CN115110143A - Production process of single crystal silicon rod - Google Patents
Production process of single crystal silicon rod Download PDFInfo
- Publication number
- CN115110143A CN115110143A CN202210809149.9A CN202210809149A CN115110143A CN 115110143 A CN115110143 A CN 115110143A CN 202210809149 A CN202210809149 A CN 202210809149A CN 115110143 A CN115110143 A CN 115110143A
- Authority
- CN
- China
- Prior art keywords
- single crystal
- silicon
- furnace
- crystal furnace
- crystals
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/002—Continuous growth
-
- 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
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
- C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
-
- 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
- C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
- C30B30/04—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using magnetic fields
Landscapes
- 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
The invention provides a production process of a silicon single crystal rod, and relates to the technical field of electronic material manufacturing. The method comprises the following steps: sorting and cleaning, batching, charging, melting, seeding, shouldering, equal-diameter growth, ending, taking out crystal bars and secondary feeding. The process adopts a magnetic field crystal pulling and continuous feeding process, improves the radial uniformity of the resistivity and the resistance value grading rate of the crystal bar, ensures that the quality of the monocrystalline silicon rod is higher than the industrial standard, and can produce lightly doped and heavily doped monocrystalline silicon rods with the resistivity range of 0.001-55 omega cm.
Description
Technical Field
The invention relates to the technical field of electronic material manufacturing, in particular to a production process of a silicon single crystal rod.
Background
Solar grade single crystal silicon wafers are the basic material for manufacturing single crystal silicon solar cells. The monocrystalline silicon rod is made from polycrystalline silicon by a zone melting method or a drawing method. The solar-grade silicon single crystal rod is produced by adopting a single crystal silicon furnace (Czochralski silicon furnace) pulling method. And after the silicon single crystal rod is successfully drawn, the silicon single crystal rod is subjected to round edge removal and is cut into a square body, and then a multi-wire cutting machine is used for cutting and processing to prepare the silicon single crystal wafer.
The prior Czochralski crystal pulling technology has two convection modes, namely natural convection and forced convection, wherein the natural convection is caused by temperature gradient, and the forced convection is caused by crystal rotation, crucible rotation and melt viscosity set during crystal pulling. In general, forced convection is relatively stable during crystal pulling; ideally, natural convection and forced convection are in a relationship tending to stabilize (critical state). However, in practical situations, the influence of natural convection is gradually strengthened, the ideal critical state is destroyed, the temperature oscillation of the crystal growth liquid surface is caused, the micro-segregation of impurities at the crystal interface is caused, and the optical property and the electrical property of the crystal are non-uniform.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a production process of a silicon single crystal rod, which solves the problems that the influence of natural convection is gradually strengthened, the ideal critical state is damaged, and the temperature of the liquid level of crystal growth is vibrated.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a production process of a single crystal silicon rod comprises the following steps:
s1, sorting and cleaning: screening out impurities in the silicon material, distinguishing the type and the resistivity of the silicon material, and cleaning and drying the screened silicon material;
s2, batching: calculating the weight of a dopant required by target resistivity by using the silicon material according to the feeding amount, crushing the silicon material into particles with the size of 5-25mm, and mixing the silicon material and the dopant in proportion;
s3, charge and melt: the method comprises the following steps of (1) filling a mixture of silicon particles and a doping agent into a secondary chamber of a single crystal furnace, filling the mixture in the secondary chamber of the single crystal furnace into a quartz crucible in a main chamber of the single crystal furnace through a feeding device, vacuumizing the single crystal furnace, heating the quartz crucible at 1450 ℃ through a graphite heating device, and then cooling to keep silicon in a solid-liquid critical state;
s4, seeding, shouldering and equal-diameter growth: electrifying a magnetic field device to generate a magnetic field in a main furnace of the single crystal furnace, then immersing the seed crystal arranged on a seeding device of the single crystal furnace into a melt, then pulling the seed crystal upwards to draw out the crystal and shrink the crystal, pulling the seed crystal to a certain length to prevent dislocation in the seed crystal from extending into the crystal for molten silicon, controlling the crystal to grow to a required diameter, pulling the seed crystal when the crystal grows to a preset diameter to ensure that the crystal vertically grows, wherein the melt silicon is conductive, the conductive fluid moves in the magnetic field, and current microelements of the fluid pass through magnetic force lines to generate ampere force acting on the magnetic force lines, and the direction of the ampere force is opposite to the movement direction of the current microelements, so that the heat convection of the fluid can be effectively reduced, and the performance and the uniformity of the crystal can be improved;
s5, ending and taking out the crystal bar: pulling the seed crystal to gradually reduce the diameter of the tail end of the crystal, leaving the melt, setting the pulling speed, cooling the crystal bar in the main chamber for a period of time, lifting the crystal bar into the auxiliary chamber of the single crystal furnace, introducing inert gas into the single crystal furnace, separating the seed crystal from the crystal bar, and taking out the crystal bar;
s6, secondary feeding: and (2) loading the mixture in the auxiliary chamber of the single crystal furnace into a quartz crucible in the main chamber of the single crystal furnace through a feeding device, vacuumizing the single crystal furnace, heating the quartz crucible at 1450 ℃ through a graphite heating device, and then cooling to keep the silicon in a solid-liquid critical state, thereby carrying out the secondary production of the silicon rod.
Preferably, the single crystal furnace is divided into a single crystal furnace main chamber and a single crystal furnace auxiliary chamber, and a seeding device, a magnetic field device and a heating device are arranged inside the single crystal furnace.
Preferably, a feeding device is arranged inside the auxiliary chamber of the single crystal furnace.
Preferably, a quartz crucible is arranged inside the main chamber of the single crystal furnace.
Preferably, an inert gas valve and a vacuum valve are arranged inside the single crystal furnace.
(III) advantageous effects
The invention provides a production process of a silicon single crystal rod. The method has the following beneficial effects:
1. the process enables the inside of the single crystal furnace to generate a magnetic field through a magnetic field device, the melt silicon is conductive, the conductive fluid moves in the magnetic field, the current infinitesimal of the fluid passes through the magnetic line of force to generate an ampere force acting on the magnetic line of force, and the direction of the force is opposite to the moving direction of the current infinitesimal, so that the thermal convection of the fluid can be effectively reduced, and the performance and the uniformity of the crystal can be improved.
2. According to the process, the silicon material and the doping agent are crushed and mixed uniformly, the mixture in the auxiliary chamber of the single crystal furnace can be filled into the quartz crucible in the main chamber of the single crystal furnace through the feeding device, the resistivity change of the silicon rod can be effectively reduced, and the quality of the monocrystalline silicon is higher.
3. By adopting the magnetic field crystal pulling and continuous feeding processes, the radial uniformity and the resistance value grading rate of the resistivity of the crystal rod are improved, the quality of the monocrystalline silicon rod is higher than the industrial standard, and the lightly doped and heavily doped monocrystalline silicon rods with the resistivity range of 0.001-55 omega cm can be produced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and 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.
The embodiment of the invention provides a production process of a silicon single crystal rod, which comprises the following steps:
s1, sorting and cleaning: screening out impurities in the silicon material, distinguishing the type and the resistivity of the silicon material, and cleaning and drying the screened silicon material;
s2, batching: calculating the weight of a dopant required by target resistivity by using the silicon material according to the feeding amount, crushing the silicon material into particles with the size of 5-25mm, and mixing the silicon material and the dopant in proportion;
s3, charge and melt: the method comprises the steps of filling a mixture of silicon particles and a doping agent into a secondary chamber of a single crystal furnace, filling the mixture in the secondary chamber of the single crystal furnace into a quartz crucible in a main chamber of the single crystal furnace through a feeding device, vacuumizing the single crystal furnace, heating the quartz crucible at 1450 ℃ through a graphite heating device, and cooling to keep silicon in a solid-liquid critical state, wherein the single crystal furnace is divided into the main chamber of the single crystal furnace and the secondary chamber of the single crystal furnace, a crystal seeding device, a magnetic field device and a heating device are arranged inside the single crystal furnace, the feeding device is arranged inside the secondary chamber of the single crystal furnace, the quartz crucible is arranged inside the main chamber of the single crystal furnace, and an inert gas valve and a vacuumizing valve are arranged inside the single crystal furnace.
S4, seeding, shouldering and equal-diameter growth: the magnetic field device is electrified to generate a magnetic field in the main furnace of the single crystal furnace, then the seed crystal arranged on the seeding device of the single crystal furnace is immersed into the melt, then the seed crystal is pulled upwards to lead out the crystal and is narrowed, the seed crystal is pulled to a certain length to prevent dislocation in the seed crystal from extending into the crystal for molten silicon, the crystal is controlled to grow to a required diameter, when the crystal grows to a preset diameter, the seed crystal is pulled to vertically grow the crystal, the melt silicon is conductive, the conductive fluid moves in the magnetic field, current microelements of the fluid pass through magnetic force lines to generate ampere force acting on the magnetic force lines, and the direction of the ampere force is opposite to the moving direction of the current microelements, so that the heat convection of the fluid can be effectively reduced, and the performance and uniformity of the crystal can be improved.
S5, ending and taking out the crystal bar: pulling the seed crystal to gradually reduce the diameter of the tail end of the crystal, leaving the melt, setting the pulling speed, cooling the crystal bar in the main chamber for a period of time, lifting the crystal bar into the auxiliary chamber of the single crystal furnace, introducing inert gas into the single crystal furnace, separating the seed crystal from the crystal bar, and taking out the crystal bar.
S6, secondary feeding: and (2) loading the mixture in the auxiliary chamber of the single crystal furnace into a quartz crucible in the main chamber of the single crystal furnace through a feeding device, vacuumizing the single crystal furnace, heating the quartz crucible at 1450 ℃ through a graphite heating device, and then cooling to keep the silicon in a solid-liquid critical state, thereby carrying out the secondary production of the silicon rod.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A production process of a single crystal silicon rod is characterized in that; the method comprises the following steps:
s1, sorting and cleaning: screening out impurities in the silicon material, distinguishing the type and the resistivity of the silicon material, and cleaning and drying the screened silicon material;
s2, batching: calculating the weight of a dopant required by target resistivity by using the silicon material according to the feeding amount, crushing the silicon material into particles with the size of 5-25mm, and mixing the silicon material and the dopant in proportion;
s3, charge and melt: the method comprises the following steps of (1) filling a mixture of silicon particles and a doping agent into a secondary chamber of a single crystal furnace, filling the mixture in the secondary chamber of the single crystal furnace into a quartz crucible in a main chamber of the single crystal furnace through a feeding device, vacuumizing the single crystal furnace, heating the quartz crucible at 1450 ℃ through a graphite heating device, and then cooling to keep silicon in a solid-liquid critical state;
s4, seeding, shouldering and equal-diameter growth: electrifying a magnetic field device to generate a magnetic field in a main furnace of the single crystal furnace, then immersing seed crystals arranged on a seeding device of the single crystal furnace into a melt, then pulling the seed crystals upwards to draw out the crystals and shrink the crystals to a certain length so as to prevent dislocation in the seed crystals from extending into the crystals for silicon in the melt shape, controlling the crystals to grow to a required diameter, pulling the seed crystals to enable the crystals to grow vertically when the crystals grow to a preset diameter, wherein the melt silicon is conductive, conductive fluid moves in the magnetic field, current microelements of the fluid pass through magnetic lines of force to generate ampere force acting on the magnetic lines, and the direction of the ampere force is opposite to the movement direction of the current microelements, so that the heat convection of the fluid can be effectively reduced, and the performance and uniformity of the crystals can be improved;
s5, ending and taking out the crystal bar: pulling the seed crystal to gradually reduce the diameter of the tail end of the crystal, leaving the melt, setting the pulling speed, cooling the crystal bar in the main chamber for a period of time, lifting the crystal bar into the auxiliary chamber of the single crystal furnace, introducing inert gas into the single crystal furnace, separating the seed crystal from the crystal bar, and taking out the crystal bar;
s6, secondary feeding: and (2) loading the mixture in the auxiliary chamber of the single crystal furnace into a quartz crucible in the main chamber of the single crystal furnace through a feeding device, vacuumizing the single crystal furnace, heating the quartz crucible at 1450 ℃ through a graphite heating device, and then cooling to keep the silicon in a solid-liquid critical state, thereby carrying out the secondary production of the silicon rod.
2. The process according to claim 1, wherein the silicon single crystal rod is produced by: the single crystal furnace is divided into a single crystal furnace main chamber and a single crystal furnace auxiliary chamber, and a seeding device, a magnetic field device and a heating device are arranged inside the single crystal furnace.
3. The process according to claim 2, wherein the silicon single crystal rod is produced by: and a feeding device is arranged in the auxiliary chamber of the single crystal furnace.
4. The process according to claim 2, wherein the silicon single crystal rod is produced by: a quartz crucible is arranged inside the main chamber of the single crystal furnace.
5. The process according to claim 1, wherein the silicon single crystal rod is produced by: an inert gas valve and a vacuum pumping valve are arranged in the single crystal furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210809149.9A CN115110143A (en) | 2022-07-11 | 2022-07-11 | Production process of single crystal silicon rod |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210809149.9A CN115110143A (en) | 2022-07-11 | 2022-07-11 | Production process of single crystal silicon rod |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115110143A true CN115110143A (en) | 2022-09-27 |
Family
ID=83332764
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210809149.9A Pending CN115110143A (en) | 2022-07-11 | 2022-07-11 | Production process of single crystal silicon rod |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115110143A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115545488A (en) * | 2022-10-11 | 2022-12-30 | 包头美科硅能源有限公司 | An automatic reporting method for the production of solar grade N-type monocrystalline silicon |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101435106A (en) * | 2008-11-21 | 2009-05-20 | 浙江瑞迪硅谷新能源科技有限公司 | Production process and apparatus for monocrystalline silicon rod |
| CN102220633A (en) * | 2011-07-15 | 2011-10-19 | 西安华晶电子技术股份有限公司 | Production technology of semiconductor grade silicon single crystal |
| CN110257901A (en) * | 2019-07-15 | 2019-09-20 | 乐山新天源太阳能科技有限公司 | The preparation process of major diameter high-efficiency N-type monocrystalline silicon |
| US20200141024A1 (en) * | 2017-04-25 | 2020-05-07 | Sumco Corporation | N-type silicon single crystal production method, n-type silicon single crystal ingot, silicon wafer, and epitaxial silicon wafer |
-
2022
- 2022-07-11 CN CN202210809149.9A patent/CN115110143A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101435106A (en) * | 2008-11-21 | 2009-05-20 | 浙江瑞迪硅谷新能源科技有限公司 | Production process and apparatus for monocrystalline silicon rod |
| CN102220633A (en) * | 2011-07-15 | 2011-10-19 | 西安华晶电子技术股份有限公司 | Production technology of semiconductor grade silicon single crystal |
| US20200141024A1 (en) * | 2017-04-25 | 2020-05-07 | Sumco Corporation | N-type silicon single crystal production method, n-type silicon single crystal ingot, silicon wafer, and epitaxial silicon wafer |
| CN110257901A (en) * | 2019-07-15 | 2019-09-20 | 乐山新天源太阳能科技有限公司 | The preparation process of major diameter high-efficiency N-type monocrystalline silicon |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115545488A (en) * | 2022-10-11 | 2022-12-30 | 包头美科硅能源有限公司 | An automatic reporting method for the production of solar grade N-type monocrystalline silicon |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106795647B (en) | Resistivity control method and n-type monocrystalline silicon | |
| CN103635613B (en) | Growth of a uniformly doped silicon ingot by doping only the initial charge | |
| CN112095141B (en) | Crystal pulling method, single crystal furnace and computer readable storage medium | |
| WO2007032799A1 (en) | Method and apparatus to produce single crystal ingot of uniform axial resistivity | |
| TW201840918A (en) | Methods for forming single crystal silicon ingots with improved resistivity control | |
| CN114959884B (en) | Seed crystal structure for growing monocrystalline silicon by Czochralski method and seeding process method | |
| CN110914483A (en) | Method for producing silicon single crystal | |
| CN115613125A (en) | Doping process of silicon material dopant | |
| CN115110143A (en) | Production process of single crystal silicon rod | |
| JP5318365B2 (en) | Silicon crystal material and method for producing FZ silicon single crystal using the same | |
| CN105239153B (en) | Single crystal furnace with auxiliary charging structure and application thereof | |
| JP2023162087A (en) | Method for growing gallium oxide single crystal by casting method, and semiconductor device including gallium oxide single crystal | |
| CN106498494A (en) | A kind of thermal field of MEMS making silicon single crystal material and preparation method | |
| CN113272479B (en) | Controlling dopant concentration in silicon melt to enhance ingot quality | |
| JP4060106B2 (en) | Unidirectionally solidified silicon ingot, manufacturing method thereof, silicon plate, solar cell substrate and sputtering target material | |
| CN117552084A (en) | Preparation method of ultralow-resistance monocrystalline silicon based on MCZ method | |
| JP5167942B2 (en) | Method for producing silicon single crystal | |
| JP2013121891A (en) | Method of manufacturing single crystal | |
| JP4595450B2 (en) | Method for producing carbon-doped silicon single crystal | |
| KR20030069822A (en) | Process for producing a highly doped silicon single crystal | |
| CN115058767B (en) | Doping method and device for preparing heavily-doped antimony monocrystal by MCZ (micro-channel chemical vapor deposition) method | |
| EP0205422A4 (en) | CONTINUOUSLY DRAWING SINGLE CRYSTAL SILICON BARS. | |
| WO2004065667A1 (en) | Process for producing single crystal | |
| KR100221087B1 (en) | Silicon single crystal growth method and silicon single crystal | |
| CN119753819A (en) | Method for preparing single crystal silicon and single crystal silicon |
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: 20220927 |
|
| RJ01 | Rejection of invention patent application after publication |