CN1095505C - Vertical pulling and zone melting process of producing monocrystalline silicon - Google Patents
Vertical pulling and zone melting process of producing monocrystalline silicon Download PDFInfo
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- CN1095505C CN1095505C CN00105518A CN00105518A CN1095505C CN 1095505 C CN1095505 C CN 1095505C CN 00105518 A CN00105518 A CN 00105518A CN 00105518 A CN00105518 A CN 00105518A CN 1095505 C CN1095505 C CN 1095505C
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- 238000004857 zone melting Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title abstract description 25
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title description 2
- 239000013078 crystal Substances 0.000 claims abstract description 91
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 55
- 239000010703 silicon Substances 0.000 claims abstract description 55
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 claims abstract description 23
- 229910052786 argon Inorganic materials 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 238000010899 nucleation Methods 0.000 claims abstract description 3
- 230000007797 corrosion Effects 0.000 claims abstract 2
- 238000005260 corrosion Methods 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000000498 cooling water Substances 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 16
- 239000001301 oxygen Substances 0.000 abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 abstract description 16
- 230000007547 defect Effects 0.000 abstract description 4
- 238000007493 shaping process Methods 0.000 abstract description 2
- 210000003739 neck Anatomy 0.000 abstract 2
- 238000005086 pumping Methods 0.000 abstract 2
- 238000003466 welding Methods 0.000 abstract 2
- 230000008602 contraction Effects 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 5
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 238000002231 Czochralski process Methods 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to Czochralski zone-melting method for producing silicon single crystals, which is completed by a Czochralski furnace and a zone-melting furnace. The method comprises the procedures: 1. materials are loaded in the Czochralski furnace for pumping vacuum and filling argon; 2. heating is carried out for melting the materials and welding seed crystals; 3. thin necks are pulled; shoulder contraction is carried out; 5. isometric growth is carried out; 6. ending is carried out; 7. cooling is carried out for the discharging materials; 8. the shaping of polycrystal rods and wash of corrosion are carried out; 9. the polycrystal rods are loaded in the zone-melting furnace for pumping vacuum and filling argon; 10. the materials are melted by preheating for welding seed crystals; crystal seeding is carried out for pulling narrow necks; 12. extension of shoulders is carried out for isometric growth; 13. tails are in tensile failure; 14. cooling is carried out for furnace shutdown and crystal discharge. The present invention overcomes the defect of high oxygen content in Czochralski silicon, the oxygen content of produced silicon single crystals is 10<16>atm/cm<3> with good thermal stability, and the defect that special solid elements can not be doped by a zone-melting method is overcome. Special solid elements can be doped, the productivity of zone-melting furnaces can be improved, production cost is reduced, and the period of production is shortened.
Description
The invention relates to a Czochralski zone melting method for producing silicon single crystals.
Almost all silicon single crystals are currently produced by the Czochralski method or the float zone method. However, the oxygen content of the silicon single crystal produced by the Czochralski method is as high as 1018atm/cm3The thermal instability and reversibility of resistivity caused by the formed oxygen donors cause the limitation and difficulty of the Czochralski silicon single crystal in the manufacturing process of power devices. Although the silicon single crystal produced by the zone melting method can reduce the oxygen content, the silicon single crystal has high production cost, is difficult to have low specific resistance, has poor radiation resistance, and can not be doped with other required special solid elements, thereby limiting the wide application of the silicon single crystal in the field of producing devices. Technologically, the silicon physical detector and the anti-radiation reinforcing device require low oxygen content (1 × 10)16atm/cm3) The silicon single crystal has good thermal stability, and is doped with special solid elements, which is difficult to achieve the full beauty of both the Czochralski method and the zone melting method.
The invention aims to provide a Czochralski zone melting method for producing silicon single crystals, which can meet the requirements of low oxygen content and doping of special solid elements.
The purpose of the invention is realized as follows: the production equipment comprises a straight pulling furnace and a zone melting furnace, and the manufacturing method comprises the following steps: (1) loading a silicon polycrystal material into a straight-pull furnace, vacuumizing and filling argon gas, (2) heating and melting a material to weld seed crystals, (3) thinning a neck, (4) shouldering and shouldering, (5) growing in an equal diameter, (6) ending, (7) cooling and discharging, (8) shaping and processing a discharged polycrystalline rod, cleaning and corroding, (9) loading into a zone melting furnace, vacuumizing and filling argon gas, (10) preheating and melting the material to weld the seed crystals, (11) seeding and thinning the neck, (12) shouldering and growing in an equal diameter, (13) breaking a tail part, (14) cooling and stopping the furnace, and discharging the crystals.
The invention adopts the Czochralski zone melting method to produce the silicon single crystal, thereby having the following characteristics:
1. overcomes the defect of high oxygen content in the silicon single crystal produced by the Czochralski method: oxygen atoms in the Czochralski silicon are generated by the high-temperature reaction of the fused silicon and the quartz crucible in the process of single crystal growth ( ) Into a silicon crystal.Oxygen content of up to 10 is generally present18atm/cm3The limitations and difficulties of czochralski silicon single crystals in power device fabrication are caused by the thermal instability and reversibility of resistivity caused by oxygen donors formed by the high oxygen content in czochralski silicon. In the process of growing zone-melting single crystal, oxygen atoms entering the melt are supplied by two parts, namely oxygen atoms in the raw material silicon polycrystalline rod and a sio film (Si-O film) generated by the reaction of trace oxygen molecules in the inert gas at high temperature (800-1350 ℃) and the raw material silicon polycrystalline rod ) The sio that enters the silicon is almost completely volatilized by the high temperature silicon melt, and only a very small fraction of the oxygen atoms eventually enter the zone-melting crystal. From a number of experimental results, although the oxygen content in the feedstock silicon rods differs by nearly 3 orders of magnitude (from 10)16atm/cm3～1018atm/cm3) However, the oxygen content of the float-zone-melted single crystal after the primary crystallization by float-zone melting tends to be 1016atm/cm3The number is extremely large. Thus the high oxygen content (10) introduced during the Czochralski process18atm/cm3) After zone melting once crystallization, the temperature is reduced to 1016atm/cm3Completely reaches the national standard.
2. Overcomes the defect that the silicon single crystal doped with special solid elements can not be produced by the zone melting method. The silicon single crystal produced by the zone melting method can not be doped with other impurities due to the process limitation, generally, the intrinsic single crystal is pulled and then is sent into a neutron reactor, and the purpose of preparing the N-type silicon single crystal by doping phosphorus can be achieved through the irradiation of the thermal (slow) neutron flow. When the Czochralski zone melting method is adopted to produce the monocrystalline silicon, the characteristic that Czochralski equipment is easy to dope can be utilized, impurities required to be doped are doped in the process of drawing a Czochralski polycrystalline rod material, and then the silicon monocrystalline doped with N-type or P-type impurities or other impurities specially required and low in oxygen content is drawn by a zone melting furnace, so that the doping purpose is achieved.
3. Greatly improves the productivity of the zone melting furnace and reduces the production period and the production cost of the zone melting silicon single crystal. The price of the zone melting furnace with the same diameter is more than eight times higher than that of the straight-pull furnace, and the zone melting method firstly purifies the silicon polycrystalline rod by the zone melting furnace, then the silicon polycrystalline rod is made into silicon single crystal by the zone melting furnace, and then neutron irradiation is carried out. The Czochralski zone melting method firstly uses the Czochralski furnace to draw the silicon polycrystal rod and then uses the zone melting furnace to prepare the silicon single crystal, and saves the time and the cost of neutron irradiation, thereby not only reducing the production cost, but also improving the production utilization rate of the zone melting furnace and shortening the production period.
Specific examples are given below to further illustrate how the invention may be implemented.
The Czochralski and float zone method for producing silicon single crystal is carried out by using a Czochralski furnace and a float zone furnace in sequence. The method comprises the following steps:
(1) 22 kg of corroded and cleaned blocky silicon polycrystalline material is put into a quartz crucible in a Czochralski furnace, and after the quartz crucible is vacuumized for 30-60 minutes until the pressure is less than or equal to 100 millitorr, argon is filled until the vacuum pressure is less than or equal to 9 torr.
(2) Cooling water is introduced before heating, a crucible rotating mechanism is started, a heating button is started, the temperature is heated to 1500-1600 ℃ for about 2.5 hours, the blocky polycrystalline material is completely melted into a molten state, a seed crystal rotating mechanism is started, the seed crystal is descended, and the seed crystal is welded.
(3) The seed travel was set to zero, the crystal potentiometer was rotated and a narrow neck of about 8mm in diameter and about 20mm in length was pulled from the molten polycrystalline material by the seed for 30 minutes.
(4) The seed crystal raising speed is reduced, a crystal growth conversion button is started, the pulling speed is controlled by a diameter controller, and the pulling diameter is enlarged from about 8mm of the thin neck to 50 mm-80 mm, in this embodiment 65mm, after about 30 minutes, the shoulder is placed.
(5) And adjusting a diameter sensor, controlling the crystal pulling speed, and carrying out the constant diameter growth process for 20 hours.
(6) The pulling speed is reduced, and the process is finished after about 3.5 hours.
(7) And (3) raising the crystal to leave the liquid level, stopping heating, rotating the crucible, raising the crystal and rotating the crystal potentiometer to zero positions, cutting off the power supply, stopping argon gas after half an hour, stopping water after four hours, closing a linear valve switch, stopping vacuumizing by a main vacuum pump, and discharging the polycrystalline rod.
(8) Carrying out ingot shape processing on the polycrystalline rod discharged from the furnace, cleaning and corroding the polycrystalline rod, then loading the polycrystalline rod into a crystal holder in a zone melting furnace, loading the seed crystal into a seed crystal fixing clamp, placing a preheating plate on the seed crystal, closing a furnace door, vacuumizing the furnace chamber to the pressure of 0.1 millitorr within about 10 minutes, and then filling argon to the pressure of 0.2 millitorr.
(9) Before heating, cooling water is introduced, the temperature of the melting zone of the crystal bar is heated to 1420 ℃ by preheating for 20 minutes, and the melting zone and the seed crystal are welded by taking 5 minutes.
(10) The melt zone was adjusted to draw a thin neck of about 8mm in diameter and about 100mm in length over 10 minutes.
(11) The conveying speed of the crystal at the lower part is reduced, shouldering is carried out, the shouldering angle is controlled to be 60 degrees by using the upper speed, the diameter of the thin neck is enlarged from 8mm to 50 mm-80 mm in 30-40 minutes, the diameter is 63mm in the embodiment, and the equal-diameter growth process is carried out for 6 hours.
(12) The upper pulling rate was gradually decreased and the tail of the crystal was pulled apart in 50 minutes.
(13) Slowly cooling until the crystal is dark, stopping heating, cutting off the power supply after ten minutes, stopping argon gas, cutting off water after twenty minutes, and stopping vacuumizing.
(14) The lower furnace chamber is opened and the crystal is taken out.
The straight-drawing furnace used in this example was a CG-3000 model straight-drawing furnace produced in USA, and the zone furnace was an FZ-14 model zone furnace produced in Denmark.
When a silicon single crystal having a specific doping requirement is produced, a raw material can be charged into a Czochralski furnace while doping with a desired impurity.
Such as: when pulling a P-type silicon single crystal, boron needs to be doped, and the calculation relation of the resistivity and the doping concentration is as follows: wherein rho: as resistivity, N: is the doping concentration
When pulling an N-type silicon single crystal, phosphorus needs to be doped, and the calculation relation of the resistivity and the doping concentration is as follows: wherein: rho is resistivity, N is concentration X-log 10 rho A0＝-3.1083A1＝-3.2626 A2＝-1.2196A3＝-0.13923 B1＝1.0265B2＝0.38755 B3＝0.041833
In addition, other elements can be doped according to different purposes, for example, a large amount of germanium-doped elements can be doped to prepare the germanium-doped silicon single crystal.
Claims (6)
1. A Czochralski and float zone method for producing silicon single crystal is carried out by using a Czochralski furnace and a float zone furnace in sequence, and comprises the following steps:
(1) loading the block-shaped silicon polycrystal material which is cleaned by corrosion into a quartz crucible in a czochralski furnace, and then vacuumizing and filling argon;
(2) cooling water is introduced before heating, the crucible rotating mechanism is started, the heating button is started, the seed crystal rotating mechanism is started after the blocky silicon polycrystal is completely melted, and the seed crystal is descended to be welded with the seed crystal;
(3) adjusting the seed crystal stroke to zero, rotating a crystal lifting potentiometer, and drawing a thin neck;
(4) descending the seed crystal raising speed, starting a crystal raising conversion button, expanding the crystal pulling diameter, and controlling the pulling speed by using a diameter controller to shoulder;
(5) adjusting a diameter sensor, and controlling the crystal pulling speed to perform equal-diameter crystal pulling;
(6) reducing the crystal pulling speed and ending;
(7) raising the temperature of the crystal leaving the liquid level, stopping heating, rotating the crucible, raising the crystal, rotating the crystal potentiometer to zero positions, cutting off the power supply, stopping argon after half an hour, stopping water after four hours, closing a linear valve switch, stopping vacuumizing by a main vacuum pump, and discharging the polycrystalline rod out of the furnace;
(8) carrying out ingot shape processing on the polycrystalline rod discharged from the furnace, cleaning and corroding the polycrystalline rod, then loading the polycrystalline rod into a crystal holder in a zone melting furnace, loading seed crystals into a seed crystal fixing chuck, placing a preheating sheet on the seed crystals, closing a furnace door, vacuumizing and filling argon;
(9) cooling water is introduced before heating, preheating and melting materials are carried out, and a crystal bar melting zone is welded with the seed crystal;
(10) adjusting a melting zone, and seeding to grow a thin neck;
(11) reducing the conveying speed of the lower crystal, shouldering, controlling the shouldering angle by using the upper speed, and starting isodiametric growth after shouldering to the required diameter;
(12) gradually reducing the upper clamping speed and breaking the tail of the crystal;
(13) slowly cooling, stopping heating until the crystal is dark, cutting off a power supply after ten minutes, stopping argon gas, and cutting off water after twenty minutes;
(14) the lower furnace chamber is opened and the crystal is taken out.
2. The Czochralski zone melting method for producing a silicon single crystal as claimed in claim 1, wherein the heating is started when the Czochralski furnace is evacuated to a pressure of 100 torr or less and argon gas is introduced to a vacuum pressure of 9 torr or less.
3. The Czochralski and float zone method for producing a silicon single crystal as claimed in claim 1, wherein the neck of the silicon polycrystalline rod drawn from the Czochralski furnace has a diameter of about 8mm, a length of about 20mm, and a shouldered diameter of 50mm to 80 mm.
4. The Czochralski zone melting method for producing a silicon single crystal as claimed in claim 1, wherein the float-zone furnace is preheated by introducing argon gas at a pressure of 0.2 mtorr while evacuating at a pressure of 0.1 mtorr.
5. The Czochralski float zone method for producing a silicon single crystal as set forth in claim 1, wherein the float zone furnace draws a silicon single crystal having a neck diameter of about8mm and a length of about 100mm and a shouldered diameter of 50mm to 80 mm.
6. The Czochralski float zone method for producing a silicon single crystal according to claim 1, wherein when a silicon single crystal doped with a specific solid state element is desired, the desired solid state element is doped at the same time as charging the silicon polycrystal raw material into the Czochralski furnace.
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| Application Number | Priority Date | Filing Date | Title |
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| CN00105518A CN1095505C (en) | 2000-03-30 | 2000-03-30 | Vertical pulling and zone melting process of producing monocrystalline silicon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00105518A CN1095505C (en) | 2000-03-30 | 2000-03-30 | Vertical pulling and zone melting process of producing monocrystalline silicon |
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| CN1267751A CN1267751A (en) | 2000-09-27 |
| CN1095505C true CN1095505C (en) | 2002-12-04 |
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| CN1325700C (en) * | 2006-04-21 | 2007-07-11 | 天津市环欧半导体材料技术有限公司 | Large-diameter zone-melting silicon single crystal growth method |
| WO2007093082A1 (en) * | 2006-02-16 | 2007-08-23 | Yonggang Jin | A process of producing silicon wafer employing float method and apparatus thereof |
| CN100339513C (en) * | 2006-04-19 | 2007-09-26 | 天津市环欧半导体材料技术有限公司 | Electric control system of zone-melted silicon single crystal furnace |
| CN100351435C (en) * | 2005-09-29 | 2007-11-28 | 天津市环欧半导体材料技术有限公司 | Process for preparing gas phase doped float-zone silicon monocrystal for solar cell |
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| CN100371505C (en) * | 2005-08-30 | 2008-02-27 | 河北工业大学 | Ge doping method of zone melting silicon single crystal by liquid smearing method |
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| WO2007093082A1 (en) * | 2006-02-16 | 2007-08-23 | Yonggang Jin | A process of producing silicon wafer employing float method and apparatus thereof |
| CN101133194B (en) * | 2006-02-16 | 2010-12-08 | 靳永钢 | Float silicon wafer manufacturing process and equipment |
| CN100339513C (en) * | 2006-04-19 | 2007-09-26 | 天津市环欧半导体材料技术有限公司 | Electric control system of zone-melted silicon single crystal furnace |
| CN1325700C (en) * | 2006-04-21 | 2007-07-11 | 天津市环欧半导体材料技术有限公司 | Large-diameter zone-melting silicon single crystal growth method |
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| WO2008067700A1 (en) * | 2006-12-06 | 2008-06-12 | Tianjin Huanou Semiconductor Material And Technology Co., Ltd. | Dislocation-free silicon monocrystal, its preparation method and a graphite heating device used |
| WO2008128378A1 (en) * | 2007-04-19 | 2008-10-30 | Tianjin Huanou Semiconductor Material And Technology Co., Ltd. | Vertical pulling and zone melting method for producing monocrystalline silicon |
| CN102304757A (en) * | 2011-10-11 | 2012-01-04 | 天津市环欧半导体材料技术有限公司 | Method for preparing 6-inch P-type solar silicon single crystals through Czochralski method and zone melting method |
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