CN112301425A - Large-argon flow crystal pulling method for large-size monocrystalline silicon rod - Google Patents
Large-argon flow crystal pulling method for large-size monocrystalline silicon rod Download PDFInfo
- Publication number
- CN112301425A CN112301425A CN201910703397.3A CN201910703397A CN112301425A CN 112301425 A CN112301425 A CN 112301425A CN 201910703397 A CN201910703397 A CN 201910703397A CN 112301425 A CN112301425 A CN 112301425A
- Authority
- CN
- China
- Prior art keywords
- argon flow
- single crystal
- argon
- stage
- diameter
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- C30B15/20—Controlling or regulating
Abstract
The invention relates to a large argon flow crystal pulling method for a large-size monocrystalline silicon rod, which comprises the steps of melting materials, stabilizing the temperature, seeding, shouldering, shoulder rotating, equalizing the diameter and ending, keeping the argon flow at 90-120SLPM in the crystal pulling process, and keeping the furnace pressure at 25Mpa, wherein the argon flow at the stages of stabilizing the temperature, seeding and shouldering is kept at 100-120 SLPM; the shoulder rotating stage keeps the argon flow at 100-; keeping the argon flow at 90-100SLPM in the equal diameter stage. The invention has the beneficial effects that: the growth requirement of a large-size single crystal silicon rod can be met by adopting large argon flow and large furnace pressure, the heat dissipation of the single crystal silicon rod is fast, the high pulling speed can be realized, the temperature in the furnace is stable, the growth of single crystals is facilitated, and the crystallization rate is higher; the pressure airflow in the furnace is ensured to be more constant by increasing the flow of argon and the furnace pressure in the production process; in order to avoid energy waste as much as possible, a staged flow method is adopted, the production requirement of the large-size single crystal silicon rod is met, and energy can be saved as much as possible.
Description
Technical Field
The invention belongs to the technical field of Czochralski silicon single crystals, and particularly relates to a large-argon flow crystal pulling method for a large-size single crystal silicon rod.
Background
In the prior art, the growth of the silicon single crystal rod is realized by using a small argon flow and small furnace pressure process for pulling the single crystal with the conventional size, the argon flow of 45-60SLPM is generally adopted, and the pressure in the furnace is kept at about 11 MPa. However, when the argon flow and the furnace pressure are used for producing the large-size (240mm-310mm) single crystal silicon rod, the gas flow in the furnace is unstable, and the liquid level is easy to shake; in addition, because the generated silicon rod is thick, the opening of the throttle valve is large due to small argon flow and small furnace pressure, so that a pipeline is blocked, waste in the furnace and generated impurities cannot be discharged in time, and the crystallization rate is influenced; due to the action of air flow, the seed crystals can shake during temperature stabilization, the shoulder-putting survival rate can be influenced by too long temperature stabilization time, and the defects of the head and the tail of the produced silicon rod are more and the dislocation is more due to the production environment; in addition, the thermal stress is increased due to the increase of the diameter of the single crystal, and the single crystal above the liquid level can be cracked due to the small argon flow and the small furnace pressure.
Disclosure of Invention
In order to solve the technical problem, the invention provides a large argon flow crystal pulling method for a large-size single crystal silicon rod.
The technical scheme adopted by the invention is as follows: a large argon flow crystal pulling method for a large-size monocrystalline silicon rod comprises the steps of melting materials, stabilizing temperature, seeding, shouldering, shoulder rotating, diameter equalizing and ending, wherein the flow of the upper argon is kept at 90-120SLPM in the processes of temperature stabilizing, seeding, shouldering, shoulder rotating and diameter equalizing, and the furnace pressure is kept at 25 Mpa.
Preferably, the upper argon flow is kept at 100-120SLPM in the stages of temperature stabilization, seeding and shouldering; the shoulder turning stage keeps the upper argon flow at 100-110 SLPM; keeping the upper argon flow at 90-100SLPM in the equal diameter stage.
Preferably, the flow of argon gas in the melting and finishing stages is maintained at 90-120 SLPM.
Preferably, the upper argon flow is maintained at 60-80SLPM during the melt and final phase.
Preferably, the lower argon flow is 20-30 SLPM.
Preferably, the upper limit of the fusion diameter of the seeding stage is 16.5mm, the lower limit of the fusion diameter is 13mm, and the minimum diameter value is 10 mm.
Preferably, the seeding gain value is 0.085.
The invention has the advantages and positive effects that: the growth requirement of a large-size single crystal silicon rod can be met by adopting large argon flow and large furnace pressure, the heat dissipation of the single crystal silicon rod is fast, the high pulling speed can be realized, the temperature in the furnace is stable, the growth of single crystals is facilitated, and the crystallization rate is higher; the pressure airflow in the furnace is ensured to be more constant by increasing the flow of argon and the furnace pressure in the production process; in order to avoid energy waste as much as possible, a staged flow method is adopted, the production requirement of the large-size single crystal silicon rod is met, and energy can be saved as much as possible.
Detailed Description
The invention relates to a large-argon flow crystal pulling method for a large-size single crystal silicon rod, which is used for producing the single crystal silicon rod with the diameter of 240mm-310 mm. The existing argon standard and furnace pressure standard for the conventional-size silicon rod cannot be used for producing the high-quality silicon single crystal rod, and in order to stably produce the high-quality large-size silicon rod, the scheme realizes the purpose by using large argon flow and large furnace pressure.
The method comprises the steps of melting materials, stabilizing temperature, seeding, shouldering, shoulder rotating, diameter equalizing and ending, wherein the argon flow is kept to be 90-120SLPM in the crystal pulling process, compared with 45-60SLPM in the traditional process, the argon flow and the furnace pressure are obviously improved, excessive argon flow in the crystal pulling process of the single crystal with the conventional size leads to easy crystallization, and in addition, the excessive argon flow can reduce the temperature in the furnace, so that the large argon flow adopted in the scheme for adapting to crystal pulling of the silicon rod with the large size can increase the stability of the crystal pulling process, the crystallization phenomenon can not occur under the synergistic effect of the large furnace pressure, and the furnace pressure is kept to be 25 Mpa. Particularly, the used argon flow is large, the high argon flow can be adopted in the whole crystal pulling process, and in order to reduce unnecessary waste, the used argon can be adjusted in each stage, so that the requirements of large-size crystal pulling can be met, and the cost can be reduced as much as possible. The melting stage can use lower argon flow which is not lower than 45SLPM, in order to be capable of stably transiting with the subsequent stage, 60-80SLPM is adopted, the temperature stabilization, seeding and shouldering stages are key steps of crystal formation, the requirement on environmental stability is higher, in order to ensure the stability of the crystal pulling environment, the argon flow is kept at 100-120SLPM, the shouldering stage can use slightly lower argon flow, 100-110SLPM is adopted, the equal diameter stage can select 90-100SLPM, and the stable environment in the rapid growth process of the crystal bar length is kept; the final stage ensures that no dislocations occur, and a lower argon flow, 60-80SLPM, may be used in this stage. The above limits are the flow value of introducing upper argon in the reaction process, and lower argon of 20-30SLPM can be continuously filled in the drawing process to balance the upper argon and keep the gas flow in the furnace constant.
In order to ensure the crystallization rate of a large-size silicon rod in the drawing process, avoid crystal transformation and shorten the use time of temperature-stabilizing fusion welding, the upper limit of the fusion diameter in the seeding stage is limited to 16.5mm, the lower limit of the fusion diameter is limited to 13mm, and the minimum diameter value is 10 mm. The seeding gain value is controlled to be 0.085, the fusion crystal forming rate can be obviously improved in the environment of large argon flow, thereby realizing high-efficiency fusion,
the invention is further illustrated by the following specific examples.
Example 1
A large-argon flow crystal pulling method for a large-size monocrystalline silicon rod comprises the steps of melting materials, stabilizing the temperature, seeding, shouldering, shoulder rotating, equal diameter and ending;
and (3) material melting stage: placing a silicon block into a quartz crucible, flushing argon, heating and melting the silicon block after the silicon block is pressurized to 25MPa to form uniform silicon melt, controlling the argon flow to be 60SLPM at the initial melting stage, increasing the argon flow along with the melting of the silicon block, controlling the argon flow to be 80SLPM after the completion of the melting stage, and preparing for the large argon flow which is obviously increased at the subsequent temperature stabilization stage;
and (3) temperature stabilization stage: the thermal field is stabilized to a proper seeding temperature to prepare for fusion welding of the seed crystal and the silicon melt, and the argon flow is rapidly increased from 80SLPM to 100SLPM in the melting stage in the temperature stabilization stage;
and (3) seeding stage: the seed crystal is welded with the silicon melt, dislocation generated during solid-liquid contact is eliminated, argon flow in a seeding stage is controlled to be 100-110SLPM, the highest argon flow cannot exceed 120SLPM, a stable environment is provided for the welding process, the seed crystal is prevented from shaking in the dissolving process, in order to improve the crystallization rate, the upper limit of the welding diameter is controlled to be 16.5mm, the lower limit of the welding diameter is controlled to be 13mm, the minimum diameter value is 10mm, and the seeding gain value is adjusted to be 0.085;
a shouldering stage: adjusting the temperature and the pulling speed, amplifying the diameter to the required crystal diameter, controlling the diameter of the single crystal silicon rod to be 240-310mm, and controlling the flow of argon gas to be 100-120SLPM in the shouldering stage;
shoulder turning stage: after the diameter of the crystal reaches the specified requirement, the pulling speed and the temperature are adjusted, shoulder turning is carried out, so that the crystal can enter the stage of equal-diameter growth, and the flow of argon gas is controlled to be 100-SLPM in the shoulder turning stage;
and (3) an equal diameter stage: after the silicon rod reaches the specified diameter, entering an equal diameter stage, and controlling the growth process of the single crystal by controlling the pulling speed of the silicon rod of the single crystal and the temperature of the melt in the furnace, wherein the growth of the crystal at the stage tends to be stable, the flow of argon can be slightly reduced, and the flow of the argon is kept at 90-100 SLPM;
and (3) ending: the molten silicon in the crucible is continuously reduced along with the growth of the crystal, after the residual material reaches a certain weight, the diameter of the single crystal silicon rod is reduced by changing the pulling speed and the temperature, the dislocation generated when the crystal is separated from the liquid level is reduced by reducing the thermal shock during the pulling-off, and the argon flow can be reduced to 60-80SLPM at the stage.
Argon is introduced into the argon gas in each stage, and argon gas is introduced into the argon gas in the whole process, wherein the argon gas is 20-30 SLPM.
Example 2
A large-argon flow crystal pulling method for a large-size monocrystalline silicon rod comprises the steps of melting materials, stabilizing the temperature, seeding, shouldering, shoulder rotating, equal diameter and ending;
and (3) material melting stage: placing the silicon block into a quartz crucible, injecting argon, pressurizing to 25MPa, and heating and melting to form uniform silicon melt;
and (3) temperature stabilization stage: stabilizing the thermal field to a proper seeding temperature to prepare for fusion welding of the seed crystal and the silicon melt;
and (3) seeding stage: the seed crystal is welded with the silicon melt, dislocation generated during solid-liquid contact is eliminated, in order to improve the crystallization rate, the upper limit of the welding diameter is controlled to be 16.5mm, the lower limit of the welding diameter is controlled to be 13mm, the minimum diameter value is 10mm, and the seeding gain value is adjusted to be 0.085;
a shouldering stage: adjusting the temperature and the pulling speed, and amplifying the diameter to the required crystal diameter, wherein the diameter of the single crystal silicon rod is 240-310 mm;
shoulder turning stage: after the diameter of the crystal reaches the specified requirement, the pulling speed and the temperature are adjusted, and shoulder turning is carried out, so that the crystal can enter the stage of equal-diameter growth;
and (3) an equal diameter stage: after the silicon rod reaches the specified diameter, entering an equal diameter stage, and controlling the growth process of the single crystal by controlling the pulling speed of the silicon single crystal rod and the temperature of the melt in the furnace;
and (3) ending: the molten silicon in the crucible is continuously reduced along with the growth of the crystal, after the residual material reaches a certain weight, the diameter of the single crystal silicon rod is reduced by changing the pulling speed and the temperature, and the dislocation generated when the crystal is separated from the liquid level is reduced by reducing the thermal shock during the pulling-off.
Controlling the flow rate of the upper argon gas to be 100SLPM and the flow rate of the lower argon gas to be 20-30 SLPM.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (7)
1. A large-argon flow crystal pulling method for a large-size single crystal silicon rod is characterized by comprising the following steps: comprises melting, temperature stabilizing, seeding, shouldering, shoulder rotating, diameter equalizing and ending, wherein the flow of argon gas is kept at 90-120SLPM in the processes of temperature stabilizing, seeding, shouldering, shoulder rotating and diameter equalizing, and the furnace pressure is kept at 25 Mpa.
2. The large argon flow pulling method for large size single crystal silicon rods according to claim 1, wherein: keeping the upper argon flow at 100-; the shoulder rotating stage keeps the upper argon flow rate at 100-110 SLPM; and keeping the upper argon flow at 90-100SLPM in the equal diameter stage.
3. The large argon flow pulling method for large size single crystal silicon rods according to claim 2, wherein: keeping the upper argon flow at 90-120SLPM in the melting and ending stage.
4. The large argon flow pulling method for large size single crystal silicon rods according to claim 2, wherein: keeping the upper argon flow at 60-80SLPM in the melting and ending stage.
5. The large argon flow pulling method for large size single crystal silicon rods according to any one of claims 1 to 4, wherein: the lower argon flow is 20-30 SLPM.
6. The large argon flow pulling method for large size single crystal silicon rods according to claims 1 to 5, wherein: the upper limit of the fusion diameter in the seeding stage is 16.5mm, the lower limit of the fusion diameter is 13mm, and the minimum diameter value is 10 mm.
7. The large argon flow pulling method for large size single crystal silicon rods according to claim 6, wherein: the seeding gain value was 0.085.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910703397.3A CN112301425A (en) | 2019-07-31 | 2019-07-31 | Large-argon flow crystal pulling method for large-size monocrystalline silicon rod |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910703397.3A CN112301425A (en) | 2019-07-31 | 2019-07-31 | Large-argon flow crystal pulling method for large-size monocrystalline silicon rod |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112301425A true CN112301425A (en) | 2021-02-02 |
Family
ID=74485875
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910703397.3A Pending CN112301425A (en) | 2019-07-31 | 2019-07-31 | Large-argon flow crystal pulling method for large-size monocrystalline silicon rod |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112301425A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115323488A (en) * | 2022-08-16 | 2022-11-11 | 三一集团有限公司 | Process method and production system for pulling straight-pulling monocrystalline silicon |
| WO2024060650A1 (en) * | 2022-09-20 | 2024-03-28 | 隆基绿能科技股份有限公司 | Crystal pulling method, single-crystal silicon rod, and single crystal furnace |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1287789A (en) * | 1968-12-06 | 1972-09-06 | Kokusai Electric Co Ltd | Crystal pulling device |
| CN1480567A (en) * | 1996-10-15 | 2004-03-10 | Memc电子材料有限公司 | Method and apppts. for controlling oxygen content of reblended antimony or arsenic in silica chip |
| CN104328494A (en) * | 2014-11-14 | 2015-02-04 | 邢台晶龙电子材料有限公司 | Production method of solar grade czochralski monocrystalline silicon |
| CN105019017A (en) * | 2015-06-30 | 2015-11-04 | 内蒙古中环光伏材料有限公司 | Method used for reducing oxygen content of czochralski silicon |
-
2019
- 2019-07-31 CN CN201910703397.3A patent/CN112301425A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1287789A (en) * | 1968-12-06 | 1972-09-06 | Kokusai Electric Co Ltd | Crystal pulling device |
| CN1480567A (en) * | 1996-10-15 | 2004-03-10 | Memc电子材料有限公司 | Method and apppts. for controlling oxygen content of reblended antimony or arsenic in silica chip |
| CN104328494A (en) * | 2014-11-14 | 2015-02-04 | 邢台晶龙电子材料有限公司 | Production method of solar grade czochralski monocrystalline silicon |
| CN105019017A (en) * | 2015-06-30 | 2015-11-04 | 内蒙古中环光伏材料有限公司 | Method used for reducing oxygen content of czochralski silicon |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115323488A (en) * | 2022-08-16 | 2022-11-11 | 三一集团有限公司 | Process method and production system for pulling straight-pulling monocrystalline silicon |
| WO2024060650A1 (en) * | 2022-09-20 | 2024-03-28 | 隆基绿能科技股份有限公司 | Crystal pulling method, single-crystal silicon rod, and single crystal furnace |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8172943B2 (en) | Single Crystal manufacturing method | |
| US9885122B2 (en) | Method of manufacturing silicon single crystal | |
| CN105019017A (en) | Method used for reducing oxygen content of czochralski silicon | |
| CN111424313A (en) | Method for preparing gallium-doped monocrystalline silicon by RCZ (controlled-temperature zone) method | |
| CN106319620A (en) | Crystal pulling method for single crystal by Czochralski pulling | |
| US10494734B2 (en) | Method for producing silicon single crystals | |
| CN108203844B (en) | Magnesium tantalate series crystal and its preparing process | |
| CN112301425A (en) | Large-argon flow crystal pulling method for large-size monocrystalline silicon rod | |
| TWI774174B (en) | Seeding method for crystal growth | |
| JP4844428B2 (en) | Method for producing sapphire single crystal | |
| CN111321460A (en) | Method for preparing large-size low-oxygen silicon single crystal by RCZ (controlled-temperature zone) method | |
| JP6458590B2 (en) | Method for producing silicon single crystal | |
| JP2018150198A (en) | LARGE-DIAMETER ScAlMgO4 SINGLE CRYSTAL, AND GROWTH METHOD AND GROWTH UNIT THEREFOR | |
| WO2021020539A1 (en) | Scalmgo4 single crystal, preparation method for same, and free-standing substrate | |
| US20130340671A1 (en) | Silica glass crucible, method for manufacturing same, and method for manufacturing silicon single crystal | |
| US20090293802A1 (en) | Method of growing silicon single crystals | |
| US9376336B2 (en) | Quartz glass crucible, method for producing the same, and method for producing silicon single crystal | |
| CN113735071A (en) | Preparation method and device of high-purity gallium telluride | |
| CN106567125A (en) | Method for improving metallurgical-method polycrystalline silicon growth interface | |
| CN107794565B (en) | Seed crystal chuck and vertical pulling single crystal furnace | |
| CN109576778A (en) | A method of reducing the impurity content that CZ method prepares monocrystalline | |
| CN105970286B (en) | A kind of method of more crucible liquid phase epitaxy SiC crystals | |
| CN107955964A (en) | The preparation method and its hot systems of a kind of MEMS hypoxemia silicon single crystal materials | |
| CN112941615B (en) | Method for ending zone-melting silicon single crystal | |
| JP4702266B2 (en) | Single crystal pulling method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210202 |
|
| RJ01 | Rejection of invention patent application after publication |