CN101899703B - Crucible for growing crystalline silicon ingot and extracting silicon raw material of crystalline silicon ingot and preparation method and application thereof - Google Patents
Crucible for growing crystalline silicon ingot and extracting silicon raw material of crystalline silicon ingot and preparation method and application thereof Download PDFInfo
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- CN101899703B CN101899703B CN2010102468319A CN201010246831A CN101899703B CN 101899703 B CN101899703 B CN 101899703B CN 2010102468319 A CN2010102468319 A CN 2010102468319A CN 201010246831 A CN201010246831 A CN 201010246831A CN 101899703 B CN101899703 B CN 101899703B
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Abstract
The invention discloses a crucible for growing a solar grade crystalline silicon ingot containing boron dopant and extracting the silicon raw material of the crystalline silicon ingot. The crucible comprises a crucible shell and a boron nitride liner covered on the internal surface of the crucible shell, wherein the thickness of the boron nitride liner is 0.001mm-4mm; the weight of boron nitride in the boron nitride liner is not more than 2% of the weight of silicon raw material added in the crucible; and the crucible shell is prepared from one or more materials of graphite, quartz and carbon/carbon composite through processing. The invention also discloses a preparation method and application of the crucible. The crucible of the invention solves the problem of the prior art that molten silicon leaks through the capillary tubes in the crucible and silicon adheres to the wall of the crucible so that the crucible or the silicon ingot is cracked or smashed, satisfies the demands of industrialization, large volume, low cost and long service life, has universal applicability and is particularly suitable for the production environment with high temperature and low pressure or the production environments with other special demands.
Description
Technical field
The technical field that the invention belongs to the growth of solar level crystalline silicon and purify is specifically related to growth of solar level boron doped agent crystal silicon ingot and silicon feedstock purification thereof with crucible and preparation and application.
Background technology
Silicon materials are the most frequently used materials of crystal silicon solar energy battery.The crystal silicon ingot is meant silicon single crystal that can be used for photovoltaic generation or the polycrystalline silicon ingot casting that adopts crystal pulling method, directional solidification method or casting production, and the purity of silicon is more than 99.999% in the common solar level crystal silicon ingot.In order to make silicon ingot or purified silicon raw material, silicon at first will at high temperature become molten state.The melting degree of silicon is generally more than 1412 ℃.The crucible that under such high temperature, holds melted silicon adopts quartz, graphite or CFC (the charcoal charcoal is compound) material usually.These materials can bear the high temperature more than 1500 ℃; But have main defective, promptly after the melted silicon cooling formed silicon ingot, silicon ingot and these materials had sticking crucible phenomenon to take place; Make crucible different owing to thermal expansivity, under the effect of thermal stresses, be damaged with silicon ingot.Usually crucible or silicon ingot can crack.
In order to address the above problem, the most frequently used method is the inner-wall spraying one deck silicon nitride (Si at crucible (being formed by graphite, quartz or CFC materials processed) in the industry at present
3N
4), silicon nitride contacts with melted silicon in the use, avoids sticking crucible phenomenon to take place.For example application number be 200810243657.5 one Chinese patent application and application number be 200820215102.5 with the Chinese patent of 200820215103.X in a kind of spraying method and device of silicon nitride are disclosed.
The crucible that is coated with silicon nitride has solved silicon ingot and crucible adhesion to a certain extent and has caused crucible or silicon ingot crackle even broken problem to occur.Yet still there is defective in silicon nitride coating, and its subject matter is that silicon nitride coating can not use in the environment of high-temperature low-pressure.Silicon nitride coating, can be gasified when using under the high-temperature low-pressure condition of pressure below 1000Pa simultaneously more than 1400 ℃ in temperature, no longer plays the purpose of the sealing coat between crucible and the melted silicon.This situation is (need under high-temperature low-pressure, carry out usually) that is unfavorable for the physics method purification of silicon raw material, also is unfavorable in order to reduce cost or to improve silicon ingot quality, the silicon ingot production that need under low pressure environment, carry out.
In addition; Under some specific production requirements; During the silicon crystal of for example production particular requirement (is the one Chinese patent application of 200810063556.X like application number); Perhaps when carrying out the silicon feedstock purification (be like application number 2009100983702 one Chinese patent application) needs to adopt plumbago crucible or CFC crucible as the container that holds melted silicon.But because the defective of material; Usually there is the capillary aperture in plumbago crucible or the CFC crucible cheaply; The melted silicon flowability is very strong; Melted silicon and graphite or CFC material are to soak into each other simultaneously, and therefore, melted silicon is usually through existing the capillary aperture to be exuded to the outside of crucible in plumbago crucible or the CFC crucible.Though highdensity plumbago crucible or CFC crucible can be avoided this problem, it is very high to improve the required manufacturing cost of the density of graphite or CFC material.
Summary of the invention
The invention provides a kind of solar level boron doped agent crystal silicon ingot growth and silicon feedstock purification thereof and use crucible; Solved that melted silicon crackle even broken problem occur through crucible or the silicon ingot that the kapillary seepage in the crucible and the adhesion of silicon on sidewall of crucible cause in the prior art; Industriallization, big volume, low cost, long requirement of life-span have not only been satisfied; And has a general applicability; Particularly go under the high-temperature low-pressure (temperature is more than 1400 ℃, and pressure is below 1000Pa) or the production environment of other particular requirement.
A kind of solar level boron doped agent crystal silicon ingot growth and silicon feedstock purification thereof are used crucible, are made up of crucible shell and the SP 1 liner that covers the crucible inner surface of outer cover, and the thickness of described SP 1 liner is 0.001mm～4mm; In the described employing of crucible shell graphite, quartz or charcoal charcoal compound (CFC) material one or more process; Wherein, the quality of SP 1 is no more than and joins 2% of the interior silicon raw materials quality of crucible in the described SP 1 liner.
In the optimized technical scheme, the thickness of described SP 1 liner is 0.01mm～2mm, and the best is preferably 0.02mm～1mm.The SP 1 liner is too thick then to have increased production cost, and coating is peeled off easily; The too thin effect that then can not play the demoulding.
Described SP 1 liner can perhaps adopt the method for plasma spraying to form boron nitride coating through forming behind the integral high-temperature sintered boron nitride powder, perhaps through additive methods such as the whole manufacturing of chemical gas phase lamination method pyrolitic boron nitride liners.
Among the present invention, described SP 1 liner is preferably formed by SP 1 (BN) materials processed, and further preferred is the SP 1 liner that raw material takes spraying method to make with the SP 1.
Specifically, described SP 1 liner is preferably made by following method:
It is 3%～40% pulpous state liquid (mass ratio of boron nitride coating and solvent is 1: 3～20) that boron nitride coating is diluted in solvent for mass concentration; Evenly spray or spread upon the internal surface of crucible shell; Dry back forms the deposition liner on the crucible inner surface of outer cover; Wherein, the quality of SP 1 is no more than and joins 2% of the interior silicon raw materials quality of crucible in the described boron nitride coating.
Described solvent is deionized water or volatile organic solvent, and described volatile organic solvent is that boiling point is lower than 80 ℃ common organic solvent, like acetone, methyl alcohol, benzene or ethanol etc., considers from cost and environmental protection aspect, preferably adopts ethanol.
Above-mentioned boron nitride coating is main raw material with the SP 1; Auxiliary curing agent wherein has silicon oxide, aluminum oxide, wilkinite etc.; There are China Shenzhen city Di Saite (DCT) metallurgical material ltd, U.S. GE Advanced Ceramics Corp (GE Advanced Ceramics Corp.) etc. in manufacturer; Can select the boron nitride coating of water base or organic solvent, by corresponding mixture ratio and deionized water or solvent preparation; Above-mentioned spraying can be carried out under normal pressure or low pressure, and above-mentioned drying can be baking or air-dry.
In order to guarantee to deposit the quality of liner, contained SP 1 is a particulate state in the described boron nitride coating, and the particulate mean diameter is not more than 300 microns.Too big boron nitride particle can cause coating to combine firmly inadequately with crucible.
Solar level boron doped agent crystal silicon ingot growth of the present invention and silicon feedstock purification thereof are prepared by following method with crucible:
In employing graphite, quartz or the charcoal carbon composite one or more make the crucible shell by ordinary method processing in the prior art; Evenly coating quality concentration is the pulpous state liquid of 3%～40% boron nitride coating on described crucible inner surface of outer cover; Dry back formation of deposits boron nitride coating; Machinery equating or polished finish obtain the uniform SP 1 liner of thickness, and wherein, the quality of SP 1 is no more than and joins 2% of the interior silicon raw materials quality of crucible in the described boron nitride coating.
In growth of solar level boron doped agent crystal silicon ingot and the silicon feedstock purification technology thereof, crucible diameter is more than the 150mm, to be generally more than the 200mm.
The present invention adopts the SP 1 liner of the internal surface that covers the crucible shell, because the resistance to elevated temperatures of SP 1 is fine, its chemicalstability is good; No sharp melting point, under low pressure (below the 1000Pa) is heat-resisting to more than 2000 ℃, the more important thing is; SP 1 at high temperature not with pasc reaction, do not soak into silicon, also not with the silicon adhesion; Thermal expansivity is low; Skin friction coefficient is little, so the SP 1 liner can be isolated melted silicon effectively and the inwall of the crucible shell processed by quartzy, graphite or CFC material, has both avoided melted silicon in the production process to be exuded to the outside of crucible through the capillary aperture on the inwall of crucible shell; Can avoid the sticking crucible of inwall of silicon ingot and crucible shell to destroy crucible and silicon ingot again; Thereby be used for the demoulding that melted silicon solidifies the back silicon ingot, and can also be applicable to the production environment of high-temperature low-pressure (temperature is more than 1400 ℃, and pressure is below 1000Pa).
It is 2% the SP 1 liner that 0.001mm～4mm and quality are no more than the silicon raw materials quality that joins in the crucible that the present invention adopts thickness; Make in growth of crystal silicon ingot or silicon feedstock purification; Because of boron (B) elemental diffusion in the SP 1 liner causes concentration that boron content in the melted silicon rises less than 0.6ppma (ppm be meant by 1,000,000 of amount of substance/); Can reach the effect of similar P type doping agent (like B, Al, Ga etc.) doped silicon liquation like this, obtain P N-type waferN silicon ingot or P N-type waferN silicon ingot is used the silicon raw material.Because when the P type mixed, when the resistivity of silicon ingot was 0.5 Ω cm, corresponding P type concentration of dopant was 0.64ppma; When the resistivity of silicon ingot was 1 Ω cm, corresponding P type concentration of dopant was 0.29ppma.As long as the resistivity of silicon ingot is controlled at more than the 0.5 Ω cm, can reaches the requirement of silicon ingot as the required resistivity of solar energy photovoltaic material.When producing N type solar energy level silicon raw material, need take in the main effect that receives of the boron that boron (B) elemental diffusion in the SP 1 liner causes, and suitably increase the consumption of N type doping agent, perhaps reduce the usage quantity of SP 1 and the thickness of SP 1 liner.Therefore, the present invention is applicable to growth of solar level crystal silicon ingot and silicon feedstock purification thereof fully.When producing P type solar level crystal silicon ingot, to a certain degree also can play the effect of saving mother alloy (doping agent B etc.), reducing cost.
Because when lacking SP 1 and directly contacting with the high temperature silicon liquation; Boron in the SP 1 is to the theoretical direction and the experimental data of the physical phenomenon of high temperature silicon liquation diffusion; Custom adopts the crucible releasing agent that silicon nitride is produced as silicon ingot in the prior art; And, then have serious technological prejudice for SP 1, think that it must cause serious boron doping and can't prepare industrial available silicon ingot.In fact; The present invention overcomes this technological prejudice; Through control to SP 1 thickness of inner lining and SP 1 quality; Realized boron (B) elemental diffusion in the SP 1 liner is caused effective control of the concentration that boron content in the melted silicon rises, simultaneously the resistivity of P N-type waferN silicon ingot has been controlled at 0.5～3 Ω cm in that the P type is adulterated, satisfied of the requirement of P type solar-grade silicon ingot fully for resistivity.Equally, this control is applicable to that also solar level P N-type waferN silicon ingot uses the silicon feedstock purification.When producing N type solar energy level silicon raw material; Because boron (B) elemental diffusion will cause a certain amount of boron doping in the solar-grade silicon ingot in the SP 1 liner; The main effect that receives that mixes and to cause to boron; Need suitably to increase the consumption of N type doping agents (like P, As etc.), realize the resistivity of being scheduled to through counter mixing, perhaps through the usage quantity (through reducing the mass ratio of SP 1 and silicon raw material) of minimizing SP 1 and the thickness of SP 1 liner.
In addition, adopt the crucible with SP 1 liner of the present invention,, reduced production cost because the good demolding performace of SP 1 liner can be avoided crucible to be damaged, thereby make crucible can access repeated use; And because the SP 1 thickness of inner lining is minimum, and spraying method manufacturing SP 1 liner cost is extremely low, therefore can after each production finishes, reuse behind the spraying formation SP 1 liner again again.In the prior art, when utilizing the casting crystalline silicon of directional solidification technique growth, adopt the container of quartz crucible usually, and quartz crucible can not recirculation use quartz crucible of every stove silicon ingot needs as running stores as the silicon raw material.Therefore, from this point, the present invention also can reduce production costs very effectively.
When crucible adopts quartz crucible as the container of silicon raw material,, then can avoid excessive oxygen element to penetrate in the melted silicon if cover the SP 1 liner at the internal surface of quartz crucible.Concerning the silicon raw material that is applied to the photovoltaic industry, when the photovoltaic silicon materials were the boron-doping material, too high oxygen level can produce photo attenuation, and caused as the decline of the solar battery efficiency of material produce.Therefore the SP 1 liner can reduce photo attenuation, improves the efficient of solar cell.
The present invention also provides growth of above-mentioned solar level boron doped agent crystal silicon ingot and silicon feedstock purification thereof with the application of crucible in solar level list/polycrystal silicon ingot is grown.
The present invention also provide growth of above-mentioned solar level boron doped agent crystal silicon ingot and silicon feedstock purification thereof with crucible in solar level list/polycrystal silicon ingot production with the application in the purification of silicon raw material.
With respect to prior art, the present invention has following useful technique effect:
The low cost of manufacture of crucible, and reuse, effectively reduce production cost; The SP 1 liner can be isolated melted silicon and the inwall of the crucible shell processed by quartzy, graphite or CFC material; Reduced the possibility of melted silicon effectively from the crucible seepage; Reduced the risk of cooling back silicon ingot and crucible outer casing rupture; And the crucible performance is more stable, can not influence the result of use of crucible following use of high-temperature low-pressure (temperature is more than 1400 ℃, and pressure is below 1000Pa).
In addition, when the SP 1 liner covered the internal surface of quartz crucible, SP 1 can play the oxygen element that stops in the quartz crucible and penetrate in the melted silicon.
Description of drawings
Fig. 1 one embodiment of the present invention;
Fig. 2 second kind of embodiment of the present invention;
Fig. 3 the third embodiment of the present invention;
Fig. 4 the 4th kind of embodiment of the present invention;
Label is in the accompanying drawing:
Single crystal growing is with shell 1, SP 1 liner 2, crucible main body 3, the crucible bottom 4 of crucible, seed crystal sleeve pipe 5, polycrystalline growth with the graphite housing 6 of crucible, polycrystalline growth with the quartz envelopes 7 of crucible, polycrystalline growth with crucible shell 8, silicon feedstock purification graphite shell 9 with crucible.
Embodiment
Embodiment 1:
A kind of crucible that is used for directional solidification method growth for solar level P type silicon single-crystal as shown in Figure 1 comprises crucible shell 1 and SP 1 liner 2.Crucible shell 1 is processed by graphite material, and SP 1 liner 2 is attached to the inner-wall surface of crucible shell 1, and the thickness of SP 1 liner 2 is 0.5mm.
Crucible integral body is divided into crucible main body 3 from top to bottom, 5 three parts of crucible bottom 4 and seed crystal sleeve pipe.In process of production, the silicon raw material is placed in the crucible main body 3, and seed crystal is placed in the seed crystal sleeve pipe 5; Distribution through controlled temperature; The silicon raw material is all melted, and make simultaneously near after the fusing of silicon part of raw materials seed crystal, the unfused seed crystal of lingering section is as the basis of seeding.Through changing the temperature field, can directional freeze produce solar level P type silicon single-crystal ingot casting.
The quality of SP 1 is to join 0.5% of the interior silicon raw materials quality of crucible in the SP 1 liner 2; Because the boron in the SP 1 is 0.1ppma to the doping of silicon; Is 0.14ppma for regulating the boron-doping mother alloy that resistance joins in the silicon raw material to the doping of silicon; The purity of silicon single-crystal ingot casting is 99.999%, and average resistivity is 1.2 Ω cm, satisfies the requirement of solar level P N-type waferN.
Embodiment 2:
Crucible use in solar level policrystalline silicon as shown in Figure 2 casting, and wherein the crucible shell is made up of double layer material, the graphite housing 6 outside being included in and in the quartz envelopes 7 of inboard.SP 1 liner 2 is coated in the internal surface of quartz envelopes 7; The employing spraying method applies; Be to be to be mixed with pulpous state liquid at 1: 10 by mass ratio with water base boron nitride coating and deionized water; And be the internal surface that is sprayed on quartz envelopes 7 under the 0.3MPa at pressure, forming on the internal surface of quartz envelopes 7 80 ℃ of dry backs of baking, its thickness is 0.2mm.Boron nitride coating is by GE Advanced Ceramics Corp. manufacturer production, and its product type is EPC.
Said crucible is used for the polycrystalline foundry furnace, and growth obtains large-sized solar level P type policrystalline silicon ingot casting.
The quality of SP 1 is to join 0.2% of the interior silicon raw materials quality of crucible in the SP 1 liner 2; Because the boron in the SP 1 is 0.06ppma to the doping of silicon; Is 0.13ppma for regulating the boron-doping mother alloy that resistance joins in the silicon raw material to the doping of silicon; The purity of silicon single-crystal ingot casting is 99.999%, and average resistivity is 1.5 Ω cm, satisfies the requirement of solar level P N-type waferN.
Embodiment 3:
Crucible is used in solar level policrystalline silicon casting as shown in Figure 3, is made up of crucible shell 8 and SP 1 liner 2.Similar with embodiment two, difference only is that crucible shell 8 processed by a kind of material, and this material is CFC (the charcoal charcoal is a compound) material.
Embodiment 4:
The crucible that is used for the silicon raw material that physics method purifying solar energy level P type silicon ingot uses as shown in Figure 4 is made up of shell 9 and SP 1 liner 2.Shell 9 adopts graphite material to be processed through machining by prior art; SP 1 liner 2 is mixed with pulpous state liquid with boron nitride coating and ethanol by certain (concrete proportioning is 1: 10) proportioning, and under normal pressure, is sprayed on the internal surface of shell 9, on the internal surface of shell 9, forms behind the natural air drying, and thickness is 0.6mm.Boron nitride coating is by GE Advanced Ceramics Corp. manufacturer production, and its product type is CPC.
In high temperature (1500 ℃～2200 ℃) and rough vacuum (under＜5Pa) the environment, to being placed on the operation of purifying of the inner melted silicon of crucible.Boron nitride material still can keep its stability under above-mentioned environment, promptly not with pasc reaction, also do not decompose or evaporate into gaseous state, played the effect of isolating graphite shell and melted silicon.After subtracting but, the silicon materials after the purification form flawless silicon ingot, not with the crucible adhesion; Used crucible is flawless also, and is repeatedly reusable.
The quality of SP 1 is to join 1% of the interior silicon raw materials quality of crucible in the SP 1 liner 2; Because the boron in the SP 1 is 0.22ppma to the doping of silicon; The purity of silicon single-crystal ingot casting is 99.999% after purifying, and average resistivity is 1.5 Ω cm, satisfies the requirement of solar energy level silicon raw material.
Claims (9)
1. solar level boron doped agent crystal silicon ingot growth and silicon feedstock purification thereof use crucible, it is characterized in that, are made up of crucible shell and the SP 1 liner that covers the crucible inner surface of outer cover, and the thickness of described SP 1 liner is 0.001mm～4mm; In the described employing of crucible shell graphite, quartz or the charcoal carbon composite one or more process;
Wherein, the quality of SP 1 is no more than and joins 2% of the interior silicon raw materials quality of crucible in the described SP 1 liner.
2. solar level boron doped agent crystal silicon ingot growth as claimed in claim 1 and silicon feedstock purification thereof are used crucible, and it is characterized in that: the thickness of described SP 1 liner is 0.01mm～2mm.
3. solar level boron doped agent crystal silicon ingot growth as claimed in claim 1 and silicon feedstock purification thereof are used crucible, and it is characterized in that: the thickness of described SP 1 liner is 0.02mm～1mm.
4. solar level boron doped agent crystal silicon ingot growth as claimed in claim 1 and silicon feedstock purification thereof are used crucible, it is characterized in that described SP 1 liner is processed by boron nitride material.
5. use crucible like arbitrary described solar level boron doped agent crystal silicon ingot growth of claim 1～4 and silicon feedstock purification thereof, it is characterized in that: described SP 1 liner is made by following method:
It is 3%～40% pulpous state liquid that boron nitride coating is diluted in solvent for mass concentration; Evenly spray or spread upon the internal surface of crucible shell; Dry back forms the deposition liner on the crucible inner surface of outer cover; Wherein, the quality of SP 1 is no more than and joins 2% of the interior silicon raw materials quality of crucible in the described boron nitride coating.
6. solar level boron doped agent crystal silicon ingot growth as claimed in claim 5 and silicon feedstock purification thereof are used crucible, and it is characterized in that: described solvent is deionized water or volatile organic solvent.
7. solar level boron doped agent crystal silicon ingot growth as claimed in claim 6 and silicon feedstock purification thereof are used crucible, and it is characterized in that: described volatile organic solvent is an ethanol.
8. solar level boron doped agent crystal silicon ingot growth as claimed in claim 5 and silicon feedstock purification thereof are with the application of crucible in solar level list/polycrystal silicon ingot growth.
9. solar level boron doped agent crystal silicon ingot as claimed in claim 5 growth and silicon feedstock purification thereof with crucible in solar level list/polycrystal silicon ingot production with the application in the purification of silicon raw material.
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| CN103305910A (en) * | 2012-03-15 | 2013-09-18 | 阿特斯(中国)投资有限公司 | Crucible for silicon ingot casting and preparation method of inner side coating thereof |
| CN103084325A (en) * | 2013-01-31 | 2013-05-08 | 天津英利新能源有限公司 | Crucible and coating method thereof |
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| CN106283183A (en) * | 2016-08-19 | 2017-01-04 | 西安华晶电子技术股份有限公司 | A kind of polycrystalline silicon casting ingot process based on boron nitride coating |
| CN106087048A (en) * | 2016-08-19 | 2016-11-09 | 西安华晶电子技术股份有限公司 | A kind of reduce the method for oxygen content bottom polycrystalline silicon ingot casting |
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| CN106283182B (en) * | 2016-08-19 | 2019-09-27 | 西安华晶电子技术股份有限公司 | A kind of polycrystalline silicon casting ingot process |
| CN106222740A (en) * | 2016-08-19 | 2016-12-14 | 西安华晶电子技术股份有限公司 | A kind of polycrystalline silicon ingot casting method reducing oxygen content bottom polycrystalline silicon ingot casting |
| CN116768653B (en) * | 2023-06-15 | 2024-04-02 | 湖南世鑫新材料有限公司 | Carbon-carbon thermal field crucible containing composite ceramic coating and preparation method thereof |
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