CN101979718A - Quartz crucible and method for casting quasi-single crystal - Google Patents
Quartz crucible and method for casting quasi-single crystal Download PDFInfo
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- CN101979718A CN101979718A CN 201010564154 CN201010564154A CN101979718A CN 101979718 A CN101979718 A CN 101979718A CN 201010564154 CN201010564154 CN 201010564154 CN 201010564154 A CN201010564154 A CN 201010564154A CN 101979718 A CN101979718 A CN 101979718A
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Abstract
The invention discloses a quartz crucible. The bottom of the quartz crucible is provided with a pit which is spontaneously generated by inducing seed crystal. The invention also discloses a method for casting quasi-single crystal by using the quartz crucible. By using the quartz crucible of the invention, the quality of grown cast crystalline silicon is effectively improved so as to improve the electrical performance of a solar cell. By the method for casting the quasi-single crystal in the invention, the diameter of the obtained crystal grain is about 5 to 10cm, tests show that the dislocation density is about 10<3>cm<-2> which is far less than a number range of 10<4> to 10<5>cm<-2> of silicon crystal obtained by the conventional casting method under the same condition; and accordingly, the minority carrier lifetime value of a silicon slice obtained by the method of the invention is about 18us which is greater than the minority carrier lifetime value of 11us of the silicon slice prepared from the same raw material by the conventional casting method.
Description
Technical field
The present invention relates to the photovoltaic industry, specifically is a kind of accurate single crystal casting quartz crucible, and a kind of accurate single crystal casting method.
Background technology
From present photovoltaic market, silicon solar cell occupies the most market share.According to the difference of employed material type, silicon solar cell can be divided into crystal-silicon solar cell and thin film silicon solar cell.Owing to apparatus expensive, technology than reason such as complexity and transformation efficiency be lower, the shared market share of thin film silicon solar cell will be far smaller than crystal-silicon solar cell, according to market statistics, crystal-silicon solar cell is about 85% at 2009 years portions.In crystal-silicon solar cell, because better simply manufacturing process of polycrystalline silicon material and relatively low manufacturing cost, since 2003, the shared market share of polysilicon surpassed single crystal silicon solar cell.
From present main flow technology, the weight of single polysilicon ingot casting can reach 450kg, be several times of the single crystal ingot weight of silicon single crystal, and the main process of growth of casting polycrystalline silicon ingot is exactly a directional freeze process, compare the process of growth (profit crystalline substance, necking down, shouldering, commentaries on classics shoulder, isodiametric growth, ending) of silicon single crystal and want much simple, this has just determined that the production cost of polysilicon chip is lower than monocrystalline silicon piece.Along with continuing to optimize of ingot casting technology, the average crystal grain diameter in the casting polycrystalline silicon can reach centimetre-sized, and like this, crystal boundary is not an especially severe just to the influence of polysilicon electric property.According to factory's scale operation data, by silicon single crystal and polycrystalline silicon solar cell that same process is made, absolute efficiency differs about 1-2%.
The basic craft course of casting generally is in quartz crucible the silicon raw material that melts to be solidified as silicon crystal gradually by the bottom to the top.In order to prevent that the crucible inwall generally applies Si from the contamination to silicon crystal of oxygen in the quartz crucible and other impurity
3N
4Coating, but still can not effectively stop in the crucible impurity particularly metallic impurity to the contamination of silicon crystal.These impurity frequents cause the raising of defective composite reactive on the defective of polysilicon, reduced the electric property of polysilicon and battery thereof.Therefore, a lot of companies and research group are devoted to develop the casting single crystal accurate single crystal technology that lives, and utilize the extremely low silicon crystal of casting growth defect density cheaply.
At present producing the company that goes before aspect the accurate monocrystalline at casting is BP Solar, and they have developed and have been called " Mono
2" accurate single crystal casting technology [Clark R. Casting single crystal silicon:Novel defect profiles from BP solar's mono (2) is wafers[J (TM) for Stoddard N; Wu B; Witting I; Wagener M; Park Y, Rozgonyi G]. Gettering and Defect Engineering in Semiconductor Technology Xii; 2008,131-133:1-8].Its basic thought is to add seed crystal in crucible bottom, charging on seed crystal again, and in the silicon melting process of raw material, seed crystal or a part of seed crystal remain solid-state, and in process of cooling, accurate monocrystalline will be along the crystal orientation crystallization of seed crystal.From the crystal that they obtain, defect concentration has obtained reducing significantly really, and is corresponding, also is improved by the solar cell of this accurate monocrystalline manufacturing and the performance of assembly.
Dendritic crystals growth is a notion common in the Metallkunde, and few people pay close attention in the silicon crystal growth.At the dendritic crystals growth crystallization initial stage, because the influence of condensate depression, certain crystal orientation speed of growth makes this crystal orientation be dendroid preferential growth in melt apparently higher than other crystal orientation.Along with the further cooling of melt, the dendritic crystalline substance that other melts go out with preferential growth gradually is that seed crystal is grown, until complete crystallization.Therefore, the crystal crystal orientation that obtains of this growth method is more single.Fujiwara is incorporated into this dendritic growth techniques in the polysilicon casting technique, utilizes silicon to obtain the casting polycrystalline silicon that crystal grain is big, crystal boundary density is lower in the crystalline growth characteristic according to qualifications of certain direction.The key of this technology is the thermal field control in the crystal boundary initial stage, obtain in crucible bottom＜112〉crystal face crystallization, the crystallization of back will be along the constantly upwards growth of this direction, finish [Fujiwara K up to crystallisation process, Pan W, Usami N, Sawada K, Tokairin M, Nose Y, Nomura A, Shishido T, Nakajima K. Growth of structure-controlled polycrystalline silicon ingots for solar cells by casting[J]. Acta Materialia, 2006,54 (12): 3191-3197].Utilize in the polysilicon that dendritic brilliant casting obtains, the obviously more common polysilicon of crystal grain is big, and crystal boundary density is obviously lower, and from the crystal orientation,＜112〉crystal orientation proportions are very high.According to report, be improved significantly by the solar cell transformation efficiency of this polysilicon manufacturing.
Yet more than all there is certain shortcoming in the accurate single crystal technology of casting.Mono for BP Solar
2Technology, accurate single crystal growing need the auxiliary of seed crystal, and the adding of seed crystal has directly increased the production cost of casting; For the accurate single crystal technology of dendritic brilliant casting, the accurate control at silicon crystal crystallization initial stage is extremely important, needs the growth of the special dendritic crystalline substance of foundry furnace ability better controlled, and early stage, the result obtained in the laboratory, and also there is certain problem in industrial production.
Summary of the invention
Goal of the invention: the objective of the invention is to overcome the deficiencies in the prior art, provide a kind of and cast the quartz crucible of accurate monocrystalline and adopt this crucible to cast the method for accurate monocrystalline.
Technical scheme: to achieve these goals, the invention provides a kind of quartz crucible, described quartz crucible bottom has the pit of inducing the spontaneous growth of seed crystal.
A kind of quartz crucible, bottom have the pit of the seeded growth of inducing.The pit of seeded growth is induced in described quartz crucible bottom, and it is shaped as horn-like or funnel-form.
The pit of seeded growth is induced in described quartz crucible bottom, is made of taper top and column bottom.The upper end, taper top of described pit is ellipse or Polygons; The bottom of column bottom is ellipse or Polygons.
Described pit full depth h is 2-14cm; The minor face d of oval minor axis of described column lower base or Polygons is 5mm ~ 50mm; Described column bottom (2) height h' is greater than 2d; The minor face D of described conical upper oval minor axis in upper end or Polygons is 30mm ~ 156mm.It is D ~ 2D that described adjacent seed crystal is induced the distance between the pit.Described quartz crucible bottom thickness is 5cm ~ 15cm.Described quartz crucible surface-coated silicon nitride coating.
The invention also discloses a kind of method of casting accurate monocrystalline, the concrete steps of this method are as follows:
(1) adopt above-mentioned quartz crucible to cast accurate monocrystalline, the silicon material of at first in quartz crucible, packing into;
(2) quartz crucible is put into foundry furnace, temperature in the stove, 1450-1580 degree centigrade;
(3) crystallization velocity of the interior silicon melt of initial stage pit is less than 1mm/min;
(4) finish whole crystalline growth with the speed of 0.5-3mm/min then;
(5) cooling is come out of the stove.
Can put into single crystal seed in the bottom pit of quartz crucible in the step described in the present invention (1), the length of described single crystal seed is 2cm～5cm, and diameter and pit lower end cylindrical region are measure-alike.
The present invention utilizes the natural selection rule of crystal growth, when crystal in than the container of minor diameter during crystallization, as shown in Figure 1, suppose to exist nucleus A, B and the C in three crystal orientation, because the crystalline anisotropy at container bottom, different crystal orientations speed of growth difference, suppose that the fastest direction of growth in B crystal orientation is parallel with wall of container, and A, the fastest direction of growth in C crystal orientation and wall of container oblique, behind the certain altitude of growing, A and C crystal orientation will only be stayed the B crystal orientation by natural selection.Utilize this principle, we just can obtain the seed crystal of follow-up crystal growth.
The present invention makes in the quartz crucible bottom and arranges the big young pit of inducing the spontaneous growth of seed crystal down suitable for reading, effectively raises the quality of the casting crystalline silicon that grows, and then has improved the electric property of solar cell.
Beneficial effect: the use of quartz crucible of the present invention effectively raises the quality of the accurate monocrystalline that grows, and then has improved the electric property of solar cell.
The method of the accurate monocrystalline of casting described in the present invention, the crystal grain diameter that obtains is about 5-10cm, and dislocation desity is 10 after tested
3Cm
-2About, in the silicon crystal that the conventional cast method obtains under the same terms 10
4-10
5Cm
-2Numerical range; Accordingly, the silicon chip minority carrier life time value that adopts the method for the invention to obtain is about 18us, the minority carrier life time value of the 11us of the silicon chip that obtains greater than the same materials ordinary casting method.
Description of drawings
Fig. 1 natural selection rule synoptic diagram.
Fig. 2 is quartz crucible structural representation described in the present invention.
Fig. 3 is quartz crucible sectional view described in the present invention.
Fig. 4 induces a kind of structural representation of the pit of seeded growth for the bottom of quartz crucible described in the present invention.
Fig. 5 induces a kind of structural representation of the pit of seeded growth for the bottom of quartz crucible described in the present invention.
Fig. 6 induces a kind of structural representation of the pit of seeded growth for the bottom of quartz crucible described in the present invention.
Fig. 7 induces a kind of structural representation of the pit of seeded growth for the bottom of quartz crucible described in the present invention.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment only is used to the present invention is described and is not used in and limit the scope of the invention, after having read the present invention, those skilled in the art all fall within the application's claims to the modification of the various equivalent form of values of the present invention and limit.
A kind of quartz crucible is shaped as squarely, and crucible bottom is provided with horn-like pit; Crucible base thickness degree is 10cm; Upper end large circle diameter D size 100mm, lower end small circle ring diameter 1cm, h ' size is 5cm, and pit depth is 8cm, and the bottom surface makes 36 of evenly distributed pits; Quartz crucible surface-coated silicon nitride coating.
A kind of method of casting accurate monocrystalline, the concrete steps of this method are as follows:
(1) adopt the quartz crucible described in the present embodiment, and the silicon ingot of the 270kg that in quartz crucible, packs into;
(2) quartz crucible is put into foundry furnace, temperature is 1450 degrees centigrade in the stove;
(3) crystallization velocity of silicon melt is 0.8mm/min in the initial stage pit;
(4) finish whole crystalline growth with the speed of 1mm/min then;
(5) cooling is come out of the stove.
A kind of quartz crucible is shaped as squarely, and the crucible bottom setting is the shape pit as shown in accompanying drawing 4; Crucible base thickness degree is 15cm; Upper end length of side D size 156mm, lower end length of side d is 30mm, and h ' size is 80mm, and pit depth h is 13cm, and the bottom surface makes 25 of evenly distributed pits; Quartz crucible surface-coated silicon nitride coating.
A kind of method of casting accurate monocrystalline, the concrete steps of this method are as follows:
(1) adopt the quartz crucible described in the present embodiment, and the silicon ingot of the 450kg that in quartz crucible, packs into;
(2) quartz crucible is put into foundry furnace, temperature is 1580 degrees centigrade in the stove;
(3) crystallization velocity of silicon melt is 0.5mm/min in the initial stage pit;
(4) finish whole crystalline growth with the speed of 3mm/min then;
(5) cooling is come out of the stove.
Embodiment 3
A kind of quartz crucible is shaped as squarely, and the crucible bottom setting is the shape pit as shown in accompanying drawing 5; Crucible base thickness degree h is 5cm; Tetragon minor face long D size in upper end is 75mm, and the long length of side equates that with the crucible length of side lower end long d of tetragon minor face is 5mm, and h ' size is 25mm, and pit depth is 13cm, and the bottom surface makes 10 of parallel evenly distributed pits; Quartz crucible surface-coated silicon nitride coating.
A kind of method of casting accurate monocrystalline, the concrete steps of this method are as follows:
(1) adopt the quartz crucible described in the present embodiment, and the silicon ingot of the 450kg that in quartz crucible, packs into;
(2) quartz crucible is put into foundry furnace, temperature is 1520 degrees centigrade in the stove;
(3) crystallization velocity of silicon melt is 0.5mm/min in the initial stage pit;
(4) finish whole crystalline growth with the speed of 0.5mm/min then;
(5) cooling is come out of the stove.
Embodiment 4
A kind of quartz crucible is shaped as squarely, and the crucible bottom setting is the shape pit as shown in accompanying drawing 6; Crucible base thickness degree h is 10cm; Tetragon minor face long D size in upper end is 30mm, and the long length of side equates that with the crucible length of side lower end long d of tetragon minor face is 5mm, and h ' size is 35mm, and pit depth is 7cm, and the bottom surface makes 25 of parallel evenly distributed pits; Quartz crucible surface-coated silicon nitride coating.
A kind of method of casting accurate monocrystalline, the concrete steps of this method are as follows:
(1) adopt the quartz crucible described in the present embodiment, and the silicon ingot of the 450kg that in quartz crucible, packs into;
(2) quartz crucible is put into foundry furnace, temperature is 1480 degrees centigrade in the stove;
(3) crystallization velocity of silicon melt is 0.5mm/min in the initial stage pit;
(4) finish whole crystalline growth with the speed of 1.5mm/min then;
(5) cooling is come out of the stove.
Embodiment 5
A kind of quartz crucible is shaped as squarely, and the crucible bottom setting is the shape pit as shown in accompanying drawing 7; Crucible base thickness degree h is 15cm; Tetragon minor face long D size in upper end is 156mm, and the long length of side equates that with the crucible length of side lower end long d of tetragon minor face is 50mm, and h ' size is 100mm, and pit depth is 14cm, and the bottom surface makes 5 of parallel evenly distributed pits; Quartz crucible surface-coated silicon nitride coating.
A kind of method of casting accurate monocrystalline, the concrete steps of this method are as follows:
(1) adopt the quartz crucible described in the present embodiment, and the silicon ingot of the 450kg that in quartz crucible, packs into;
(2) quartz crucible is put into foundry furnace, temperature is 1480 degrees centigrade in the stove;
(3) crystallization velocity of silicon melt is 0.3mm/min in the initial stage pit;
(4) finish whole crystalline growth with the speed of 2.5mm/min then;
(5) cooling is come out of the stove.
Embodiment 6
A kind of quartz crucible is shaped as squarely, and the crucible bottom setting is the shape pit as shown in accompanying drawing 4; Crucible base thickness degree is 15cm; Upper end length of side D size 156mm, lower end length of side d is 30mm, and h ' size is 80mm, and pit depth h is 13cm, and the bottom surface makes 25 of evenly distributed pits; Quartz crucible surface-coated silicon nitride coating.
A kind of method of casting accurate monocrystalline, the concrete steps of this method are as follows:
(1) be 30mm in the crucible bottom pit, putting into the bottom surface length of side respectively, (100) crystal orientation seed crystal of length 2-5cm;
(2) adopt the quartz crucible described in the present embodiment, and the silicon ingot of the 450kg that in quartz crucible, packs into;
(3) quartz crucible is put into foundry furnace, stay-warm case promotes 5cm than the original position, guarantees that seed crystal can not melt fully, and controls 1540 degrees centigrade of the interior temperature of stove;
(4) crystallization velocity of silicon melt is 1mm/min in the initial stage pit;
(5) finish whole crystalline growth with the speed of 3mm/min then;
(6) cooling is come out of the stove.
Claims (9)
1. a quartz crucible is characterized in that: the pit that has the seeded growth of inducing bottom the described quartz crucible.
2. a kind of quartz crucible according to claim 1 is characterized in that: the pit of seeded growth is induced in described quartz crucible bottom, and it is shaped as horn-like or funnel-form.
3. a kind of quartz crucible according to claim 2 is characterized in that: the pit of seeded growth is induced in described quartz crucible bottom, is made of taper top (1) and column bottom (2).
4. a kind of quartz crucible according to claim 3 is characterized in that: the upper end, taper top (1) of described pit is ellipse or Polygons; The bottom of column bottom (2) is ellipse or Polygons.
5. a kind of quartz crucible according to claim 3 is characterized in that: described pit full depth h is 2-14cm; The minor face d of oval minor axis in described column bottom (2) bottom or Polygons is 5mm ~ 50mm; Described column bottom (2) height h' is greater than 2d; The minor face D of oval minor axis in described conical upper (1) upper end or Polygons is 30mm ~ 156mm; It is D ~ 2D that described adjacent seed crystal is induced the distance between the pit.
6. according to the described a kind of quartz crucible of arbitrary claim among the claim 1-5, it is characterized in that: described quartz crucible bottom thickness is 5cm ~ 15cm.
7. a kind of quartz crucible according to claim 1 is characterized in that: described quartz crucible surface-coated silicon nitride coating.
One kind the casting accurate monocrystalline method, it is characterized in that: the concrete steps of this method are as follows:
(1) adopts the described quartz crucible of arbitrary claim among the right 1-5, in quartz crucible, pack into silicon ingot or single crystal seed;
(2) quartz crucible is put into foundry furnace, the design temperature scope is 1450-1580 degree centigrade in the stove;
(3) initial stage makes the crystallization velocity of silicon melt in the pit less than 1mm/min by control stay-warm case pulling speed or crucible bottom speed of cooling;
(4) finish whole crystalline growth by control stay-warm case pulling speed or crucible bottom speed of cooling with the speed of 0.5-3mm/min then;
(5) cooling is come out of the stove.
9. a kind of method of casting accurate monocrystalline according to claim 7, it is characterized in that: can put into single crystal seed in the bottom pit of quartz crucible in the described step (1), the length of described single crystal seed is 2cm～5cm, and diameter and pit lower end cylindrical region are measure-alike.
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| CN102605418A (en) * | 2012-01-16 | 2012-07-25 | 上澎太阳能科技(嘉兴)有限公司 | Solar cell substrate, manufacturing method of solar cell and crucible used for same |
| CN102766904A (en) * | 2012-08-15 | 2012-11-07 | 常熟华融太阳能新型材料有限公司 | Silica ceramic crucible |
| CN102776554A (en) * | 2012-04-01 | 2012-11-14 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot, preparation method of polycrystalline silicon ingot and polycrystalline silicon slice |
| FR2979638A1 (en) * | 2011-09-05 | 2013-03-08 | Commissariat Energie Atomique | DEVICE FOR MANUFACTURING CRYSTALLINE MATERIAL FROM A NON-UNIFORM THERMAL RESISTANCE CUP |
| CN103255475A (en) * | 2012-02-15 | 2013-08-21 | 昆山中辰矽晶有限公司 | Silicon crystal ingot containing nucleation promoting particles and method for producing same |
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| CN103628132A (en) * | 2012-08-21 | 2014-03-12 | 国硕科技工业股份有限公司 | Polycrystalline silicon chip, polycrystalline silicon ingot and method for manufacturing polycrystalline silicon ingot |
| CN103806096A (en) * | 2012-11-15 | 2014-05-21 | 茂迪股份有限公司 | Crucible and filling method of crucible silicon material |
| CN104342752A (en) * | 2013-07-29 | 2015-02-11 | 晶科能源有限公司 | Method for ingoting polycrystalline silicon |
| CN107974710A (en) * | 2017-11-21 | 2018-05-01 | 浙江师范大学 | The growing method of high-performance polycrystal silicon based on quartzy seed crystal |
| CN111778548A (en) * | 2019-04-04 | 2020-10-16 | 天合光能股份有限公司 | Crucible for casting monocrystalline silicon and method for casting monocrystalline silicon |
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| US9945046B2 (en) | 2011-09-05 | 2018-04-17 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Device for manufacturing a crystalline material from a crucible having non-uniform heat resistance |
| CN103917699A (en) * | 2011-09-05 | 2014-07-09 | 原子能和代替能源委员会 | Device for manufacturing a crystalline material from a crucible having non-uniform heat resistance |
| FR2979638A1 (en) * | 2011-09-05 | 2013-03-08 | Commissariat Energie Atomique | DEVICE FOR MANUFACTURING CRYSTALLINE MATERIAL FROM A NON-UNIFORM THERMAL RESISTANCE CUP |
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| CN103255475A (en) * | 2012-02-15 | 2013-08-21 | 昆山中辰矽晶有限公司 | Silicon crystal ingot containing nucleation promoting particles and method for producing same |
| CN102776554A (en) * | 2012-04-01 | 2012-11-14 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot, preparation method of polycrystalline silicon ingot and polycrystalline silicon slice |
| CN102776554B (en) * | 2012-04-01 | 2015-09-16 | 江西赛维Ldk太阳能高科技有限公司 | A kind of polycrystal silicon ingot and preparation method thereof and polysilicon chip |
| CN102766904A (en) * | 2012-08-15 | 2012-11-07 | 常熟华融太阳能新型材料有限公司 | Silica ceramic crucible |
| CN103628132A (en) * | 2012-08-21 | 2014-03-12 | 国硕科技工业股份有限公司 | Polycrystalline silicon chip, polycrystalline silicon ingot and method for manufacturing polycrystalline silicon ingot |
| CN103628132B (en) * | 2012-08-21 | 2017-04-12 | 国硕科技工业股份有限公司 | Polycrystalline silicon chip, polycrystalline silicon ingot and method for manufacturing polycrystalline silicon ingot |
| CN103806096A (en) * | 2012-11-15 | 2014-05-21 | 茂迪股份有限公司 | Crucible and filling method of crucible silicon material |
| CN103806096B (en) * | 2012-11-15 | 2016-09-07 | 茂迪股份有限公司 | The packing method of crucible silicon material |
| CN104342752A (en) * | 2013-07-29 | 2015-02-11 | 晶科能源有限公司 | Method for ingoting polycrystalline silicon |
| CN103590105A (en) * | 2013-11-25 | 2014-02-19 | 天津英利新能源有限公司 | Silicon ingot casting device |
| CN107974710A (en) * | 2017-11-21 | 2018-05-01 | 浙江师范大学 | The growing method of high-performance polycrystal silicon based on quartzy seed crystal |
| CN111778548A (en) * | 2019-04-04 | 2020-10-16 | 天合光能股份有限公司 | Crucible for casting monocrystalline silicon and method for casting monocrystalline silicon |
| CN112899777A (en) * | 2019-11-19 | 2021-06-04 | 苏州阿特斯阳光电力科技有限公司 | Seed wafer, preparation method thereof and preparation method of crystalline silicon ingot |
| CN112899777B (en) * | 2019-11-19 | 2022-05-13 | 苏州阿特斯阳光电力科技有限公司 | Seed wafer, preparation method thereof and preparation method of crystalline silicon ingot |
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Application publication date: 20110223 |