CN102732943A - Method for producing monocrystalline silicon cast ingot - Google Patents
Method for producing monocrystalline silicon cast ingot Download PDFInfo
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- CN102732943A CN102732943A CN2011100832606A CN201110083260A CN102732943A CN 102732943 A CN102732943 A CN 102732943A CN 2011100832606 A CN2011100832606 A CN 2011100832606A CN 201110083260 A CN201110083260 A CN 201110083260A CN 102732943 A CN102732943 A CN 102732943A
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Abstract
The invention discloses a method for producing a monocrystalline silicon cast ingot, which comprises the following steps: 1) placing seed crystals in a seed crystal groove at the bottom of a crucible according to same crystal orientation, adding a silicon material and a doping agent in the crucible; 2) melting the silicon material and the doping agent over the seed crystals, and partially melting the seed crystals; 3) carrying out directional solidification on the silicon melt from bottom to top by using a crucible descending method, and inducing the growth of the quasi monocrystalline by unmelted seed crystals to finally form the monocrystalline silicon cast ingot. The obtained monocrystalline silicon has the characteristics of less dislocation density, less oxygen stacking fault and better consistence of crystal orientation, and can satisfy a texturing process of a monocrystalline silicon solar energy battery, the monocrystalline silicon sheets are corroded to textures with a pyramid state along (100) the crystal orientation, thereby the absorbancy of the battery on light can be increased.
Description
Technical field
The present invention relates to a kind of making method of solar level silicon single crystal, the working method of the silicon single crystal ingot casting of particularly a kind of integrated vertical pulling method silicon single crystal and ingot casting polysilicon advantage.
Background technology
Solar level silicon single crystal mainly is to produce with vertical pulling method (CZ method) or zone melting method (FZ method) at present.Vertical pulling method is slowly pulled out from the molten silicon pond through steps such as seed crystal seeding necking downs.For the FZ method, the solid material charging is solidified through melting zone and at the opposite side of melting zone again.The silicon single crystal of making by these modes comprises radially-arranged impurity and defective, and for example L&S line defect, oxygen cause " whirlpool " defective or the vacancy cluster in stacking fault ring and gap.The CZ method is used as main monocrystalline silicon growing mode, because it can be used for making solar cell efficiently.But on cost, CZ method too expensive.
For casting polycrystalline silicon, molten silicon is contained in the quartz ceramic crucible, and cools off through the mode of control, thereby makes silicon crystallization wherein.The polysilicon that this mode is produced is the reunion of crystal grain, and within the wafer of processing thus, crystal grain orientation to each other is actually at random.
The random orientation of the crystal grain in the conventional polysilicon makes and is difficult to resulting wafer surface is carried out decorative pattern.Decorative pattern is to be used for through reducing luminous reflectance and improving the efficient that the absorption that sees through battery surface luminous energy improves battery.In addition, form on the crystal boundary between the polysilicon grain " kinking " tend to bunch or the dislocation line form become the nuclear of textural defect.These dislocations and their gettering effect cause the compound fast of current carrier in the battery that polysilicon processes, and cause the reduction of battery efficiency.In view of the cost of polysilicon lower, and in the battery processing effectively the defective passivation eliminate the dangling bonds on battery sheet surface, polysilicon generally is used for solar cell.
Bottom seed crystal method is the combination of falling crucible method and flux method, generally is used to produce non-congruent melting compound monocrystalline.Through structure and principle analysis, the mode of new similar polysilicon casting growing single-crystal silicon has been proposed: bottom seed crystal method growing single-crystal silicon to itself and ingot furnace.This method has solved an issuable seed crystal fusing control and a floating difficult problem when using flat crucible melting silicon material.
Summary of the invention
The object of the invention is exactly in order to provide a kind of working method of silicon single crystal ingot casting, to prepare the consistent solar level silicon single crystal in crystal orientation with big crystal grain, crystal grain.
The object of the invention can be realized through following technical scheme: a kind of working method of silicon single crystal ingot casting may further comprise the steps:
A, seed crystal is positioned over according to identical crystal orientation in the seed slot of crucible bottom, in crucible, adds polycrystalline silicon material then and doping agent covers seed crystal;
B, crucible is placed ingot furnace, vacuumize the back and feed argon gas, polycrystalline silicon material under argon shield above the heat fused seed crystal and doping agent, and make the part seed crystal fusing near polycrystalline silicon material and doping agent, formation silicon melt;
C, adopt falling crucible method to impel silicon melt, induce the growth of accurate monocrystalline, finally form the silicon single crystal ingot casting by unfused seed crystal by the bottom directional freeze that makes progress;
Ingot is got in D, cooling.
The crystal orientation of described seed crystal is < 100 >.
Described seed slot stretches out downwards from crucible bottom, and the height that is positioned over the seed crystal in the seed slot is higher than the height of seed slot.
Described seed slot be shaped as cube shaped or the cylinder bodily form, corresponding seed crystal is shaped as cube shaped or the cylinder bodily form.
Described crucible is the quartz ceramic crucible with silicon nitride coating.
Described doping agent is boron, phosphorus or gallium.
The vacuum degree control that vacuumizes described in the step B is below 5Pa, and Heating temperature is for being heated to 1550 ℃.
During falling crucible method directional freeze described in the step C, the speed control that crucible descends is at 5-15mm/h, and adopts the recirculated water cooling in crucible bottom.
The height of the aspect ratio seed slot of described seed crystal exceeds 8-10mm.
Described crucible is cube shaped or the cylinder bodily form, and its bottom is provided with funnel-shaped structure recessed down; Described seed slot is connected at the bottom of the bucket of this funnel-shaped structure.
The present invention makes it compared with prior art owing to adopted above technical scheme, has following advantage and characteristics:
1, uses bottom seed crystal method growing single-crystal silicon, compare casting polycrystalline silicon and have littler crystal boundary density, bigger crystal grain, more consistent grain orientation;
2, compare vertical pulling method silicon single crystal, have lower energy consumption, output that can be big;
3, owing to do not use quartz crucible, oxygen level is lacked than pulling of silicon single crystal, has reduced optical attenuation;
4, the reduction of crystal boundary density makes alkali alcohol hybrid corrosion liquid carry out anisotropic corrosion to silicon chip, makes silicon chip surface have suede structure (light trapping structure), can effectively strengthen the absorption of silicon chip to the incident sunshine, thereby improve photogenerated current.
Description of drawings
Fig. 1 is for the crucible that adopts among the present invention and be positioned over seed crystal and the synoptic diagram of polycrystalline silicon material in the crucible.
Embodiment
Below in conjunction with accompanying drawing 1 and specific embodiment the present invention is elaborated.
Embodiment 1
1) dislocation-free raw material monocrystalline silico briquette is put into the seed slot 2 of crucible 1 as seed crystal 3, crucible is selected the square quartz ceramic crucible of silicon nitride coating for use, and the crucible main body is 450Kg level 840mm*840mm*400mm, confirms seed crystal < 100>crystal orientation straight up; Again 450Kg polysilicon 4 is placed on the raw material monocrystalline silico briquette 3, and add P type doping agent boron, make the crystal resistivity after the doping remain on 1.5-2 Ω cm.
2) the ingot furnace furnace chamber back that is evacuated is directly fed argon gas.The position of adjustment crucible makes doping agent, polysilicon and be heated near the part seed crystal of polysilicon; Be heated to gradually and make more than 1412 ℃ that polysilicon begins to melt; And maintain the temperature at for some time more than 1412 ℃; Make doping agent, polysilicon and be melted into liquid forming silicon melt, and the seed crystal in the crucible bottom seed slot does not melt near the part material monocrystalline silico briquette of polysilicon.Whenever measured long brilliant situation at a distance from one hour with quartz pushrod.
3) cool off crucible bottom with recirculated cooling water; Make the heat exchange of silicon melt mainly occur in crucible bottom, with the speed decline crucible of 5-15mm/h, furnace temperature is reduced to 1450 ℃ by 1550 ℃ simultaneously; Make silicon melt from the bottom directional freeze gradually upwards; Because crucible bottom remains with not the part silicon single crystal that melts, at this as the seed crystal induced growth, thereby grow the silicon single crystal ingot casting.
4) ingot is got in cooling.Carry out 1100 ℃ of annealing after crystal growth finishes, reduce heating power gradually, stop heating, the crystal ingot naturally cooling after 700 ℃.
1) dislocation-free raw material monocrystalline silico briquette is put into the seed slot 2 of crucible 1 as seed crystal 3, crucible is selected the circular quartz ceramic crucible of silicon nitride coating for use, and the crucible main body is 18 inches crucibles of 60Kg level, is 450mm highly, confirms seed crystal < 100>crystal orientation straight up; Again 50Kg polysilicon 4 is placed on 3 of the raw material silicon single crystal, and add P type doping agent boron, make the crystal resistivity after the doping remain on 1.5-2 Ω cm.
2) the ingot furnace furnace chamber back that is evacuated is directly fed argon gas.The position of crucible in the adjustment stove makes doping agent, polysilicon and be heated near the part seed crystal of polysilicon; Be heated to gradually and make more than 1412 ℃ that polysilicon begins to melt; And maintain the temperature at for some time more than 1412 ℃; Make doping agent, polysilicon and be melted into liquid forming silicon melt, and seed crystal does not melt in the crucible bottom seed slot near the part material monocrystalline silico briquette of polysilicon.Whenever measured long brilliant situation at a distance from one hour with quartz pushrod.
3) cool off crucible bottom with recirculated cooling water; Make the heat exchange of silicon melt mainly occur in crucible bottom, with the speed decline crucible of 5-15mm/h, furnace temperature is reduced to 1450 ℃ by 1550 ℃ simultaneously; Make silicon melt from the bottom directional freeze gradually upwards; Because crucible bottom remains with not the part silicon single crystal that melts, at this as the seed crystal induced growth, thereby grow casting monocrystalline silicon.
4) ingot is got in cooling.Carry out 1100 ℃ of annealing after crystal growth finishes, reduce heating power gradually, stop heating, the crystal ingot naturally cooling after 700 ℃.
After silicon single crystal ingot takes out through evolution, the tail that detects, decaptitates, process little side's ingot.Can see that through butt the silicon single crystal crystal boundary density of being grown by bottom seed crystal method is little, crystal grain is vertically grown, and the chip area pattern area of its side's ingot surface concentrates on 60-80mm
2What the interval was interior accounts for 90%.The monocrystalline silicon piece of producing with the present invention is carried out minority carrier life time detect, the life-span concentrates in the 3-7 μ s scope, and mean lifetime is 4 μ s.
Claims (10)
1. the working method of a silicon single crystal ingot casting is characterized in that, may further comprise the steps:
A, seed crystal is positioned over according to identical crystal orientation in the seed slot of crucible bottom, in crucible, adds polycrystalline silicon material then and doping agent covers seed crystal;
B, crucible is placed ingot furnace, vacuumize the back and feed argon gas, polycrystalline silicon material under argon shield above the heat fused seed crystal and doping agent, and make the part seed crystal fusing near polycrystalline silicon material and doping agent, formation silicon melt;
C, adopt falling crucible method to impel silicon melt, induce the growth of accurate monocrystalline, finally form the silicon single crystal ingot casting by unfused seed crystal by the bottom directional freeze that makes progress;
Ingot is got in D, cooling.
2. the working method of silicon single crystal ingot casting according to claim 1 is characterized in that: the crystal orientation of described seed crystal is < 100 >.
3. the working method of silicon single crystal ingot casting according to claim 1 is characterized in that: described seed slot stretches out downwards from crucible bottom, and the height that is positioned over the seed crystal in the seed slot is higher than the height of seed slot.
4. the working method of silicon single crystal ingot casting according to claim 1 is characterized in that: described seed slot be shaped as cube shaped or the cylinder bodily form, corresponding seed crystal is shaped as cube shaped or the cylinder bodily form.
5. the working method of silicon single crystal ingot casting according to claim 1 is characterized in that: described crucible is the quartz ceramic crucible with silicon nitride coating.
6. the working method of silicon single crystal ingot casting according to claim 1 is characterized in that: described doping agent is boron, phosphorus or gallium.
7. the working method of silicon single crystal ingot casting according to claim 1 is characterized in that: the vacuum degree control that vacuumizes described in the step B is below 5Pa, and Heating temperature is for being heated to 1550 ℃.
8. the working method of silicon single crystal ingot casting according to claim 1 is characterized in that: during falling crucible method directional freeze described in the step C, the speed control that crucible descends is at 5-15mm/h, and adopts the recirculated water cooling in crucible bottom.
9. the working method of silicon single crystal ingot casting according to claim 3 is characterized in that: the height of the aspect ratio seed slot of described seed crystal exceeds 8-10mm.
10. the working method of silicon single crystal ingot casting according to claim 1 is characterized in that: described crucible is cube shaped or the cylinder bodily form, and its bottom is provided with funnel-shaped structure recessed down; Described seed slot is connected at the bottom of the bucket of this funnel-shaped structure.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103205798A (en) * | 2013-03-21 | 2013-07-17 | 南昌大学 | Method for manufacturing cast silicon and method for manufacturing solar cells by cast silicon solids |
| CN104047052A (en) * | 2013-03-11 | 2014-09-17 | 三菱综合材料株式会社 | Silicon member for semiconductor apparatus and method of producing same |
| CN104846435A (en) * | 2015-06-02 | 2015-08-19 | 江苏协鑫硅材料科技发展有限公司 | P type gallium-doped crystalline silicon and preparation method thereof |
| CN105648520A (en) * | 2016-03-18 | 2016-06-08 | 江苏中电振华晶体技术有限公司 | Seed crystal capable of reinforcing seeding temperature signals and seeding method thereof |
| CN112226809A (en) * | 2020-11-11 | 2021-01-15 | 浙江普智能源装备有限公司 | Crucible for ingot casting monocrystalline silicon |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201362752Y (en) * | 2009-03-23 | 2009-12-16 | 浙江碧晶科技有限公司 | Crucible used for growth of silicon single crystals |
| CN101928980A (en) * | 2010-09-17 | 2010-12-29 | 浙江碧晶科技有限公司 | Seeding guidance die for growing silicon crystal by directional solidification method |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201362752Y (en) * | 2009-03-23 | 2009-12-16 | 浙江碧晶科技有限公司 | Crucible used for growth of silicon single crystals |
| CN101928980A (en) * | 2010-09-17 | 2010-12-29 | 浙江碧晶科技有限公司 | Seeding guidance die for growing silicon crystal by directional solidification method |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104047052A (en) * | 2013-03-11 | 2014-09-17 | 三菱综合材料株式会社 | Silicon member for semiconductor apparatus and method of producing same |
| US9878915B2 (en) | 2013-03-11 | 2018-01-30 | Mitsubishi Materials Corporation | Silicon member for semiconductor apparatus and method of producing the same |
| CN104047052B (en) * | 2013-03-11 | 2018-10-19 | 三菱综合材料株式会社 | The manufacturing method of semiconductor device silicon parts and semiconductor device silicon parts |
| CN103205798A (en) * | 2013-03-21 | 2013-07-17 | 南昌大学 | Method for manufacturing cast silicon and method for manufacturing solar cells by cast silicon solids |
| CN103205798B (en) * | 2013-03-21 | 2016-02-24 | 南昌大学 | A kind of to cast the method for manufacturing solar battery that silicon entity is material |
| CN104846435A (en) * | 2015-06-02 | 2015-08-19 | 江苏协鑫硅材料科技发展有限公司 | P type gallium-doped crystalline silicon and preparation method thereof |
| CN105648520A (en) * | 2016-03-18 | 2016-06-08 | 江苏中电振华晶体技术有限公司 | Seed crystal capable of reinforcing seeding temperature signals and seeding method thereof |
| CN112226809A (en) * | 2020-11-11 | 2021-01-15 | 浙江普智能源装备有限公司 | Crucible for ingot casting monocrystalline silicon |
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Application publication date: 20121017 |