CN102560641A - N-type casting policrystalline silicon with uniform doping resistivity and preparation method thereof - Google Patents
N-type casting policrystalline silicon with uniform doping resistivity and preparation method thereof Download PDFInfo
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- CN102560641A CN102560641A CN2012100738134A CN201210073813A CN102560641A CN 102560641 A CN102560641 A CN 102560641A CN 2012100738134 A CN2012100738134 A CN 2012100738134A CN 201210073813 A CN201210073813 A CN 201210073813A CN 102560641 A CN102560641 A CN 102560641A
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Abstract
The invention discloses an N-type casting policrystalline silicon with a uniform doping resistivity and a preparation method thereof. The preparation method comprises the following steps of: mixing a polycrystalline silicon material, a phosphorus doping agent and gallium; then fusing; and growing a polycrystalline silicon body by using a casting method. According to the N-type casting policrystalline silicon with the uniform doping resistivity, the resistivity of about 90% N-type phosphorus doping phosphorus doping cast ingots can be controlled in the range of 1.0-2.0 omega.cm, therefore, the utilization rate of the N-type polycrystalline silicon crystal in the process of manufacturing an efficient solar cell is beneficially improved, the manufacturing cost of the efficient solar cell is remarkably lowered, the preparation method is simple to operate and easy to popularize and use in the photovoltaic industry.
Description
Technical field
The invention belongs to the solar cell material field, be specifically related to the uniform N mold casting of a kind of doped resistor rate policrystalline silicon and preparation method thereof.
Background technology
Sun power is inexhaustible, nexhaustible clean energy, utilizes the light transfer characteristic of semiconductor material, is prepared into solar cell, can change sun power into electric energy.In nearest 10 years, the output of solar cell is with the speed increment of annual 30-40%, and solar energy industry becomes one of industry with fastest developing speed in the market.
Casting polycrystalline silicon is one of main raw of preparation solar cell, accounts for about 50% of photovoltaic market at present.In traditional solar-photovoltaic technology, the P mold casting polysilicon of boron-doping is widely used in the preparation of solar cell.But under illumination, the P mold casting polysilicon of boron-doping will cause less sub-carrier lifetime to decline to a great extent, thereby cause the relaxation phenomenon of cell photoelectric efficiency of conversion owing to the generation of boron oxygen complex body.This photo attenuation phenomenon can cause the photoelectric transformation efficiency of solar cell to reduce 1-2%, and generating is very disadvantageous to solar cell photovoltaic for this.Replace the N mold casting polysilicon that boron prepares through phosphorus, can avoid the generation of boron oxygen complex body, suppress the optical attenuation phenomenon.In addition, N mold casting polysilicon is better than P mold casting polysilicon to the tolerance of transition metal such as iron, so generally speaking, N mold casting polysilicon has higher minority carrier lifetime, and this is very favorable to preparation high conversion efficiency solar cell.
For crystal silicon solar energy battery, its photoelectric transformation efficiency is closely-related with the resistivity of crystal silicon chip.Generally speaking, for preparation N type high-efficiency crystal silicon solar cell, the optimal resistivity of material should be controlled at the scope of 1.0-2.0 Ω .cm.If resistivity too high (＞2.0 Ω .cm), its corresponding doping content is just low, causes the potential barrier of the PN junction built in field in the solar cell of subsequent preparation low, is unfavorable for obtaining high open circuit voltage, thereby must influences the efficiency of conversion of battery; If resistivity too low (＜1.0 Ω .cm), the indirect complex effect effect of impurity strengthens in auger recombination and the silicon forbidden band, will limit less sub-carrier lifetime, is unfavorable for obtaining high short-circuit current, equally also can influence the efficiency of conversion of battery.When phosphorus cast silicon polycrystalline is mixed in the directional solidification method growth, because the segregation coefficient of phosphorus is 0.35, much smaller than 1, so after the polycrystalline silicon ingot casting growth was accomplished, resistivity was big along crystal ingot direction of growth distribution plastisied dispersion.For whole polycrystalline silicon ingot casting; Resistivity distribution polycrystalline silicon ingot casting useful length in 1.0-2.0 Ω .cm scope, that can be used for preparing efficient solar battery only accounts for the 50-65% of whole polycrystalline silicon ingot casting; And for the polycrystalline silicon ingot casting of remaining 35-50%, conventional batteries technology can not be prepared high performance solar batteries at present.
Publication number is that the patented claim of CN101918314A provides a kind of method that compensated feedstock silicon forms the resistivity of silicon ingot process that is used for controlling; Through in metallurgical compensated feedstock silicon, adding the aluminium or the gallium of pre-determined quantity; Increase the share of P type silicon materials in the silicon ingot, keep the consistence of resistivity in the P type silicon ingot.Publication number is that the patented claim of CN101654804A provides a kind of method that gallium pulling of crystals silicon resistivity is mixed in control in crystal growing process; When the resistivity of P N-type waferN during at 1.0-1.2 Ω .cm; To the extra adding part of excess silicon melt solution phosphorus, reach the purpose of regulation and control resistivity.The method of control resistivity evenness when above-mentioned two patented claims disclose the growing P-type silicon crystal, the N type silicon crystal that grows for overcompensation part is as waste disposal.
In recent years, received increasing attention, remained a difficult problem for homogeneity how to control N type phosphorus doping cast silicon polycrystalline resistivity along with N type silicon crystal is used for preparing solar cell.Therefore, seek the homogeneity that a kind of reasonable and effective method is controlled N type phosphorus doping cast silicon polycrystalline resistivity, the utilization ratio, the reduction battery cost that the raising silicon crystal are prepared solar cell have very important significance.
Summary of the invention
The invention provides a kind of method for preparing the uniform N mold casting of doped resistor rate policrystalline silicon; Can the resistivity of at least 90% N type phosphor doped polysilicon ingot casting be controlled in the 1.0-2.0 Ω .cm scope; It is big to have solved the axial variation range of N type phosphor doped polysilicon ingot casting resistivity, the low problem of preparation high performance solar batteries material use efficiency.
A kind of method for preparing the uniform N mold casting of doped resistor rate policrystalline silicon comprises the steps: polycrystalline silicon material, phosphorus dopant and gallium are mixed the back fusion, utilizes casting grown silicon polycrystal again.
Described being melted under the temperature that is higher than the silicon fusing point gets final product, and selects 1410 ℃ usually for use,, under this temperature, polysilicon is a melting, if temperature is higher, then is unfavorable for energy-conservation.
Described melting process carries out under the protection of vacuum or argon gas; This is to have good crystalline structure for the polysilicon that guarantees the casting growth; If under protective condition, do not carry out; Then polysilicon can produce defective, thereby can not better controlled resistivity, influences the efficient of the solar cell that subsequent preparation goes out.
The ratio of described polycrystalline silicon material, phosphorus dopant and gallium does not have particular restriction, but its proportion relation need make the electronics net dopant concentration of policrystalline silicon of at least 90% height that generate subsequent grows at 2.0e15～5.0e15cm
-3In the scope.
Described casting can adopt prior art, under vacuum or argon shield, and fusion polycrystalline silicon material, phosphorus dopant and gallium; Promote stay-warm case in the stove then, cool off crucible bottom simultaneously, melt temperature begins from the bottom to reduce; Crystalline silicon at first forms in the bottom, and is upwards growth of column.
After the directional solidification growth of polycrystalline silicon ingot casting is accomplished, the impurity enriched part (accounting for 10%) at excision polycrystalline silicon ingot casting top, remaining polycrystalline silicon ingot casting is the resistivity uniformity on its whole axial length, and resistivity distribution is in 1.0-2.0 Ω .cm scope.
As preferably, described polycrystalline silicon material is high pure electronic grade silicon material or metallurgical grade compensation silicon material.
When described polycrystalline silicon material is a high pure electronic grade silicon material, use only phosphorous and gallium in the N type policrystalline silicon body that this method prepares, avoided generating the boron oxygen complex body that causes optical attenuation.
When described polycrystalline silicon material is a metallurgical grade compensation silicon material, the phosphorus that is added in the N type policrystalline silicon body that uses this method to prepare can compensate the electroactive of boron atom in the metallurgical grade compensation silicon material, effectively reduces the optical attenuation effect.
The present invention also provides a kind of usefulness N type policrystalline silicon body that described method prepares.
Described N type policrystalline silicon body electronics net dopant concentration is at 2.0e15～5.0e15cm
-3In the scope, in this scope, the resistivity distribution that can guarantee N type policrystalline silicon body always makes the solar cell that utilizes this policrystalline silicon body to prepare have higher photoelectric transformation efficiency in 1.0～2.0 Ω .cm scopes.
Described N type policrystalline silicon body resistivity is distributed in 1.0～2.0 Ω .cm scopes.Resistivity uniformity on its whole axial length.If resistivity too high (＞2.0 Ω .cm), its corresponding doping content is just low, causes the potential barrier of the PN junction built in field in the solar cell of subsequent preparation low, is unfavorable for obtaining high open circuit voltage, thereby must influences the efficiency of conversion of battery; If resistivity too low (＜1.0 Ω .cm), the indirect complex effect effect of impurity strengthens in auger recombination and the silicon forbidden band, will limit less sub-carrier lifetime, is unfavorable for obtaining high short-circuit current, equally also can influence the efficiency of conversion of battery.
The present invention prepares the method for the uniform N mold casting of doped resistor rate policrystalline silicon; Can 90% N mold casting policrystalline silicon resistivity be controlled at the scope of 1.0～2.0 Ω .cm; Help improving the utilization ratio of N type policrystalline silicon when the preparation high performance solar batteries; Thereby significantly reduce the manufacturing cost of solar cell, the inventive method is simple to operate, is easy in the photovoltaic industry large-scale application.
Description of drawings
Fig. 1 be embodiment 1 preparation N N-type waferN silicon chip curing degree and resistivity concern synoptic diagram.
Fig. 2 be embodiment 2 preparation N N-type waferN silicon chip curing degree and resistivity concern synoptic diagram.
Embodiment
Earlier the phosphorus of 53.04mg and the gallium of 1.74g are put into crucible bottom, again the high pure electronic grade polycrystalline silicon material of 240kg is put into quartz crucible, shove charge.Under argon shield,, phosphorus and gallium are fused in the polysilicon solution at 1410 ℃ of fusion polycrystalline silicon materials; Speed with 2mm/min promotes stay-warm case in the stove; Simultaneously be blown into cooling gas in crucible bottom, the heat exchange of silicon melt mainly occurs in crucible bottom, through the directional solidification growth of polycrystalline silicon ingot casting.In the different sites sampling of the polycrystalline silicon ingot casting of growing, pass through the axial distribution of the resistivity of four probe method test vector generation for testing IC polycrystalline silicon ingot casting then, shown in accompanying drawing 1.Can see that the resistivity of about 90% polycrystalline silicon ingot casting all is distributed in 1.0-2.0 Ω .cm.Thereby with respect to the polycrystalline silicon ingot casting that does not pass through the gallium doping compensation, the utilization ratio of silicon materials has improved 20%.These resistivity in the efficient of the solar cell of the N type polysilicon chip of 1.0-2.0 Ω .cm preparation all more than 18%, unglazed decay.
Embodiment 2
Earlier the phosphorus of 45.46mg and the gallium of 2.49g are put into crucible bottom, again the metallurgical grade boron phosphorus compensation silicon material (total contains the boron of 2.35mg and the phosphorus of 30.29mg) of 240kg is put into crucible.Under argon shield,, phosphorus and gallium are fused in the polysilicon solution at 1410 ℃ of fusion polycrystalline silicon materials; Speed with 5mm/min promotes stay-warm case in the stove; Simultaneously be blown into cooling gas in crucible bottom, the heat exchange of silicon melt mainly occurs in crucible bottom, through directional solidification growth of polycrystalline silicon ingot.In the different sites sampling of the polycrystal silicon ingot of growing, pass through the axial distribution of the resistivity of four probe method test vector generation for testing IC polycrystal silicon ingot then, shown in accompanying drawing 2.Can see that the resistivity of about 90% polycrystal silicon ingot all is distributed in 1.0-2.0 Ω .cm.Thereby with respect to the polycrystal silicon ingot that does not pass through the gallium doping compensation, the utilization ratio of silicon materials has improved 25%.All more than 17%, light decay reduces these resistivity in the efficient of the solar cell of the N type polysilicon chip of 1.0-2.0 Ω .cm preparation, and absolute efficiency decays in 0.5% scope.
Claims (8)
1. a method for preparing the uniform N mold casting of doped resistor rate policrystalline silicon is characterized in that: polycrystalline silicon material, phosphorus dopant and gallium are mixed the back fusion, utilize casting grown silicon polycrystal again.
2. the method for preparing the uniform N mold casting of doped resistor rate policrystalline silicon as claimed in claim 1 is characterized in that: described phosphorus dopant is phosphorus powder or phosphorus silicon mother alloy.
3. the method for preparing the uniform N mold casting of doped resistor rate policrystalline silicon as claimed in claim 1 is characterized in that: described fusion and casting grown silicon polycrystalline carry out under the protection of vacuum or argon gas.
4. the method for preparing the uniform N mold casting of doped resistor rate policrystalline silicon as claimed in claim 1 is characterized in that: described polycrystalline silicon material is a high pure electronic grade silicon material.
5. the method for preparing the uniform N mold casting of doped resistor rate policrystalline silicon as claimed in claim 1 is characterized in that: described polycrystalline silicon material is a metallurgical grade compensation silicon material.
6. the N mold casting policrystalline silicon for preparing like each described method for preparing the uniform N mold casting of doped resistor rate policrystalline silicon of claim 1～5.
7. N mold casting policrystalline silicon as claimed in claim 6 is characterized in that the electronics net dopant concentration is 2.0e15～5.0e15cm
-3
8. N mold casting policrystalline silicon as claimed in claim 7 is characterized in that, resistivity is 1.0～2.0 Ω .cm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102817075A (en) * | 2012-08-18 | 2012-12-12 | 安阳市凤凰光伏科技有限公司 | Master alloy production method by using polycrystalline foundry furnace |
| CN102877122A (en) * | 2012-10-24 | 2013-01-16 | 英利能源（中国）有限公司 | Processing technology for silicon doping agent |
| CN103361724A (en) * | 2013-06-21 | 2013-10-23 | 东海晶澳太阳能科技有限公司 | Boron-gallium co-doped efficient polycrystalline silicon and preparation method thereof |
| CN104746134A (en) * | 2015-03-30 | 2015-07-01 | 江苏盎华光伏工程技术研究中心有限公司 | N-type monocrystalline silicon drawing method by using compensation silicon material |
| CN104928486A (en) * | 2015-06-11 | 2015-09-23 | 重庆大学 | Method for separating out silicon and aluminum-silicon alloy |
| CN105755538A (en) * | 2016-05-05 | 2016-07-13 | 中国科学院合肥物质科学研究院 | Preparation method for tin-doped metallurgical polycrystalline silicon casting ingot |
| CN105951173A (en) * | 2016-05-30 | 2016-09-21 | 上海超硅半导体有限公司 | N type monocrystalline silicon crystal ingot and manufacturing method thereof |
| CN106012010A (en) * | 2016-08-15 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Method and apparatus for secondary addition of doping agent |
| CN109554751A (en) * | 2017-09-25 | 2019-04-02 | 中美矽晶制品股份有限公司 | N-type polysilicon crystal, method for manufacturing the same, and N-type polysilicon wafer |
| CN109576787A (en) * | 2019-01-14 | 2019-04-05 | 浙江晶科能源有限公司 | Using the polycrystal silicon ingot and polycrystalline silicon rod and method of the silicon material preparation of physical method purification |
| CN110438566A (en) * | 2019-08-09 | 2019-11-12 | 湖南红太阳光电科技有限公司 | Preparation method, more doping silicon ingots and the silicon wafer of more doping silicon ingots |
| CN112195515A (en) * | 2020-09-29 | 2021-01-08 | 晶科能源有限公司 | Silicon crystal and preparation method thereof |
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| CN102817075A (en) * | 2012-08-18 | 2012-12-12 | 安阳市凤凰光伏科技有限公司 | Master alloy production method by using polycrystalline foundry furnace |
| CN102877122A (en) * | 2012-10-24 | 2013-01-16 | 英利能源（中国）有限公司 | Processing technology for silicon doping agent |
| CN103361724A (en) * | 2013-06-21 | 2013-10-23 | 东海晶澳太阳能科技有限公司 | Boron-gallium co-doped efficient polycrystalline silicon and preparation method thereof |
| CN104746134A (en) * | 2015-03-30 | 2015-07-01 | 江苏盎华光伏工程技术研究中心有限公司 | N-type monocrystalline silicon drawing method by using compensation silicon material |
| CN104928486A (en) * | 2015-06-11 | 2015-09-23 | 重庆大学 | Method for separating out silicon and aluminum-silicon alloy |
| CN105755538A (en) * | 2016-05-05 | 2016-07-13 | 中国科学院合肥物质科学研究院 | Preparation method for tin-doped metallurgical polycrystalline silicon casting ingot |
| CN105951173A (en) * | 2016-05-30 | 2016-09-21 | 上海超硅半导体有限公司 | N type monocrystalline silicon crystal ingot and manufacturing method thereof |
| CN106012010A (en) * | 2016-08-15 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Method and apparatus for secondary addition of doping agent |
| CN109554751A (en) * | 2017-09-25 | 2019-04-02 | 中美矽晶制品股份有限公司 | N-type polysilicon crystal, method for manufacturing the same, and N-type polysilicon wafer |
| US10510830B2 (en) | 2017-09-25 | 2019-12-17 | Sino-American Silicon Products Inc. | N-type polysilicon crystal, manufacturing method thereof, and N-type polysilicon wafer |
| CN109576787A (en) * | 2019-01-14 | 2019-04-05 | 浙江晶科能源有限公司 | Using the polycrystal silicon ingot and polycrystalline silicon rod and method of the silicon material preparation of physical method purification |
| CN110438566A (en) * | 2019-08-09 | 2019-11-12 | 湖南红太阳光电科技有限公司 | Preparation method, more doping silicon ingots and the silicon wafer of more doping silicon ingots |
| CN112195515A (en) * | 2020-09-29 | 2021-01-08 | 晶科能源有限公司 | Silicon crystal and preparation method thereof |
| CN112195515B (en) * | 2020-09-29 | 2022-03-01 | 晶科能源股份有限公司 | Silicon crystal and preparation method thereof |
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