CN114457408A - Preparation method of gettering tank for cleaning impurity bottom materials in single crystal furnace - Google Patents
Preparation method of gettering tank for cleaning impurity bottom materials in single crystal furnace Download PDFInfo
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- CN114457408A CN114457408A CN202011421649.2A CN202011421649A CN114457408A CN 114457408 A CN114457408 A CN 114457408A CN 202011421649 A CN202011421649 A CN 202011421649A CN 114457408 A CN114457408 A CN 114457408A
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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
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Abstract
A method for preparing a gettering tank for cleaning impurity bed charge in a single crystal furnace comprises the steps of respectively manufacturing the tank body, a sealing plate and a gettering pipe, sequentially splicing and molding the tank body, the sealing plate and the gettering pipe to obtain a gettering tank green compact, sintering the gettering tank green compact to obtain a finished product, and finally inspecting to be qualified. The method is reasonable in design and easy to operate, the prepared gettering tank can suck out crucible bed charge with high impurity content left after the single crystal furnace is pulled, and the problems that after the single crystal furnace is pulled for multiple times, more crystal bars cannot be pulled due to impurity enrichment and the quality of the crystal bars is reduced in the later period are effectively solved.
Description
Technical Field
The invention relates to the technical field of single crystal pulling, in particular to a preparation method of a gettering sink for cleaning an impurity primer in a single crystal furnace.
Background
At present, because a secondary feeding mode is adopted for a single crystal pulling rod, the shutdown of one rod is obviously improved compared with the shutdown of one traditional rod, and the shutdown of a plurality of rods can be generally realized in the prior art. However, since impurities are enriched at the bottom of the crucible due to multiple charging, the continuous rod pulling cannot be performed in a secondary charging mode after a plurality of single crystal rods are pulled, and the single crystal rods need to be shut down for cleaning, so that the cost is increased invisibly; and due to the enrichment of impurities, the quality of the crystal bar also shows a remarkable reduction trend after the crystal bar is drawn to three.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a method for preparing a gettering sink for cleaning impurity bed charge in a single crystal furnace.
The technical problem to be solved by the present invention is achieved by the following technical means. The invention relates to a method for preparing a gettering sink for cleaning impurity bed charge in a single crystal furnace, which comprises the following steps:
(1) manufacturing a tank body:
firstly splicing 2 moulds with the shape of a half of gettering tank body, pouring slurry into the mould splicing space, then absorbing slurry for 2-3h by adopting a single-side slurry absorbing method, and pouring out the residual slurry after the wall thickness of the tank body reaches 8-20mm to obtain the tank body of the gettering tank;
(2) manufacturing a gettering pipe:
firstly splicing 2 molds with half of the shape of the gettering pipe, then inserting a forming rod in the space between the molds after splicing, then pouring slurry between the molds and the forming rod, pulling out the forming rod after the slurry is completely cured, and disassembling the molds to obtain the gettering pipe;
(3) manufacturing a sealing plate:
placing the forming ring with the same shape at the bottom of the tank body on a forming plate, then pouring slurry into the forming ring, and obtaining a sealing plate after the slurry is solidified and formed;
(4) placing the formed tank body, the gettering pipe and the sealing plate in an oven for curing for 4-8 h;
(5) splicing and finishing the surfaces of the solidified tank body, the impurity absorbing pipe and the sealing plate according to the specific size requirement of the impurity absorbing tank, digging a mounting hole matched with the impurity absorbing pipe on the tank body, and cleaning by using compressed air;
(6) installing the gettering pipe on the tank body, inserting the gettering pipe into the installation hole, positioning, pouring slurry into a gap between the gettering pipe and the installation hole, and curing for 2-3 h;
(7) mounting the sealing plate on the tank body, firstly placing the sealing plate at the bottom of the tank body, positioning, then pouring slurry into a gap between the sealing plate and the tank body, and then curing for 2-3 h;
(8) putting the mounted tank body into an oven, drying for 3-8h at 45-100 ℃, cooling the tank body to room temperature, and then carrying out repair inspection to obtain a raw blank of the gettering tank;
(9) sintering the green body of the gettering tank at 1050 ℃ and 1100 ℃ for 65-75h to obtain a finished product of the gettering tank;
(10) checking the air tightness of the sintered gettering tank finished product, and then cleaning and drying the gettering tank finished product;
the technical problem to be solved by the invention can be further realized by the following technical scheme, and for the above preparation method of the gettering sink for cleaning the impurity bed charge in the single crystal furnace, in the step (8), the concrete operation of repairing and checking is as follows: repairing and flattening the uneven areas among the impurity suction pipe, the sealing plate and the tank body, and then blowing the tank body clean by using compressed air.
The technical problem to be solved by the invention can be further realized by the following technical scheme that in the preparation method of the gettering sink for cleaning the impurity bottom material in the single crystal furnace, in the step (9), a tunnel kiln is adopted to sinter the green body of the gettering sink.
The technical problem to be solved by the invention can be further realized by the following technical scheme that in the preparation method of the gettering tank for cleaning the impurity bottom material in the single crystal furnace, in the step (10), the air tightness of a finished product of the gettering tank is checked by using a water soaking method, and then the finished product of the gettering tank is cleaned by using pure water;
the technical problem to be solved by the invention can be further realized by the following technical scheme that in the step (10), the drying temperature is 100-150 ℃, and the drying time is 45-100 min.
The technical problem to be solved by the invention can be further realized by the following technical scheme that the slurry adopted by the method for preparing the gettering sink for cleaning the impurity bottom material in the single crystal furnace is high-purity silicon dioxide or aluminum oxide.
The technical problem to be solved by the invention can be further realized by the following technical scheme that the preparation method of the gettering sink for cleaning the impurity backing material in the single crystal furnace comprises a tank body, wherein one end of the tank body is sealed by a sealing plate, a gettering pipe is inserted into the other end of the tank body, one end of the gettering pipe penetrates through the tank body from outside to inside and extends into the tank body, a gettering chamber convenient for containing the impurity backing material is formed between the gettering pipe in the tank body and the inner wall of the tank body, and a gettering gap convenient for the impurity backing material to enter the gettering chamber is formed between the end part of the gettering pipe in the tank body and the sealing plate.
The technical problem to be solved by the invention can be further realized by the following technical scheme that in the preparation method of the impurity suction tank for cleaning the impurity bottom material in the single crystal furnace, the tank body is cylindrical, the sealing plate is disc-shaped, and the impurity suction pipe is in a circular pipe shape.
Compared with the prior art, the method is designed aiming at the problems that after the pulling rod of the single crystal furnace is fed for multiple times, more crystal rods cannot be pulled due to impurity enrichment and the quality of the later crystal rods is reduced, the impurity suction tank prepared by the method can suck out crucible bed charge with high impurity content left after the pulling rod, so that the pulling purpose of increasing the pulling rod amount is achieved, and the difference of the quality of the pulling rod crystal rods for multiple times is obviously reduced due to the fact that the crucible bed charge with high impurity content is sucked out, so that the aims of reducing the crystal pulling cost and improving the product quality are comprehensively achieved; when the device is used, the tank body of the gettering tank, the gettering pipe and the sealing plate are manufactured respectively and then assembled in sequence. The method is reasonable in design and easy to operate, the prepared gettering tank can suck out crucible bed charge with high impurity content left after the single crystal furnace is pulled, and the problems that after the single crystal furnace is pulled for multiple times, more crystal bars cannot be pulled due to impurity enrichment and the quality of the crystal bars is reduced in the later period are effectively solved.
Drawings
FIG. 1 is a schematic view of the construction of a gettering can made by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the method for preparing the gettering sink for cleaning the impurity bed charge in the single crystal furnace comprises the following steps of:
(1) manufacturing a tank body 1:
firstly splicing 2 moulds with the shape of a half of a gettering tank body 1, pouring slurry into a mould splicing space, then sucking slurry for 2-3h by adopting a single-side slurry sucking method, preferably sucking slurry for 2.5h, pouring out the residual slurry after the wall thickness of the tank body 1 reaches 8-20mm, preferably, the wall thickness of the tank body 1 is 15mm, and thus obtaining the tank body 1 of the gettering tank;
(2) manufacturing a gettering pipe 3:
firstly splicing 2 molds with half of the shape of the gettering pipe 3, then inserting a forming rod in the space after the molds are spliced, pouring slurry between the molds and the forming rod, pulling out the forming rod after the slurry is completely cured, and disassembling the molds to obtain the gettering pipe 3; the forming roller is a stainless steel round roller;
(3) manufacturing a sealing plate 2:
placing the forming ring with the same shape at the bottom of the tank body 1 on a forming plate, then pouring slurry into the forming ring, and obtaining a sealing plate 2 after the slurry is solidified and formed; the forming ring adopts a stainless steel ring, and the forming plate adopts a gypsum board;
(4) placing the formed tank body 1, the gettering pipe 3 and the sealing plate 2 in an oven for curing for 4-8h, preferably 6 h;
(5) splicing and finishing the surfaces of the solidified tank body 1, the gettering pipe 3 and the sealing plate 2 according to the specific size requirement of the gettering tank, digging a mounting hole matched with the gettering pipe 3 on the tank body 1, and cleaning by using compressed air;
(6) installing the gettering pipe 3 on the tank body 1, inserting the gettering pipe 3 into the installation hole, positioning, pouring slurry into a gap between the gettering pipe 3 and the installation hole, and curing for 2-3h, preferably 3 h;
(7) mounting a sealing plate 2 on a tank body 1, firstly placing the sealing plate 2 at the bottom of the tank body 1, positioning, then pouring slurry into a gap between the sealing plate 2 and the tank body 1, and then curing for 2-3h, preferably 3 h;
(8) putting the installed tank body 1 into an oven, drying for 3-8h at 45-100 ℃, preferably drying for 6h at 80 ℃, then cooling the tank body 1 to room temperature, and then carrying out repair inspection, wherein the specific operation of the repair inspection is as follows: repairing and flattening the uneven areas among the gettering pipe 3, the sealing plate 2 and the tank body 1, and then blowing the tank body 1 clean by using compressed air to obtain a gettering tank green body;
(9) sintering the green body of the gettering tank by adopting a tunnel kiln, wherein the sintering temperature is 1050-1100 ℃, and the sintering time is 65-75h, so as to obtain a finished product of the gettering tank, preferably, the sintering temperature is 1080 ℃, and the sintering time is 72 h;
(10) checking the air tightness of the finished product of the gettering tank by using a water soaking method, cleaning the finished product of the gettering tank by using pure water, and if no abnormity is detected, cleaning and drying by using the pure water, wherein the drying temperature is 100-; preferably, the drying temperature is 120 ℃ and the drying time is 60 min.
The slurry adopted by the method is high-purity silicon dioxide or alumina; high purity silica generally means silica having a total metal impurity content of less than one ten million and a single non-metal impurity content of less than one ten million, and is mainly used as a filler for an integrated circuit encapsulant and a raw material for manufacturing high purity quartz glass. High temperature resistance: the softening point temperature of the silicon dioxide glass is about 1730 ℃, the silicon dioxide glass can be used for a long time at 1180 ℃, and the maximum use temperature in a short time can reach 1450 ℃; alumina is an inorganic substance, has a chemical formula of Al2O3, is a high-hardness compound, has a melting point of 2054 ℃ and a boiling point of 2980 ℃, is an ionic crystal which can be ionized at high temperature, and is commonly used for manufacturing refractory materials; the tank body 1, the sealing plate 2 and the impurity absorbing pipe 3 are made of high-purity silicon dioxide or aluminum oxide, so that the high-temperature environment of the single crystal furnace can be effectively applied.
The gettering tank prepared by the method comprises a tank body 1, wherein one end of the tank body 1 is sealed by a sealing plate 2, a gettering pipe 3 is inserted into the other end of the tank body 1, one end of the gettering pipe 3 penetrates through the tank body 1 from outside to inside and extends into the tank body 1, a gettering chamber convenient for containing impurity backing materials is formed between the gettering pipe 3 in the tank body 1 and the inner wall of the tank body 1, and a gettering gap convenient for the impurity backing materials to enter the gettering chamber is formed between the end part of the gettering pipe 3 in the tank body 1 and the sealing plate 2. One end of the tank body 1 is sealed by a sealing plate 2, and the other end is inserted with a gettering pipe 3, so that a closed space is formed in the tank body 1, only one inlet and outlet of the gettering pipe 3 is provided, so that the gettering pipe 3 can be conveniently extended into the single crystal furnace, and an impurity bed charge in the single crystal furnace is sucked from the gettering pipe 3 by using pressure difference and enters a gettering chamber through a gettering gap, so that the single crystal furnace is not stopped, the rod pulling amount of the single crystal furnace is increased, and the rod pulling quality of the single crystal furnace is ensured; the gettering chamber is arranged to prevent the impurity substrate from dropping from the tank body 1 when the gettering pipe 3 is pulled out of the single crystal furnace, thereby ensuring the gettering effect.
The gettering pipe 3 is vertically inserted in the tank body 1, so that the gettering pipe 3 is conveniently and fixedly connected with the tank body 1, the gettering pipe 3 is also convenient to use, and when the gettering pipe 3 is extended into the single crystal furnace, the tank body 1 is not easy to collide with the single crystal furnace.
The tank body 1 is cylindrical, the sealing plate 2 is disc-shaped, the impurity suction pipe 3 is in a circular pipe shape, design and manufacturing are facilitated, and meanwhile the impurity suction pipe 3 is convenient to insert into the single crystal furnace to suck impurity backing materials in the single crystal furnace.
Claims (8)
1. A preparation method of a gettering sink for cleaning up impurity bed charge in a single crystal furnace is characterized in that: the gettering tank prepared by the method comprises a tank body, a sealing plate and a gettering pipe, and comprises the following specific steps:
(1) manufacturing a tank body:
firstly splicing 2 moulds with the shape of a half of gettering tank body, pouring slurry into the mould splicing space, then absorbing slurry for 2-3h by adopting a single-side slurry absorbing method, and pouring out the residual slurry after the wall thickness of the tank body reaches 8-20mm to obtain the tank body of the gettering tank;
(2) manufacturing a gettering pipe:
firstly splicing 2 molds with half of the shape of the gettering pipe, then inserting a forming rod in the space between the molds after splicing, then pouring slurry between the molds and the forming rod, pulling out the forming rod after the slurry is completely cured, and disassembling the molds to obtain the gettering pipe;
(3) manufacturing a sealing plate:
placing the forming ring with the same shape at the bottom of the tank body on a forming plate, then pouring slurry into the forming ring, and obtaining a sealing plate after the slurry is solidified and formed;
(4) placing the formed tank body, the gettering pipe and the sealing plate in an oven for curing for 4-8 h;
(5) splicing and finishing the surfaces of the solidified tank body, the impurity absorbing pipe and the sealing plate according to the specific size requirement of the impurity absorbing tank, digging a mounting hole matched with the impurity absorbing pipe on the tank body, and cleaning by using compressed air;
(6) installing the gettering pipe on the tank body, inserting the gettering pipe into the installation hole, positioning, pouring slurry into a gap between the gettering pipe and the installation hole, and curing for 2-3 h;
(7) mounting the sealing plate on the tank body, firstly placing the sealing plate at the bottom of the tank body, positioning, then pouring slurry into a gap between the sealing plate and the tank body, and then curing for 2-3 h;
(8) putting the mounted tank body into an oven, drying for 3-8h at 45-100 ℃, cooling the tank body to room temperature, and then carrying out repair inspection to obtain a raw blank of the gettering tank;
(9) sintering the green body of the gettering tank at 1050 ℃ and 1100 ℃ for 65-75h to obtain a finished product of the gettering tank;
(10) and checking the air tightness of the sintered gettering tank finished product, and then cleaning and drying the gettering tank finished product.
2. The method for manufacturing a gettering sink of cleaning foreign substances bed material in a single crystal furnace according to claim 1, characterized in that: in the step (8), the concrete operations of repairing and checking are as follows: repairing and flattening the uneven areas among the impurity suction pipe, the sealing plate and the tank body, and then blowing the tank body clean by using compressed air.
3. The method for manufacturing a gettering sink of cleaning foreign substances bed material in a single crystal furnace according to claim 1, characterized in that: and (9) sintering the green bodies of the adsorption tanks by adopting a tunnel kiln.
4. The method for manufacturing a gettering sink of cleaning foreign substances bed material in a single crystal furnace according to claim 1, characterized in that: in the step (10), the air tightness of the finished gettering tank is checked by a water soaking method, and then the finished gettering tank is cleaned by pure water.
5. The method for manufacturing a gettering sink of cleaning foreign substances bed material in a single crystal furnace according to claim 1 or 4, characterized in that: in the step (10), the drying temperature is 100-150 ℃, and the drying time is 45-100 min.
6. The method for manufacturing a gettering sink of cleaning foreign substances bed material in a single crystal furnace according to claim 1, characterized in that: the slurry adopted by the method is high-purity silicon dioxide or alumina.
7. The method for manufacturing a gettering sink of cleaning foreign substances bed material in a single crystal furnace according to claim 1, characterized in that: the gettering tank prepared by the method comprises a tank body, wherein one end of the tank body is sealed by a sealing plate, a gettering pipe is inserted into the other end of the tank body, one end of the gettering pipe penetrates through the tank body from outside to inside and extends into the tank body, a gettering chamber convenient for containing impurity backing materials is formed between the gettering pipe in the tank body and the inner wall of the tank body, and a gettering gap convenient for the impurity backing materials to enter the gettering chamber is formed between the end part of the gettering pipe in the tank body and the sealing plate.
8. The method for on-line cleaning of an impurity primer in a single crystal furnace according to claim 7, wherein: the tank body is cylindrical, the sealing plate is disc-shaped, and the impurity absorbing pipe is in a circular pipe shape.
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| CN202011421649.2A CN114457408A (en) | 2020-12-08 | 2020-12-08 | Preparation method of gettering tank for cleaning impurity bottom materials in single crystal furnace |
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| CN202011421649.2A CN114457408A (en) | 2020-12-08 | 2020-12-08 | Preparation method of gettering tank for cleaning impurity bottom materials in single crystal furnace |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976333A (en) * | 2012-12-13 | 2013-03-20 | 青岛隆盛晶硅科技有限公司 | Method and equipment for controlled directional solidification and purification of polycrystalline silicon through taking tailing by graphite tube |
| CN102976334A (en) * | 2012-12-13 | 2013-03-20 | 青岛隆盛晶硅科技有限公司 | Method and equipment for rapid collection and purification of polycrystalline silicon through directional solidification of tailing |
| CN103043664A (en) * | 2012-12-13 | 2013-04-17 | 青岛隆盛晶硅科技有限公司 | Method and device for directionally solidifying and purifying polysilicon by vacuum extraction of tailing |
| CN111111333A (en) * | 2019-12-26 | 2020-05-08 | 西安奕斯伟硅片技术有限公司 | Single crystal growing furnace dust removal filtration system |
-
2020
- 2020-12-08 CN CN202011421649.2A patent/CN114457408A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976333A (en) * | 2012-12-13 | 2013-03-20 | 青岛隆盛晶硅科技有限公司 | Method and equipment for controlled directional solidification and purification of polycrystalline silicon through taking tailing by graphite tube |
| CN102976334A (en) * | 2012-12-13 | 2013-03-20 | 青岛隆盛晶硅科技有限公司 | Method and equipment for rapid collection and purification of polycrystalline silicon through directional solidification of tailing |
| CN103043664A (en) * | 2012-12-13 | 2013-04-17 | 青岛隆盛晶硅科技有限公司 | Method and device for directionally solidifying and purifying polysilicon by vacuum extraction of tailing |
| CN111111333A (en) * | 2019-12-26 | 2020-05-08 | 西安奕斯伟硅片技术有限公司 | Single crystal growing furnace dust removal filtration system |
Non-Patent Citations (1)
| Title |
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| 王丽: "《光电子与光通信实验》", 北京工业大学出版社, pages: 86 * |
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