CN102817069A - Preparation technology of compound heating heat radiation resistant Czochralski polysilicon or monocrystalline silicon - Google Patents
Preparation technology of compound heating heat radiation resistant Czochralski polysilicon or monocrystalline silicon Download PDFInfo
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- CN102817069A CN102817069A CN2012102049352A CN201210204935A CN102817069A CN 102817069 A CN102817069 A CN 102817069A CN 2012102049352 A CN2012102049352 A CN 2012102049352A CN 201210204935 A CN201210204935 A CN 201210204935A CN 102817069 A CN102817069 A CN 102817069A
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Abstract
The invention discloses a preparation technology of compound heating heat radiation resistant Czochralski polysilicon or monocrystalline silicon, comprising the following steps of: a) charging: putting a polysilicon or monocrystalline silicon raw material and impurities into a quartz crucible, wherein the impurities contain boron, phosphorus and nitrogen; b) melting: turning off and vacuumizing a crystal growth furnace after the polysilicon or monocrystalline silicon raw material is added into the quartz crucible, filling the crystal growth furnace with high-pure nitrogen gas, turning on the power of a graphite heater, heating to the melting temperature of more than 1420 DEG C, melting the polysilicon or monocrystalline silicon raw material, letting an upper heater and a lower heater simultaneously operate when melting the material, and reducing heater power after melting the material. The above heaters are main heaters for growth; the temperature of the bottom of a thermal field is reduced without influencing crystal growth, and the temperature difference between the top and bottom of a traditional thermal field is minimized; and 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
The invention discloses the many or silicon single crystal preparation technology of a kind of compound heating radioprotective formula vertical pulling, make the bottom temp decline of thermal field and do not influence the crystalline growth, reduced the temperature difference of traditional thermal field top and bottom; Strengthened argon (nitrogen) air-flow to the brushing of solid-liquid interface, 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.
Technical scheme of the present invention is following:
Many or the silicon single crystal preparation technology of compound heating radioprotective formula 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, upper heater in the body of heater, well heater down, upper heater, well heater is right against top, the bottom of quartz crucible respectively down; Upper heater, following well heater are connected with power-supply system respectively, and upper heater, following well heater are the square wave shape respectively, 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, upper heater, following well heater are worked simultaneously when changing material; Changing material and finish back reduction heater power down, is that primary heater is grown with the upper heater;
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), the purity of nitrogen is 99.9%, and nitrogen pressure is 0.14MPa, and nitrogen flow 90L/min opens the graphite heater power supply then, is heated to 1570 ℃ of temperature of fusion, with polysilicon or the fusing of silicon single crystal raw material.
Temperature of the present invention field is meant the temperature distribution in the hot system, and is of crucial importance to the crystalline growth.Warm field is divided into warm of static state and dynamically warm field.Temperature field when not carrying out crystal growth is called static temperature field, is decided by the shape and size of well heater and heat-insulation system.Temperature field when carrying out crystal growth is referred to as dynamically temperature field.Have crystallization latent heat to discharge in the crystallisation process, pulling rate is fast more, and crystallization rate is high more, and the latent heat of release is many more.Flowing of the variation of crystal diameter, length and bushing position and melt all produces bigger influence to the temperature field.Because the factor of this respect has changed static temperature, the dynamic following test that therefore will pass through crystal pulling technique is revised static temperature, could make dynamic warm the requirement of satisfying crystal growth.In melt, longitudinal temperature gradient suitably increases, and helps the thermal conduction of crystallization latent heat in distributing and carries out, and helps carrying out smoothly of crystallisation process.
The present invention descends the bottom temp of thermal field and does not influence the crystalline growth, has reduced the temperature difference of traditional thermal field top and bottom; Strengthened argon (nitrogen) air-flow to the brushing of solid-liquid interface, 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.
Embodiment
Many or the silicon single crystal preparation technology of compound heating radioprotective formula 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, upper heater in the body of heater, well heater down, upper heater, well heater is right against top, the bottom of quartz crucible respectively down; Upper heater, following well heater are connected with power-supply system respectively, and upper heater, following well heater are the square wave shape respectively, 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, upper heater, following well heater are worked simultaneously when changing material; Changing material and finish back reduction heater power down, is that primary heater is grown with the upper heater;
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 compound heating radioprotective formula 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, upper heater in the body of heater, well heater down, upper heater, well heater is right against top, the bottom of quartz crucible respectively down; Upper heater, following well heater are connected with power-supply system respectively, and upper heater, following well heater are the square wave shape respectively, 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, upper heater, following well heater are worked simultaneously when changing material; Changing material and finish back reduction heater power down, is that primary heater is grown with the upper heater;
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; It is characterized in that: in step b), 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016183071A (en) * | 2015-03-26 | 2016-10-20 | 株式会社Sumco | Manufacturing method of silicon single crystal |
| 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 |
| CN110685011A (en) * | 2019-10-21 | 2020-01-14 | 大同新成新材料股份有限公司 | Intelligent processing equipment for producing single-product silicon thermal field crucible and processing method thereof |
Citations (1)
| 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 |
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- 2012-06-20 CN CN2012102049352A patent/CN102817069A/en active Pending
Patent Citations (1)
| 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 |
Non-Patent Citations (2)
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| 任丙彦等: "大直径直拉硅单晶炉热场的改造及数值模拟", 《人工晶体学报》 * |
| 刘立新等: "单晶硅生长原理及工艺", 《长春理工大学学报(自然科学版)》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016183071A (en) * | 2015-03-26 | 2016-10-20 | 株式会社Sumco | Manufacturing method of silicon single crystal |
| 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 |
| CN110685011A (en) * | 2019-10-21 | 2020-01-14 | 大同新成新材料股份有限公司 | Intelligent processing equipment for producing single-product silicon thermal field crucible and processing method thereof |
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