CN106319621A - Large-size czochralski silicon single crystal growth method - Google Patents
Large-size czochralski silicon single crystal growth method Download PDFInfo
- Publication number
- CN106319621A CN106319621A CN201610841931.3A CN201610841931A CN106319621A CN 106319621 A CN106319621 A CN 106319621A CN 201610841931 A CN201610841931 A CN 201610841931A CN 106319621 A CN106319621 A CN 106319621A
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- Prior art keywords
- single crystal
- silicon single
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- large scale
- growth
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Classifications
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
-
- 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
- C30B15/14—Heating of the melt or the crystallised materials
-
- 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
Abstract
The invention relates to the field of single crystal silicon growth manufacturing, in particular to the technical field of large-size czochralski silicon single crystal growth. A large-size czochralski silicon single crystal growth method comprises the steps of charging, vacuum pumping, material melting through heating, seeding temperature regulation and seeding, shouldering, shoulder rotation, equal-diameter growth, finishing annealing and cooling, and is characterized in that a sealed tubular graphite heater group consisting of a plurality of arc flaky graphite heaters is used for heating a crucible for material melting; in the silicon single crystal growth process, each graphite heater maintains identical temperature; in the equal-diameter growth process, argon air flow enters a heat field system through a flow guide tube; a cooler is arranged at the inner side of the flow guide tube and is parallel to the guide flow tube. The method has the advantages that through the process, the heat convection in the horizontal direction is improved; the product quality is further improved; the growth interface is effectively cooled; the yield is improved to a certain degree.
Description
Technical field:
The present invention relates to monocrystalline silicon growing and manufacture field, particularly relate to a kind of large scale Modelling of Crystal Growth in CZ-Si Pulling technology neck
Territory.
Background technology
The growing technology of silicon single crystal can be divided into czochralski silicon monocrystal (CZ), zone-melted silicon single crystal (FZ), magnetic by process at present
Drawing silicon single crystal (MCZ) etc., these several growing methods are all growing silicon single crystals from melt.Additionally also have pedestal pulling method, platy-monocrystal
Growth method, web shape crystal growth method etc..In the above method for monocrystal growth, vertical pulling method (CZ) has equipment and technique is simple
Advantage, and easily realize Automated condtrol and become the main method of current silicon monocrystal growth.
The present age, czochralski silicon monocrystal developed towards high-purity, high integrality, high uniformity and large scale.But, silicon list
Crystal orientation large scale development, inventory sharply increases, and big melt produces serious thermal convection current, not only affects crystal mass, even can break
Bad crystal growth；Single crystal growing furnace single inventory increases, and thermal field of single crystal furnace size increases, the interval of heater distance melt central point
Elongated, in order to ensure single crystal growing furnace production safety, heating power can be strengthened accordingly, to ensure that Solutions Center point reaches suitable liquid level
Temperature, its operating rate has certain reduction, to reach the steady of growth interface, therefore, meeting as well as the rising of power simultaneously
Face the problem that growth rate is on the low side.
In order to solve thermal convection current problem, take now the way of magnetic field crystal pulling when growing large diameter silicon monocrystal, obtain
The large diameter silicon monocrystal that oxygen content is relatively low.Horizontal magnetic field unidirectional magnetic line of force structure so that the free convection of vertical direction
Viscosity strengthen, thermal convection current is effectively suppressed, but is horizontally oriented owing to its flow velocity direction is parallel with magnetic line of force direction, no
Being acted on by Lorentz force, so vertical direction relies primarily on conduction of heat and carries out heat transmission, and horizontal direction Heat transmission is still
Rely primarily on thermal convection current, be unfavorable for the growth of large scale high-quality monocrystal silicon.
The problem on the low side in order to solve growth rate, argon flow amount and argon are purged position by 201510970073.8 to be changed
Enter, enhance the action effect that growth interface is cooled down by argon, after ensureing that thermal field size increases, be positioned at optimal at growth interface
Crystal growth temperature range, overcomes the problem that large scale thermal field growth rate is on the low side, but argon passes through inside guide shell list
Crystalline silicon rod growth interface purges, and easily causes solution internal convection, may introduce impurity, affect monocrystal silicon quality.
Summary of the invention:
It is an object of the invention to provide a kind of large scale vertical pulling method of growing silicon single crystal, improve large size single crystal silicon further
Quality, improves the problem that growth rate is on the low side simultaneously.
For achieving the above object, the present invention is by the following technical solutions: a kind of large scale vertical pulling method of growing silicon single crystal, bag
Including following steps: charging, evacuation, add hot melt, seeding temperature regulation and seeding, shouldering, turn shoulder, isodiametric growth, ending is moved back
Fire and cooling, the closed tube graphite heater group using some arc sheet graphite heaters to form adds hot melt, silicon to crucible
After material fusing, during silicon monocrystal growth, each graphite heater heating mode is temp-controled mode, and each graphite heater keeps
Temperature is consistent, and during isodiametric growth, argon stream is through guide shell internal entrance thermal field system, and cooler is arranged in guide shell
Survey, and parallel with guide shell.
Preferably, the arc sheet graphite heater sheet number of the closed tube graphite heater group of composition is wanted by silicon single crystal quality
Asking decision, 3～5 preferably.
Preferably, adding hot melt, elect each graphite heater heating mode as power control mode, pressure pattern is elected as very
Empty pattern, uses low-voltage and high-current to make heater itself generate heat, and heats segmentation and carries out, heating power be gradually increased to 45～
55kw。
Preferably, seeding temperature regulation and seeding, after heating silicon material to fusing, each graphite heater heating mode is changed into
Temp-controled mode, regulation makes each graphite heater reach mutually synthermal, controls silicon liquid level of solution temperature so that it is reach solid-liquid and face
Boundary's temperature.
Preferably, seeding temperature regulation and seeding, after heating silicon material to fusing, first each graphite heater heating mode is changed
For temp-controled mode into, afterwards pressure pattern is changed gas mode, be first set as when gas mode is in 1200 DEG C giving vent to anger
Pattern, rises high-temperature and is set as air inlet pattern after 1500 DEG C.
Preferably, turn shoulder and improve pull rate, make raising speed be higher than isodiametric growth process pull rate more than 1.5 times.
Preferably, guide shell surface-coated heat-sink shell.
Preferably, cooler surface coating heat-sink shell.
More selection of land, heat-sink shell is graphite linings.
Compared with prior art, the invention have the advantages that
(1) the closed tube graphite heater group using some arc sheet graphite heaters to form adds hot melt to crucible,
After melting silicon materials, during silicon monocrystal growth, each graphite heater heating mode is temp-controled mode, it is achieved the essence to temperature
Really regulation and control, each graphite heater keeps temperature consistent so that melt level direction temperature contrast is effectively improved, and presses down to a certain extent
Having made the thermal convection current of horizontal direction, so while horizontal magnetic field suppression vertical direction thermal convection current, horizontal direction thermal convection current is also
It is effectively controlled, reduces the impurity such as the oxygen that thermal convection current causes, improve the quality of silicon single crystal；
(2) argon stream is through guide shell internal entrance thermal field system, and cooler is surveyed in being arranged on guide shell, and and guide shell
Parallel, increase film-cooled heat, effectively cool down growth interface, guide shell coats heat-sink shell with cooler surface, effectively absorbs hot spoke
Penetrating, strengthen cooling effect, above-mentioned process improves when pulling rate is fast, and the unit interval latent heat of release is many, causes knot
The problem of crystal boundary face Bending Influence product quality, improves the problem that growth rate is on the low side to a certain extent, improves productivity.
Accompanying drawing illustrates:
Fig. 1 is embodiment heating system partial top view；
Fig. 2 is embodiment single-crystal furnace guide shell fragmentary sectional view.
Detailed description of the invention:
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
Release the present invention, the present invention will not be constituted any restriction.
A kind of large scale vertical pulling method of growing silicon single crystal, comprises the following steps:
Charging, evacuation, be placed in silicon material in silica crucible 1, and evacuation takes out the air in stove, inserts high-purity argon
Gas, maintains certain negative pressure state, furnace pressure 100mbar in making stove；
Add hot melt, use the closed tube graphite heater group 2 of 4 arc sheet graphite heater 21 compositions to crucible 1
Heating, elects each graphite heater 21 heating mode as power control mode, and pressure pattern elects vacuum mode as, due to ingot furnace
Heater cold stage temperature controls instability, it is difficult to accurate temperature controlling, therefore elects heating mode as power control mode；With
Time, owing to there may be certain moisture in just starting stove or on silicon material, by selecting vacuum as pressure pattern, it is possible to be easy to
Drying heating furnace and silicon material.Using low-voltage and high-current to make heater itself generate heat, setting power is 20kw, and crucible is heated 10
Minute；Changing power into 30kw, it is constant that other arranges holding, continues to heat crucible 20 minutes；Change power into 40kw, other
It is constant that holding is set, continues crucible is heated 60 minutes；Changing power into 50kw, it is constant that other arranges holding, continues crucible
Heat 240 minutes；
Seeding temperature regulation and seeding, after heating silicon material to fusing, change each graphite heater 21 heating mode into temperature
Control model, changes by pressure pattern as gas mode into simultaneously, and regulation makes each graphite heater 21 reach mutually synthermal 1170 DEG C, gas
Bulk-mode is the pattern of giving vent to anger, and the impurity simultaneously making melting silicon materials process produce takes furnace chamber out of with gas, temperature-gradient method to 1200 DEG C,
Furnace pressure segmentation therewith rises to 500mbar, then temperature is upgraded to 1500 DEG C, and furnace pressure 500mbar, gas mode is for changing
For air inlet pattern, it is passed through argon gas and guarantees that silicon material is not oxidized in the condition of high temperature, control silicon liquid level of solution temperature so that it is reach
Solid-liquid critical temperature, the most slowly decline seed crystal is to chaotropic face 3～5mm distance, drops to solution surface, enter after making seed crystal preheating
Row seeding；
Shouldering, turn shoulder, seeding slows down pull rate after completing, reduce and make each graphite heater 21 reach mutually synthermal 1400
DEG C, reduce silicon solution temperature, make crystal grow to target size, improve pull rate 1.5mm/min, carry out turning shoulder.
Isodiametric growth, pull rate 0.6mm/min, argon stream is through guide shell 3 internal entrance thermal field system, cooler 4
Survey in being arranged on guide shell 3, and parallel with guide shell 3, argon stream cooling growth interface, guide shell 3 is coated with cooler 4 surface
Cover graphite linings, increase thermal-radiating absorption, improve cooling effect, to a certain degree improve isodiametric growth speed；
Ending annealing, each graphite heater 21 heating mode changes power control mode into, and pressure pattern remains gas mould
Formula, eliminates produced thermal stress in growth course, reduces dislocation；
Cooling, heating mode is converted to power control mode, and power gradually reduces to zero, and pressure pattern continues to remain
Gas mode, persistently leads to argon in stove, cool down 4.5h.
The present embodiment obtained silicon single crystal product do not improve the silicon single crystal product oxygen atom content of growing method have dropped 1 ×
10-6Above, productivity improves more than 5%.
Claims (9)
1. a large scale vertical pulling method of growing silicon single crystal, comprises the following steps: charging, evacuation, adds hot melt, seeding temperature
Regulation and seeding, shouldering, turn shoulder, isodiametric growth, ending annealing and cooling, it is characterised in that: use some arc sheet graphite to add
The closed tube graphite heater group of hot device composition adds hot melt to crucible, after melting silicon materials, during silicon monocrystal growth, and each stone
Ink heater heating mode is temp-controled mode, and each graphite heater keeps temperature consistent, during isodiametric growth, and argon gas
Flowing through guide shell internal entrance thermal field system, cooler is surveyed in being arranged on guide shell, and parallel with guide shell.
2. a kind of large scale vertical pulling method of growing silicon single crystal as claimed in claim 1, it is characterised in that: the closed tube of composition
The arc sheet graphite heater sheet number of graphite heater group is determined by silicon single crystal prescription, and 3～5 preferably.
3. a kind of large scale vertical pulling method of growing silicon single crystal as claimed in claim 1, it is characterised in that: add hot melt, by institute
Stating each graphite heater heating mode and elect power control mode as, pressure pattern elects vacuum mode as, uses low-voltage and high-current
Making heater itself generate heat, heating segmentation is carried out, and heating power is gradually increased to 45～55kw.
4. large scale vertical pulling method of growing silicon single crystal as claimed in claim 1 a kind of, it is characterised in that: seeding temperature regulation with
Seeding, after heating silicon material to fusing, changes by described each graphite heater heating mode as temp-controled mode into, and regulation makes each graphite
Heater reaches mutually synthermal, controls silicon liquid level of solution temperature so that it is reach solid-liquid critical temperature.
5. large scale vertical pulling method of growing silicon single crystal as claimed in claim 1 a kind of, it is characterised in that: seeding temperature regulation with
Seeding, after heating silicon material to fusing, first changes described each graphite heater heating mode into temp-controled mode, afterwards by pressure
Pattern changes gas mode into, is first set as the pattern of giving vent to anger when gas mode is in 1200 DEG C, rises high-temperature and sets after 1500 DEG C
It is set to air inlet pattern.
6. a kind of large scale vertical pulling method of growing silicon single crystal as claimed in claim 1, it is characterised in that: turn shoulder and improve lifting speed
Degree, makes raising speed be higher than isodiametric growth process pull rate more than 1.5 times.
7. a kind of large scale vertical pulling method of growing silicon single crystal as claimed in claim 1, it is characterised in that: described guide shell surface
Coating heat-sink shell.
8. a kind of large scale vertical pulling method of growing silicon single crystal as claimed in claim 1, it is characterised in that: described cooler surface
Coating heat-sink shell.
9. a kind of large scale vertical pulling method of growing silicon single crystal, it is characterised in that: described heat-sink shell
For graphite linings.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610841931.3A CN106319621A (en) | 2016-09-22 | 2016-09-22 | Large-size czochralski silicon single crystal growth method |
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| CN201610841931.3A CN106319621A (en) | 2016-09-22 | 2016-09-22 | Large-size czochralski silicon single crystal growth method |
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| CN201610841931.3A Withdrawn CN106319621A (en) | 2016-09-22 | 2016-09-22 | Large-size czochralski silicon single crystal growth method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106676625A (en) * | 2017-02-21 | 2017-05-17 | 洛阳金诺机械工程有限公司 | Blowing device for drawing silicon cores |
| CN107268071A (en) * | 2017-06-06 | 2017-10-20 | 界首市七曜新能源有限公司 | A kind of solar panel monocrystal silicon preparation technology |
| WO2020181795A1 (en) * | 2019-03-08 | 2020-09-17 | 宁夏隆基硅材料有限公司 | Heat shield apparatus for czochralski monocrystalline silicon and monocrystalline silicon production equipment |
| CN113604869A (en) * | 2021-08-11 | 2021-11-05 | 晶澳太阳能有限公司 | Growth method of monocrystalline silicon and seeding structure |
| TWI805508B (en) * | 2022-05-18 | 2023-06-11 | 大陸商西安奕斯偉材料科技股份有限公司 | Water cooling jacket and single crystal furnace |
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Application publication date: 20170111 |