CN102817071A - Preparation technology of heat radiation resistant Czochralski polysilicon or monocrystalline silicon - Google Patents
Preparation technology of heat radiation resistant Czochralski polysilicon or monocrystalline silicon Download PDFInfo
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- CN102817071A CN102817071A CN2012102049348A CN201210204934A CN102817071A CN 102817071 A CN102817071 A CN 102817071A CN 2012102049348 A CN2012102049348 A CN 2012102049348A CN 201210204934 A CN201210204934 A CN 201210204934A CN 102817071 A CN102817071 A CN 102817071A
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- heat shielding
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- polysilicon
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- 238000005516 engineering process Methods 0.000 title claims abstract description 25
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 17
- 229920005591 polysilicon Polymers 0.000 title claims abstract description 17
- 230000005855 radiation Effects 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 64
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 53
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 49
- 239000010703 silicon Substances 0.000 claims abstract description 49
- 230000012010 growth Effects 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000010453 quartz Substances 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- 239000012535 impurity Substances 0.000 claims description 6
- 230000001680 brushing effect Effects 0.000 claims description 5
- 230000004927 fusion Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 239000002019 doping agent Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- PWKWDCOTNGQLID-UHFFFAOYSA-N [N].[Ar] Chemical compound [N].[Ar] PWKWDCOTNGQLID-UHFFFAOYSA-N 0.000 abstract description 6
- 238000002425 crystallisation Methods 0.000 abstract description 6
- 230000008025 crystallization Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract 3
- 238000002844 melting Methods 0.000 abstract 3
- 238000007664 blowing Methods 0.000 abstract 1
- 230000007423 decrease Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 5
- 230000002950 deficient Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002210 silicon-based material Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- VJTAZCKMHINUKO-UHFFFAOYSA-M chloro(2-methoxyethyl)mercury Chemical compound [Cl-].COCC[Hg+] VJTAZCKMHINUKO-UHFFFAOYSA-M 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005094 computer simulation Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003913 materials processing Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation technology of heat radiation resistant Czochralski polysilicon or monocrystalline silicon, comprising the following steps of: a) melting: adding a polysilicon or monocrystalline silicon raw material into a quartz crucible, turning off and vacuumizing a crystal growth furnace, filling it with high-pure nitrogen gas, turning on the power of a graphite heater, heating to the melting temperature of 1570 DEG C, and melting the polysilicon or monocrystalline silicon raw material; and b) shouldering growth: growing a fine neck, and reducing the temperature and pull speed to make the diameter of the silicon single crystal gradually increase to an expected size. A thermal shielding is arranged around a silicon single-crystal rod. As the thermal shielding decreases heat radiation of the heater on crystal and simultaneously reduces the heat radiation intensity on a solid-liquid interface, the vertical temperature gradient of molten silicon is increased to a certain extent. In the meantime, after the adoption of the thermal shielding, blowing of an argon (nitrogen) airstream on the solid-liquid interface is enhanced, and the effect of the argon (nitrogen) airstream carrying crystallization latent heat is strengthened so as to promote single crystal growth, raise crystallization rate and further increase the pull speed.
Description
Technical field
The present invention relates to the many or silicon single crystal preparation field of vertical pulling, specifically belong to the many or silicon single crystal preparation technology of thermal radiation resistant vertical pulling.
Background technology
Current, silicon materials in semiconductor applications and field of solar energy still in occupation of main status.Along with development of science and technology and development of technology, unicircuit and manufacture of solar cells technology have all proposed new requirement to silicon materials, and the growing technology of major diameter, high quality silicon single crystal becomes the research and development focus of current field of semiconductor materials and field of solar energy.
In recent years, the silicon materials processing technology has obtained many impressive progresses.One of most important progress in silicon crystal growth aspect is that 12 inches silicon monocrystal growth technology are ripe.The main silicon single-crystal manufacturer in the world comprises SHIN-ETSU HANTOTAI, SUMCO; MEMC, watt gram etc. all adopts the single crystal growing furnace that is suitable for 12 inches silicon monocrystal growths, mostly adopts magnetic field Czochralski method; Every stove charge reaches the 300-350 kilogram, and main application 28 or 32 inches crucibles and thermal field carry out silicon single-crystal production.Cutting edge technology comprises both at home and abroad at present: 1) thermal field designing technique, promptly utilize computer modeling technique, and the temperature of thermal field and the distribution situation of gradient thereof reach the improvement of crystal mass during the analogue crystals growth;
2) heat shielding technology promptly utilizes heat shielding to reduce thermal radiation and calorific loss, reduces thermal convection, accelerates the volatilization of vaporised gas, accelerates the crystalline cooling; 3) double-heater technology is promptly utilized, and two well heaters guarantee that solid-liquid interface has suitable thermograde down; 4) magnetic field technique, i.e. the convection current of applying a magnetic field control melt suppresses the fluctuating of bath surface temperature and the concentration of reduction silicon single crystal inside clearance oxygen; 5) seed crystal technology because the weight of large diameter silicon monocrystal is more and more heavy, is developed secondary and is grabbed shoulder technology, no necking down seed crystal technology etc.In addition, also develop the charging again and the PNEUMATICALLY CONTROLLED PERISTALTIC SOLIDS of pulling of crystals.
Another impressive progress of silicon crystal growth aspect is effectively to have controlled the formation of primary particle (COP) defective in the crystal.The size of COP defective exists in 8 inches silicon chips about 100 nanometers already, but along with line widths shrink to 100 nanometers when following, this problem becomes more outstanding.Because the COP defective can cause the degeneration and the isolated inefficacy of gate oxide integrity, MEMC company has at first developed this technology, and other main wafer fabrication plant merchants also develop similar techniques afterwards.These technology are based on the optimum temperature at best pulling rate and solid-liquid interface place, on the whole length of crystal ingot and diameter, suppress the formation of two types of height injurous defects.Use the silicon polished requirement that can satisfy device fully of silicon single-crystal preparation of these technology drawings, thereby improved the yield rate of device greatly, reduced cost.
Summary of the invention
Provide a kind of thermal radiation resistant vertical pulling many or silicon single crystal preparation technology on the object of the invention; Because heat shielding has weakened well heater to the crystalline thermal radiation; Also weakened solid-liquid interface thermal radiation dynamics simultaneously, increased the longitudinal temperature gradient of molten silicon to a certain extent.After adopting heat shielding simultaneously, strengthened argon (nitrogen) air-flow, strengthened the effect that argon (nitrogen) air-flow carries crystallization latent heat and therefore helped single crystal growing, and can improve crystallization rate, and then improved pulling rate the brushing of solid-liquid interface.
Technical scheme of the present invention is following:
Many or the silicon single crystal preparation technology of thermal radiation resistant vertical pulling includes following operation steps:
A), reinforced: polysilicon or silicon single crystal raw material and impurity are put into quartz crucible, and the kind of impurity is decided according to the N of resistance or P type, and dopant species has boron, phosphorus, nitrogen;
B), melt: add polysilicon or silicon single crystal raw material in quartz crucible after; Charge into high pure nitrogen after long brilliant stove must cut out and be evacuated, the purity of nitrogen is more than 98%, and nitrogen pressure is 0.06-0.2MPa; Nitrogen flow 80-100L/min; Open the graphite heater power supply then, be heated to temperature of fusion more than 1420 ℃, with polysilicon or the fusing of silicon single crystal raw material;
C), necking down growth: after the temperature-stable of silicon melt, seed crystal is slowly immersed in the silicon melt, seed crystal is upwards promoted fast, the reduced that makes the seed crystal that grows is to 4-6mm;
D), shouldering growth: grown after the thin neck, must reduce temperature and pulling rate, made the diameter of silicon single-crystal increase to required size gradually; Outside silicon single crystal bar, be provided with heat shielding, the upper end of heat shielding is connected with the heat shielding loam cake, and the below of heat shielding loam cake is provided with heat-preservation cylinder; Heat shielding is made up of heat shielding shell, heat shielding inner casing and intermediary heat shielding thermal insulation layer, and it is round table-like that heat shielding is, and have centre gangway; Angle between heat shielding and the heat shielding loam cake is 40-50 °; The longitudinal section of centre gangway is trapezoidal, and nitrogen gas stream feeds from centre gangway, has strengthened nitrogen gas stream brushing solid-liquid interface;
E), isodiametric growth: grown after thin neck and the shoulder, borrowed the continuous adjustment of pulling rate and temperature, boule diameter is maintained between the positive and negative 2mm, the part of this section fixed diameter promptly is called equal-diameter part, and monocrystalline silicon piece is taken from equal-diameter part;
F), afterbody growth: after having grown equal-diameter part, must slowly dwindle by first diameter with crystal bar, separate with liquid level up to becoming a cusp, the crystal bar of having grown is risen to furnace chamber and is taken out after cooling for some time, promptly accomplishes growth cycle one time.
In step b), add polysilicon or silicon single crystal raw material in quartz crucible after, charge into high pure nitrogen after long brilliant stove must cut out and be evacuated; The purity of nitrogen is 99.9%; Nitrogen pressure is 0.14MPa, and nitrogen flow 90L/min opens the graphite heater power supply then; Be heated to 1570 ℃ of temperature of fusion, with polysilicon or the fusing of silicon single crystal raw material.
The present invention has also weakened solid-liquid interface thermal radiation dynamics because heat shielding has weakened well heater to the crystalline thermal radiation simultaneously, has increased the longitudinal temperature gradient of molten silicon to a certain extent.After adopting heat shielding simultaneously, strengthened argon (nitrogen) air-flow, strengthened the effect that argon (nitrogen) air-flow carries crystallization latent heat and therefore helped single crystal growing, and can improve crystallization rate, and then improved pulling rate the brushing of solid-liquid interface.
Embodiment
Many or the silicon single crystal preparation technology of thermal radiation resistant vertical pulling includes following operation steps:
A), reinforced: polysilicon or silicon single crystal raw material and impurity are put into quartz crucible, and the kind of impurity is decided according to the N of resistance or P type, and dopant species has boron, phosphorus, nitrogen;
B), melt: add polysilicon or silicon single crystal raw material in quartz crucible after; Charge into high pure nitrogen after long brilliant stove must cut out and be evacuated, the purity of nitrogen is 99.9%, and nitrogen pressure is 0.14MPa; Nitrogen flow 90L/min; Open the graphite heater power supply then, be heated to 1570 ℃ of temperature of fusion, with polysilicon or the fusing of silicon single crystal raw material;
C), necking down growth: after the temperature-stable of silicon melt, seed crystal is slowly immersed in the silicon melt, seed crystal is upwards promoted fast, the reduced that makes the seed crystal that grows is to 4-6mm;
D), shouldering growth: grown after the thin neck, must reduce temperature and pulling rate, made the diameter of silicon single-crystal increase to required size gradually; Outside silicon single crystal bar, be provided with heat shielding, the upper end of heat shielding is connected with the heat shielding loam cake, and the below of heat shielding loam cake is provided with heat-preservation cylinder; Heat shielding is made up of heat shielding shell, heat shielding inner casing and intermediary heat shielding thermal insulation layer, and it is round table-like that heat shielding is, and have centre gangway; Angle between heat shielding and the heat shielding loam cake is 40-50 °; The longitudinal section of centre gangway is trapezoidal, and nitrogen gas stream feeds from centre gangway, has strengthened nitrogen gas stream brushing solid-liquid interface;
E), isodiametric growth: grown after thin neck and the shoulder, borrowed the continuous adjustment of pulling rate and temperature, boule diameter is maintained between the positive and negative 2mm, the part of this section fixed diameter promptly is called equal-diameter part, and monocrystalline silicon piece is taken from equal-diameter part;
F), afterbody growth: after having grown equal-diameter part, must slowly dwindle by first diameter with crystal bar, separate with liquid level up to becoming a cusp, the crystal bar of having grown is risen to furnace chamber and is taken out after cooling for some time, promptly accomplishes growth cycle one time.
Claims (2)
1. the many or silicon single crystal preparation technology of thermal radiation resistant vertical pulling is characterized in that, includes following operation steps:
A), reinforced: polysilicon or silicon single crystal raw material and impurity are put into quartz crucible, and the kind of impurity is decided according to the N of resistance or P type, and dopant species has boron, phosphorus, nitrogen;
B), melt: add polysilicon or silicon single crystal raw material in quartz crucible after; Charge into high pure nitrogen after long brilliant stove must cut out and be evacuated, the purity of nitrogen is more than 98%, and nitrogen pressure is 0.06-0.2MPa; Nitrogen flow 80-100L/min; Open the graphite heater power supply then, be heated to temperature of fusion more than 1420 ℃, with polysilicon or the fusing of silicon single crystal raw material;
C), necking down growth: after the temperature-stable of silicon melt, seed crystal is slowly immersed in the silicon melt, seed crystal is upwards promoted fast, the reduced that makes the seed crystal that grows is to 4-6mm;
D), shouldering growth: grown after the thin neck, must reduce temperature and pulling rate, made the diameter of silicon single-crystal increase to required size gradually; Outside silicon single crystal bar, be provided with heat shielding, the upper end of heat shielding is connected with the heat shielding loam cake, and the below of heat shielding loam cake is provided with heat-preservation cylinder; Heat shielding is made up of heat shielding shell, heat shielding inner casing and intermediary heat shielding thermal insulation layer, and it is round table-like that heat shielding is, and have centre gangway; Angle between heat shielding and the heat shielding loam cake is 40-50 °; The longitudinal section of centre gangway is trapezoidal, and nitrogen gas stream feeds from centre gangway, has strengthened nitrogen gas stream brushing solid-liquid interface;
E), isodiametric growth: grown after thin neck and the shoulder, borrowed the continuous adjustment of pulling rate and temperature, boule diameter is maintained between the positive and negative 2mm, the part of this section fixed diameter promptly is called equal-diameter part, and monocrystalline silicon piece is taken from equal-diameter part;
F), afterbody growth: after having grown equal-diameter part, must slowly dwindle by first diameter with crystal bar, separate with liquid level up to becoming a cusp, the crystal bar of having grown is risen to furnace chamber and is taken out after cooling for some time, promptly accomplishes growth cycle one time.
2. the many or silicon single crystal preparation technology according to the said thermal radiation resistant vertical pulling of claim 1 is characterized in that: in step b), add polysilicon or silicon single crystal raw material in quartz crucible after; Charge into high pure nitrogen after long brilliant stove must cut out and be evacuated, the purity of nitrogen is 99.9%, and nitrogen pressure is 0.14MPa; Nitrogen flow 90L/min; Open the graphite heater power supply then, be heated to 1570 ℃ of temperature of fusion, with polysilicon or the fusing of silicon single crystal raw material.
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| CN2012102049348A CN102817071A (en) | 2012-06-20 | 2012-06-20 | Preparation technology of heat radiation resistant Czochralski polysilicon or monocrystalline silicon |
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| CN2012102049348A CN102817071A (en) | 2012-06-20 | 2012-06-20 | Preparation technology of heat radiation resistant Czochralski polysilicon or monocrystalline silicon |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177703A (en) * | 2015-10-13 | 2015-12-23 | 邢台晶龙电子材料有限公司 | Method for slender neck leading in process of preparing single crystal silicon rods by Czochralski method |
| 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 |
| CN108277530A (en) * | 2018-03-19 | 2018-07-13 | 卡姆丹克太阳能（江苏）有限公司 | A kind of preparation method of N-type solar energy silicon single crystal material |
| CN115383534A (en) * | 2022-09-13 | 2022-11-25 | 成都青洋电子材料有限公司 | Production process of monocrystalline silicon wafer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1417386A (en) * | 2001-11-01 | 2003-05-14 | 北京有色金属研究总院 | Heat shielding method and heat shield for vertically pulling crystal furnace |
| CN1422989A (en) * | 2002-12-02 | 2003-06-11 | 浙江大学 | Method for growing micro nitrogen silicon single crystal from polysilicon melting and nitrogen-doping |
| CN101597787A (en) * | 2009-06-24 | 2009-12-09 | 浙江大学 | Method for casting nitrogen-doped single crystal silicon with controllable nitrogen concentration under nitrogen |
-
2012
- 2012-06-20 CN CN2012102049348A patent/CN102817071A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1417386A (en) * | 2001-11-01 | 2003-05-14 | 北京有色金属研究总院 | Heat shielding method and heat shield for vertically pulling crystal furnace |
| CN1422989A (en) * | 2002-12-02 | 2003-06-11 | 浙江大学 | Method for growing micro nitrogen silicon single crystal from polysilicon melting and nitrogen-doping |
| CN101597787A (en) * | 2009-06-24 | 2009-12-09 | 浙江大学 | Method for casting nitrogen-doped single crystal silicon with controllable nitrogen concentration under nitrogen |
Non-Patent Citations (2)
| Title |
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| 刘寄声: "《单晶硅与多晶硅生产技术问答》", 30 April 2012, 化学工业出版社 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177703A (en) * | 2015-10-13 | 2015-12-23 | 邢台晶龙电子材料有限公司 | Method for slender neck leading in process of preparing single crystal silicon rods by Czochralski method |
| 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 |
| CN108277530A (en) * | 2018-03-19 | 2018-07-13 | 卡姆丹克太阳能（江苏）有限公司 | A kind of preparation method of N-type solar energy silicon single crystal material |
| CN115383534A (en) * | 2022-09-13 | 2022-11-25 | 成都青洋电子材料有限公司 | Production process of monocrystalline silicon wafer |
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