CN109023522A - The preparation method of polycrystal silicon ingot - Google Patents
The preparation method of polycrystal silicon ingot Download PDFInfo
- Publication number
- CN109023522A CN109023522A CN201811137295.1A CN201811137295A CN109023522A CN 109023522 A CN109023522 A CN 109023522A CN 201811137295 A CN201811137295 A CN 201811137295A CN 109023522 A CN109023522 A CN 109023522A
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- Prior art keywords
- crucible
- separation layer
- ingot
- preparation
- seed layer
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 56
- 239000010703 silicon Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 61
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 10
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 10
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical group N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 230000008961 swelling Effects 0.000 claims description 4
- 229920005591 polysilicon Polymers 0.000 claims 2
- 238000000034 method Methods 0.000 abstract description 16
- 230000006911 nucleation Effects 0.000 abstract description 12
- 238000010899 nucleation Methods 0.000 abstract description 12
- 239000000523 sample Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 238000005266 casting Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002210 silicon-based material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000010485 coping Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention is suitable for technical field of solar batteries, provides a kind of preparation method of polycrystal silicon ingot.This method comprises: the inner surface in the crucible of coating seed layer coats separation layer, wherein the separation layer of the crucible bottom is loose and porous structure；It is put into polycrystalline silicon raw material in the crucible after separation layer coating, and the crucible is placed in ingot furnace；Melt the polycrystalline silicon raw material, and make the polycrystalline silicon raw material on the basis of seed layer crystalline growth at polycrystal silicon ingot.The present invention makes silicon liquid penetrate into the lower section of separation layer by the gap of separation layer, contacts with seed layer, using seed layer as nucleation point, keep heterogeneous nucleation rate higher, crystal grain is more uniform by coating loose porous separation layer in crucible bottom.
Description
Technical field
The invention belongs to technical field of solar batteries more particularly to a kind of preparation methods of polycrystal silicon ingot.
Background technique
First procedure of the polycrystal silicon ingot technology as photovoltaic module industrial chain generates key to the efficiency of photovoltaic cell
It influences.The preparation process of polycrystal silicon ingot is will be after melting silicon materials, and being frozen into again by the way of oriented growth has certain crystalline substance
The square silicon ingot of kernel structure and resistivity.
Currently, the conventional process for preparing polycrystal silicon ingot is fine melt technique, i.e., seed layer is coated in crucible bottom, in seed layer
Upper surface be coated with nitride spacer, these seed layers will form concaveconvex structure in crucible bottom, pass through control technique item
Part, silicon material forming core crystallization on these concave-convex points after fusing.But since the partial size of silicon nitride is less than the grain of seed layer
Diameter, silicon nitride can be embedded into pit, reduce nucleation rate, form strip dendrite.
Summary of the invention
In view of this, the embodiment of the invention provides a kind of preparation method of polycrystal silicon ingot, to solve to lead in the prior art
When crossing fine melt technique and preparing polycrystal silicon ingot, the low problem of nucleation rate.
The first aspect of the embodiment of the present invention provides a kind of preparation method of polycrystal silicon ingot, comprising:
Separation layer is coated in the inner surface of the crucible of coating seed layer, wherein the separation layer of the crucible bottom is loose
Porous structure；
It is put into polycrystalline silicon raw material in the crucible after separation layer coating, and the crucible is placed in ingot furnace；
Melt the polycrystalline silicon raw material, and make the polycrystalline silicon raw material on the basis of seed layer crystalline growth at more
Crystal silicon ingot.
In a kind of implementation, the separation layer of the crucible bottom with a thickness of 1 millimeter to 1.5 millimeters, the crucible side
The separation layer of wall with a thickness of 2 millimeters to 3 millimeters.
In a kind of implementation, the material of the separation layer of the crucible bottom is silicon nitride, water and swelling agent；The crucible
The material of the separation layer of side wall is silicon nitride and water.
In a kind of implementation, the separation layer density of the crucible bottom is the 1/ of the separation layer density of the crucible wall
3 to 1/2.
In a kind of implementation, the fusing polycrystalline silicon raw material, and make the polycrystalline silicon raw material in the seed layer
On the basis of crystalline growth at polycrystal silicon ingot, comprising:
The temperature of the ingot furnace is increased to the first preset temperature, the polycrystalline silicon raw material is made all to be fused into silicon liquid；
Within a preset time, the temperature of the crucible is maintained into the second preset temperature, makes seed described in the silicon liquid corrode
Crystal layer；
The temperature for reducing the ingot furnace, crystalline growth is at polycrystalline on the basis of making seed layer of the silicon liquid after corrode
Silicon ingot.
In a kind of implementation, the corrode depth of the seed layer is the 1/3 to 1/2 of the seed crystal layer height.
In a kind of implementation, second preset temperature is 1360 degrees Celsius to 1365 degrees Celsius, preset time 13
Minute was to 17 minutes.
In a kind of implementation, second preset temperature is 1365 degrees Celsius to 1370 degrees Celsius, and preset time is 8 points
Clock was to 12 minutes.
In a kind of implementation, second preset temperature is 1370 degrees Celsius to 1375 degrees Celsius, and preset time is 3 points
Clock was to 7 minutes.
In a kind of implementation, further includes:
Seed layer is coated in crucible bottom, wherein the partial size of the seed layer is 50 mesh to 80 mesh.
Existing beneficial effect is the embodiment of the present invention compared with prior art: the embodiment of the present invention passes through in crucible bottom
Loose porous separation layer is coated, so that silicon liquid is penetrated into the lower section of separation layer by the gap of separation layer, is contacted with seed layer,
Using seed layer as nucleation point, keep heterogeneous nucleation rate higher, crystal grain is more uniform.It changes in conventional fine melt technique using recessed
The mode of male structure forming core solves the problems, such as that nucleation rate caused by covering because of separation layer declines.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to embodiment or description of the prior art
Needed in attached drawing be briefly described, it should be apparent that, the accompanying drawings in the following description is only of the invention some
Embodiment for those of ordinary skill in the art without any creative labor, can also be according to these
Attached drawing obtains other attached drawings.
Fig. 1 is the implementation process schematic diagram of the preparation method of polycrystal silicon ingot provided in an embodiment of the present invention；
Fig. 2 is the schematic diagram of the preparation method of polycrystal silicon ingot provided in an embodiment of the present invention；
Fig. 3 is the implementation process schematic diagram of step S103 provided in an embodiment of the present invention.
Specific embodiment
In being described below, for illustration and not for limitation, the tool of such as particular system structure, technology etc is proposed
Body details, to understand thoroughly the embodiment of the present invention.However, it will be clear to one skilled in the art that there is no these specific
The present invention also may be implemented in the other embodiments of details.In other situations, it omits to well-known system, device, electricity
The detailed description of road and method, in case unnecessary details interferes description of the invention.
In order to illustrate technical solutions according to the invention, the following is a description of specific embodiments.
Referring to FIG. 1, Fig. 1 is the implementation flow chart of the preparation method for the polycrystal silicon ingot that one embodiment of the invention provides, it should
Method the following steps are included:
Step S101 coats separation layer in the inner surface of the crucible of coating seed layer, wherein the isolation of the crucible bottom
Layer is loose and porous structure.
In embodiments of the present invention, the bottom and side wall by spray coating method in crucible sprays separation layer, wherein crucible wall
Separation layer be conventional insulation layer structure, the separation layer of crucible bottom is loose and porous structure.Spray coating method includes but is not limited to
Round brush method, high-pressure spray gun spray coating method or manual brushing method.
Step S102 is put into polycrystalline silicon raw material coating, and the crucible is placed in ingot casting in the crucible after separation layer
In furnace.
In embodiments of the present invention, it after inner surface of crucible sprays separation layer, will charge after crucible standing and drying, after charging
Crucible is put into ingot furnace, and by ingot casting stove evacuation.
Step S103 melts the polycrystalline silicon raw material, and ties the polycrystalline silicon raw material on the basis of seed layer
Crystals growth is at polycrystal silicon ingot.
In embodiments of the present invention, the temperature for setting ingot furnace, makes polycrystalline silicon raw material all be fused into silicon liquid.Such as Fig. 2 institute
Show, silicon liquid 21 can penetrate into the lower section of separation layer by the gap of separation layer 22, contact with seed layer 23, then reduce ingot casting
The temperature of furnace crystallizes silicon liquid 21 on the basis of seed layer 23.
The embodiment of the present invention makes gap of the silicon liquid by separation layer by coating loose porous separation layer in crucible bottom
The lower section for penetrating into separation layer, contacts with seed layer, using seed layer as nucleation point, keeps heterogeneous nucleation rate higher, crystal grain
It is more uniform.It changes in conventional fine melt technique in the way of concaveconvex structure forming core, caused by solving because of separation layer covering
The problem of nucleation rate declines.
As an embodiment of the present invention, before step S101 further include: coat seed layer in crucible bottom, wherein
The partial size of the seed layer is 50 mesh to 80 mesh.
In embodiments of the present invention, the material of seed layer can be for silicon carbide, silica etc., the shape of crystal grain in seed layer
Shape can be one of spherical, hemispherical and polygon with corner angle or a variety of.
As an embodiment of the present invention, the separation layer of the crucible bottom with a thickness of 1 millimeter to 1.5 millimeters, institute
State the separation layer of crucible wall with a thickness of 2 millimeters to 3 millimeters.
In embodiments of the present invention, by reducing the spraying number and spray pressure of crucible bottom separation layer, make crucible bottom
The thickness of the separation layer in portion is less than the thickness of the separation layer of crucible wall, prevents the thickness of crucible bottom separation layer is too thick from leading to silicon
Liquid is difficult to penetrate into below separation layer.
As an embodiment of the present invention, the material of the separation layer of the crucible bottom is silicon nitride, water and swelling agent；
The material of the separation layer of the crucible wall is silicon nitride and water.
In embodiments of the present invention, silicon nitride material can play effective buffer action, and chemical property is stablized, not with earthenware
Crucible and silicon liquid react, and have enough adhesive strengths in inner surface of crucible, do not fall off at high temperature, not blistering.Pass through
Swelling agent is added in Silicon nitride solution, keeps separation layer fluffy, generates and conveys porous structure, silicon liquid is enable to seep by gap
It penetrates into below separation layer.
As an embodiment of the present invention, the separation layer density of the crucible bottom is the separation layer of the crucible wall
The 1/3 to 1/2 of density.
In embodiments of the present invention, the density of the separation layer of crucible wall is conventional separation layer density, in crucible bottom
Separation layer material in be added a large amount of water, reduce the density of crucible bottom separation layer, make the separation layer density of crucible bottom
It is the 1/3 to 1/2 of the separation layer density of crucible wall, it is easier to form loose porous structure.
As an embodiment of the present invention, as shown in figure 3, a kind of possible implementation of step S103 includes following
Step:
The temperature of the ingot furnace is increased to the first preset temperature by step S301, keeps the polycrystalline silicon raw material all molten
It is melted into silicon liquid.
In embodiments of the present invention, the temperature for increasing ingot furnace, is completely melt polycrystalline silicon raw material.Setting two in ingot furnace
A temperature probe, wherein the temperature probe TC1 at top is used to control the temperature of heater, for example, make temperature in ingot furnace by
It edges up up to 1520 degrees Celsius to 1540 degrees Celsius, to provide heat melts whole silicon material.Another temperature probe TC2 setting exists
On the heat exchange platform of crucible bottom, for monitoring the temperature of crucible bottom.In polycrystalline silicon raw material fusion process, temp probe
TC2 detects the temperature in crucible and is gradually increasing, and the slope of ascending curve lowers, after polycrystalline silicon raw material all melts, by
Thermally conductive in crucible bottom can accelerate, and TC2 detects the meeting rapid increase of the temperature in crucible, when there is inflection point in temperature curve,
Polycrystalline silicon raw material is all fused into silicon liquid.
The temperature of the crucible is maintained the second preset temperature within a preset time by step S302, keeps the silicon liquid molten
Lose the seed layer.
In embodiments of the present invention, silicon liquid can be reacted with the generation of the crystal grain in seed layer corrode, by control crucible
Temperature and time controls the depth of corrode, makes seed layer part corrode.
Step S303 reduces the temperature of the ingot furnace, makes to crystallize on the basis of seed layer of the silicon liquid after corrode
Grow into polycrystal silicon ingot.
In embodiments of the present invention, after the corrode of seed layer part, the temperature of ingot furnace, seed crystal of the silicon liquid after corrode are reduced
Forming core on the basis of layer, and crystalline growth is at polycrystal silicon ingot.
As an embodiment of the present invention, the corrode depth of the seed layer is the 1/3 to 1/ of the seed crystal layer height
2。
In embodiments of the present invention, it during corrode, needs accurately to control corrode depth.If burn-out time is too short, lead
Corrode does not occur for cause or corrode is too shallow, and the silicon liquid for penetrating into separation layer is very little, causes nucleation rate too low, if burn-out time is too long,
Seed crystal can be by excessive corrode, and the contact angle of heterogeneous forming core is excessive at this time, and nucleation rate equally declines, it could even be possible to seed layer is complete
Portion's fusing, separation layer are destroyed completely, cause silicon ingot and crucible base adhesion, cause accident.Reasonable corrode depth should control
The 1/3 to 1/2 of seed crystal layer height.
In embodiments of the present invention, temperature in crucible (i.e. the temperature of temperature probe TC2 measurement) is different, when the corrode of control
Between it is different.The temperature of TC2 measurement is 1360 degrees Celsius to 1365 degrees Celsius, and burn-out time is 13 minutes to 17 minutes, for example, molten
Losing the time is 15 minutes.The temperature of TC2 measurement is 1365 degrees Celsius to 1370 degrees Celsius, and burn-out time is 8 minutes to 12 minutes,
For example, burn-out time is 10 minutes.TC2 measurement temperature be 1370 degrees Celsius to 1375 degrees Celsius, burn-out time be 3 minutes extremely
7 minutes, for example, burn-out time is 5 minutes.
It should be understood that the size of the serial number of each step is not meant that the order of the execution order in above-described embodiment, each process
Execution sequence should be determined by its function and internal logic, the implementation process without coping with the embodiment of the present invention constitutes any limit
It is fixed.
Embodiment described above is merely illustrative of the technical solution of the present invention, rather than its limitations；Although referring to aforementioned reality
Applying example, invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each
Technical solution documented by embodiment is modified or equivalent replacement of some of the technical features；And these are modified
Or replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution should all
It is included within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of polycrystal silicon ingot characterized by comprising
Separation layer is coated in the inner surface of the crucible of coating seed layer, wherein the separation layer of the crucible bottom is loose porous
Structure；
It is put into polycrystalline silicon raw material in the crucible after separation layer coating, and the crucible is placed in ingot furnace；
Melt the polycrystalline silicon raw material, and make the polycrystalline silicon raw material on the basis of seed layer crystalline growth at polysilicon
Ingot.
2. the preparation method of polycrystal silicon ingot as described in claim 1, which is characterized in that the thickness of the separation layer of the crucible bottom
Degree be 1 millimeter to 1.5 millimeters, the separation layer of the crucible wall with a thickness of 2 millimeters to 3 millimeters.
3. the preparation method of polycrystal silicon ingot as described in claim 1, which is characterized in that the material of the separation layer of the crucible bottom
Matter is silicon nitride, water and swelling agent；The material of the separation layer of the crucible wall is silicon nitride and water.
4. the preparation method of polycrystal silicon ingot as described in claim 1, which is characterized in that the separation layer density of the crucible bottom
It is the 1/3 to 1/2 of the separation layer density of the crucible wall.
5. such as the preparation method of the described in any item polycrystal silicon ingots of Claims 1-4, which is characterized in that the fusing is described more
Crystal silicon raw material, and make the polycrystalline silicon raw material on the basis of seed layer crystalline growth at polycrystal silicon ingot, comprising:
The temperature of the ingot furnace is increased to the first preset temperature, the polycrystalline silicon raw material is made all to be fused into silicon liquid；
Within a preset time, the temperature of the crucible is maintained into the second preset temperature, makes seed layer described in the silicon liquid corrode；
The temperature for reducing the ingot furnace, crystalline growth is at polysilicon on the basis of making seed layer of the silicon liquid after corrode
Ingot.
6. the preparation method of polycrystal silicon ingot as claimed in claim 5, which is characterized in that the corrode depth of the seed layer is institute
State the 1/3 to 1/2 of seed crystal layer height.
7. such as the preparation method of polycrystal silicon ingot described in claim 5 or 6, which is characterized in that second preset temperature is
1360 degrees Celsius to 1365 degrees Celsius, preset time is 13 minutes to 17 minutes.
8. such as the preparation method of polycrystal silicon ingot described in claim 5 or 6, which is characterized in that second preset temperature is
1365 degrees Celsius to 1370 degrees Celsius, preset time is 8 minutes to 12 minutes.
9. such as the preparation method of polycrystal silicon ingot described in claim 5 or 6, which is characterized in that second preset temperature is
1370 degrees Celsius to 1375 degrees Celsius, preset time is 3 minutes to 7 minutes.
10. such as the preparation method of the described in any item polycrystal silicon ingots of Claims 1-4, which is characterized in that further include:
Seed layer is coated in crucible bottom, wherein the partial size of the seed layer is 50 mesh to 80 mesh.
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Application publication date: 20181218 |