.
8. The method as claimed in claim 7, wherein the heating system is removed from the bottom to the top of the quartz tubular container, so that there is a time difference between the solidification process of the silicon liquid at the bottom of the quartz tubular container and the crystallization solidification process of the silicon liquid at the top, and the silicon liquid at the bottom is crystallized and solidified before the silicon liquid at the top.
9. The method of claim 8, wherein the heating system is removed uniformly in a bottom-to-top direction of the quartz tubular vessel.
10. The method of claim 8, wherein the time for complete removal of the heating system is 25-30 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110901326.1A CN113584584A (en) | 2021-08-06 | 2021-08-06 | Method for producing silicon core rod by casting |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110901326.1A CN113584584A (en) | 2021-08-06 | 2021-08-06 | Method for producing silicon core rod by casting |
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| Publication Number | Publication Date |
|---|---|
| CN113584584A true CN113584584A (en) | 2021-11-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202110901326.1A Pending CN113584584A (en) | 2021-08-06 | 2021-08-06 | Method for producing silicon core rod by casting |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492980A (en) * | 2011-12-16 | 2012-06-13 | 国电宁夏太阳能有限公司 | Method and device for preparing silicon cores for polycrystalline silicon deposition |
| CN204918845U (en) * | 2015-07-24 | 2015-12-30 | 北京京运通科技股份有限公司 | Silicon core furnace |
| CN110241457A (en) * | 2019-07-01 | 2019-09-17 | 江阴东升新能源股份有限公司 | Silicon core side ingot ingot casting device and its casting technique |
| CN112176407A (en) * | 2020-10-21 | 2021-01-05 | 苏州昀丰半导体装备有限公司 | Thermal field structure of square silicon core ingot furnace and preparation method |
-
2021
- 2021-08-06 CN CN202110901326.1A patent/CN113584584A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492980A (en) * | 2011-12-16 | 2012-06-13 | 国电宁夏太阳能有限公司 | Method and device for preparing silicon cores for polycrystalline silicon deposition |
| CN204918845U (en) * | 2015-07-24 | 2015-12-30 | 北京京运通科技股份有限公司 | Silicon core furnace |
| CN110241457A (en) * | 2019-07-01 | 2019-09-17 | 江阴东升新能源股份有限公司 | Silicon core side ingot ingot casting device and its casting technique |
| CN112176407A (en) * | 2020-10-21 | 2021-01-05 | 苏州昀丰半导体装备有限公司 | Thermal field structure of square silicon core ingot furnace and preparation method |
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Application publication date: 20211102 |