CN106987901A - A kind of crystalline silicon and preparation method thereof - Google Patents
A kind of crystalline silicon and preparation method thereof Download PDFInfo
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- CN106987901A CN106987901A CN201710200003.3A CN201710200003A CN106987901A CN 106987901 A CN106987901 A CN 106987901A CN 201710200003 A CN201710200003 A CN 201710200003A CN 106987901 A CN106987901 A CN 106987901A
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- 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
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- 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
- C30B27/00—Single-crystal growth under a protective fluid
-
- 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
Abstract
The invention provides a kind of preparation method of crystalline silicon, including：The silicon melt of molten condition is loaded in crucible, temperature is then adjusted, into crystal growing stage, during long crystalline substance, continue into crucible or be discontinuously passed through air until long crystalline substance terminates, the flow of the air is 1L/min 6L/min, after annealed cooling, crystalline silicon is obtained.The preparation method for the crystalline silicon that the present invention is provided, air is passed through by the crystal growing stage prepared in crystalline silicon, is reduced the carbon and content of carborundum impurities in crystalline silicon, is improved the volume recovery of crystalline silicon, reduces the dislocation of crystalline silicon.Present invention also offers a kind of crystalline silicon, the crystalline silicon dislocation is less, and minority carrier life time is higher, and quality is preferable.
Description
Technical field
The present invention relates to solar cell material technical field, and in particular to a kind of crystalline silicon and preparation method thereof.
Background technology
In recent years, solar energy has become the heat of people's R and D as a kind of emerging renewable green energy resource
Point.Along with the fast development of solar cell industry, cost it is low and suitable for large-scale production polysilicon or class monocrystalline silicon turn into
One of topmost photovoltaic material in industry, and progressively replace traditional pulling of silicon single crystal in solar cell material market
Leading position.
The insulation material in ingot furnace, heater for preparing crystalline silicon, the material such as breather pipe, cover plate is all carbon materials
Matter, during ingot casting, the small carbon particle volatilized at high temperature is easily accessible in crucible to react with silicon melt and generated
Carborundum hard impurity.On the one hand these impurity enter influences the volume recovery of silicon ingot in silicon ingot, on the other hand can also cause dislocation
Generation.Therefore, it is necessary to provide a kind of preparation method of new crystalline silicon.
The content of the invention
To solve the above problems, the invention provides a kind of preparation method of new crystalline silicon.The present invention is preparing crystal
The oxygen in air, air is introduced during silicon can reduce impurity content, and the nitrogen of air can reduce the propagation of dislocation.
The preparation method for the crystalline silicon that the present invention is provided, technique is simple to operation.
First aspect present invention provides a kind of preparation method of crystalline silicon, including：
The silicon melt of molten condition is loaded in crucible, temperature is then adjusted, into crystal growing stage, in the long brilliant process
In, continue into the crucible or be discontinuously passed through air until long crystalline substance terminates, the flow of the air is 1L/min-6L/
Min, after annealed cooling, obtains crystalline silicon.
Wherein, the flow of the air is 3L/min-4L/min.
Wherein, it is described be discontinuously passed through air operation be：The air is passed through once every 5min-60min, it is logical every time
The time entered is 5min-60min.
Wherein, it is described be discontinuously passed through air operation be：The air is passed through once every 10min-30min, every time
The time being passed through is 10min-30min.
Wherein, in the crystal growing stage, argon gas is continually fed into the crucible, the flow of the argon gas is 10L/
min-60L/min。
Wherein, the flow-rate ratio of the air and the argon gas is 1:1.67-1:60.
Wherein, in the crystal growing stage, the pressure in the crucible is 400mbar-800mbar.
Wherein, the air source is in air or compressed air.
The preparation method for the crystalline silicon that first aspect present invention is provided, sky is passed through by the crystal growing stage prepared in crystalline silicon
Gas, reduces the carbon and content of carborundum impurities in crystalline silicon, improves the volume recovery of crystalline silicon, reduce the position of crystalline silicon
It is wrong.
Second aspect of the present invention provides a kind of crystalline silicon, is made according to the preparation method described in above-mentioned first aspect.
Wherein, impurity fraction defective average out to is below 0.5% in the crystalline silicon, and minority carrier life time is less than 4 μ in the crystalline silicon
The average proportions that s region accounts for the whole crystalline silicon are less than 6%.
The crystalline silicon that second aspect of the present invention is provided, dislocation is less, and minority carrier life time is higher, and quality is preferable.
To sum up, beneficial effect of the present invention includes the following aspects：
1st, the preparation method for the crystalline silicon that the present invention is provided, is passed through air by the crystal growing stage prepared in crystalline silicon, subtracts
Lack the carbon and content of carborundum impurities in crystalline silicon, improved the volume recovery of crystalline silicon, reduce the dislocation of crystalline silicon；
2nd, the crystalline silicon that the present invention is provided, impurity is less, and crystalline silicon quality is preferable.
Brief description of the drawings
Fig. 1 is the impurity fraction defective of polycrystal silicon ingot made from embodiment 1；
Fig. 2 is the dislocation accounting of polycrystal silicon ingot made from embodiment 1；
Fig. 3 is the minority carrier life time figure of polycrystal silicon ingot made from embodiment 1.
Embodiment
As described below is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications are also considered as
Protection scope of the present invention.
Embodiment of the present invention first aspect provides a kind of preparation method of crystalline silicon, including：
The silicon melt of molten condition is loaded in crucible, temperature is then adjusted, into crystal growing stage, in the long brilliant process
In, continue into the crucible or be discontinuously passed through air until long crystalline substance terminates, the flow of the air is 1L/min-6L/
Min, after annealed cooling, obtains crystalline silicon.
In embodiment of the present invention, the operation of the silicon melt of molten condition is loaded in crucible to be included：Loaded in crucible
Silicon material, heating makes melting silicon materials formation silicon melt, or the silicon melt melted in another crucible is poured onto in the crucible.
In embodiment of the present invention, the crystalline silicon is class monocrystal silicon or polycrystal silicon ingot, when crystalline silicon is class monocrystalline silicon
During ingot, crucible bottom is provided with inculating crystal layer.The routine techniques that is set to of inculating crystal layer is selected, and particular determination is not done herein.Alternatively, when
When crystalline silicon is class monocrystal silicon, the operation that regulation temperature enters crystal growing stage includes：
Seed crystal formation inculating crystal layer is laid in crucible；The silicon melt of molten condition, control are set above the inculating crystal layer
The crucible bottom temperature is less than the fusing point of the seed crystal so that the inculating crystal layer is not completely melted；Regulation thermal field was formed
Cold state, makes the silicon melt start long crystalline substance on the basis of the inculating crystal layer and enters crystal growing stage.
In embodiment of the present invention, it is passed through and introduces air in crystal growing stage, normal composition of air is calculated by volume fraction
It is:Nitrogen (N2) account for 78%, oxygen (O2) account for 21%, rare gas account for 0.94% (helium He, neon Ne, argon Ar, krypton Kr, xenon Xe,
Radon Rn).Under the composition and volume fraction, the oxygen in air can at high temperature be carried out instead with entering the carbon particle in crucible
Should, carbon dioxide is generated, then carbon dioxide is carried out outside crucible, reduces the carbon and carborundum in crystalline silicon
Impurity content, so that the volume recovery of silicon ingot is improved, probability of the reduction silicon ingot in slicing processes interrupt line.In addition, the nitrogen in air
Gas being capable of pinning crystalline silicon Dislocations, the propagation of reduction dislocation.Alternatively, the air source is in air or compressed air.
Alternatively, the flow of the air is 3L/min-4L/min.The present invention can be effectively reduced crucible under the air mass flow
In impurity and be effectively reduced the propagation of dislocation.Still optionally further, the flow of the air is 4L/min-5L/min.Tool
Body, the flow of the air is 1L/min, 1.5L/min, 2L/min, 2.5L/min, 3L/min, 3.5L/min, 4L/min,
4.5L/min、5L/min、5.5L/min、6L/min.Alternatively, it is described be discontinuously passed through air operation be：Every 5min-
60min is passed through once the air, and the time being passed through every time is 5min-60min.Still optionally further, it is described to be discontinuously passed through
The operation of air is：The air is passed through once every 10min-30min, the time being passed through every time is 10min-30min.Enter one
Step alternatively, the air is passed through once every 5min-30min, and the time being passed through every time is 5min-30min.It is further optional
Ground, the air is passed through once every 30min-60min, and the time being passed through every time is 30min-60min.Specifically, every
5min, 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min, 60min are passed through one
The secondary air.Specifically, the time being passed through every time be 5min, 10min, 15min, 20min, 25min, 30min, 35min,
40min、45min、50min、55min、60min.Alternatively, after long crystalline substance terminates, stopping is passed through air, and subsequent technique is with conventional
Casting ingot process.
In embodiment of the present invention, in the crystal growing stage, argon gas is continually fed into the crucible, the argon gas
Flow is 10L/min-60L/min.Alternatively, the purity of argon gas is more than 99.99%.Argon gas is set to enter crucible together with air
In, it is filled with the effect mainly regulation furnace pressure of argon gas and carries the effect of the pernicious gas produced during ingot casting.When in air
Oxygen and crucible in carbon particle reaction production carbon dioxide after can by argon gas flowing carry out outside crucible.In crystalline silicon
Other preparatory phases can also be continually fed into argon gas.
In embodiment of the present invention, the flow-rate ratio of the air and the nitrogen is 1:1.67-1:60.In such flow
Than under the conditions of, the oxygen in air can both react with the carbon particle in crucible, it is to avoid carbon particle enters in silicon melt, meanwhile,
Air will not destroy the carbon insulation material in ingot furnace again.Alternatively, the flow-rate ratio of the air and the nitrogen is 1:1.67-
1:30.Alternatively, the flow-rate ratio of the air and the nitrogen is 1:30-1:60.Alternatively, the air and the nitrogen
Flow-rate ratio is 1:1.67、1:3、1:5、1:7、1:10、1:15、1:20、1:25、1:30、1:35、1:40、1:45、1:50、1:55、
1:60。
In embodiment of the present invention, in the crystal growing stage, the pressure in the crucible is 400mbar-800mbar.
Alternatively, the pressure that the furnace chamber is kept is 400,450,500,550,600,650,700,750,800mbar.Here in crucible
Pressure and the pressure of whole furnace chamber of ingot furnace be identical.
In embodiment of the present invention, the air is passed through by the surface position of the crucible.
The preparation method for the crystalline silicon that first aspect present invention is provided, sky is passed through by the crystal growing stage prepared in crystalline silicon
Gas, reduces the carbon and content of carborundum impurities in silicon ingot, improves the volume recovery of silicon ingot, reduce the dislocation of silicon ingot.
Embodiment of the present invention second aspect provides a kind of crystalline silicon, according to preparation method system as described in relation to the first aspect
.
In embodiment of the present invention, the impurity fraction defective average out to of the crystalline silicon is few in the crystalline silicon below 0.5%
The sub- life-span, to account for the ratio of the whole crystalline silicon be less than 6% to the region less than 4 μ s.Wherein, the definition of impurity fraction defective is institute
State influence to crystalline silicon volume recovery of carborundum impurity in crystalline silicon and cause the average down ratio of volume recovery.Such as crystalline silicon
Impurity fraction defective be less than 0.5% to mean that carborundum impurity is in crystalline silicon to the average influence of crystalline silicon volume recovery
Less than 0.5%, alternatively, the crystalline silicon includes polysilicon and class monocrystalline silicon, when crystalline silicon is polysilicon, the crystalline silicon
Impurity fraction defective average out to below 0.5%, region of the minority carrier life time less than 4 μ s accounts for the whole crystalline silicon in the crystalline silicon
Ratio be less than 6%；When crystalline silicon is class monocrystalline silicon, the impurity fraction defective average out to of the crystalline silicon is below 0.5%, institute
It is less than 4% to state the ratio that region of the minority carrier life time less than 4 μ s accounts for the whole crystalline silicon in crystalline silicon.
The crystalline silicon that second aspect of the present invention is provided, impurity is less, improves the volume recovery of crystalline silicon, reduces crystalline silicon
Dislocation, crystalline silicon quality is preferable.
The embodiment of the present invention third aspect provides a kind of ingot furnace for being used to prepare crystalline silicon, including crucible and setting
Gas passage above the crucible, the gas passage is provided with a lateral, and the lateral connects with air-source
Connect, for being passed through air to the crucible.
In embodiment of the present invention, alternatively, the lateral is provided with valve and flowmeter.When need not be to crucible
When being passed through air, valve is fastened, when needing to be passed through air to crucible, valve is opened.
In embodiment of the present invention, alternatively, gas passage is connected with argon gas source, for being passed through argon gas to the crucible.
The use process of ingot furnace of the present invention is：When entering crystal growing stage, the valve of lateral is opened, allows air to lead to
Cross gas pipeline to enter in crucible, the valve is closed after the time of being passed through when the air being passed through reaches, crystalline silicon is cooled down by annealing
Deng operation after complete ingot casting.
The ingot furnace for preparing crystalline silicon that third aspect present invention is provided, a branch is set in conventional ingot furnace
Pipeline is used to be passed through air to crucible, and structure is very simple, it is not necessary to larger change is carried out to ingot furnace, and will not shadow
Ring the application function of ingot furnace script.
Embodiment 1：
A kind of preparation method of polycrystal silicon ingot, including：
(1) silica crucible (internal diameter 840mm × 840mm) is taken, various block silicon materials are loaded in crucible.It is equipped with above-mentioned
The crucible of silicon material is fitted into ingot furnace, starts ingot casting program, vacuumizes and heat, be heated to silicon melting temperature, make silicon material slowly
It is fused into silicon melt.
(2) when silicon material is completely melt；Temperature edge in control crucible is gradually increasing perpendicular to crucible bottom upwardly direction
Thermograde is formed, into crystal growing stage, silicon melt starts long brilliant formation crystal；In crystal growing stage, continue into the crucible
Ground is passed through air until long crystalline substance terminates, while being passed through argon gas, the flow of air is 6L/min, and the flow of argon gas is 10L/min.
(3) after whole silicon melts have been crystallized, stopping is passed through air, and annealed cooling obtains polycrystal silicon ingot.
Embodiment 2：
The preparation method of one species monocrystal silicon, including：
(1) silica crucible (internal diameter 840mm × 840mm) is taken, seed crystal is laid in crucible bottom, the seed that thickness is 10mm is formed
Crystal layer, then loads various block silicon materials above inculating crystal layer.The above-mentioned crucible equipped with silicon material is fitted into ingot furnace, started
Ingot casting program, vacuumizes and heats, and is heated to silicon melting temperature, silicon material is slowly fused into silicon melt.
(2) control crucible bottom temperature is less than the fusing point of seed crystal so that inculating crystal layer is not completely melted；Control in crucible
Temperature perpendicular to crucible bottom upwardly direction along being gradually increasing to form thermograde, and into crystal growing stage, silicon melt is in seed crystal
On the basis of start long brilliant to form crystal；In crystal growing stage, air is constantly passed through into the crucible until long crystalline substance terminates, simultaneously
Argon gas is passed through, the flow of air is 1L/min, and the flow of argon gas is 60L/min.
(3) after whole silicon melts have been crystallized, stopping is passed through air, and annealed cooling obtains class monocrystal silicon.
Embodiment 3：
A kind of preparation method of polycrystal silicon ingot, including：
(1) silica crucible (internal diameter 840mm × 840mm) is taken, various block silicon materials are loaded in crucible.It is equipped with above-mentioned
The crucible of silicon material is fitted into ingot furnace, starts ingot casting program, vacuumizes and heat, be heated to silicon melting temperature, make silicon material slowly
It is fused into silicon melt.
(2) when silicon material is completely melt；Temperature edge in control crucible is gradually increasing perpendicular to crucible bottom upwardly direction
Thermograde is formed, into crystal growing stage, silicon melt starts long brilliant formation crystal；In crystal growing stage, continue into the crucible
Ground is passed through air until long crystalline substance terminates, while being passed through argon gas, the flow of air is 4L/min, and the flow of argon gas is 40L/min.
(3) after whole silicon melts have been crystallized, stopping is passed through air, and annealed cooling obtains polycrystal silicon ingot.
Embodiment 4：
A kind of preparation method of polycrystal silicon ingot, including：
(1) silica crucible (internal diameter 840mm × 840mm) is taken, various block silicon materials are loaded in crucible.It is equipped with above-mentioned
The crucible of silicon material is fitted into ingot furnace, starts ingot casting program, vacuumizes and heat, be heated to silicon melting temperature, make silicon material slowly
It is fused into silicon melt.
(2) when silicon material is completely melt；Temperature edge in control crucible is gradually increasing perpendicular to crucible bottom upwardly direction
Thermograde is formed, into crystal growing stage, silicon melt starts long brilliant formation crystal；In crystal growing stage, it is interrupted into the crucible
Ground is passed through air until long crystalline substance terminates, while being passed through argon gas, the flow of air is 3L/min, and primary air is passed through every 5min,
The time that is passed through of each air is 5min, and the flow of argon gas is 30L/min.
(3) after whole silicon melts have been crystallized, stopping is passed through air, and annealed cooling obtains polycrystal silicon ingot.
Embodiment 5：
A kind of preparation method of polycrystal silicon ingot, including：
(1) silica crucible (internal diameter 840mm × 840mm) is taken, various block silicon materials are loaded in crucible.It is equipped with above-mentioned
The crucible of silicon material is fitted into ingot furnace, starts ingot casting program, vacuumizes and heat, be heated to silicon melting temperature, make silicon material slowly
It is fused into silicon melt.
(2) when silicon material is completely melt；Temperature edge in control crucible is gradually increasing perpendicular to crucible bottom upwardly direction
Thermograde is formed, into crystal growing stage, silicon melt starts long brilliant formation crystal；In crystal growing stage, it is interrupted into the crucible
Ground is passed through air until long crystalline substance terminates, while being passed through argon gas, the flow of air is 5L/min, and primary air is passed through every 60min,
The time that is passed through of each air is 60min, and the flow of argon gas is 20L/min.
(3) after whole silicon melts have been crystallized, stopping is passed through air, and annealed cooling obtains polycrystal silicon ingot.
Embodiment 6：
A kind of preparation method of polycrystal silicon ingot, including：
(1) silica crucible (internal diameter 840mm × 840mm) is taken, various block silicon materials are loaded in crucible.It is equipped with above-mentioned
The crucible of silicon material is fitted into ingot furnace, starts ingot casting program, vacuumizes and heat, be heated to silicon melting temperature, make silicon material slowly
It is fused into silicon melt.
(2) when silicon material is completely melt；Temperature edge in control crucible is gradually increasing perpendicular to crucible bottom upwardly direction
Thermograde is formed, into crystal growing stage, silicon melt starts long brilliant formation crystal；In crystal growing stage, it is interrupted into the crucible
Ground is passed through air until long crystalline substance terminates, while being passed through argon gas, the flow of air is 4L/min, and primary air is passed through every 10min,
The time that is passed through of each air is 10min, and the flow of argon gas is 40L/min.
(3) after whole silicon melts have been crystallized, stopping is passed through air, and annealed cooling obtains polycrystal silicon ingot.
Embodiment 7：
A kind of preparation method of polycrystal silicon ingot, including：
(1) silica crucible (internal diameter 840mm × 840mm) is taken, various block silicon materials are loaded in crucible.It is equipped with above-mentioned
The crucible of silicon material is fitted into ingot furnace, starts ingot casting program, vacuumizes and heat, be heated to silicon melting temperature, make silicon material slowly
It is fused into silicon melt.
(2) when silicon material is completely melt；Temperature edge in control crucible is gradually increasing perpendicular to crucible bottom upwardly direction
Thermograde is formed, into crystal growing stage, silicon melt starts long brilliant formation crystal；In crystal growing stage, it is interrupted into the crucible
Ground is passed through air until long crystalline substance terminates, while being passed through argon gas, the flow of air is 5L/min, and primary air is passed through every 30min,
The time that is passed through of each air is 30min, and the flow of argon gas is 20L/min.
(3) after whole silicon melts have been crystallized, stopping is passed through air, and annealed cooling obtains polycrystal silicon ingot.
Effect example
To verify the effect of the embodiment of the present invention, the present invention is also provided with effect example.
Comparative example 1 is the conventional method for preparing polycrystal silicon ingot, and differing only in during ingot casting for embodiment 1 does not have
It is passed through air.
Polycrystal silicon ingot made from polycrystal silicon ingot made from embodiment 1 and comparative example 1 is subjected to the test of impurity fraction defective, dislocation
Accounting is tested and minority carrier lifetime.Wherein the test of impurity fraction defective is to be obtained using infrared acquisition (IR).Pass through infrared spy
Survey can detect the impure point in silico briquette.The position for having impure point need to be removed with band sawing, further according to the length being cut out
Divided by the theoretical length (theoretical can break area be excision minority carrier life time is less than 2 μ s end to end region) that can be cut into slices just is calculated
To impurity fraction defective.That ordinate is represented is one because of the removed length of impure point divided by the theoretical length computation that can be cut into slices
Percentage ratio, abscissa represents the silicon ingot number that same stove is continuously done, and each point represents an ingot.Dislocation accounting is tested
What the method according to Application No. 201210237553.X was tested.What ordinate was represented in Fig. 2 is low minority carrier life time region
(refer to minority carrier life time be more than 2 μ s be less than 4 μ s region) account for whole silico briquette can break area ratio (theoretical area of cutting into slices
Domain is the region that excision minority carrier life time is less than 2 μ s end to end).Abscissa represents the silicon ingot number that same ingot casting stove is continuously done, often
One point represents an ingot.Caused by low few subregion is mainly due to dislocation, so with this intuitive way come indirect table
Levy the height of dislocation.
Test result as Figure 1-3, wherein, Fig. 1 is the impurity fraction defective of polycrystal silicon ingot made from embodiment 1, and Fig. 2 is
The dislocation accounting of polycrystal silicon ingot made from embodiment 1, Fig. 3 is the minority carrier life time figure of polycrystal silicon ingot made from embodiment 1.From Fig. 1
In as can be seen that the vertical line left side the situation for not filling air for comparative example 1, the vertical line left side is the situation for being passed through air, can be seen
Go out, it can be seen that the impurity fraction defective of unaerated is 2% or so, the impurity fraction defective of inflation is less than 0.5%.It is passed through air
Polycrystal silicon ingot reach the purpose of carborundum hard impurity in reduction silicon ingot, so as to improve the volume recovery of silicon ingot, reduction is in section
During the probability that breaks.From figure 2 it can be seen that the situation for not filling air for comparative example 1 on the vertical line left side, the vertical line left side is
It is passed through the situation of air, it can be seen that minority carrier life time 2-4 μ s average accounting drops to less than 6% from 8%.Introduce micro
Nitrogen, nitrogen being capable of pinning silicon Dislocations, the increment of reduction dislocation.As can be seen from Figure 3, (A) is schemed wherein in Fig. 3 not fill air
The few subgraph of silico briquette, figure (B) is the few subgraph of silico briquette for filling air, it can be seen that few sub- longevity of silico briquette can be improved by being passed through air
Life.
To sum up, the oxygen that the embodiment of the present invention is passed through during polycrystal silicon ingot is prepared in air, air can be with entrance
Carbon particle in crucible is reacted at high temperature, generates carbon dioxide, and then carbon dioxide is carried out crucible,
The carbon and content of carborundum impurities in crystalline silicon are reduced, so as to improve the volume recovery of silicon ingot, reduction silicon ingot is in slicing processes
The probability of broken string.In addition, the nitrogen in air being capable of pinning crystalline silicon Dislocations, the propagation of reduction dislocation.
Embodiment described above only expresses the several embodiments of the present invention, and it describes more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of preparation method of crystalline silicon, it is characterised in that including：
The silicon melt of molten condition is loaded in crucible, temperature is then adjusted, into crystal growing stage, during the long crystalline substance,
Continue into the crucible or be discontinuously passed through air until long crystalline substance terminates, the flow of the air is 1L/min-6L/min, warp
After annealing cooling, crystalline silicon is obtained.
2. the preparation method of crystalline silicon as claimed in claim 2, it is characterised in that the flow of the air is 3L/min-4L/
min。
3. the preparation method of crystalline silicon as claimed in claim 1, it is characterised in that the operation for being discontinuously passed through air
For：The air is passed through once every 5min-60min, the time being passed through every time is 5min-60min.
4. the preparation method of crystalline silicon as claimed in claim 3, it is characterised in that the operation for being discontinuously passed through air
For：The air is passed through once every 10min-30min, the time being passed through every time is 10min-30min.
5. the preparation method of crystalline silicon as claimed in claim 1, it is characterised in that in the crystal growing stage, to the earthenware
Argon gas is continually fed into crucible, the flow of the argon gas is 10L/min-60L/min.
6. the preparation method of crystalline silicon as claimed in claim 1, it is characterised in that the flow-rate ratio of the air and the argon gas
For 1:1.67-1:60.
7. the preparation method of crystalline silicon as claimed in claim 1, it is characterised in that in the crystal growing stage, the crucible
Interior pressure is 400mbar-800mbar.
8. the preparation method of crystalline silicon as claimed in claim 1, it is characterised in that the air source is empty in air or compression
Gas.
9. a kind of crystalline silicon, it is characterised in that be made according to the preparation method as any one of claim 1-8.
10. crystalline silicon as claimed in claim 9, it is characterised in that the impurity fraction defective average out to 0.5% of the crystalline silicon with
Under, the average proportions that region of the minority carrier life time less than 4 μ s accounts for the whole crystalline silicon in the crystalline silicon are less than 6%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710200003.3A CN106987901A (en) | 2017-03-30 | 2017-03-30 | A kind of crystalline silicon and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710200003.3A CN106987901A (en) | 2017-03-30 | 2017-03-30 | A kind of crystalline silicon and preparation method thereof |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066762A (en) * | 2007-04-12 | 2007-11-07 | 宋德忠 | High purity silicon preparing oxygen and chlorine refining process and apparatus |
| CN101423220A (en) * | 2008-11-17 | 2009-05-06 | 上海普罗新能源有限公司 | Method for purifying and ingot casting multi-temperature zones silicon material and apparatus thereof |
| CN101597790A (en) * | 2009-06-24 | 2009-12-09 | 浙江大学 | The method of preparing cast polycrystalline silicon through melting silicon and doping nitrogen under nitrogen |
| CN101680110A (en) * | 2007-04-27 | 2010-03-24 | 弗赖贝格化合物原料有限公司 | Device and process for producing poly-crystalline or multi-crystalline silicon |
| CN201495107U (en) * | 2009-08-12 | 2010-06-02 | 管悦 | Polycrystal furnace with high-quality purification polysilicon |
| CN101850975A (en) * | 2009-04-01 | 2010-10-06 | 高文秀 | Method for purifying silicon by removing phosphorus and metal impurities |
| CN102336408A (en) * | 2011-03-31 | 2012-02-01 | 宜兴市昱元能源装备技术开发有限公司 | Novel method for purifying silicon |
| CN102807220A (en) * | 2011-05-31 | 2012-12-05 | 比亚迪股份有限公司 | Silicon purification method |
-
2017
- 2017-03-30 CN CN201710200003.3A patent/CN106987901A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066762A (en) * | 2007-04-12 | 2007-11-07 | 宋德忠 | High purity silicon preparing oxygen and chlorine refining process and apparatus |
| CN101680110A (en) * | 2007-04-27 | 2010-03-24 | 弗赖贝格化合物原料有限公司 | Device and process for producing poly-crystalline or multi-crystalline silicon |
| CN101423220A (en) * | 2008-11-17 | 2009-05-06 | 上海普罗新能源有限公司 | Method for purifying and ingot casting multi-temperature zones silicon material and apparatus thereof |
| CN101850975A (en) * | 2009-04-01 | 2010-10-06 | 高文秀 | Method for purifying silicon by removing phosphorus and metal impurities |
| CN101597790A (en) * | 2009-06-24 | 2009-12-09 | 浙江大学 | The method of preparing cast polycrystalline silicon through melting silicon and doping nitrogen under nitrogen |
| CN201495107U (en) * | 2009-08-12 | 2010-06-02 | 管悦 | Polycrystal furnace with high-quality purification polysilicon |
| CN102336408A (en) * | 2011-03-31 | 2012-02-01 | 宜兴市昱元能源装备技术开发有限公司 | Novel method for purifying silicon |
| CN102807220A (en) * | 2011-05-31 | 2012-12-05 | 比亚迪股份有限公司 | Silicon purification method |
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