CN102758253A - Czochralski polycrystalline silicon or monocrystal silicon preparation technology - Google Patents
Czochralski polycrystalline silicon or monocrystal silicon preparation technology Download PDFInfo
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- CN102758253A CN102758253A CN2012102049333A CN201210204933A CN102758253A CN 102758253 A CN102758253 A CN 102758253A CN 2012102049333 A CN2012102049333 A CN 2012102049333A CN 201210204933 A CN201210204933 A CN 201210204933A CN 102758253 A CN102758253 A CN 102758253A
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Abstract
The invention discloses a Czochralski polycrystalline silicon or monocrystal silicon preparation technology which comprises the following operation steps of: a) charging: putting polycrystalline silicon or monocrystal silicon raw material and impurities into a quartz crucible, wherein the types of the impurities are determined by the N type or P type of a resistor and comprise B, P and N; b) melting: after the polycrystalline silicon or monocrystal silicon raw material is added into the quartz crucible, closing and vacuumizing a long crystal furnace, and filling high-purity nitrogen into the long crystal furnace, wherein the purity of the nitrogen is more than 98%, the nitrogen pressure is 0.06-0.2MPa and the flow rate of the nitrogen is 80-100L/min; turning on a power supply of a graphite heater, heating up until the melting temperature is more than 1420 DEG C and melting the polycrystalline silicon or monocrystal silicon raw material; and c) necking down growth: after the temperature of silicon melt is stable, slowly soaking seed crystals into the silicon melt, rapidly lifting the seed crystals upwards and leading the diameter of the growing seed crystals to be reduced to 4-6mm. The technology uses nitrogen flow to replace argon flow, so that the microdefect in the silicon can be greatly inhibited, the mechanical strength of the silicon material is enhanced, and the slice yield is greatly increased; and furthermore, the slice damage rate is low, so that the production cost of the monocrystal silicon is lowered, and the service life of a minority carrier is obviously prolonged.
Description
Technical field
The present invention relates to the preparation field of silicon single crystal or polysilicon, specifically belong to the many or silicon single crystal preparation technology of 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
The invention discloses the many or silicon single crystal preparation technology of a kind of vertical pulling; Replace existing argon gas stream with nitrogen gas stream, suppressed the microdefect in the silicon greatly, strengthened the physical strength of silicon materials; Piece rate is improved greatly; And the fragmentation rate is low, thereby reduces the production cost of silicon single crystal, and minority carrier life time is significantly improved simultaneously.
Technical scheme of the present invention is following:
Many or the silicon single crystal preparation technology of 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 crystalline diameter increase to required size gradually;
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.
The concentration of described nitrogen is 2 * 10
13-4 * 10
15/ cm
3
The present invention replaces existing argon gas stream with nitrogen gas stream; Suppressed the microdefect in the silicon greatly, strengthened the physical strength of silicon materials, piece rate is improved greatly; And the fragmentation rate is low; Thereby reduce the production cost of silicon single crystal, minority carrier life time is significantly improved simultaneously, and the raw-material quality of solar cell is an important factor that influences efficiency of solar cell and solar cell life-span.Minority carrier life time is high more, and the photo-generated carrier diffusion length is big more, and the open circuit voltage of solar cell is high more, and the efficient of solar cell is also just high more.Few daughter life-span is the most directly parameter of weighing material self impurity and defective.Few daughter life-span is high more, and the density in the deep energy level of material deathnium content more little or impurity own is more little, and the quality of material self is just high more.
The present invention replaces existing argon gas stream with nitrogen gas stream, because nitrogen can strengthen the Internal Gettering of Silicon Wafers ability, nitrating can also improve the silicon chip physical strength in this external czochralski silicon monocrystal, suppresses void-type defect.Suppressed the microdefect in the silicon greatly, strengthened the physical strength of silicon materials, piece rate is improved greatly, and the fragmentation rate has been low, thereby reduced the production cost of silicon single crystal, minority carrier life time is significantly improved simultaneously.
Embodiment
Many or the silicon single crystal preparation technology of 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, and the concentration of nitrogen is 2 * 10
13-4 * 10
15/ cm
3
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 crystalline diameter increase to required size gradually;
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 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 crystalline diameter increase to required size gradually;
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 vertical pulling of claim 1, it is characterized in that: the concentration of described nitrogen is 2 * 10
13-4 * 10
15/ cm
3
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104389015A (en) * | 2014-11-13 | 2015-03-04 | 宁晋松宫电子材料有限公司 | Production technique capable of controlling single crystal black edge |
| CN104911694A (en) * | 2015-06-01 | 2015-09-16 | 宁晋晶兴电子材料有限公司 | Doping process for production of silicon single crystal rods |
| CN105063744A (en) * | 2015-07-15 | 2015-11-18 | 包头市山晟新能源有限责任公司 | Silicon single crystal drawing method |
| 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 |
| CN109518269A (en) * | 2017-09-20 | 2019-03-26 | 内蒙古中环光伏材料有限公司 | Doped monocrystalline silicon stick and its production method |
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| JPH0639352B2 (en) * | 1987-09-11 | 1994-05-25 | 信越半導体株式会社 | Single crystal manufacturing equipment |
| WO1999007922A1 (en) * | 1997-08-08 | 1999-02-18 | Memc Electronic Materials, Inc. | Non-dash neck method for single crystal silicon growth |
| JP2000128691A (en) * | 1998-10-16 | 2000-05-09 | Shin Etsu Handotai Co Ltd | Silicon seed crystal and production of silicon single crystal |
| US6548886B1 (en) * | 1998-05-01 | 2003-04-15 | Wacker Nsce Corporation | Silicon semiconductor wafer and method for producing the same |
| US20060016386A1 (en) * | 2002-12-23 | 2006-01-26 | Hyon-Jong Cho | Silicon wafer and method for producing silicon single crystal |
| CN101435105A (en) * | 2008-12-01 | 2009-05-20 | 浙江碧晶科技有限公司 | Preparation of low oxygen content silicon crystal |
| CN101798704A (en) * | 2009-12-31 | 2010-08-11 | 峨嵋半导体材料研究所 | Process for growing phi 8'' solar-grade Czochralski silicon by using 18-inch thermal field |
| CN102367588A (en) * | 2011-11-07 | 2012-03-07 | 东方电气集团峨嵋半导体材料有限公司 | Straight-pull eight-inch silicon single crystal thermal field and production method of eight-inch silicon single crystal |
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2012
- 2012-06-20 CN CN2012102049333A patent/CN102758253A/en active Pending
Patent Citations (11)
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|---|---|---|---|---|
| CN85100295A (en) * | 1985-04-01 | 1986-02-10 | 浙江大学 | The nitrogen atmosphere of vertical pulling (czochralski therapy) silicon single-crystal |
| CN87105811A (en) * | 1987-08-22 | 1988-02-24 | 浙江大学 | The gas phase nitrogen-doping method of czochralski silicon monocrystal |
| JPH0639352B2 (en) * | 1987-09-11 | 1994-05-25 | 信越半導体株式会社 | Single crystal manufacturing equipment |
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| WO1999007922A1 (en) * | 1997-08-08 | 1999-02-18 | Memc Electronic Materials, Inc. | Non-dash neck method for single crystal silicon growth |
| US6548886B1 (en) * | 1998-05-01 | 2003-04-15 | Wacker Nsce Corporation | Silicon semiconductor wafer and method for producing the same |
| JP2000128691A (en) * | 1998-10-16 | 2000-05-09 | Shin Etsu Handotai Co Ltd | Silicon seed crystal and production of silicon single crystal |
| US20060016386A1 (en) * | 2002-12-23 | 2006-01-26 | Hyon-Jong Cho | Silicon wafer and method for producing silicon single crystal |
| CN101435105A (en) * | 2008-12-01 | 2009-05-20 | 浙江碧晶科技有限公司 | Preparation of low oxygen content silicon crystal |
| CN101798704A (en) * | 2009-12-31 | 2010-08-11 | 峨嵋半导体材料研究所 | Process for growing phi 8'' solar-grade Czochralski silicon by using 18-inch thermal field |
| CN102367588A (en) * | 2011-11-07 | 2012-03-07 | 东方电气集团峨嵋半导体材料有限公司 | Straight-pull eight-inch silicon single crystal thermal field and production method of eight-inch silicon single crystal |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104389015A (en) * | 2014-11-13 | 2015-03-04 | 宁晋松宫电子材料有限公司 | Production technique capable of controlling single crystal black edge |
| CN104911694A (en) * | 2015-06-01 | 2015-09-16 | 宁晋晶兴电子材料有限公司 | Doping process for production of silicon single crystal rods |
| CN105063744A (en) * | 2015-07-15 | 2015-11-18 | 包头市山晟新能源有限责任公司 | Silicon single crystal drawing method |
| CN109518269A (en) * | 2017-09-20 | 2019-03-26 | 内蒙古中环光伏材料有限公司 | Doped monocrystalline silicon stick and its production method |
| 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 |
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Application publication date: 20121031 |