CN107923064A - Method for molten solids silicon - Google Patents
Method for molten solids silicon Download PDFInfo
- Publication number
- CN107923064A CN107923064A CN201680041964.8A CN201680041964A CN107923064A CN 107923064 A CN107923064 A CN 107923064A CN 201680041964 A CN201680041964 A CN 201680041964A CN 107923064 A CN107923064 A CN 107923064A
- Authority
- CN
- China
- Prior art keywords
- crucible
- silicon
- solid silicon
- upper opening
- solid
- 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
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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
- C30B15/14—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
-
- 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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
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)
- Silicon Compounds (AREA)
Abstract
A kind of method for molten solids silicon, including with solid silicon loaded crucible, at least a portion of wherein solid silicon is granular polycrystalline silicon；Heating crucible is to melt solid silicon present in crucible；With distributing for heat radiation is being prevented by upper opening in crucible during solid silicon melts；Once having changed into melt with solid silicon, then distributing for heat radiation is promoted by the upper opening in crucible.
Description
The present invention relates to the method for molten solids silicon, and the purpose is to provide for producing the molten of silicon single crystal according to CZ methods
Body.
CZ methods are the growing methods using the crucible equipped with melt, it is necessary to which the melt grows list as charging
It is brilliant.Before monocrystalline is grown, crucible is mounted with solid silicon and heats until melt composition.Growing through for monocrystalline allows at it
The crystal seed of upper growth monocrystalline starts with melt contacts.
It can be entered by the upper opening with circular cross section inside crucible.The diameter of cross section is usually with crucible
The increase for the melt volume for wanting to include and increase, and depending on monocrystalline diameter.
The solid silicon that crucible is loaded is typically polycrystalline.Nevertheless, crucible can also be mounted with such as monocrystalline into
Divide the monocrystalline silicon for being not suitable for production semiconductor crystal wafer.Polysilicon (Polycrystalline silicon) (abbreviation polysilicon
(polysilicon)) bulk form that can be particularly ground into rod provides.Rod by vapor deposited silicon by being formed.
When crucible is mounted with the bulk of polysilicon, considerable volume of unused storage space is left between bulk.In order to subtract
Granular silicon, can completely or partially be filled into crucible by few unused storage space.Granular silicon by fluid bed by gas
Mutually deposit silicon and formed, also polycrystalline.Granular polycrystalline silicon (Granular polycrystalline silicon) (letter
Claim granular polycrystalline silicon (granular polysilicon)) the gas such as hydrogen and chlorine of trace are included, these gases are in gas
Mutually it is incorporated to during deposition silicon.
2014/051539 A1 of WO are reported during the melting of granular polycrystalline silicon, the trace present in the granular polycrystalline silicon
When amount gas discharges suddenly, it may occur that the splashing of melt.
This splash from melt may also cause problem during crystal-pulling, particularly if in cooling
They are fallen into melt during crystal growth when being in solid-state afterwards.Splash from melt may for example be adhered to and be intended to shield
The monocrystalline of growth is covered from cooling down on the heat shield of laterally-incident heat radiation and on it.
The purpose of the present invention is reliably reduce the problem of such.
The purpose realizes that it includes by the method for molten solids silicon
With solid silicon loaded crucible, at least a portion of wherein solid silicon is granular polycrystalline silicon；
Heating crucible is to melt solid silicon present in crucible；With
Distributing for heat radiation is prevented by the upper opening in crucible during solid silicon melts；With
Once solid silicon has changed into melt, then distributing for heat radiation is promoted by the upper opening in crucible.
The inventors have studied the melting situation of granular polycrystalline silicon in crucible, and speculate in the melt relatively
Big temperature difference has played effect with the native oxide layer around granular polycrystalline silicon.The oxide skin(coating) is adiabatic, therefore grain
Shape polysilicon easily overheats, this is promoted by the temperature difference in melt.The superheat state causes the spontaneous molten of granular polycrystalline silicon
Melt, so as to cause the unexpected release of gas.
In order to avoid this sequence of events during melting, it is proposed that opened during solid silicon melts by the top in crucible
Mouth prevents distributing for heat radiation.The measure as a result, inside crucible more uniform temperature be distributed, this generates granular polycrystalline
Silicon is slowly and the condition that equably melts.
The preferred embodiment of the present invention is included in is used as heat radiation obstacle afterwards with solid silicon loaded crucible
Upper opening in lid covering crucible.Once solid silicon melts, then it will cover and remove to obtain the melt led to for crystal growth
Passage.
Lid is arranged in above solid silicon and preferably extends radially outward from the axis by crucible center.Lid is covered
Crucible in upper opening area preferably correspond to not less than crucible upper opening cross-sectional area 35%.If
Heat shield is arranged in above crucible and around the axis by crucible center, then the diameter covered is preferably no less than heat shield lower end
Internal diameter 85% and be less than the internal diameter.Lid is preferably placed at the certain altitude above crucible, in the height and crucible of its middle cover
Difference in height between brim height is preferably not less than zero.Beeline of the lid away from solid silicon is preferably more than 150mm.
The solid silicon that crucible loads includes a certain proportion of granular polycrystalline silicon.Weight fraction is preferably not less than 10%.Crucible
In solid silicon can also be entirely granular silicon.The solid silicon that crucible loads is preferably the mixture of bulk silicon and granular silicon.
According to a preferred embodiment of the invention, the slow and uniform melting of the solid silicon in crucible is by making earthenware
Crucible is in argon atmospher and the pressure of the atmosphere increases to the program of final pressure from initial pressure during solid silicon melts
To promote.The pressure increase is preferably realized in the constant flow rate lower linear of the argon gas by reactor shell.Initial pressure
It is preferred that in the range of 1kPa to 1.5kPa, final pressure is preferably in the range of 5kPa to 6kPa.
Attached drawing cited below shows herein below：
Fig. 1 is the side for the vertical cross-section for being used for the device according to CZ farads of silicon single crystal processed before molten solids silicon in crucible
View.It illustrate only the feature that the simplified present invention illustrates.The device includes the reactor with gas access 2 and gas vent 3
Housing 1.Atmosphere in reactor shell 1 is substantially made of argon gas, and argon gas introduces reactor shell 1 simultaneously via gas access 2
Discharged by gas vent 3 from reactor shell 1.Supported made of quartz, by support crucible (support crucible) 5
Crucible 4 be shelved on the rotatable axis 6 of liftable.Crucible 4 is mounted with the solid silicon of 8 form of bulk 7 and granular polycrystalline silicon.Institute
The device shown includes two heating units-side heater 9 and bottom heater 10, it provides the thermal energy needed for molten solids silicon.Earthenware
Crucible 4 has upper opening 12, which is limited by top edge 11 and to enter inside crucible.In crucible
4 tops are disposed with heat shield 13, it is intended to influence of the monocrystalline that shielding is then grown from the heat radiation sent by side heater 9.
Around an axis, which passes through on the extended line of the center of crucible 4 and the rotation axis in axis 6 heat shield 13.Once
Heating crucible 4, then heat radiation are also distributed by silicon just melted present in crucible 4 and molten.The heat radiation passes through earthenware
The lid 14 for distributing the upper opening 12 covered after with solid silicon loaded crucible 4 in crucible 4 of upper opening 12 in crucible 4
Stop.Lid 14 is arranged in above solid silicon and extends radially outward from the axis by 4 center of crucible.Once in crucible 4
Solid silicon melt completely, then withdraw lid 14 upwards, this is conducive to distribute heat radiation by the upper opening in crucible.With
Afterwards, in the position of lid 14, crystal seed is reduced to melt, to start crystal growth.
Fig. 2 is shown, is kept away during solid silicon melts by the suppression that the heat radiation of the upper opening in crucible distributes
Temperature Distribution in the case of exempting from and after being melted in the case that the suppression is not avoided by solid silicon at bath surface.
Due to inhibiting distributing for heat radiation by the upper opening in crucible, the temperature T along on the bath surface of crucible radius R
The distribution of (solid line) compares when the measure is avoided by (dotted line) significantly evenly.
Embodiment：
Silicon single crystal is produced according to CZ methods and compares the yield changed with the application of method according to the present invention.In solid
Silicon melt during by upper opening in crucible hinder heat radiation distribute realize 10% yield increase.
Claims (6)
1. a kind of method for solid silicon melting, including
With solid silicon loaded crucible, wherein at least a portion of the solid silicon is granular polycrystalline silicon；
The crucible is heated to melt solid silicon present in the crucible；With
Distributing for heat radiation is prevented by the upper opening in the crucible during the solid silicon melts；With
Once the solid silicon has changed into melt, then distributing for heat radiation is promoted by the upper opening in the crucible.
2. according to the method described in claim 1, including
The upper opening being used as after with solid silicon loaded crucible in the lid covering crucible of heat radiation obstacle；With
Once the solid silicon has become melt, then the lid is removed.
3. according to the method described in claim 2, wherein described drop cloth is put above solid silicon and preferably from by the earthenware
The axis at crucible center extends radially outward.
4. according to the method described in claim 3, it is characterized in that the lid covers pair of the upper opening in the crucible
35% areas of the Ying Yu not less than the cross-sectional area of the upper opening of the crucible.
5. method according to any one of claim 2 to 4, wherein the drop cloth is put away from the solid silicon certain distance
Place, the beeline of solid silicon described in its middle-range are no more than 150mm.
6. method according to any one of claim 1 to 5, wherein the crucible is subjected to argon atmospher, wherein described solid
The pressure of the atmosphere increases to final pressure from initial pressure during body silicon melts.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102015213474.1A DE102015213474A1 (en) | 2015-07-17 | 2015-07-17 | Process for melting solid silicon |
| DE102015213474.1 | 2015-07-17 | ||
| PCT/EP2016/061025 WO2017012733A1 (en) | 2015-07-17 | 2016-05-17 | Method for melting solid silicon |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107923064A true CN107923064A (en) | 2018-04-17 |
Family
ID=54053857
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201680041964.8A Pending CN107923064A (en) | 2015-07-17 | 2016-05-17 | Method for molten solids silicon |
Country Status (4)
| Country | Link |
|---|---|
| CN (1) | CN107923064A (en) |
| DE (1) | DE102015213474A1 (en) |
| TW (1) | TWI600807B (en) |
| WO (1) | WO2017012733A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110106546A (en) * | 2019-05-24 | 2019-08-09 | 浙江大学 | A kind of high finished product rate casting monocrystalline silicon growing method and thermal field structure |
| CN113862772A (en) * | 2021-09-27 | 2021-12-31 | 云南北方光学科技有限公司 | Preparation device of germanium window material for large-size infrared optics and method for preparing germanium window material for large-size infrared optics by using preparation device |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20220064816A1 (en) * | 2020-09-01 | 2022-03-03 | Globalwafers Co., Ltd. | Crystal pulling systems having a cover member for covering the silicon charge and methods for growing a melt of silicon in a crucible assembly |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1824848A (en) * | 2005-02-10 | 2006-08-30 | 硅电子股份公司 | Process for producing a silicon single crystal with controlled carbon content |
| TWM485251U (en) * | 2014-04-03 | 2014-09-01 | Globalwafers Co Ltd | Crystal growth apparatus and thermal insulation cover thereof |
| CN104685113A (en) * | 2012-09-10 | 2015-06-03 | Gtatip控股有限责任公司 | Continuous CZ method and apparatus |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03193694A (en) * | 1989-12-21 | 1991-08-23 | Sumitomo Metal Ind Ltd | Crystal growing device |
| US6313398B1 (en) * | 1999-06-24 | 2001-11-06 | Shin-Etsu Chemical Co., Ltd. | Ga-doped multi-crytsalline silicon, Ga-doped multi-crystalline silicon wafer and method for producing the same |
| JP5413354B2 (en) * | 2010-10-22 | 2014-02-12 | 株式会社Ｓｕｍｃｏ | Silicon single crystal pulling apparatus and silicon single crystal manufacturing method |
| WO2014051539A1 (en) * | 2012-09-25 | 2014-04-03 | Memc Electronic Materials S.P.A. | Method for preparing molten silicon melt using high pressure meltdown |
-
2015
- 2015-07-17 DE DE102015213474.1A patent/DE102015213474A1/en not_active Ceased
-
2016
- 2016-05-17 CN CN201680041964.8A patent/CN107923064A/en active Pending
- 2016-05-17 WO PCT/EP2016/061025 patent/WO2017012733A1/en active Application Filing
- 2016-07-12 TW TW105121889A patent/TWI600807B/en active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1824848A (en) * | 2005-02-10 | 2006-08-30 | 硅电子股份公司 | Process for producing a silicon single crystal with controlled carbon content |
| CN104685113A (en) * | 2012-09-10 | 2015-06-03 | Gtatip控股有限责任公司 | Continuous CZ method and apparatus |
| TWM485251U (en) * | 2014-04-03 | 2014-09-01 | Globalwafers Co Ltd | Crystal growth apparatus and thermal insulation cover thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110106546A (en) * | 2019-05-24 | 2019-08-09 | 浙江大学 | A kind of high finished product rate casting monocrystalline silicon growing method and thermal field structure |
| CN113862772A (en) * | 2021-09-27 | 2021-12-31 | 云南北方光学科技有限公司 | Preparation device of germanium window material for large-size infrared optics and method for preparing germanium window material for large-size infrared optics by using preparation device |
Also Published As
| Publication number | Publication date |
|---|---|
| TWI600807B (en) | 2017-10-01 |
| TW201704558A (en) | 2017-02-01 |
| WO2017012733A1 (en) | 2017-01-26 |
| DE102015213474A1 (en) | 2015-09-24 |
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| 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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180417 |