CN1200147C - Method of speeding smelting of polycrystalline material and bottom heater for pulling monocrystal - Google Patents
Method of speeding smelting of polycrystalline material and bottom heater for pulling monocrystal Download PDFInfo
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- CN1200147C CN1200147C CNB021176035A CN02117603A CN1200147C CN 1200147 C CN1200147 C CN 1200147C CN B021176035 A CNB021176035 A CN B021176035A CN 02117603 A CN02117603 A CN 02117603A CN 1200147 C CN1200147 C CN 1200147C
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- heating element
- bottom heater
- hole
- discoid
- heating unit
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- 238000000034 method Methods 0.000 title abstract description 24
- 239000000463 material Substances 0.000 title description 2
- 238000003723 Smelting Methods 0.000 title 1
- 238000010438 heat treatment Methods 0.000 claims abstract description 62
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 229910002804 graphite Inorganic materials 0.000 claims description 16
- 239000010439 graphite Substances 0.000 claims description 16
- 239000013078 crystal Substances 0.000 abstract description 49
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 30
- 229910052710 silicon Inorganic materials 0.000 abstract description 30
- 239000010703 silicon Substances 0.000 abstract description 30
- 239000010453 quartz Substances 0.000 abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 23
- 229910052732 germanium Inorganic materials 0.000 abstract description 6
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 abstract 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 22
- 229920005591 polysilicon Polymers 0.000 description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 4
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 241000033695 Sige Species 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
The present invention relates to a method and a device for accelerating fusing of polycrystal raw materials during drawing single crystals, which is a method for accelerating fusing of polycrystal raw materials during controlling single crystals and a bottom heating unit device. The present invention can be used for accelerating fusing of polycrystal silicon and polycrystalline germanium. The method comprises the following steps: direct current is led into a main heating unit; direct current is led into the bottom heating unit (a discoid heating unit); a quartz crucible is heated respectively from the side surface and the bottom of the quartz crucible. The device of the present invention is composed of a discoid heating unit and two electrodes, wherein a through hole groove and two electrode holes are positioned on the discoid heating unit. The present invention shortens the fusing time of polycrystal silicon raw materials and increases the yield of single crystal silicon in unit time. The bottom heating unit has the advantages of simple structure, easy production and obvious effect.
Description
(1) technical field
When the present invention relates to pulling monocrystal, accelerate the device of polycrystal raw material melting method, more specifically say so when drawing the silicon single-crystal germanium single crystal, accelerate the heating element that install polysilicon polycrystalline germanium method of fusion and single crystal growing furnace thereof bottom.
(2) background technology
The major part of semiconductor silicon single crystal body is all with cutting krousky (Czochralski) manufactured.In this method, polysilicon is put in the quartz crucible, heat fused then, will melt silicon and slightly do cooling, give certain condensate depression, the silicon single crystal of a particular crystal orientation (being called seed crystal) is contacted with melt silicon, and temperature by adjusting melt and the seed crystal pulling speed that makes progress is when making seed body grow up to the close-target diameter, improve pulling speed, make the nearly permanent growth in thickness of single crystal.In the last stage of process of growth, the interior silicon melt not completely dissolve as yet of crucible this moment, by the heat supplied that increases the crystalline pulling speed and adjust crystal diameter is reduced to form a tail shape cone gradually to crucible, when sharp enough hour of cone, crystal will break away from melt, thereby finishes the crystalline process of growth.
Czochralski silicon monocrystal roughly is divided into so several stages during fabrication: the dress polycrystal, find time, growth, equal diameter growth, the growth of afterbody crystalline, the crystal cooling of unmelted polycrystalline silicon, neck and shoulder, wherein most of process is an endothermic process, that is to say to want outside heat supplied.A heating element (graphite system) is generally arranged in the single crystal growing furnace, and direct current on its two ends lead to produces heat.Heating element is in the outside of heat-absorbing body, that is to say, heat is ecto-entad conduction (radially).Increasing (Φ 200mm along with the silicon single-crystal diameter, Φ 300mm, more than the Φ 300mm), the size of thermal field of single crystal furnace becomes increasing, caused that the thermal field radial temperature difference strengthens (temperature head at thermal field core temperature and polysilicon supporting apparatus edge), thermal field is temperature head also very big (the central upper portion temperature of polycrystalline supporting apparatus bottom centre's temperature and polycrystalline supporting apparatus poor) longitudinally, and this makes polysilicon melt (tens time) for a long time fully.
Because the single crystal growing furnace that is used for pulling monocrystal of the prior art, especially the monocrystal stove of pulling monocrystal silicon all is a heating element, between the quartz crucible supporting apparatus 14 and heat-preservation cylinder 18 of the graphite system of being installed in, silicon single-crystal, germanium single crystal enlarged diameter, thus cause the radial temperature difference of thermal field and thermal field longitudinally the temperature difference strengthen, polysilicon is melted fully need be for a long time, production efficiency reduces, in order to enhance productivity, shorten the fusing time of polysilicon, just become the anxious technical issues that need to address.
(3) summary of the invention
Purpose of the present invention just is to work out a kind of heating means of new polysilicon, makes polycrystal raw material, and especially the fusing time of polysilicon shortens greatly.
Another object of the present invention is developed in the single crystal growing furnace exactly, the bottom heater device one secondary heating element device of the thermal field bottom of (especially in the monocrystal stove), and the technology that unmelted polycrystalline silicon is especially accelerated in the fusing of quickening polycrystal raw material is achieved.
Accelerate the melting method of polycrystal raw material during a kind of pulling monocrystal of the present invention, in quartz crucible, add polycrystal raw material, furnace chamber closes, and vacuumize, in single crystal growing furnace, be installed in the quartz crucible supporting apparatus and the main heating element between the heat-preservation cylinder of graphite system, feed direct current, side heat quartz crucible from quartz crucible, in the bottom of single crystal growing furnace the bottom heater device is housed, to main heating element feed galvanic to the time, feed direct current in the discoid heating element in the bottom heater device,, accelerate the molten method of polycrystal raw material from the bottom heating quartz crucible of quartz crucible.
Close behind the furnace chamber, be evacuated to 1.33 * 10
3-1.33 * 10
4Pa is for well.Said polycrystal raw material is a polysilicon, wherein a kind of of many SiGes, feeding galvanic voltage in main heating element is the 20-60 volt, electric current is the 1500-5000 ampere, the galvanic voltage that feeds in the discoid heating element of bottom heater device is the 10-60 volt, and electric current is the 500-1000 ampere.
A kind of bottom heater device of accelerating the polycrystal raw material fusing when being used for pulling monocrystal of the present invention, comprise graphite rounding plate-like heating element 22 and two electrodes 21, there is a central circular hole 23 in discoid heating element central authorities, with central circular hole 23 is that the center has the sensing disc circumference, cross section is rectangular through-hole groove 24, there is required distance on the top 25 of through-hole groove 24 with the periphery of disk, having from the cross section of disc circumference sensing central circular hole 23 between two through-hole grooves 24 is rectangular through-hole groove 26, the top 27 and the central circular hole 23 of through-hole groove 26 have required distance, two electrode holes 28 are arranged at the top of two through-hole grooves 24, two electrodes 21 are connected with discoid heating element 22 by two electrode holes 28.
For well, the top 25 of through-hole groove 24 is 1.0mm-150mm with the distance of disc circumference to the cross section on the top 25 of through-hole groove 24 with circular arc, and the cross section on the top 27 of through-hole groove 26 is that circular arc is advisable.The top 27 of through-hole groove 26 is 10mm-150mm with the distance of central circular hole 23.Two electrode holes 28 are with good to being called.Discoid heating element and electrode are made by semiconductor-grade graphite.The thickness of graphite rounding plate-like heating element is 10-50mm.Main heating element has 4 electrodes 20, and bottom heater (discoid heating element, secondary heating element) has two electrodes 21.The wide of through-hole groove 24,26 is 5mm-50mm.The diameter of discoid heating element is 500mm-1000mm.The diameter of central circular hole 23 is 50-200mm.
Be installed in the graphite axis by discoid heating element central circular hole in use,, be connected with discoid heating element, and the method for all knowing with those skilled in the art is with they good insulation with bottom heater electrode 21 by two electrode holes 28.
With polycrystal raw material for example after the polycrystalline silicon raw material fusing, the method pulling monocrystal body of all knowing with those skilled in the art, for example silicon single-crystal barred body.
In the silicon monocrystal growth process, be negative pressure state in the stove, must constantly charge into argon shield, make the argon gas that contains silicon monoxide remain on 1.33 * 10
3-1.33 * 10
4Pa, the temperature of progressively falling silicon melt makes quartz crucible and seed crystal reverse rotation near the fusing point of silicon, and the quartz crucible speed of rotation is 4-20 rev/min, and the speed of rotation of seed crystal is 8-30 rev/min.Silicon seed is slowly descended, and contact with silicon melt, the back upwards promotes seed crystal with the speed of 0.8mm/min-5mm/min.The purpose of this process mainly is to eliminate the dislocation defects that forms because of thermal shocking in the seed crystal, when treating that seed crystal rises to certain-length (50mm-300mm), pulling speed is slowed to 0.4mm/min-0.6mm/min, reduce simultaneously about the temperature to 1418 ℃ of silicon melt, make the seed crystal enlarged diameter, when the seed crystal diameter increases to than the low approximately 10mm-20mm of aimed dia, increase pulling speed to 1.27mm/min-2.5mm/min, make crystal be close to the equal diameter growth, it is the so-called isodiametric growth stage, generally be about about 1.5mm/min at isodiametric growth stage pulling rate, be reduced to about 0.4mm/min-0.8mm/min gradually.The silicon material of storing in quartz crucible enters the ending stage not for a long time, and pulling rate is 0.6mm/min-1.2mm/min, suitably increase the power of heating simultaneously, make crystal diameter be changed to a back taper, when boring point enough hour, it can break away from silicon melt, and at this moment the crystalline process of growth finishes.Be cooled to when being close to room temperature in crystal, crystal is taken off.The crystal bar that is generated is a conical object, has a central shaft, a seed crystal end cone and a tail cone body, and be the right cylinder of near constant diameter between two cones.
The advantage that a kind of pulling monocrystal of the present invention is accelerated polycrystal raw material method of fusion and bottom heater device just is:
1. improved the temperature of graphite system quartz crucible supporting apparatus bottom with method of the present invention, changed temperature distribution in original thermal field, changed the heat-supplying mode of thermal field of single crystal furnace, reduced radially, the temperature difference longitudinally, shortened the time that polycrystal raw material melts fully greatly, especially greatly shorten the complete fusing time of polysilicon, and increased the concentration of oxygen in the czochralski silicon monocrystal.This is because the heat that provides makes the oxygen in the quartz crucible diapire be easy to enter silicon melt with the form of SiO.Save electric energy, increased the output of silicon single crystal in the unit time.
Table 1 bottom heater is to the influence of the complete fusing time of polysilicon
Whether use the bottom heater total power, KW (the complete fusing time of bottom disc shape polysilicon,
Heating element 22+ main heating element 7) hour
Do not use bottom heater 0+,100 7
Use bottom disc shape heating 13,+87 5.5
Body
2. of the present invention having wide range of applications is applicable to that not only accelerating polysilicon melts fully, also can accelerate polycrystalline germanium and melt fully.
3. of the present invention when being used for pulling monocrystal silicon, accelerate the bottom heater device of polycrystal fusing, it is simple in structure, is easy to make, and has shortened the time that polycrystal raw material melts fully greatly, has shortened the time of fusing fully of polysilicon especially greatly.
(4) description of drawings
Fig. 1 has the single crystal growing furnace diagrammatic cross-section of cutting krousky (vertical pulling) manufactured silicon single-crystal of bottom heater.
Omit supporting structure, bell, crystal in the drawings and lifted the cabin, lifting rod, the form part, segregaion valve, the single crystal growing furnace shell is made by stainless steel.
Among the figure, 1 is seed crystal, and 3 is silicon single crystal bar, 4 is loam cake, 5 carbon lagging materials, and 6 is the temperature signal hole, 7 is graphite heater, and 8 is crystal growing chamber, and 9 is venting port, 10 are anti-drain cap, and 11 is the graphite axis, and 12 is the carbon thermal insulation layer, 13 is silicon melt, and 14 is the quartz crucible supporting apparatus of graphite system, and 16 is quartz crucible, 17 is the bottom heater device, and 18 is heat-preservation cylinder.
The discoid heating element diagrammatic cross-section of Fig. 2 bottom heater device 17.
Among the figure, 22 is discoid heating element, 23 is discoid heating element central circular hole, 24 cross sections for the sensing disc circumference are the rectangular through holes groove, 25 for cross section be the top of rectangular through holes groove 24,26 cross sections for periphery sensing central circular hole 23 are the rectangular through holes groove, and 27 for cross section is the top of rectangular through holes groove 26, and 28 is electrode hole.
What Fig. 3 increased silicon monocrystal growth chamber behind the bottom heater just cuts open synoptic diagram.
Among the figure, 8 is crystal growing chamber, and 19 is the crystal growing chamber bottom surface, and 20 is main heating element electrode (totally four), and 21 is the electrode (totally 2) of discoid heating element (secondary heating element).
(5) embodiment
Below the present invention is further illustrated with indefiniteness embodiment, can help the better understanding to the present invention and advantage thereof, effect, and protection scope of the present invention is decided by claim.
Embodiment 1
Accelerate the melting method of silicon single crystal during the pulling monocrystal silicon of present embodiment, in quartz crucible, add polysilicon 120Kg, the furnace chamber that closes, and be evacuated to 2.66 * 10
3Pa is installed in the quartz crucible supporting apparatus of graphite system and the main heating element 7 between the heat-preservation cylinder in monocrystal stove, feed direct current, and its voltage is 30 volts, and 2900 amperes in electric current, power are 87Kw, from the side heat quartz crucible of quartz crucible.Bottom heater (discoid heating element) is housed in the bottom of monocrystal stove, feeds direct current in bottom heater (disk heating element 22), its voltage is 20 volts, 650 amperes in electric current, power 13Kw from quartz crucible bottom heating quartz crucible, makes polysilicon fusing fully in 5.5 hours.
Present embodiment be used for pulling monocrystal the time accelerate the bottom heater device of unmelted polycrystalline silicon, form by graphite rounding plate-like heating element 22 and two electrodes 21, there is a central circular hole 23 in the central authorities of discoid heating element 22, with central circular hole 23 is that the cross section that points to disc circumference is arranged is rectangular through-hole groove 24 at the center, totally 10, the vertical cross section of through-hole groove 24 is a circular arc, the top 25 of through-hole groove 24 is 10mm with the distance with disc circumference, having from the cross section of disc circumference sensing central circular hole 23 between two through-hole grooves 24 is rectangular through-hole groove 26, totally 10, the vertical cross section of through-hole groove 26 is a circular arc, the top 27 of through-hole groove 26 is 10mm with the distance of central circular hole 23, two symmetric electrode holes 28 are arranged at the top of two through-hole grooves 24, by electrode hole 28, two electrodes 21 are connected with discoid heating element 22, discoid heating element 22 and electrode 21 are made by semiconductor-grade graphite, the thickness of graphite rounding plate-like heating element is 35mm, through-hole groove 24, the wide of through-hole groove 26 is 5mm.The diameter of discoid heating element is 500mm.The diameter of central circular hole is 100mm.Main heating element has 4 electrodes 20, and discoid heating element 22 (secondary heating element) has two electrodes.
Comparing embodiment
Its working method and equipment are substantially with embodiment 1, only different is not add bottom heater (discoid heating element) only to feed direct current in monocrystal stove in main heating element, 40 volts of its voltages, 2500 amperes in electric current, fusing fully in polysilicon 120Kg7 hour.
Embodiment 2
Its working method and equipment are substantially with embodiment 1, and only different is that bottom heater (discoid heating element) feeds galvanic current, and its voltage is 60 volts, 883 amperes in electric current, add main heating element power, total power is 100KW, and the time that the 120kg polysilicon melts fully is 4.5 hours.
Embodiment 3
Its working method and equipment are fully with embodiment 1, and only different is heat fused 120kg polycrystalline germanium, and Rong Hua time is 1 hour fully.
Claims (6)
1. a bottom heater device of accelerating the polycrystal raw material fusing when being used for pulling monocrystal is characterized in that,
1) comprise graphite disk shape heating element (22) and two electrodes (21),
2) there is a central circular hole (23) in discoid heating element central authorities, are that the center has and points to disc circumference with central circular hole (23), and cross section is rectangular through-hole groove (24), and the top (25) of through-hole groove (24) is 10mm-150mm with the distance of the periphery of disk,
3) having from the cross section of disc circumference sensing central circular hole (23) between two through-hole grooves (24) is rectangular through-hole groove (26), and the top (27) of through-hole groove (26) is 10mm-150mm with the distance of central circular hole (23),
4) at the top of two through-hole grooves (24) two electrode holes (28) are arranged,, two electrodes (21) are connected with discoid heating element (22) by two electrode holes (28).
2. accelerate the bottom heater device of polycrystal raw material fusing when being used for pulling monocrystal according to claim 1 a kind of, it is characterized in that the cross section on the top (25,27) of through-hole groove (24) and through-hole groove (26) is circular arc.
3. accelerate the bottom heater device of polycrystal raw material fusing when being used for pulling monocrystal according to claim 1 a kind of, it is characterized in that two electrode holes (28) symmetry.
4. accelerate the bottom heater device of polycrystal raw material fusing when being used for pulling monocrystal according to claim 1 a kind of, it is characterized in that the thickness of discoid heating element is 10-50mm.
5. accelerate the bottom heater device of polycrystal raw material fusing when being used for pulling monocrystal according to claim 1 a kind of, it is characterized in that, through-hole groove (24), the width of through-hole groove (26) is 5mm-50mm.
6. accelerate the bottom heater device of polycrystal raw material fusing when being used for pulling monocrystal according to claim 1 a kind of, it is characterized in that the diameter of discoid heating element (22) is 500mm-1000mm; The diameter of its central circular hole (23) is 50mm-200mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021176035A CN1200147C (en) | 2001-10-30 | 2002-05-08 | Method of speeding smelting of polycrystalline material and bottom heater for pulling monocrystal |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN01134282.X | 2001-10-30 | ||
| CN01134282 | 2001-10-30 | ||
| CNB021176035A CN1200147C (en) | 2001-10-30 | 2002-05-08 | Method of speeding smelting of polycrystalline material and bottom heater for pulling monocrystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1417388A CN1417388A (en) | 2003-05-14 |
| CN1200147C true CN1200147C (en) | 2005-05-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021176035A Expired - Lifetime CN1200147C (en) | 2001-10-30 | 2002-05-08 | Method of speeding smelting of polycrystalline material and bottom heater for pulling monocrystal |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102505145B (en) * | 2011-10-28 | 2014-12-10 | 江西赛维Ldk太阳能多晶硅有限公司 | Graphite preheating piece, semiconductor preheating device, silicon core furnace and phosphorus detection furnace |
| CN103545162B (en) * | 2012-07-09 | 2016-06-08 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Plasma reaction device and quartz window heating means |
| CN105239154A (en) * | 2015-09-10 | 2016-01-13 | 上海超硅半导体有限公司 | Czochralski method single-crystal silicon growth flow field control technology |
| CN109554755A (en) * | 2018-12-19 | 2019-04-02 | 西安奕斯伟硅片技术有限公司 | A kind of heating equipment and production of polysilicon equipment |
| CN114293256B (en) * | 2021-12-30 | 2023-06-27 | 中国有研科技集团有限公司 | Thermal field and growth process for growing dislocation-free germanium single crystal by Czochralski method |
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