CN104372404B - Preparation method of polycrystalline silicon ingot, polycrystalline silicon ingot furnace and silicon wafer - Google Patents
Preparation method of polycrystalline silicon ingot, polycrystalline silicon ingot furnace and silicon wafer Download PDFInfo
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- CN104372404B CN104372404B CN201410659691.6A CN201410659691A CN104372404B CN 104372404 B CN104372404 B CN 104372404B CN 201410659691 A CN201410659691 A CN 201410659691A CN 104372404 B CN104372404 B CN 104372404B
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Abstract
The invention relates to a preparation method of a polycrystalline silicon ingot. The preparation method comprises the following steps: arranging molten silicon materials in a crucible, wherein the inner bottom surface of the crucible is an inclined surface arranged obliquely relatively to the horizontal direction, and the thicknesses of the bottom of the crucible is gradually increased in the horizontal direction; controlling the thermal field in crystal growth, so that the horizontal temperature gradient is greater than longitudinal temperature gradient, and silicon material grows along the horizontal direction or in the direction with an acute angle with the vertical direction. During the growth of silicon ingot, a solid-liquid interface is not perpendicular to the axial direction of the crucible (i.e., vertical direction), so that the small-angle grain boundary in the silicon ingot can be reduced, and the dislocation density is grown outside the crystals before high dislocation density is formed. Therefore, silicon wafers with low grain boundary density and low dislocation density can be obtained through cutting, and the conversion efficiency of the silicon wafers can be improved. In addition, the invention further provides a polycrystalline silicon ingot furnace implementing the method.
Description
Technical field
The present invention relates to solar energy photovoltaic material preparation field is and in particular to a kind of preparation method of polycrystal silicon ingot, polycrystalline
Silicon ingot furnace and silicon chip.
Background technology
Crystal silicon battery occupies more than 90% market share in photovoltaic generation market at present, wherein does substrate based on polysilicon chip
Polycrystalline battery occupy crystal silicon battery 70% about the market share.Solid silicon material puts in the crucible of ingot furnace, passes through
Graphite resistance or sensing heating, melting silicon materials, the thermograde then being constructed by ingot casting thermal field are erected bottom-up
Nogata to long brilliant, then prepare polycrystal silicon ingot through annealing, cooling.Polycrystal silicon ingot after evolution working procedure processing Cheng little Fang ingot,
Again polysilicon chip is cut into along parallel or vertical crystal growth direction by multi-thread chopper and slicer.Photovoltaic generation is to extensive
Application it is necessary to improve generating efficiency and reduce cost of electricity-generating.At present, ingot casting polysilicon chip is with respect to pulling of crystals silicon chip
Speech, has absolute cost advantage, so by the raising of polysilicon chip quality, and then lifting polycrystalline battery efficiency just seems outstanding
For important.
Current efficient polycrystalline silicon ingot, mainly promotes layer induction long brilliant by nucleation, it can be broken silicon that nucleation promotes layer
Material, single crystal silicon square rods or other fusing point > 1400 DEG C of solid particles, after induction nucleation, crystal grain grows up along vertical direction.Many
Crystal silicon ingot evolution Cheng little Fang ingot, cuts into polysilicon chip further along parallel or vertical crystal growth direction.But this method is only capable of
Suppress initial bit density by increasing number of grain boundaries, can not effectively reduce the dislocation of later stage crystal grain growth course straight up
Propagation, along with excessive crystal boundary, as shown in the pl photo of Fig. 1, limits the continuation that such method prepares high-efficiency polycrystalline efficiency
Lifting.
Content of the invention
Based on this it is necessary to provide a kind of preparation method of the polycrystal silicon ingot that can lift polysilicon chip transformation efficiency.
A kind of preparation method of polycrystal silicon ingot, comprises the following steps: arranges the silicon material of molten condition, wherein institute in crucible
State the inclined-plane that the inner bottom surface of crucible is obliquely installed for relatively horizontal orientation, the thickness of the bottom of described crucible in the horizontal direction by
Step increases；Thermal field when controlling long brilliant, makes Transverse Temperature Gradient be more than longitudinal temperature gradient, make silicon material in the horizontal direction or with perpendicular
Nogata is to direction growth at an acute angle.
Wherein in an embodiment, the described thermal field controlling during long crystalline substance, make Transverse Temperature Gradient be more than longitudinal temperature ladder
Degree, make silicon material in the horizontal direction or the step of direction at an acute angle with vertical direction growth in: make heat-insulation cage near described crucible
The one side of bottom thinnest part first individually rise；After the scheduled time, then the other parts of heat-insulation cage are made to increase together.
A kind of polycrystalline silicon ingot or purifying furnace is also proposed, including body of heater, the heat-insulation cage being placed in body of heater, heat-insulated top board, heat insulation bottom board,
Positioned at the heat exchange platform in heat-insulation cage, the crucible on heat exchange platform, it is placed in the heater top in heat-insulation cage and side heater,
Described heat-insulation cage can lift with respect to described heat insulation bottom board, and the inner bottom surface of described crucible is obliquely installed for relatively horizontal orientation
Inclined-plane, the thickness of the bottom of described crucible incrementally increases in the horizontal direction, and heat-insulation cage is near the bottom thinnest part of described crucible
One side can self-movement with respect to the remainder of heat-insulation cage.
Wherein in an embodiment, the thermal conductivity of the one side near the bottom thinnest part of described crucible for the described heat-insulation cage is big
Thermal conductivity in heat-insulation cage remainder.
Wherein in an embodiment, described crucible includes four medial surface, in four medial surface of described crucible, closes on
Forming core is scribbled on the crucible medial surface of the bottom thinnest part of described crucible and promotes layer.
Wherein in an embodiment, described crucible arrange forming core promote the thermal conductivity of the medial surface of layer be more than crucible remaining
The thermal conductivity in each face.
Wherein in an embodiment, described side heater is three face heating, and described side heater removes setting shape from crucible
Other sides beyond core promotes layer are heated.
Wherein in an embodiment, the angle of inclination of the inner bottom surface of described crucible is 5 °～20 °.
Wherein in an embodiment, described crucible be formed around side guard plate, described side guard plate closes on described crucible
The thermal conductivity of the one side of bottom thinnest part is more than the thermal conductivity in other three faces of side guard plate.
A kind of silicon chip is also proposed, the polycrystal silicon ingot cutting that method described in aforementioned any one for the described silicon chip is obtained forms.
The preparation method of above-mentioned polycrystal silicon ingot, by controlling thermal field, makes Transverse Temperature Gradient be more than longitudinal temperature gradient, makes
Crystal grain is in the horizontal direction or the direction at an acute angle with vertical direction grows, in silicon ingot growth course, due to solid liquid interface out of plumb
In crucible axially (i.e. vertical direction), it is possible to reduce the low-angle boundary in silicon ingot, be conducive to before high dislocation density is formed, will
Dislocation density grows outside crystal.Therefore, subsequently can cut the silicon chip obtaining low grain boundary density and low-dislocation-density, lift silicon
The conversion efficiency of piece.
Above-mentioned polycrystalline silicon ingot or purifying furnace, can pass through during use to control the motion of heat-insulation cage, in conjunction with crucible, side guard plate, heater,
Produce the thermal field that Transverse Temperature Gradient is more than longitudinal temperature gradient, make crystal grain in the horizontal direction or at an acute angle with vertical direction
Direction grows, and subsequently can cut the silicon chip obtaining low grain boundary density and low-dislocation-density, the conversion efficiency of lifting silicon chip.
Above-mentioned silicon chip, the polycrystal silicon ingot cutting being obtained by aforesaid method is obtained, and grain boundary density is low, and dislocation density is low.
Brief description
Fig. 1 is the pl photo of the silicon chip of traditional method；
Fig. 2 is the flow chart of the preparation method of polycrystal silicon ingot；
Fig. 3 is the schematic diagram of polycrystalline silicon ingot or purifying furnace；
Fig. 4 is the schematic diagram of crucible；
Fig. 5 is the pl photo of the silicon chip that embodiment one is obtained；
Fig. 6 is the pl photo of the silicon chip that embodiment three is obtained.
Specific embodiment
Refer to Fig. 2, the present invention provides a kind of preparation method of polycrystal silicon ingot, comprises the following steps.
Step s110, the silicon material of molten condition is set in crucible, the inner bottom surface of wherein said crucible is relative level side
To the inclined-plane being obliquely installed, the thickness of the bottom of described crucible incrementally increases in the horizontal direction.The inner bottom surface of crucible tilts one
Determine angle, angular range is 5 °～20 °.So, the bottom thickness of crucible is inconsistent, incrementally increases in the horizontal direction, so that
During follow-up liquid silicon material length crystalline substance, crystal grain horizontally or diagonally grows.
The silicon material arranging molten condition in crucible can be obtained by following several ways less.
Mode one: load solid silicon material in crucible；Described crucible is carried out with heating makes solid silicon material melt.Mode
Two: heat solid silicon material, the silicon material of prepared molten condition in another crucible, then the silicon material of molten condition is poured into length
In crucible used by crystalline substance.
Thermal field when step s120, control are long brilliant, makes Transverse Temperature Gradient be more than longitudinal temperature gradient, makes silicon material along level
Direction or the direction at an acute angle with vertical direction growth.
In this step, following manner is taken to obtain the thermal field that Transverse Temperature Gradient is more than longitudinal temperature gradient: to make polysilicon
The heat-insulation cage of ingot furnace first individually rises near the one side of the bottom thinnest part of crucible；After Preset Time, then make heat-insulation cage
Other parts rise together.Traditional heat-insulation cage control mode is the overall temperature rising with respect to heat insulation bottom board, obtaining longitudinal direction
Gradient.And in this step, so that heat-insulation cage is first individually increased near the one side of crucible bottom thinnest part, then make heat-insulation cage other parts
Rise together, so, silicon material starts brilliant along level or the direction length at an acute angle with vertical direction from the side of crucible.
In silicon ingot growth course, because solid liquid interface is not orthogonal to crucible axially (i.e. vertical direction), it is possible to reduce silicon
Low-angle boundary in ingot, is conducive to before high dislocation density is formed, outside dislocation density is grown crystal.After prepared silicon ingot,
First along vertical direction by silicon ingot processing Cheng little Fang ingot, further along horizontal direction, little side's ingot is cut into silicon chip, can obtain low
Grain boundary density and the silicon chip of low-dislocation-density.
Refer to Fig. 3 and Fig. 4, the present invention also provides a kind of polycrystalline silicon ingot or purifying furnace 100 implementing said method, and it includes
Body of heater 110, the heat-insulation cage 120 being placed in body of heater 110, heat-insulated top board 130, heat insulation bottom board 140,120 heat in heat-insulation cage
Board 150, the crucible 160 being located on heat exchange platform 150, are placed in the heater 170 in 120 in heat-insulation cage, and are located at crucible
The side guard plate 180 of 160 surroundings and the bottom backplate 190 of crucible 160 bottom.
The inner bottom surface of crucible 160 is obliquely installed, and angle of inclination is 5 °～20 °, makes the bottom of crucible 160 in the horizontal direction
Variable thickness causes.Heater 170 includes the heater top 172 crucible 160 being heated from crucible 160 top and from sidepiece pair
The side heater 174 that crucible 160 is heated.
Heat-insulation cage 120 can lift with respect to heat insulation bottom board 140.Silicon material heating melting stage, heat-insulation cage 120 and heat-insulated top board
130th, heat insulation bottom board 140 is collectively forming closed cavity.Crystal growing stage, heat-insulation cage 120 then can rise with respect to heat insulation bottom board 140.
Traditional heat-insulation cage, is integral elevating with respect to heat insulation bottom board.In the present invention, heat-insulation cage 120 is near crucible 160
First face 122 of bottom thinnest part and the up and down motion in other three faces of heat-insulation cage 120 can be separately controlled.That is, heat-insulation cage
120 can self-movement with respect to the remainder of heat-insulation cage 120 near the first face 122 of the bottom thinnest part of crucible 160.Use
Two sets of drive mechanisms control two parts of heat-insulation cage 120 to can achieve that two parts can be separately controlled the purpose of motion respectively.
When long brilliant, the control mode of heat-insulation cage 120 is: first make can self-movement one side individually with respect to heat insulation bottom board 140
Rise, due to crucible 160 bottom thickness in the horizontal direction (in Fig. 3 along away from the first face 122 direction) be gradually increased, obtain
Obtained relatively larger transverse thermograde；After the scheduled time, then so that other three faces is risen overally, obtain longitudinal temperature gradient,
Horizontal thermograde is more than longitudinal temperature gradient.So, silicon material start along level or with vertical direction from the side of crucible be in
The direction length of acute angle is brilliant.In silicon ingot growth course, because solid liquid interface is not orthogonal to crucible axially (i.e. vertical direction), permissible
Reduce the low-angle boundary in silicon ingot, be conducive to before high dislocation density is formed, outside dislocation density is grown crystal.
The square configuration that crucible 160 opens wide for top.Crucible 160 has four medial surface, wherein closes on the bottom of crucible 160
Scribble on one medial surface of portion's thinnest part forming core promote layer 162, this medial surface near heat-insulation cage 120 can self-movement first
Face 122, the two orientation in ingot furnace is consistent.It is higher than the material of silicon fusing point that forming core promotes the material of layer 162, can be stone
Sand or carborundum, silicon oxide.Forming core promotes the induced nucleation of layer 162, can reduce initial bit density.
The thermal conductivity of the medial surface of layer 162 is promoted to be more than the thermal conductivity in other each faces additionally, crucible 160 arranges forming core.Every
Hot cage 120 can self-movement the first face 122 thermal conductivity be more than heat-insulation cage 120 remainder thermal conductivity, such as by
The method of the heat-insulation layer of setting different-thickness obtains.Side heater 174 is three face heating, and it only enters from the three of crucible lateral surface
Row heating, is not heated at the lateral surface being promoted the corresponding crucible 160 of layer 162 with forming core.Side guard plate 180 closes on crucible
The thermal conductivity of 160 one side of bottom thinnest part be more than other three faces of side guard plate 180 thermal conductivity, for example, thermal conductivity high one
The material in face can be using the high isostatic pressing formed graphite of thermal conductivity, and other three faces can be multiple with the carbon carbon that use intensity is high, thermal conductivity is low
Condensation material.The material of bottom backplate 190 is that intensity is high, and thermal conductivity is in the carbon carbon composite of 0.15～10w/ (m.k).Heat exchange platform
150 is also such, can be using the material that intensity is high, thermal conductivity is low.Above-mentioned improved feature, is for better ensuring that vertical
It is less than Transverse Temperature Gradient to thermograde, enable heat-insulation cage 120 when moving, to better ensure that silicon liquid arranges shape from crucible 160
Core promotes the side of layer 162 to start long crystalline substance, can coordinate aforementioned ingot furnace 120 and crucible using multinomial improved feature simultaneously
160 it is also possible to only choose the improved feature of one of which.
To further explain how below by specific embodiment to implement above-mentioned preparation side using above-mentioned polycrystalline silicon ingot or purifying furnace
Method.
Embodiment 1
The silicon material of 750kg is put in crucible 160, a medial surface of crucible 160 is coated with silicon carbide layer or quartz
Layer of sand.The angle of inclination of the inner bottom surface of crucible 160 is 5 °.
Heat-insulation cage 120 forms closed cavity with heat-insulated top board 130, heat insulation bottom board 140.Using heater top 172 from top
Silicon material is heated, from three lateral surface of crucible 160, silicon material is heated using side heater 174.
After melting silicon materials, the first face 122 of the self-movement of heat-insulation cage 120 is controlled individually to rise, after rising 8cm, then
The other parts controlling heat-insulation cage 120 rise together, silicon liquid nucleation under the promotion of carborundum, and open from the side of crucible 160
Begin to obtain polycrystal silicon ingot along level or the long crystalline substance in direction at an acute angle with vertical direction.Along vertical direction by silicon ingot processing Cheng little Fang
Little side's ingot is cut into silicon chip along horizontal direction, can obtain the silicon chip of low grain boundary density and low-dislocation-density by ingot.
Prepared silicon chip is carried out with photoluminescence (photoluminescence, pl) test, result is as shown in Figure 5.Permissible
See, grain boundary density and dislocation density are significantly less than the silicon chip of the traditional scheme of Fig. 1.Silicon chip is made after cell piece, test effect
Rate finds that the conversion efficiency of the cell piece that the silicon chip of embodiment 1 is made reaches 18.01%, compared with the normal casting polysilicon shown in Fig. 1
Piece improves 0.11%.
Embodiment 2
The silicon material of 700kg is put in crucible 160, a medial surface of crucible 160 is coated with quartz sand layer.Crucible
The angle of inclination of 160 inner bottom surface is 10 °.
Heat-insulation cage 120 forms closed cavity with heat-insulated top board 130, heat insulation bottom board 140.Using heater top 172 from top
Silicon material is heated, from three lateral surface of crucible 160, silicon material is heated using side heater 174.
After melting silicon materials, the first face 122 of the self-movement of heat-insulation cage 120 is controlled individually to rise, after rising 8cmm, then
The other parts controlling heat-insulation cage 120 rise together, silicon liquid nucleation under the promotion of carborundum, and open from the side of crucible 160
Begin to obtain polycrystal silicon ingot along level or the long crystalline substance in direction at an acute angle with vertical direction.Along vertical direction by silicon ingot processing Cheng little Fang
Little side's ingot is cut into silicon chip along horizontal direction, can obtain the silicon chip of low grain boundary density and low-dislocation-density by ingot.
Silicon chip is made after cell piece, testing efficiency finds that the conversion efficiency of the cell piece that the silicon chip of embodiment 2 is made reaches
18.04%, improve 0.14% compared with the normal polysilicon chip shown in Fig. 1.
Embodiment 3
The silicon material of 650kg is put in crucible 160, a medial surface of crucible 160 is coated with quartz sand layer.Crucible
The angle of inclination of 160 inner bottom surface is 20 °.
Heat-insulation cage 120 forms closed cavity with heat-insulated top board 130, heat insulation bottom board 140.Using heater top 172 from top
Silicon material is heated, from three lateral surface of crucible 160, silicon material is heated using side heater 174.
After melting silicon materials, the first face 122 of the self-movement of heat-insulation cage 120 is controlled individually to rise, after rising 10cm, then
The other parts controlling heat-insulation cage 120 rise together, silicon liquid nucleation under the promotion of carborundum, and open from the side of crucible 160
Begin to obtain polycrystal silicon ingot along level or the long crystalline substance in direction at an acute angle with vertical direction.Along vertical direction by silicon ingot processing Cheng little Fang
Little side's ingot is cut into silicon chip along horizontal direction, can obtain the silicon chip of low grain boundary density and low-dislocation-density by ingot.
Prepared silicon chip is carried out with photoluminescence (photoluminescence, pl) test, result is as shown in Figure 6.Permissible
See, grain boundary density and dislocation density are significantly less than the silicon chip of the traditional scheme of Fig. 1.Silicon chip is made after cell piece, test effect
Rate finds that the conversion efficiency of the cell piece that the silicon chip of embodiment 3 is made reaches 18.10%, compared with the normal casting polysilicon shown in Fig. 1
Piece improves 0.2%.
Embodiment described above only have expressed the several embodiments of the present invention, and its description is more concrete and detailed, but simultaneously
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, some deformation can also be made and improve, these broadly fall into the guarantor of the present invention
Shield scope.Therefore, the protection domain of patent of the present invention should be defined by claims.
Claims (9)
1. a kind of preparation method of polycrystal silicon ingot is it is characterised in that comprise the following steps:
The silicon material of molten condition is set in crucible, the inner bottom surface of wherein said crucible for relatively horizontal orientation be obliquely installed oblique
Face, the thickness of the bottom of described crucible incrementally increases in the horizontal direction；
Thermal field when controlling long brilliant, makes Transverse Temperature Gradient be more than longitudinal temperature gradient, make silicon material in the horizontal direction or with vertical
Direction direction growth at an acute angle.
2. the preparation method of polycrystal silicon ingot according to claim 1 is it is characterised in that thermal field when described control length is brilliant,
Make Transverse Temperature Gradient be more than longitudinal temperature gradient, make silicon material in the horizontal direction or direction at an acute angle with vertical direction growth
In step:
Heat-insulation cage is made first individually to increase near the one side of the bottom thinnest part of described crucible；
After the scheduled time, then the other parts of heat-insulation cage are made to increase together.
3. a kind of polycrystalline silicon ingot or purifying furnace, including body of heater, the heat-insulation cage being placed in body of heater, heat-insulated top board, heat insulation bottom board, positioned at heat-insulated
Heat exchange platform in cage, the crucible being located on heat exchange platform, are placed in the heater top in heat-insulation cage and side heater, described heat-insulated
Cage can lift with respect to described heat insulation bottom board it is characterised in that the inner bottom surface of described crucible tilts to set for relatively horizontal orientation
The inclined-plane put, the thickness of the bottom of described crucible incrementally increases in the horizontal direction, and heat-insulation cage is near the bottom of described crucible
The one side at thin place can self-movement with respect to the remainder of heat-insulation cage.
4. polycrystalline silicon ingot or purifying furnace according to claim 3 is it is characterised in that described heat-insulation cage is near the bottom of described crucible
The thermal conductivity of the one side of thinnest part is more than the thermal conductivity of heat-insulation cage remainder.
5. polycrystalline silicon ingot or purifying furnace according to claim 3 is it is characterised in that described crucible includes four medial surface, described
In four medial surface of crucible, the crucible medial surface of the bottom thinnest part closing on described crucible scribbles forming core and promotes layer.
6. polycrystalline silicon ingot or purifying furnace according to claim 5 is it is characterised in that described crucible arranges the inner side that forming core promotes layer
The thermal conductivity in face is more than the thermal conductivity in remaining each face of crucible.
7. polycrystalline silicon ingot or purifying furnace according to claim 5 is it is characterised in that described side heater is three face heating, described
Side heater from crucible, heated by other sides in addition to setting forming core promotes layer.
8. polycrystalline silicon ingot or purifying furnace according to claim 3 is it is characterised in that the angle of inclination of the inner bottom surface of described crucible is
5 °～20 °.
9. polycrystalline silicon ingot or purifying furnace according to claim 3 it is characterised in that described crucible be formed around side guard plate, institute
The thermal conductivity stating the one side of bottom thinnest part that side guard plate closes on described crucible is more than the thermal conductivity in other three faces of side guard plate.
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