CN102277618B - Polysilicon ingot, manufacturing method and growing furnace thereof, as well as bottom plate and solar cell of growing furnace - Google Patents
Polysilicon ingot, manufacturing method and growing furnace thereof, as well as bottom plate and solar cell of growing furnace Download PDFInfo
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- CN102277618B CN102277618B CN2011102131884A CN201110213188A CN102277618B CN 102277618 B CN102277618 B CN 102277618B CN 2011102131884 A CN2011102131884 A CN 2011102131884A CN 201110213188 A CN201110213188 A CN 201110213188A CN 102277618 B CN102277618 B CN 102277618B
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Abstract
The embodiment of the invention discloses a polysilicon ingot, a manufacturing method and a growing furnace thereof, as well as a bottom plate and a solar cell of the growing furnace. The method comprises the following steps: spreading crystal seeds at the bottom of a vessel in the polysilicon ingot growing furnace to form a crystal seed layer, wherein a plurality of mutually crossed grooves are formed on the a bottom plate positioned under the vessel, and the grooves and gaps among the crystal seeds inside the vessel are positioned on the same vertical plane; loading a solid-state silicon raw material on the crystal seed layer; melting the silicon raw material and partial crystal seed layer to form a liquid layer, introducing an inert gas in the grooves on the bottom plate in the processof melting the partial crystal seed layer, and at least maintaining part of the crystal seed layer, which contacts the bottom of the vessel, to be in a solid state; and controlling the thermal field in the polysilicon ingot growing furnace, and crystallizing the liquid layer until the growth of the polysilicon ingot is completed. The polysilicon ingot cast by adopting the method includes most monosilicon areas, the crystal boundary density in the polysilicon ingot is reduced, and the photoelectric conversion efficiency of the solar cell produced by adopting the polysilicon ingot is improved.
Description
Technical field
The present invention relates to the manufacturing technology of polysilicon, relate in particular to a kind of manufacture method of polycrystal silicon ingot.
Background technology
The energy and environment are the two large problems of world today's extensive concern, and sun power becomes the focus of people's R and D naturally as a kind of reproducible green energy resource.Be accompanied by the fast development of solar cell industry, cost polysilicon lower and that be suitable for scale operation has become one of topmost photovoltaic material, and progressively replaces the dominant position of traditional pulling of silicon single crystal in the middle of solar cell material market.
At present, the method of the polycrystal silicon ingot of preparation used for solar batteries is mainly directional solidification method, namely in the raw silicon process of setting of fusion, by the thermograde of control solid-liquid interface, to carry out controlled directional freeze process, form polycrystalline column crystal (hereinafter to be referred as polycrystal silicon ingot).
Above-mentioned directional solidification method refers in particular to directional freeze systems approach (Directional solidification system is called for short DSS) the stove crystal technique that the present GT Solar that generally adopts provides.Directional solidification method is a kind of method of casting polycrystalline silicon, its mainly comprise heating, melt, solidify processing steps such as long crystalline substance, annealing, cooling, in heating and melting process, thermal insulator in the polycrystal silicon ingot growth furnace is sealed, with thermal insulator lifting all around, below crucible, leave the openning of a heat transfer when length is brilliant, the silicon raw material of molten state is begun to cool down from the bottom, realize silicon raw material directional freeze from lower to upper, thereby finish the castingprocesses of polycrystal silicon ingot gradually.DSS growing technology can grow big polycrystal silicon ingot thereby the output height of polysilicon.The process of growth of the relative silicon single crystal of this technology controlling and process in addition, the process of growth of polysilicon is simple, and production cost is low, and this technology can produce big square polysilicon chip, has reduced the cost of downstream cell processing course.
But find in the actual production process, the solar cell that the polycrystal silicon ingot that adopts the DSS method to produce is produced, often there are problems such as photoelectric transformation efficiency is low, the contriver discovers, the reasons for the above problems are that foreign matter content and the defect concentration in the polycrystal silicon ingot of producing in the prior art is all higher, and this has just directly influenced the photoelectric transformation efficiency of solar cell.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of manufacture method of polycrystal silicon ingot, reduced foreign matter content and the defect concentration in the polycrystal silicon ingot, and the photoelectric transformation efficiency of the solar cell that the polycrystal silicon ingot in the employing embodiment of the invention is produced is improved.
For addressing the above problem, the embodiment of the invention provides following technical scheme:
A kind of manufacture method of polycrystal silicon ingot comprises:
Container bottom in the polycrystal silicon ingot growth furnace is laid seed crystal, form inculating crystal layer, in described polycrystal silicon ingot growth furnace, be positioned on the base plate of described container below and have the cross one another groove of multiple tracks, the seed crystal of described groove and internal tank and the slit between seed crystal are positioned on the same vertical plane;
Solid-state silicon raw material is loaded into the top of described inculating crystal layer;
Described container is heated, melt described silicon raw material and the described inculating crystal layer of part, with the formation liquid level, and in the described inculating crystal layer melting process of part, groove on described base plate feeds rare gas element, and the part inculating crystal layer that keeps at least contacting with described container bottom is solid-state;
Control the thermal field in the described polycrystal silicon ingot growth furnace, described liquid level is carried out crystallization, so that solid-liquid interface moves to the direction away from described container bottom, finish until the polycrystal silicon ingot growth.
Preferably, described liquid level is carried out in the crystallisation process, the temperature that is positioned at the place, slit between the seed crystal of described groove top is higher than the temperature of other position, and place, the slit crystal growth rate between seed crystal is less than the crystal growth rate of other position.
Preferably, described polycrystal silicon ingot contains continuous large-sized monocrystalline silicon region, and the crystalline orientation of described monocrystalline silicon region is identical with the crystalline orientation of the described seed crystal that is positioned at its below.
Preferably, the process of the described silicon raw material of described fusing and the described inculating crystal layer of part comprises: described container top and/or container side wall are heated, keep the container top temperature to be higher than the fusing point of silicon, the container bottom temperature is lower than the fusing point of silicon, formation is perpendicular to the thermograde of container bottom, make silicon raw material and the fusing successively from top to bottom of part seed crystal in the described container, and the part inculating crystal layer that maintenance contacts with described container bottom is solid-state.
Preferably, described described container is carried out in the heat-processed, keep described solid-liquid interface substantially parallel with the bottom of described container.
Preferably, described liquid level is carried out crystallisation process to be comprised: open described container thermal insulator all around, and by the water-cooling system around the described container described container is cooled off, formation is perpendicular to the thermograde of container bottom, described liquid level is carried out crystallization, and the temperature in the described container rises gradually along the direction that makes progress perpendicular to container bottom.
Preferably, described liquid level is carried out crystallisation process, the temperature of described internal tank rises slowly along the direction that makes progress perpendicular to container bottom.
Preferably, described seed crystal is that crystalline orientation is the silicon single crystal of (100), (110) or (111) orientation.
Preferably, the process that forms described inculating crystal layer is specially: adopt the bulk seed crystal splicing paving that crystalline orientation is identical and have the geometrical shape of rule, to cover the most of zone of described container bottom, have the slit between described bulk seed crystal.
Preferably, described bulk seed crystal is square seed crystal or rectangle seed crystal.
Preferably, the minor face of described bulk seed crystal is 100mm-160mm.
Preferably, also comprise: when described bulk seed crystal can not cover described container bottom fully, adopt the bar shaped seed crystal identical with the crystalline orientation of described bulk seed crystal to fill zone between described bulk seed crystal edge and described container side wall.
Preferably, the width in the slit between the slit between described bulk seed crystal and/or described bulk seed crystal and bar shaped seed crystal is in 10mm.
Preferably, has chamfering on described bulk seed crystal and/or bar shaped seed crystal and the one side that the silicon raw material contacts.
Preferably, the degree of depth of described chamfering is in 10mm-30mm.
Preferably, the angle of described chamfering is in 70 °.
Preferably, the thickness of described inculating crystal layer is 10mm-30mm.
Preferably, the process that solid-state silicon raw material is loaded into the top of described inculating crystal layer is specially:
Silica flour is loaded into the top of described inculating crystal layer, to fill slit between described seed crystal and the slit between described inculating crystal layer and described container side wall;
The silicon raw material of large volume is loaded into the top of described silica flour.
Compared with prior art, technique scheme has the following advantages:
The technical scheme that the embodiment of the invention provides, adopt the method for casting to produce polycrystal silicon ingot, form inculating crystal layer by laying the big area seed crystal at container bottom, growth by seed crystal guiding monocrystalline silicon region, make and comprise continuous large-sized monocrystalline silicon region in the polycrystal silicon ingot of producing, the polycrystal silicon ingot that namely casts out is by most of monocrystalline silicon region consistent with the seed crystal orientation, and the polysilicon region of small part composition.
And, in the inculating crystal layer melting process, groove on described base plate has fed rare gas element, in the long brilliant stage, the gas temperature that groove feeds has obtained rising, because the thermal conductivity of rare gas element is much smaller than the thermal conductivity of graphite, therefore described liquid level is being carried out in the crystallisation process, be positioned at the temperature that the temperature at the place, slit between the seed crystal of groove top will a little higher than other position, thereby make the slit between seed crystal locate crystal growth rate less than the crystal growth rate of other position, and then probability and the content of the polysilicon of crystal boundary place generation will be reduced, thereby further reduced the crystal boundary density in the polycrystal silicon ingot.And owing to contain continuous large-sized monocrystalline silicon region in the polycrystal silicon ingot, therefore, the photoelectric transformation efficiency of the solar cell that the polycrystal silicon ingot that adopts the embodiment of the invention to provide is produced is improved.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art, to do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below, apparently, accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the schematic flow sheet of the manufacture method of the disclosed polycrystal silicon ingot of the embodiment of the invention;
Fig. 2 is the sectional view of the disclosed receptacle support means of the embodiment of the invention;
Fig. 3 is the vertical view of the disclosed polycrystal silicon ingot growth furnace of embodiment of the invention base plate;
Fig. 4 is the sectional view of the disclosed polycrystal silicon ingot growth furnace of the embodiment of the invention;
Fig. 5 is the schematic flow sheet of the manufacture method of the disclosed polycrystal silicon ingot of another embodiment of the present invention;
Fig. 6 and Fig. 7 are the disclosed seed crystal paving mode of another embodiment of the present invention vertical view;
Fig. 8 is the structural representation of the disclosed seed crystal edge chamfer of another embodiment of the present invention;
Fig. 9 is the sectional view of the polycrystal silicon ingot produced in another embodiment of the present invention.
Embodiment
Just as described in the background section, the photoelectric transformation efficiency of the solar cell that the polycrystal silicon ingot that the DSS mode of employing prior art is produced is made is low, the contriver discovers, the reason that this problem occurs is because polycrystal silicon ingot foreign matter content height, defect concentration are big on the one hand, concrete, oxygen and carbon are main light-element impurities in the polycrystal silicon ingot of casting, especially the concentration of carbon will be higher than the concentration in the pulling of silicon single crystal, also has impurity such as metallic element, nitrogen, hydrogen also can cause detrimentally affect to polycrystalline silicon material and Solar cell performance in addition; Be because the polycrystal silicon ingot that casts out has highdensity crystal boundary, dislocation and microdefect on the other hand, these defectives become the deathnium of minority carrier in the silicon materials, make electric charge carrier compound fast, cause minority carrier life time low, and, because the orientation of intergranule is at random, be difficult to adopt chemical process that texture is carried out on its surface, thereby can not reduce polysilicon surface to the reflection of light rate, can not improve the characteristics such as specific absorption to light, cause the polysilicon solar cell photoelectric transformation efficiency low.
Based on above reason, the contriver considers, Comparatively speaking, the efficiency of conversion of monocrystaline silicon solar cell is than the efficiency of conversion height of polysilicon solar cell, its major cause is the grain orientation unanimity of silicon single crystal, therefore there are not defectives such as crystal boundary, comprise large-sized monocrystalline silicon region if make in the polycrystal silicon ingot of production, should be able to solve the low shortcoming of polysilicon solar cell efficiency of conversion in the prior art to a certain extent.
It more than is the application's core concept, below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is clearly and completely described, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
A lot of details have been set forth in the following description so that fully understand the present invention, but the present invention can also adopt other to be different from alternate manner described here and implement, those skilled in the art can do similar popularization under the situation of intension of the present invention, so the present invention is not subjected to the restriction of following public specific embodiment.
Secondly, the present invention is described in detail in conjunction with synoptic diagram, when the embodiment of the invention is described in detail in detail; for ease of explanation; the sectional view of expression device architecture can be disobeyed general ratio and be done local the amplification, and described synoptic diagram is example, and it should not limit the scope of protection of the invention at this.The three-dimensional space size that in actual fabrication, should comprise in addition, length, width and the degree of depth.
On the basis based on above-mentioned research, the embodiment of the invention provides a kind of manufacture method of polycrystal silicon ingot, and the schema of this method may further comprise the steps as shown in Figure 1:
Step S101: the container bottom in the polycrystal silicon ingot growth furnace is laid seed crystal, form inculating crystal layer, in described polycrystal silicon ingot growth furnace, be positioned on the base plate of described container below and have the cross one another groove of multiple tracks, the seed crystal of described groove and internal tank and the slit between seed crystal are positioned on the same vertical plane;
Wherein, described seed crystal is the fixing silicon single crystal of crystalline orientation, described inculating crystal layer comprises the monocrystalline silicon layer of at least a crystalline orientation, preferably, seed crystal in the present embodiment is that crystalline orientation is the silicon single crystal of (100), (110) or (111), preferred, it is the silicon single crystal paving formation of (100) that the inculating crystal layer in the present embodiment all adopts crystalline orientation.
This does not limit the shape and size of described seed crystal present embodiment, described inculating crystal layer can be the big or small and essentially identical bulk seed crystal of shape with container bottom, also can be pieced together by the polylith seed crystal and form, if the latter, for the convenience of process of deployment and the needs that satisfy complete tiling, seed crystal preferably has the geometrical shape of rule, preferred described seed crystal is shaped as rectangle, more preferably square, to select bigger seed crystal as far as possible, so that the slit of piecing together between the seed crystal of formation is as far as possible little, to guarantee the quality of polycrystal silicon ingot.Describe in detail in following examples about the shape of described seed crystal, size, paving mode etc., do not do concrete restriction in the present embodiment.
And, also specifically do not limit the paving mode of described inculating crystal layer in the present embodiment, but in order to guarantee the quality of the silicon single crystal in the polycrystal silicon ingot, preferably, described seed crystal is layed in the region intermediate of described container, in addition, in order better to control making processes and the quality of described polycrystal silicon ingot, described inculating crystal layer should keep substantially parallel or approximate parallel with described container bottom.
Same, also specifically do not limit the thickness of described inculating crystal layer in the present embodiment, decide with concrete production process and working condition, preferably, the thickness of described inculating crystal layer is 10mm-30mm.
Container described in the present embodiment is generally square crucible, more general is ceramic crucible, certainly, what described container can also be selected other castingprocesses that can be used for polycrystal silicon ingot can disposable crucible or reusable crucible, as quartz crucible, molybdenum crucible or tungsten crucible etc.
And, adapt with the polycrystal silicon ingot manufacture method in the present embodiment, a kind of base plate is also disclosed in the present embodiment, and the polycrystal silicon ingot growth furnace with this base plate, as Fig. 2-shown in Figure 4, Fig. 2 is the sectional view of the receptacle support means in this polycrystal silicon ingot growth furnace, and Fig. 3 is the vertical view of this base plate, and Fig. 4 is the sectional view of this polycrystal silicon ingot growth furnace.
As shown in Figure 4, this polycrystal silicon ingot growth furnace comprises:
Body of heater 28;
Be positioned at the receptacle support means of described bottom of furnace body, described bracing or strutting arrangement comprises base plate 26, and namely this base plate 26 is positioned at the container below of polycrystal silicon ingot growth furnace, to carry described container;
Be positioned at the container of described base plate 26 tops, can lay inculating crystal layer and silicon raw material in the described container, container described in the present embodiment is preferably crucible 22;
Wherein, have the cross one another groove 27 of multiple tracks on the described base plate 26, seed crystal and the slit between seed crystal that described groove 27 and internal tank are laid are positioned on the same vertical plane, as shown in Figures 2 and 3.
Need to prove, distribution situation to groove 27 in the present embodiment is not done concrete restriction, be that the position of described groove 27 on base plate 26 is the shape of the seed crystal laid according to container bottom and fixed, have groove as long as guarantee the base plate corresponding position of the slit correspondence between seed crystal.
Concrete, be example with square seed crystal, corresponding with the shape of seed crystal, groove 27 also is horizontal vertical intersecting vertically, as shown in Figure 3.The width of groove can be corresponding with the width in slit between seed crystal, the degree of depth of groove can with silicon raw material in the thickness of base plate and the container what and decide, preferably, the depth of groove in the present embodiment is 5mm-15mm, width is 10mm-20mm, and described base plate is preferably the graphite base plate.
In addition, need to prove, container shapes in the polycrystal silicon ingot growth furnace in the present embodiment and material are by deciding in the polycrystal silicon ingot growth furnace that adopts in the production process, generally speaking, owing to be to adopt the mode of casting to produce polycrystal silicon ingot in the present embodiment, generally adopt directional solidification method (DirectionalSolidification System is called for short DSS) stove crystal technique at present, adopt this technology can produce big square polysilicon chip, reduced downstream battery cost of processing.Can adopt the growth furnace (DSS growth furnace) of directional solidification method in the present embodiment, also can adopt other polycrystal silicon ingot growing principle and the similar growth furnace of DSS growth furnace, to not doing too much restriction in this present embodiment.
Accordingly, as shown in Figure 4, be example with the DSS stove, this polycrystal silicon ingot growth furnace also comprises: inlet mouth 29, air outlet 30, heat-insulation cage 31, well heater 32(comprise the well heater of top and sidewall), and, described bracing or strutting arrangement also comprises: the side plate 33 of its supporting roles of crucible 22 periphery, and side plate 33 is connected with base plate 26, and 33 of base plate 26 and side plates are detachably; Be positioned at the DS piece of base plate 26 belows, play and support base plate 26, and the effect of heat radiation, the DS piece in the present embodiment is preferably graphite material; Be positioned at the hard charcoal felt 35 of DS piece periphery, to play insulation effect.
And, in order to be convenient in groove, to feed gas in process of production, also can increase an inlet mouth (not shown) at polycrystalline silicon growth furnace bottom or other position.
Container described in the present embodiment is generally square crucible, more general is ceramic crucible, certainly, what described container can also be selected other castingprocesses that can be used for polycrystal silicon ingot can disposable crucible or reusable crucible, as quartz crucible, molybdenum crucible or tungsten crucible etc.
In addition; it will be appreciated by those skilled in the art that; be example with the DSS stove only in the present embodiment; to the structure of polycrystalline silicon growth stove and utilize its method for preparing polycrystal silicon ingot to describe; if select the polycrystalline silicon growth stove of other type for use; just change the position of type of heating, inlet mouth and air outlet etc. accordingly; but; the variation of growth furnace type; do not influence the juche idea of present embodiment; no matter namely adopt the growth furnace of which kind of type, as long as adopted the juche idea of present embodiment, all within the scope of present embodiment protection.
Step S102: the top that solid-state silicon raw material is loaded into described inculating crystal layer;
Do not limit the mode of loading described solid-state silicon raw material in the present embodiment, concrete mode of loading the silicon raw material is decided according to the paving mode of the inculating crystal layer that adopts, as long as guarantee the quality of the monocrystalline silicon region in the polycrystal silicon ingot, as reduce defectives such as crystal boundary, fault as far as possible.
Step S103: described container is heated, melt described silicon raw material and the described inculating crystal layer of part, form liquid level, and in the described inculating crystal layer melting process of part, groove on described base plate feeds rare gas element, and the part inculating crystal layer that keeps at least contacting with described container bottom is solid-state;
Adopt different polycrystal silicon ingot growth furnace, the method that described container is heated also just is not quite similar, as adopt heat-exchanging method growth furnace, adopt the growth furnace of Bridgman method or adopt the growth furnace of the two technology that combines, its heating means are had nothing in common with each other, as long as can be with solid-state silicon raw material and the fusing of part inculating crystal layer, the fusing demand that satisfies this step gets final product.
For the growth furnace that adopts directional solidification method casting polycrystalline silicon ingot, usually adopt the heating installation (being generally well heater) of container top and/or container side wall, container top and/or container side wall are heated, in the heat-processed, for melted silicon raw material as soon as possible, keep the container top temperature to be higher than the fusing point of silicon, and in order to guarantee that the inculating crystal layer bottom keeps solid-state in the heat-processed, the container bottom temperature should be lower than the fusing point of silicon, and then formation is perpendicular to the thermograde of container bottom, make the fusing successively from top to bottom of silicon raw material in the described container and part seed crystal, and the part inculating crystal layer that remains close to container bottom is solid-state.
Be example with the DSS stove, generally speaking, silicon raw material heating phase and silicon raw material fusion stage preceding half section, be in vacuum stages in the growth furnace, in the second half section of silicon raw material fusion stage, namely when the silicon raw material is about to fusing and will finish, this moment the temperature in the growth furnace generally up to 1200 ℃ in addition more than, until silicon ingot process of growth, annealing process and process of cooling whole process, all can in the polycrystal silicon ingot growth furnace, feed rare gas element by inlet mouth 29, simultaneously also can be from the air outlet 30 extract certain gas out, to discharge the impurity in the stove, this process need guarantees the stable gas pressure in growth furnace, the amount that can adjust air inlet automatically and give vent to anger according to the variation of stove internal gas pressure.
And, in described inculating crystal layer melting process, groove 27 places on described base plate 26 feed rare gas element, generally speaking, also be when inculating crystal layer is about to fusing and will finish, feed the rare gas element of normal temperature at groove 27 places, when the inculating crystal layer fusing is finished, can close the inlet mouth that gas is provided for groove 27 places, and also can not feed gas to groove again in the long brilliant stage.Described rare gas element is preferably argon gas, is generally the argon gas of normal temperature, also can select other rare gas element for use certainly, as helium etc., in the present embodiment this is not done too much restriction.
In addition, need to prove, do not limit the contact condition of solid-liquid interface and container bottom in this step, difference according to the growth furnace that adopts, solid-liquid interface can have little angle with container bottom, perhaps solid-liquid interface has a spot of rough zone, it is the solid-liquid interface undulate, the arc of W shape or top bump etc., certainly solid-liquid interface also can be substantially parallel with container bottom, but the quality for the polysilicon that guarantees to produce, be preferably in the present embodiment, container is being carried out in the heat-processed, keep solid-liquid interface substantially parallel with described container bottom or approximate parallel as far as possible.
Concrete, when if solid-liquid interface is positioned at the height zone of inculating crystal layer, and when solid-liquid interface is uneven, the height of the vertex of need assurance solid-liquid interface is smaller or equal to the end face of inculating crystal layer, the height of the lower-most point of solid-liquid interface is greater than the bottom surface of inculating crystal layer, in other words, even the difference of altitude between the vertex of solid-liquid interface and lower-most point is less than the thickness of inculating crystal layer, to guarantee that the part inculating crystal layer near container bottom is solid-state, so that solid-state part inculating crystal layer can play the effect of seeding, guarantee the normal growth of the monocrystalline silicon region in the polycrystal silicon ingot.
Step S104: control the thermal field in the described polycrystal silicon ingot growth furnace, described liquid level is carried out crystallization, so that described solid-liquid interface moves to the direction away from described container bottom, finish until the polycrystal silicon ingot growth, obtain polycrystal silicon ingot.
Similar with previous step, adopt different polycrystal silicon ingot growth furnace, also inequality to the method that molten silicon cools off, can utilize the refrigerating unit heat absorption of growth furnace bottom, also can pass through the mode of the power of reduction growth furnace bottom heater, reduce the temperature of crucible bottom, make equally and form the thermograde vertical with crucible bottom in the burner hearth, to realize the crystallisation process from the bottom up of molten silicon.For the DSS growth furnace or with the similar growth furnace of its principle, specifically can be by opening described container thermal insulator (being generally heat-insulation cage) all around, and by the water-cooling system around the described container described container is cooled off, formation is perpendicular to the thermograde of container bottom, described liquid level is carried out crystallization, and the temperature in the described container rises gradually along the direction that makes progress perpendicular to container bottom.
Different growth furnace, the mode of opening heat-insulation cage are also different, as promote heat-insulation cage, open heat-insulation cage top or bottom, the heat-insulation cage etc. of outwarding winding, no matter after taking which kind of mode to open heat-insulation cage, all need cool off container by the water-cooling system of external container.
Need to prove, the temperature of internal tank described in the crystallisation process of present embodiment rises slowly along the direction that makes progress perpendicular to container bottom, namely make progress along container bottom, the rising gradient of temperature is less, thereby can guarantee in the directional freeze process, growth velocity is stable, make the silicon impurities in raw materials (as silicon carbide, silicon nitride etc.) there is time enough to carry out fractional condensation, have little time to separate out with the silicon impurities in raw materials of avoiding causing because the speed of growth is too fast, thereby be deposited in the polycrystalline silicon ingot casting, form impurity enriched layer and hard point, thereby influence the quality of product.The control of actual temp gradient in which kind of size can be decided according to the particular case of actual production process.
And, because in later stage seed crystal fusion stage, 27 places have fed rare gas element at groove, thereby make in the long brilliant stage, the gas temperature that groove 27 places feed has obtained rising, and because the thermal conductivity of rare gas element is much smaller than the thermal conductivity of graphite, therefore described liquid level is being carried out in the crystallisation process, be positioned at the temperature that the temperature at the place, slit between the seed crystal of groove 27 tops will a little higher than other position, thereby make the slit between seed crystal locate crystal growth rate less than the crystal growth rate of other position, and then the probability and the content that make crystal boundary 25 places derive polysilicon will reduce, thereby further reduced the crystal boundary density in the polycrystal silicon ingot, increase the monocrystalline silicon region 21 in the polycrystal silicon ingot, improved the quality of product.
The technical scheme that the embodiment of the invention provides, adopt the method for casting to produce polycrystal silicon ingot, form inculating crystal layer by laying the big area seed crystal at container bottom, growth by seed crystal guiding monocrystalline silicon region, make and comprise continuous large-sized monocrystalline silicon region in the polycrystal silicon ingot of producing, and the polysilicon region of small part, the crystalline orientation of described monocrystalline silicon region is identical with the crystalline orientation of the described seed crystal that is positioned at its below.
Present embodiment is in the inculating crystal layer melting process, groove on described base plate has fed rare gas element, in the long brilliant stage, the gas temperature that groove feeds has obtained rising, because the thermal conductivity of rare gas element is much smaller than the thermal conductivity of graphite, therefore described liquid level is being carried out in the crystallisation process, be positioned at the temperature that the temperature at the place, slit between the seed crystal of groove top will a little higher than other position, thereby make the slit between seed crystal locate crystal growth rate less than the crystal growth rate of other position, and then probability and the content of the polysilicon of crystal boundary place generation will be reduced, thereby further reduced the crystal boundary density in the polycrystal silicon ingot.Therefore, the solar cell that the polycrystal silicon ingot that adopts the embodiment of the invention to provide is produced, polysilicon solar cell photoelectric transformation efficiency more of the prior art is higher.
And, because thermograde is less in the long brilliant process of present embodiment, long brilliant speed is slow and stable, be about 9cm/h-14cm/h, make impurity (as silicon carbide, silicon nitride etc.) have time enough to carry out fractional condensation, thereby avoided impurity to have little time to separate out and be deposited in the crystalline region that has solidified, and then hard point and impurity enriched layer in the cast main body of polysilicon have been reduced, defect concentration in the polycrystal silicon ingot of producing is reduced greatly, also improve minority carrier life time to a certain extent, improved the photoelectric transformation efficiency of solar cell.
The schema of the castmethod of disclosed polycrystal silicon ingot as shown in Figure 5 in another embodiment of the present invention, different with a last embodiment is, in the present embodiment selection of described seed crystal, the generation type of inculating crystal layer and the process of loading silicon raw material are specialized, this method may further comprise the steps:
Step S201: the container bottom in the polycrystal silicon ingot growth furnace, adopt the bulk seed crystal splicing paving that crystalline orientation is identical and have the geometrical shape of rule, to cover the most of zone of described container bottom, have the slit between described bulk seed crystal;
For adopting DSS mode producer conformal polysilicon ingot, the seed crystal of bulk described in the present embodiment is preferably square seed crystal or rectangle seed crystal, and is preferred, and the minor face of described bulk seed crystal is 100mm-160mm.
Step S202: when described bulk seed crystal can not cover described container bottom fully, adopt the bar shaped seed crystal identical with the crystalline orientation of described bulk seed crystal to fill zone between described bulk seed crystal edge and described container side wall, after described bulk seed crystal and the paving of described bar shaped seed crystal are finished, form described inculating crystal layer;
In other words, this step can be understood as, after the bulk seed crystal arranges, when the bulk seed crystal of a monoblock can not be placed in container bottom and its sidewall junction, can adopt the bar shaped seed crystal of fritter to fill up these regional seed crystal vacancies, not limit length and the width of bar shaped seed crystal in the present embodiment, as long as can be suitable with practical condition, in addition, when the bar shaped seed crystal was put, its edge also can keep certain slit with bulk seed crystal and container side wall.
The silicon single crystal paving that is preferably (100) orientation in the present embodiment forms described inculating crystal layer, be the silicon single crystal that described bulk seed crystal and described bar shaped seed crystal are (100) orientation, preferably, the area of described inculating crystal layer occupies the per-cent of described container bottom area, namely to account for the per-cent of polycrystal silicon ingot cumulative volume be 50%-99% to the volume of the monocrystalline silicon region in the final polycrystal silicon ingot that forms, preferred, the area of described inculating crystal layer occupies the 70%-99% of described container bottom area, preferred, the area of described inculating crystal layer occupies the 90%-99% of described container bottom area, preferred, the area of described inculating crystal layer occupies the 95%-99% of described container bottom area.
And; the width in the slit between the slit between described bulk seed crystal and/or described bulk seed crystal and bar shaped seed crystal is in 0mm-10mm; to guarantee that grain boundary area meets the demands; generally speaking; the area of single crystal grain is about 2cm*2cm; if the temperature of long brilliant process, growth velocity control are better, crystal grain also can be bigger.
Concrete, seed crystal in the present embodiment at the vertical view of the arrangement mode of container bottom as shown in Figure 6 and Figure 7, shape in conjunction with growth furnace and container bottom, bulk seed crystal with square and rectangle (refering in particular to rectangle in the present embodiment) is example respectively, and the paving mode of inculating crystal layer in the present embodiment is described.
Among Fig. 6 for adopting the square seed crystal 11 of bulk and fritter bar shaped seed crystal 12 to finish the synoptic diagram of the inculating crystal layer after the paving, among Fig. 7 for adopting bulk rectangle seed crystal 13 and fritter bar shaped seed crystal 12 to finish the synoptic diagram of the inculating crystal layer after the paving.Present embodiment is that example describes with the seed crystal of (100) crystalline orientation only, do not limit the size of bulk seed crystal and fritter bar shaped seed crystal in addition in the present embodiment, can be with the size of container (crucible) internal diameter close or be slightly smaller than the internal diameter of crucible as the length of the rectangle bulk seed crystal among Fig. 4, its width is preferably controlled at 100mm-160mm and is advisable, gauge control is advisable at 10mm-30mm, the size of bar shaped seed crystal is selected according to practical situation, as the uncomfortable timing of the length of side crucible width of square seed crystal, or with the width of rectangle seed crystal and the uncomfortable timing of crucible width, can adopt one or more bar shaped seed crystal to remedy its vacancy.
Because the restriction of paving mode, inculating crystal layer can not occupy the entire area of container bottom, preferably, each limit of the inculating crystal layer that is formed by bulk seed crystal and the paving of fritter bar shaped seed crystal in the present embodiment and the distance of container edge are approximate, and be more even with the monocrystalline silicon region in the polycrystal silicon ingot that guarantees to cast out.
Step S203: short grained silicon raw material and/or silica flour are loaded into the top of described inculating crystal layer, to fill slit between described seed crystal and the slit between described inculating crystal layer and described container side wall;
In the present embodiment for fear of in castingprocesses, slit between the slit between seed crystal and described inculating crystal layer and described container side wall causes occurring in the cast main body defectives such as cavity easily, thereby influence quality product, adopt short grained silicon raw material and/or silica flour blind, can avoid the cavity blemish in the cast main body on the one hand, can also get rid of the foreign gas in the slit, to reduce swirl defect and various oxygen is induced defective etc., and can utilize small-particle silicon raw material and silica flour to have bigger specific surface area, the advantage of comparatively easy heat absorption fusing, blind, utilization ratio and the quality of raising polycrystal silicon ingot.
In addition, in the present embodiment in order better to fill these slits, as shown in Figure 8, the corner angle of the upper surface that each seed crystal contacts with top silicon raw material have all carried out chamfered, be described bulk seed crystal and/or bar shaped seed crystal with one side that the silicon raw material contacts on have chamfering, preferred, the degree of depth of described chamfering is in 10mm-30mm, the angle a of chamfering is in 70 °, and namely the angle b at two seed crystal edge contact positions is in 140 °.In addition, in order to reduce impurity as far as possible, also need seed crystal and crucible bottom contact part need be cleaned up.
Because the setting of chamfering, slit and the slit between seed crystal and crucible wall between two seed crystals can be littler, even can directly closely contact, and, on the one hand the existence of chamfering is equivalent to be provided with in the seed crystal contact site a little gradient, when filling small-particle silicon raw material or silica flour, can make arranging of small-particle silicon raw material between the slit or silica flour tightr, further reduced between the seed crystal slit and the foreign gas between seed crystal and crucible wall slit etc., further improved the quality of polycrystal silicon ingot; On the other hand when putting seed crystal, if the people is for putting, chamfered area provides placement space for hand, can be used as the zone of putting forth effort of hand simultaneously, be that operator can control seed crystal at chamfer site it is not dropped, and it closely can be contacted with other seed crystal edge or crucible wall when putting, and can not touch the seed crystal of having put, it is as the same that use equipment is put seed crystal.
In addition, for the seed crystal of being more convenient for put and make arranging of small-particle silicon raw material and silica flour tightr, chamfer site can arrange certain radian, the size of radian, shape etc. can not done concrete restriction herein according to the practical situation setting.
Step S204: the silicon raw material of large volume is loaded into the top of described small-particle silicon raw material and/or silica flour, is filled until container (crucible), namely finish the loading process of silicon raw material.
Performing step S205 and step S206 melt-crystallisation process described silicon raw material and part inculating crystal layer afterwards, and step S103 and step S104 among this process and the last embodiment are similar, repeat no more here.
The sectional view of the polycrystal silicon ingot that the method for employing present embodiment is produced as shown in Figure 9, the middle portion of this polycrystal silicon ingot is monocrystalline silicon region 21, monocrystalline silicon region 21 has consistent crystalline orientation with the seed crystal of its below, around monocrystalline silicon region 21, because the impurity in crucible 22 inwalls very easily diffuses to the surface of crucible 22 inwalls, the inner wall surface that causes crucible 22 is nucleation very easily, therefore around monocrystalline silicon region 21, form crystalline orientation polysilicon region 23 at random, also has unfused inculating crystal layer 24 in crucible bottom, owing to have slit or chamfering between the seed crystal of paving, what filled at slit or chamfering place is short grained silicon raw material or silica flour, thereby may there be crystal boundary 25 in 21 of the monocrystalline silicon regions of the polycrystal silicon ingot of producing, but because the chip area of monocrystalline silicon region 21 is big, therefore, polycrystal silicon ingot more of the prior art, density and the foreign matter content of the crystal boundary 25 of the polycrystal silicon ingot of making in the present embodiment greatly reduce.
Another embodiment of the present invention discloses the method polycrystal silicon ingot of producing and the solar wafer and the solar cell that adopt the polycrystal silicon ingot making that casts out that adopts above each embodiment.
Wherein, the continuous large-sized monocrystalline silicon region that comprises the crystalline orientation unanimity in the described polycrystal silicon ingot, after the impurity enriched layer excision with described polycrystal silicon ingot two ends, other body region cutting is obtained solar wafer, utilize described wafer fabrication solar cell, described solar cell comprises:
Wafer, the continuous large-sized monocrystalline silicon region that has the crystalline orientation unanimity on the described wafer;
P-N knot in the described wafer;
Conductive contact on the described wafer.
Also comprise in addition being coated with the antireflective coating that is plated on the described wafer, to reduce wafer to reflection of light, strengthen the absorption to light.
The content of oxygen, carbon and other impurity is all lower in the polycrystal silicon ingot in the present embodiment, and defective such as crystal boundary density reduces greatly.
Because the monocrystalline silicon region that the wafer that obtains has the crystalline orientation unanimity of continuous large-area, therefore can adopt chemical process preferential etch pyramid matte, wafer surface is carried out texture, increase is to the absorption of light, and, lower crystal boundary density in the wafer can effectively have been avoided the low defective of photoelectric transformation efficiency because of the too high solar battery sheet that causes of crystal boundary density in the material.
In sum, with respect to polysilicon solar cell of the prior art, the solar cell in the present embodiment has higher photoelectric transformation efficiency.
Various piece adopts the mode of going forward one by one to describe in this specification sheets, and what each part stressed is and the difference of other parts that identical similar part is mutually referring to getting final product between the various piece.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be apparent concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments herein.Therefore, the present invention will can not be restricted to embodiment illustrated herein, but will meet the wideest scope consistent with principle disclosed herein and features of novelty.
Claims (18)
1. the manufacture method of a polycrystal silicon ingot is characterized in that, comprising:
Container bottom in the polycrystal silicon ingot growth furnace is laid seed crystal, form inculating crystal layer, in described polycrystal silicon ingot growth furnace, be positioned on the base plate of described container below and have the cross one another groove of multiple tracks, the seed crystal of described groove and internal tank and the slit between seed crystal are positioned on the same vertical plane;
Solid-state silicon raw material is loaded into the top of described inculating crystal layer;
Described container is heated, melt described silicon raw material and the described inculating crystal layer of part, with the formation liquid level, and in the described inculating crystal layer melting process of part, groove on described base plate feeds rare gas element, and the part inculating crystal layer that keeps at least contacting with described container bottom is solid-state;
Control the thermal field in the described polycrystal silicon ingot growth furnace, described liquid level is carried out crystallization, so that solid-liquid interface moves to the direction away from described container bottom, finish until the polycrystal silicon ingot growth.
2. the manufacture method of polycrystal silicon ingot according to claim 1, it is characterized in that, described liquid level is carried out in the crystallisation process, the temperature that is positioned at the place, slit between the seed crystal of described groove top is higher than the temperature of other position, and place, the slit crystal growth rate between seed crystal is less than the crystal growth rate of other position.
3. the manufacture method of polycrystal silicon ingot according to claim 2 is characterized in that, described polycrystal silicon ingot contains continuous large-sized monocrystalline silicon region, and the crystalline orientation of described monocrystalline silicon region is identical with the crystalline orientation of the described seed crystal that is positioned at its below.
4. the manufacture method of polycrystal silicon ingot according to claim 3, it is characterized in that, the process of the described silicon raw material of described fusing and the described inculating crystal layer of part comprises: described container top and/or container side wall are heated, keep the container top temperature to be higher than the fusing point of silicon, the container bottom temperature is lower than the fusing point of silicon, formation is perpendicular to the thermograde of container bottom, make silicon raw material and the fusing successively from top to bottom of part seed crystal in the described container, and the part inculating crystal layer that maintenance contacts with described container bottom is solid-state.
5. the manufacture method of polycrystal silicon ingot according to claim 3 is characterized in that, described described container is carried out in the heat-processed, keeps described solid-liquid interface substantially parallel with the bottom of described container.
6. the manufacture method of polycrystal silicon ingot according to claim 3, it is characterized in that, described liquid level is carried out crystallisation process to be comprised: open described container thermal insulator all around, and by the water-cooling system around the described container described container is cooled off, formation is perpendicular to the thermograde of container bottom, described liquid level is carried out crystallization, and the temperature in the described container rises gradually along the direction that makes progress perpendicular to container bottom.
7. the manufacture method of polycrystal silicon ingot according to claim 6 is characterized in that, described liquid level is carried out crystallisation process, and the temperature of described internal tank rises slowly along the direction that makes progress perpendicular to container bottom.
8. the manufacture method of polycrystal silicon ingot according to claim 3 is characterized in that, described seed crystal is that crystalline orientation is the silicon single crystal of (100), (110) or (111) orientation.
9. the manufacture method of polycrystal silicon ingot according to claim 3, it is characterized in that, the process that forms described inculating crystal layer is specially: adopt the bulk seed crystal splicing paving that crystalline orientation is identical and have the geometrical shape of rule, to cover the most of zone of described container bottom, has the slit between described bulk seed crystal.
10. the manufacture method of polycrystal silicon ingot according to claim 9 is characterized in that, described bulk seed crystal is square seed crystal or rectangle seed crystal.
11. the manufacture method of polycrystal silicon ingot according to claim 10 is characterized in that, the minor face of described bulk seed crystal is 100mm-160mm.
12. the manufacture method of polycrystal silicon ingot according to claim 10, it is characterized in that, also comprise: when described bulk seed crystal can not cover described container bottom fully, adopt the bar shaped seed crystal identical with the crystalline orientation of described bulk seed crystal to fill zone between described bulk seed crystal edge and described container side wall.
13. the manufacture method of polycrystal silicon ingot according to claim 12 is characterized in that, the width in the slit between the slit between described bulk seed crystal and/or described bulk seed crystal and bar shaped seed crystal is in 10mm.
14. the manufacture method of polycrystal silicon ingot according to claim 13 is characterized in that, has chamfering on described bulk seed crystal and/or bar shaped seed crystal and the one side that the silicon raw material contacts.
15. the manufacture method of polycrystal silicon ingot according to claim 14 is characterized in that, the degree of depth of described chamfering is in 10mm-30mm.
16. the manufacture method of polycrystal silicon ingot according to claim 15 is characterized in that, the angle of described chamfering is in 70 °.
17. the manufacture method of polycrystal silicon ingot according to claim 1 is characterized in that, the thickness of described inculating crystal layer is 10mm-30mm.
18. the manufacture method of polycrystal silicon ingot according to claim 1 is characterized in that, the process that solid-state silicon raw material is loaded into the top of described inculating crystal layer is specially:
Silica flour is loaded into the top of described inculating crystal layer, to fill slit between described seed crystal and the slit between described inculating crystal layer and described container side wall;
The silicon raw material of large volume is loaded into the top of described silica flour.
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| CN102797037B (en) * | 2011-05-26 | 2015-08-12 | 浙江昱辉阳光能源有限公司 | Polycrystal silicon ingot and manufacture method, solar cell |
| CN102586857B (en) * | 2012-02-28 | 2014-11-26 | 常州天合光能有限公司 | Method for controlling melting residual height of seed crystals of ingot monocrystalline silicon in non-contact manner |
| DE102012203524B4 (en) * | 2012-03-06 | 2016-10-27 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Process for the production of silicon ingots |
| CN102747414A (en) * | 2012-06-20 | 2012-10-24 | 常州天合光能有限公司 | Production method for ingot casting monocrystalline silicon |
| CN103628125A (en) * | 2012-08-21 | 2014-03-12 | 浙江昱辉阳光能源有限公司 | Polysilicon ingot furnace and polysilicon ingot casting method |
| CN103628126A (en) * | 2012-08-21 | 2014-03-12 | 浙江昱辉阳光能源有限公司 | Manufacturing method for monocrystalloid crystalline silica ingot and polysilicon ingot furnace |
| CN102877129B (en) * | 2012-09-11 | 2015-08-05 | 江西赛维Ldk太阳能高科技有限公司 | A kind of crystalline silicon and preparation method thereof |
| CN103014833B (en) * | 2012-12-26 | 2015-11-18 | 阿特斯(中国)投资有限公司 | The preparation method of silicon ingot |
| TWI541396B (en) * | 2013-12-20 | 2016-07-11 | 中美矽晶製品股份有限公司 | Cooling device for ingot casting furnace and method of casting ingot |
| CN103834994A (en) * | 2014-03-13 | 2014-06-04 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot and preparation method thereof and polycrystalline silicon wafer |
| CN105603521A (en) * | 2016-02-03 | 2016-05-25 | 江西赛维Ldk太阳能高科技有限公司 | Seed crystal laying method, preparation method of monocrystalline silicon-like ingot and monocrystalline silicon-like piece |
| CN107475770A (en) * | 2017-08-30 | 2017-12-15 | 晶科能源有限公司 | One species single crystal seed and class method for monocrystal growth |
| CN107747121A (en) * | 2017-11-07 | 2018-03-02 | 晶科能源有限公司 | The laying method of one species single crystal seed |
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| JP2002193610A (en) * | 2000-12-26 | 2002-07-10 | Mitsubishi Materials Corp | Apparatus for producing crystal silicon |
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| JP2002193610A (en) * | 2000-12-26 | 2002-07-10 | Mitsubishi Materials Corp | Apparatus for producing crystal silicon |
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