CN101892518A - System and method for manufacturing polycrystalline ingots - Google Patents
System and method for manufacturing polycrystalline ingots Download PDFInfo
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- CN101892518A CN101892518A CN 201010228251 CN201010228251A CN101892518A CN 101892518 A CN101892518 A CN 101892518A CN 201010228251 CN201010228251 CN 201010228251 CN 201010228251 A CN201010228251 A CN 201010228251A CN 101892518 A CN101892518 A CN 101892518A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 26
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
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- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 claims description 5
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Abstract
The invention discloses a system for manufacturing polycrystalline ingots, which comprises an upper furnace body, a lower furnace body, a crucible, at least one heater, a crucible holder, a crucible support, a heat insulating part and a heat exchange unit, wherein the crucible is arranged in a furnace space and is arranged to accommodate feed; the at least one heater is used heating the crucible and melting the feed accommodated in the crucible; the crucible holder is used for holding the crucible; the crucible holder accommodating the crucible is arranged on the crucible support; the heat insulating part is accommodated in the furnace space and is arranged in a manner of longitudinally moving relative to the crucible; and the heat exchange unit is used for controlling the dissipation of the heat from the bottom of the crucible, and a flow path for heat dissipation is formed below the crucible support in a polycrystalline ingot solidification and/or cooling process. The invention also discloses a method for manufacturing the polycrystalline ingots by directional solidification. When the system and the method are used, the quality of the polycrystalline ingots can be guaranteed and the production efficiency of the polycrystalline ingots can be improved.
Description
Technical field
The present invention relates to the manufacturing process of polycrystalline ingot, especially relate to a kind of method that is used to make the system of polycrystalline ingot and makes polycrystalline ingot by directional freeze.
Background technology
In the manufacturing process of existing solar energy battery adopted silicon chip, need usually earlier monocrystalline or polycrystalline ingot to be carried out butt.After this, to the monocrystalline after the butt or polycrystalline ingot polishes or acid corrosion,, after this clean to obtain described solar energy battery adopted silicon chip with the clean surface line section of going forward side by side.Thus, just need provide a kind of manufacturing installation and equipment of making polycrystalline ingot.Existing polycrystalline ingot technical process is as follows: at first feed; Vacuumize heating then, change material, after material all melts, it is carried out directional freeze, need during this time to vacuumize and logical argon gas, after directional freeze, need be incubated preset time the polycrystalline ingot that forms, cool off then, and come out of the stove to obtain described polycrystalline ingot.
But in existing polycrystal silicon ingot producing apparatus, because the restriction of self structure has caused having to prolong its corresponding time in directional freeze and refrigerating work procedure.Describe in detail with reference to Fig. 1 below, Fig. 1 has shown the synoptic diagram according to existing polycrystal silicon ingot producing apparatus 100 ', this polycrystal silicon ingot producing apparatus 100 ' has wherein shown the gas circuit distribution schematic diagram in the directional freeze process by upper furnace body 101 ' and lower furnace body 102 ' airtight forming.Wherein shown and in crucible 1 ', carried out directional freeze.In the process of directional freeze, need be from the rare gas element of downward general rule in the center of heat shielding 31 such as Ar gas, rare gas element is because the structural limitations of heat-insulation cage 4 ', flow and be discharged from along gas circuit B1 ', B2 ', B3 ', C1 ', C2 ', also have the part rare gas element also finally to be discharged from addition by stream B4 ' formation loop by aspirating hole 103 '.Heat-insulation cage 4 ' moves on slowly in the process of directional freeze, and the translational speed of heat-insulation cage 4 ' must be controlled very slow, otherwise the solid-liquid interface 11 ' that can cause appearing in the crucible significantly becomes recessed downwards, as shown in Figure 2.This is that rare gas element stream B1 ' and C1 ' at first can cool off the molten silicon of the side part of crucible 1 ' because in the process of moving on whole, and this heat-sinking capability of molten silicon of centre portions that causes crucible 1 ' is less than the molten silicon of peripheral part, thereby causes this phenomenon.In addition, in the lifting process of heat-insulation cage 4 ', the gas circuit B4 ' that rare gas element forms dies down until disappearance gradually to the cooling power of the bottom of crucible 1 ', thereby be difficult to improve solid-liquid interface and become recessed phenomenon, these all can cause the polycrystalline ingot quality to become bad, that is can not form bigger crystal grain, and cause more lattice defect, especially in zone near quartz crucible.
In the refrigerative process, exist polycrystalline ingot upper surface heat radiation to concentrate, insufficient problem is dispelled the heat in the bottom.The polycrystalline ingot internal stress that these problems can cause being produced increases, and crystal ingot inside is prone to crackle.In existing scheme, can only guarantee the quality of polycrystalline ingot by prolongation directional freeze and refrigerative time.
This shows, because the restriction in the existing installation, can not reach the purpose of the directional freeze of accelerating molten silicon by the pulling speed that improves heat-insulation cage, promptly around crucible, form and have good thermograde, avoid causing solid-liquid interface as shown in Figure 2 to be bent downwardly simultaneously, thereby cause polycrystalline ingot generation quality to become bad situation.
The contriver finds by measuring, and is example with the 450Kg charge amount, and directional freeze approximately needed about 30 hours, and cooling needs 5-10 hour.This shows the manufacturing processed overlong time of whole polycrystalline ingot, production efficiency is lower.
Summary of the invention
In view of this, a kind of system of new manufacturing polycrystalline ingot need be provided, described system can improve the production efficiency of whole polycrystalline ingot by when forming controlled thermograde around the crucible and guaranteeing the quality of polycrystalline ingot or even improve the polycrystalline ingot quality.
Further, a kind of method of new manufacturing polycrystalline ingot need be provided, described method can improve the production efficiency of whole polycrystalline ingot by when forming controlled thermograde around the crucible and guaranteeing the quality of polycrystalline ingot or even improve the polycrystalline ingot quality, reduces manufacturing cost.
According to an aspect of the present invention, provide a kind of system that makes polycrystalline ingot, described system comprises: upper furnace body; Lower furnace body, described lower furnace body match with described upper furnace body to form furnace space; Crucible, described crucible are arranged in the furnace space and are configured to hold feed; At least one well heater, described well heater are used for heating crucible and melt the feed that is contained in crucible; The crucible retainer, described crucible retainer is used to keep described crucible; The crucible bearing, the described crucible retainer that accommodates described crucible is arranged on the described crucible bearing; Heat insulating member, described heat insulating member is contained in the described furnace space, and be configured to vertically removable with respect to described crucible, to control the directional freeze of the polycrystal silicon ingot in the described crucible; And heat exchange unit, described heat exchange unit is arranged under the described crucible bearing, the heat that is used to control from crucible bottom dissipates, and polycrystalline ingot solidify and/or the refrigerative process in the stream that under the crucible bearing, is formed for dispelling the heat.
According to one embodiment of present invention, described heat exchange unit comprises: gas duct, an end of described gas duct is arranged near the bottom center of described crucible bearing, another termination source of the gas of described gas duct.
According to one embodiment of present invention, described heat exchange unit also comprises: the air-flow guiding piece, and the bottom surface of described air-flow guiding piece and described crucible bearing is oppositely arranged, and described gas duct penetrates described air-flow guiding piece.
According to one embodiment of present invention, described air-flow guiding piece comprises: the air-flow guiding material layer that is oppositely arranged with the bottom surface of described crucible bearing, the described first air-flow guiding material layer center is formed with first perforate, and the described first air-flow guiding material layer is combined to form by graphite, carbon-carbon composite, carbon fibre material, tungsten, molybdenum, insulation charcoal felt material or above-mentioned materials.
According to one embodiment of present invention, described air-flow guiding piece further comprises: the second air-flow guiding material layer, the described second air-flow guiding material layer is arranged under the described first air-flow guiding material layer also coupled, the center of the described second air-flow guiding material layer is formed with second perforate corresponding with described first perforate, and the described second air-flow guiding material layer is formed by insulation charcoal felt.
According to one embodiment of present invention, the bottom of described crucible bearing is formed with radiating groove, and the top and the quartz crucible of described radiating groove are adjacent, and described gas duct is inserted in the described radiating groove.
According to one embodiment of present invention, described radiating groove forms any one in cone table, sphere, rectangular parallelepiped, right cylinder, the cone.
According to one embodiment of present invention, be formed with adiabator layer on the lower surface of described crucible bearing.
According to one embodiment of present invention, described heat insulating member forms heat-insulation cage, and described heat-insulation cage covers described well heater, and the lower peripheral edge of described heat-insulation cage is provided with the flange that stretches out towards the inboard, so that the air-flow of heat exchange unit is difficult for flowing in the heat-insulation cage.
According to one embodiment of present invention, the position relative with described gas duct is provided with first air inlet port on the described lower furnace body.
According to one embodiment of present invention, with N
2, Ar, He or its mixed gas be supplied to described gas duct by first air inlet port.
According to one embodiment of present invention, the top of described upper furnace body is provided with second inlet mouth, and described second inlet mouth is connected with second gas circuit with first gas circuit respectively, and described first gas circuit is used for feeding N to quartz crucible
2, Ar or its mixed gas; Described gas duct is connected with described second gas circuit, is used for feeding N to described gas duct
2, Ar, He or its mixed gas.
According to the system that should make polycrystalline ingot of the present invention, by improving the temperature gradient distribution around the crucible, thereby when guaranteeing the polycrystalline ingot quality, reduced the time of directional freeze and refrigerating work procedure, improved production efficiency.Simultaneously, the shape of solid-liquid interface when this system can change directional freeze changes into from the spill interface as far as possible near horizontal interface or dimpling interface upwards, thereby can be used to control the grain-size of polycrystalline ingot casting, improves crystal mass.
According to a further aspect of the invention, provide a kind of method by directional freeze manufacturing polycrystalline ingot, comprised the steps: the polycrystalline feed is put into the intravital crucible of stove, described crucible is by the crucible seat supports; Heating and melt described polycrystalline feed; The polycrystalline feed that melts in the described crucible is carried out directional freeze; Movably heat insulating member is set in body of heater vertically, and described heat insulating member is configured to move with respect to crucible is directed, to promote the directional freeze of polycrystalline ingot; And the heat exchange unit of operation setting under crucible, described heat exchange unit forms the heat radiation gas flow path in the bottom surface of crucible bearing, move and the cooperation of the gas flow path that dispels the heat maintenance level or the dimpling upwards so that solid-liquid interface in the crucible is tried one's best by heat insulating member.
According to one embodiment of present invention, described heat exchange unit comprises: gas duct, an end of described gas duct is arranged near the bottom center of described crucible bearing, another termination source of the gas of described gas duct.
According to one embodiment of present invention, described heat exchange unit also comprises: the air-flow guiding piece, and the bottom surface of described air-flow guiding piece and described crucible bearing is oppositely arranged, and described gas duct penetrates described air-flow guiding piece.
According to one embodiment of present invention, described air-flow guiding piece comprises: the first air-flow guiding material layer that is oppositely arranged with the bottom surface of described crucible bearing, the described first air-flow guiding material layer center is formed with first perforate, and the described first air-flow guiding material layer is combined to form by graphite, carbon-carbon composite, carbon fibre material, tungsten, molybdenum, insulation charcoal felt material or above-mentioned materials.
According to one embodiment of present invention, described air-flow guiding piece further comprises: the second air-flow guiding material layer, the described second air-flow guiding material layer is arranged under the described first air-flow guiding material layer also coupled, the center of the described second air-flow guiding material layer is formed with second perforate corresponding with described first perforate, and the described second air-flow guiding material layer is formed by insulation charcoal felt.
According to one embodiment of present invention, the bottom of described crucible bearing is formed with radiating groove, and the top and the quartz crucible of described radiating groove are adjacent, and described gas duct is inserted in the described radiating groove.
According to one embodiment of present invention, described radiating groove forms any one in cone table, sphere, rectangular parallelepiped, right cylinder, the cone.
Make the method for polycrystalline ingot according to of the present invention by directional freeze, by improving the temperature gradient distribution around the crucible, thereby when guaranteeing the polycrystalline ingot quality, reduced the time of directional freeze and refrigerating work procedure, improved production efficiency.
Simultaneously, the shape of solid-liquid interface when this system can change directional freeze changes into from the spill interface as far as possible near horizontal interface or dimpling interface, thereby can be used to control the grain-size of polycrystalline ingot casting, improves crystal mass.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage are from obviously and easily understanding becoming the description of embodiment below in conjunction with accompanying drawing, wherein:
Fig. 1 has shown according to the synoptic diagram of existing polycrystal silicon ingot producing apparatus in the directional freeze process;
Fig. 2 has shown according to the solid-liquid interface synoptic diagram in the crucible in the existing polycrystal silicon ingot producing apparatus;
Fig. 3 has shown the structural representation of polycrystal silicon ingot manufacturing system according to an embodiment of the invention;
Fig. 4 has shown the interior solid-liquid interface synoptic diagram of crucible of polycrystal silicon ingot manufacturing system according to an embodiment of the invention;
Fig. 5 has shown the structural representation of polycrystal silicon ingot manufacturing system according to another embodiment of the invention;
Fig. 6 has shown the structural representation of bottom according to an embodiment of the invention heat shielding;
Fig. 7 has shown the structural representation of crucible bearing according to an embodiment of the invention;
Fig. 8 has shown the internal structure synoptic diagram of polycrystal silicon ingot manufacturing system according to an embodiment of the invention;
Fig. 9 A, 9B have shown the structural representation of gas duct according to an embodiment of the invention;
Figure 10 has shown the gas circuit distribution schematic diagram of polycrystal silicon ingot manufacturing system according to an embodiment of the invention; And
Figure 11 has shown the schema of making the method for polycrystalline ingot by directional freeze according to an embodiment of the invention.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, and wherein identical from start to finish or similar label is represented identical or similar elements or the element with identical or similar functions.Below by the embodiment that is described with reference to the drawings is exemplary, only is used to explain the present invention, and can not be interpreted as limitation of the present invention.
Fig. 3 has shown the structural representation of polycrystal silicon ingot manufacturing system 100 according to an embodiment of the invention.The system 100 of this manufacturing polycrystalline ingot comprises: upper furnace body 101; Lower furnace body 102, described lower furnace body 102 match with described upper furnace body 101 to form furnace space 104; Crucible 1, described crucible 1 are arranged in the lower furnace body 102 and are configured to hold the feed (not shown); At least one well heater, described well heater are used for heating crucible 1 and melt the feed that is contained in crucible 1; Crucible retainer 5, described crucible retainer 5 is used to keep described crucible 1; Crucible bearing 6, the described crucible retainer 5 that holds described crucible 1 is arranged on the described crucible bearing 6; Heat insulating member, described heat insulating member is contained in the described furnace space, and be configured to vertically removable with respect to described crucible 1, to control the directional freeze of the polycrystal silicon ingot in the described crucible 1; And heat exchange unit, described heat exchange unit is arranged under the described crucible bearing 6, and the heat that is used to control from crucible 1 dissipates, and the stream that is formed for dispelling the heat in the process that polycrystalline ingot solidifies under crucible bearing 6.
In according to one embodiment of present invention, described crucible 1 can need to have required shape, and is not limited to square, cylindrical, taper etc.In the present invention,, adopt the quadrate crucible, but need to prove for the purpose of example, herein only for purposes of illustration, rather than in order to limit protection scope of the present invention.Described crucible 1 is kept by crucible retainer 5, as shown in Figure 4.Described crucible retainer 5 can comprise retaining plate 51,52 and 53.Described retaining plate 51,52 and 53 can be formed by graphite cake.In according to one embodiment of present invention, described at least one well heater comprises: top heater 31, side well heater 32.Described top heater 31, side well heater 32 cover described crucible 1 when work, be placed on wherein feed with fusing.After upper furnace body 101 and lower furnace body 102 closures, described top heater 31 and sidewall well heater 32 cover above the reaching all around of described crucible 1.
According to one embodiment of present invention, described lower furnace body 102 is vertically removable with respect to described upper furnace body 101, thereby can utilize fork truck etc. to put into and take out crucible 1 easily.
According to one embodiment of present invention, this system 100 can also comprise the heat shielding 2 that is arranged between crucible 1 and the top heater 31, the center of this heat shielding 2 has gas entrance hole 21, can be provided with a plurality of fixed part (not shown) that interfix with retaining plate 51,52 and 53 around the heat shielding 2.Heat shielding 2 can stop the volatile matter of silicon melt directly to deposit on the top heater 31 and other lagging materials of quartz crucible 1 top, gas entrance hole 21 by heat shielding 2 centers can also import to the rare gas element of for example argon gas (Ar) etc. the silicon melt surface in the crucible 1, and a plurality of air outlet openings outflows that are provided with around the top by quartz crucible 1, thereby can take away various volatile matters by described rare gas element.
According to one embodiment of present invention, heat insulating member forms heat-insulation cage 4, when upper furnace body 101 and lower furnace body 102 are closed, make top heater 31 and sidewall well heater 32 be loaded into crucible 1 around, and heat-insulation cage 4 entangles quartz crucible 1 to prevent the heat outflow in the process of changing material.In the process of the directional freeze after the feed of crucible 1 fusing is incubated, can upwards promote described heat-insulation cage 4 lentamente, keeping the temperature of not solidified liquid-state silicon material, and control the directional freeze of the interior polycrystal silicon ingot of described crucible 1.
According to one embodiment of present invention, below described crucible bearing 6, be provided with heat exchange unit.The gas circuit D1 that described heat exchange unit is formed for dispelling the heat in the polycrystalline ingot process of setting under crucible bearing 6, D2, described gas circuit D1, D2 flow along the lower surface of crucible bearing 6, thereby can provide the fusion feed to being positioned at the crucible centre to carry out the refrigerative gas flow path.By controlling moving and described gas flow path of described heat-insulation cage 4, make solid-liquid interface in the described crucible maintenance level or dimpling as far as possible in the process of condensation.
Fig. 4 has shown the solid-liquid interface synoptic diagram in the crucible 1 of polycrystal silicon ingot manufacturing system 100 according to an embodiment of the invention.As shown in Figure 4, by this heat exchange unit being set in bottom surface at crucible bearing 6, make the crucible 1 interior solid-liquid interface 11 among the present invention significantly flatten or dimpling, thereby improved, increased the size of the crystal grain of peripheral part polycrystalline ingot in the quality of polycrystalline ingot in the directional freeze process.
According to one embodiment of present invention, described heat exchange unit comprise gas duct 8 and with described gas duct 8 vertically disposed air-flow guiding pieces 7, described air-flow guiding piece 7 is oppositely arranged with the bottom surface of described crucible 1 support; Described gas duct 8 passes the adjacent setting in bottom surface of described air-flow guiding piece 7 and an end and described crucible 1 support, another termination source of the gas of gas duct 8.By current path D1, the D2 that between the lower surface of described air-flow guiding piece 7 and described crucible bearing 6, forms, thereby improve the temperature gradient distribution under the crucible effectively, thereby improved the quality of polycrystalline ingot in the directional freeze process.
In order better to play cooling performance, as shown in Figure 5, in one embodiment of the invention, bottom at crucible 1 support is formed with radiating groove 61, the top of radiating groove 61 can be adjacent with quartz crucible 1, gas duct 8 can be inserted in the radiating groove 61, thereby can be with the more direct central position that is blown into crucible bottom of air-flow, thereby can play the liquid-state silicon of cooling crucible center position or the purpose of solid silicon ingot.
Fig. 6 has shown the structural representation of air-flow guiding piece 7 according to an embodiment of the invention.Described air-flow guiding piece 7 comprises: the first air-flow guiding material layer 710 that is oppositely arranged with the bottom surface of described crucible 1 support, the described first air-flow guiding material layer 710 center are formed with first perforate 720, and are combined to form by graphite, carbon-carbon composite, carbon fibre material, tungsten, molybdenum, insulation charcoal felt material or above-mentioned materials.According to one embodiment of present invention, described air-flow guiding piece 7 further comprises: the second air-flow guiding material layer 730, the described second air-flow guiding material layer 730 is arranged under the described first air-flow guiding material layer 710 and is coupled, and the center of the described second air-flow guiding material layer 730 is formed with and the second corresponding perforate 740 of described first perforate 720.According to one embodiment of present invention, the described second air-flow guiding material layer 730 can be formed by insulation charcoal felt.
Wherein, radiating groove 61 in the foregoing description can form any one in cone table, sphere, rectangular parallelepiped, right cylinder, the cone etc., as shown in Figure 7, structural representation for the crucible bearing of the embodiment of the invention, radiating groove 61 can be cone table in this embodiment, but those skilled in the art obviously can also adopt the radiating groove of other shapes.
According to one embodiment of present invention, as shown in Figure 8, on the lower surface of crucible bearing 6, can be formed with adiabator layer 10, thus can be so that this layer adiabator layer 10 can cooperatively interact with gas duct 8, and the interface control of polycrystalline ingot becomes more easy when making to directional freeze.This adiabator layer can be so that when cooling off by described gas duct 8 feeding gases, described temperature gradient distribution be more even.
Simultaneously, in another embodiment of the present invention, as shown in Figure 8, lower peripheral edge at heat-insulation cage 4 is provided with the flange 9 that stretches out towards the inboard, like this after heat-insulation cage 4 covers well heater 31 and 32, flange 9 can stop that the air-flow that enters by gas duct 8 enters in the heat-insulation cage 4, thereby may cause the supercooling to the side of crucible.
Shown in Fig. 9 A, be gas duct 8 structure iron of one embodiment of the invention, in this embodiment, described gas duct 8 comprises first pipe 81, this described first pipe 81 is formed by graphite, C-C composite, molybdenum or stainless steel.Shown in Fig. 9 B, be gas duct 8 structure iron of another embodiment of the present invention, described gas duct 8 also comprises second pipe 82, described second pipe, 82 nested described first pipes 81, described second pipe 82 can be formed by insulation charcoal felt material.
Provide also for source of the gas of the present invention and can adopt multiple mode, for example in one embodiment of the invention, an air inlet port can be set respectively on lower furnace body on the body of heater, as shown in figure 10, second air inlet port is set on upper furnace body 101, this second air inlet port enters in the heat-insulation cage 4 by first gas circuit 11, and passes heat shielding 2 with the surface of Ar air-blowing to melt, and simultaneously the position relative with described gas duct 8 is provided with first air inlet port 1021 on the lower furnace body 102.What be different from an embodiment is, in another embodiment of the present invention, an air inlet port can only be provided on body of heater, also as shown in figure 10, the top of described upper furnace body 101 is provided with second inlet mouth 1011, described second inlet mouth 1011 is connected with second gas circuit 12 with first gas circuit 11 respectively, described first gas circuit 11 is used for to crucible 1 by rare gas elementes such as Ar gas, described gas duct 8 is connected with described the 3rd gas circuit 13, wherein said second gas circuit 12 is connected with the 3rd gas circuit 13 by gas interface 14, is used for feeding rare gas element to described gas duct 8.Need to prove, the present invention's purpose for simplicity, in Figure 10, show this two kinds of plenum systems simultaneously, but it will be appreciated by those skilled in the art that this dual mode realizes respectively, and those skilled in the art also can make modification or the variation that is equal to these two embodiment, for example only in the bottom of body of heater an air inlet port etc. are set.In the above-described embodiments, not only Ar can be fed, also N can be fed
2, gas such as He, the perhaps mixed gas of these gases.
According to one embodiment of present invention, according to the system 100 that should make polycrystalline ingot of the present invention, by improving the temperature gradient distribution around the crucible 1, thereby when guaranteeing the polycrystalline ingot quality, reduce the time of directional freeze and refrigerating work procedure, improved production efficiency.Simultaneously, the shape of solid-liquid interface when this system 100 can change directional freeze changes into from the spill interface as far as possible near level or dimpling interface, thereby can be used to control the grain-size of polycrystalline ingot casting, improves crystal mass.
According to a further aspect of the invention, provide a kind of method that adopts directional freeze to make polycrystalline ingot, may further comprise the steps:
Step S101 puts into the intravital crucible of stove with the polycrystalline feed, and wherein, crucible is by the crucible seat supports.
Step S102, the polycrystalline feed that heating and fusing are put into.
Step S103 carries out directional freeze to the polycrystalline feed that melts in the crucible, and movably heat insulating member is set in body of heater vertically simultaneously, and heat insulating member is configured to move with respect to crucible is directed, to promote the directional freeze of polycrystalline ingot.
Step S104, the heat exchange unit of operation setting under crucible, described heat exchange unit forms the heat radiation gas flow path in the bottom surface of crucible bearing, move and the cooperation of the gas flow path that dispels the heat by heat insulating member, so that the solid-liquid interface in the crucible keeps level or dimpling shape.
Make the method for polycrystalline ingot according to of the present invention by directional freeze, by improving the temperature gradient distribution around the crucible 1, thereby when guaranteeing the polycrystalline ingot quality, reduced the time of directional freeze and refrigerating work procedure, improved production efficiency.
Simultaneously, the shape of solid-liquid interface when this system 100 can change directional freeze changes into from the spill interface as far as possible near horizontal interface or dimpling interface, thereby can be used to control the grain-size of polycrystalline ingot casting, improves crystal mass.
Any mentioning " embodiment ", " embodiment ", " illustrative examples " etc. mean concrete member, structure or the characteristics described in conjunction with this embodiment and are contained among at least one embodiment of the present invention.Not necessarily refer to identical embodiment in this schematic statement everywhere of this specification sheets.And when describing concrete member, structure or characteristics in conjunction with any embodiment, what advocated is, realizes that in conjunction with other embodiment such member, structure or characteristics all drop within those skilled in the art's the scope.
Although the specific embodiment of the present invention is described in detail with reference to a plurality of illustrative examples of the present invention, but it must be understood that, those skilled in the art can design multiple other improvement and embodiment, and these improve and embodiment will drop within the spirit and scope.Particularly, within the scope of aforementioned open, accompanying drawing and claim, can make rational modification and improvement aspect the layout of component and/or subordinate composite configuration, and can not break away from spirit of the present invention.Except the modification and the improvement of component and/or layout aspect, its scope is limited by claims and equivalent thereof.
Claims (19)
1. system that makes polycrystalline ingot, described system comprises:
Upper furnace body;
Lower furnace body, described lower furnace body match with described upper furnace body to form furnace space;
Crucible, described crucible are arranged in the furnace space and are configured to hold feed;
At least one well heater, described well heater are used for heating crucible and melt the feed that is contained in crucible;
The crucible retainer, described crucible retainer is used to keep described crucible;
The crucible bearing, the described crucible retainer that accommodates described crucible is arranged on the described crucible bearing;
Heat insulating member, described heat insulating member is contained in the described furnace space, and be configured to vertically removable with respect to described crucible, to control the directional freeze of the polycrystal silicon ingot in the described crucible; And
Heat exchange unit, described heat exchange unit are arranged under the described crucible bearing, and the heat that is used to control from crucible bottom dissipates, and polycrystalline ingot solidify and/or the refrigerative process in the stream that under the crucible bearing, is formed for dispelling the heat.
2. system according to claim 1 is characterized in that, described heat exchange unit comprises:
Gas duct, an end of described gas duct is arranged near the bottom center of described crucible bearing, another termination source of the gas of described gas duct.
3. system according to claim 2 is characterized in that, described heat exchange unit also comprises:
The air-flow guiding piece, the bottom surface of described air-flow guiding piece and described crucible bearing is oppositely arranged, and described gas duct penetrates described air-flow guiding piece.
4. system according to claim 3 is characterized in that, described air-flow guiding piece comprises:
The air-flow guiding material layer that is oppositely arranged with the bottom surface of described crucible bearing, the described first air-flow guiding material layer center is formed with first perforate, and the described first air-flow guiding material layer is combined to form by graphite, carbon-carbon composite, carbon fibre material, tungsten, molybdenum, insulation charcoal felt material or above-mentioned materials.
5. system according to claim 4 is characterized in that, described air-flow guiding piece further comprises:
The second air-flow guiding material layer, the described second air-flow guiding material layer is arranged under the described first air-flow guiding material layer also coupled, the center of the described second air-flow guiding material layer is formed with second perforate corresponding with described first perforate, and the described second air-flow guiding material layer is formed by insulation charcoal felt.
6. system according to claim 2 is characterized in that the bottom of described crucible bearing is formed with radiating groove, and the top and the quartz crucible of described radiating groove are adjacent, and described gas duct is inserted in the described radiating groove.
7. system according to claim 6 is characterized in that described radiating groove forms any one in cone table, spheroid, rectangular parallelepiped, right cylinder, the cone.
8. system according to claim 6 is characterized in that, is formed with adiabator layer on the lower surface of described crucible bearing.
9. system according to claim 2, it is characterized in that described heat insulating member forms heat-insulation cage, and described heat-insulation cage covers described well heater, the lower peripheral edge of described heat-insulation cage is provided with the flange that stretches out towards the inboard, so that the air-flow of heat exchange unit is difficult for flowing in the heat-insulation cage.
10. system according to claim 2 is characterized in that, position relative with described gas duct on the described lower furnace body is provided with first air inlet port.
11. system according to claim 10 is characterized in that, with N
2, Ar, He or its mixed gas be supplied to described gas duct by first air inlet port.
12. system according to claim 3 is characterized in that, the top of described upper furnace body is provided with second inlet mouth, and described second inlet mouth is connected with second gas circuit with first gas circuit respectively, and described first gas circuit is used for feeding Ar, N to quartz crucible
2Perhaps its mixed gas;
Described gas duct is connected with described second gas circuit, is used for feeding N to described gas duct
2, Ar, He or its mixed gas.
13. the method by directional freeze manufacturing polycrystalline ingot comprises the steps:
The polycrystalline feed is put into the intravital crucible of stove, and described crucible is by the crucible seat supports;
Heating and melt described polycrystalline feed;
The polycrystalline feed that melts in the described crucible is carried out directional freeze;
Movably heat insulating member is set in body of heater vertically, and described heat insulating member is configured to move with respect to crucible is directed, to promote the directional freeze of polycrystalline ingot; And
The heat exchange unit of operation setting under crucible, described heat exchange unit form the heat radiation gas flow path in the bottom surface of crucible bearing, move and the cooperation of the gas flow path that dispels the heat by heat insulating member, so that the solid-liquid interface in the crucible keeps the level or the shape of dimpling upwards.
14. method according to claim 13 is characterized in that, described heat exchange unit comprises:
Gas duct, an end of described gas duct is arranged near the bottom center of described crucible bearing, another termination source of the gas of described gas duct.
15. method according to claim 14 is characterized in that, described heat exchange unit also comprises:
The air-flow guiding piece, the bottom surface of described air-flow guiding piece and described crucible bearing is oppositely arranged, and described gas duct penetrates described air-flow guiding piece.
16. method according to claim 13 is characterized in that, described air-flow guiding piece comprises:
The first air-flow guiding material layer that is oppositely arranged with the bottom surface of described crucible bearing, the described first air-flow guiding material layer center is formed with first perforate, and the described first air-flow guiding material layer is combined to form by graphite, carbon-carbon composite, carbon fibre material, tungsten, molybdenum, insulation charcoal felt material or above-mentioned materials.
17. method according to claim 16 is characterized in that, described air-flow guiding piece further comprises:
The second air-flow guiding material layer, the described second air-flow guiding material layer is arranged under the described first air-flow guiding material layer also coupled, the center of the described second air-flow guiding material layer is formed with second perforate corresponding with described first perforate, and the described second air-flow guiding material layer is formed by insulation charcoal felt.
18. method according to claim 14 is characterized in that, the bottom of described crucible bearing is formed with radiating groove, and the top and the quartz crucible of described radiating groove are adjacent, and described gas duct is inserted in the described radiating groove.
19. method according to claim 18 is characterized in that, described radiating groove forms any one in cone table, sphere, rectangular parallelepiped, right cylinder, the cone.
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| CN102703968A (en) * | 2012-06-05 | 2012-10-03 | 湖南红太阳光电科技有限公司 | Method and device for controlling seed crystal melting degree through gas flow in single crystal casting process |
| CN103160934A (en) * | 2011-12-18 | 2013-06-19 | 洛阳金诺机械工程有限公司 | Device and method of temperature gradient control in growth process of crystal material |
| CN103290473A (en) * | 2012-02-28 | 2013-09-11 | 三菱综合材料株式会社 | Quartz crucible, production method of the same, and casting apparatus |
| CN103334154A (en) * | 2013-05-29 | 2013-10-02 | 浙江晟辉科技有限公司 | Preparation method of polycrystalline silicon ingots based on thermal exchange technology |
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| CN104131345A (en) * | 2014-07-17 | 2014-11-05 | 大连理工大学 | Polysilicon semi-fusion casting device adopting bottom air cooling and technology using the same |
| CN105586636A (en) * | 2016-02-18 | 2016-05-18 | 安徽旭能光伏电力有限公司 | Manufacturing technology for directional-solidification growth of polycrystalline silicon ingots used for solar cells |
| CN110923803A (en) * | 2019-12-25 | 2020-03-27 | 南京晶升能源设备有限公司 | Semiconductor silicon material consumable material growth furnace and silicon material preparation method |
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| CN114645325A (en) * | 2022-04-04 | 2022-06-21 | 扬州晶樱光电科技有限公司 | Efficient polycrystalline ingot furnace for producing polycrystalline silicon ingots and production method thereof |
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