CN108315813A - A kind of preparation method of polycrystalline silicon ingot casting - Google Patents
A kind of preparation method of polycrystalline silicon ingot casting Download PDFInfo
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- CN108315813A CN108315813A CN201810008373.1A CN201810008373A CN108315813A CN 108315813 A CN108315813 A CN 108315813A CN 201810008373 A CN201810008373 A CN 201810008373A CN 108315813 A CN108315813 A CN 108315813A
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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
- 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
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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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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Abstract
The present invention relates to a kind of preparation methods of polycrystalline silicon ingot casting, wherein includes the following steps：After silicon raw material is added into ingot furnace, the first preset time is persistently vacuumized, until the air pressure in stove is the first preset pressure；Continue to heat the second preset time, until in-furnace temperature is the first preset temperature；In-furnace temperature is increased to the second preset temperature, air pressure is gone up to the second preset pressure, and fusing operation third preset time is carried out；It is passed through hydrogeneous purified into stove, and the temperature in stove is set as third preset temperature, carries out the 4th preset time of long brilliant operation；Continue to be passed through the hydrogeneous purified, the temperature in stove is set as the 4th preset temperature, carries out the 5th preset time of annealing operation；In-furnace temperature is cooled to the 5th preset temperature, furnace pressure is gone up to third preset pressure, finished product is to obtain the polycrystalline silicon ingot casting in taking-up stove.The present invention improves the overall distribution uniformity of few son in silicon ingot, promotes crystal quality and transfer efficiency.
Description
Technical field
The present invention relates to technical field of crystal growth, more particularly to a kind of preparation method of polycrystalline silicon ingot casting.
Background technology
Since entering this century, photovoltaic industry becomes fastest-rising new high-tech industry in the world.It is all kinds of too
In positive energy battery, crystalline silicon (monocrystalline, polycrystalline) solar cell occupies extremely important status.
Currently, crystal silicon solar energy battery has occupied the share of 75% or more photovoltaic market.Crystal silicon solar energy battery
Opto-electronic conversion is realized using the photovoltaic effect of p~n knots.From the viewpoint of development, crystal silicon solar energy battery is not
A period of time to grow very much will occupy leading position.Due to the unique advantage of crystal silicon solar energy battery, in recent years to it
Application demand also rising year by year, therefore the growth-promoting industrialization production of solar cell.
In solar cells, polysilicon chip is one of those very important building block, wherein polysilicon chip
Total quality directly affects the transfer efficiency of solar cell.However, in existing polysilicon chip, there are still higher concentrations
Defect and impurity, defect itself and the impurity in fault location aggregation can form the complex centre of electron-hole, cause polycrystalline few
The problem of sub- service life reduction, few sub- distributing homogeneity is poor, bulk crystal mass deviation.
Invention content
Based on this, the purpose of the present invention is to solve in the prior art, there are the defects of higher concentration in polysilicon chip
And impurity, cause the reduction of polycrystalline minority carrier life time, the problem of few sub- distributing homogeneity difference.
The present invention proposes a kind of preparation method of polycrystalline silicon ingot casting, wherein includes the following steps：
After silicon raw material is added into ingot furnace, the first preset time is persistently vacuumized, until the air pressure in stove is first pre-
If air pressure；
Continue to heat the second preset time, until in-furnace temperature is the first preset temperature；
In-furnace temperature is increased to the second preset temperature, air pressure is gone up to the second preset pressure, and fusing operation third is carried out
Preset time；
It is passed through hydrogeneous purified into stove, and the temperature in stove is set as third preset temperature, carries out long brilliant operation the 4th
Preset time；
Continue to be passed through the hydrogeneous purified, the temperature in stove is set as the 4th preset temperature, carries out annealing operation the 5th
Preset time；
In-furnace temperature is cooled to the 5th preset temperature, furnace pressure is gone up to third preset pressure, is taken out in stove
Finished product is to obtain the polycrystalline silicon ingot casting.
Hydrogeneous purified is added in polycrystalline cast ingot process, in high temperature in the preparation method of polycrystalline silicon ingot casting proposed by the present invention
Under environment, the H and Si in hydrogeneous purified is chemically reacted, and forms covalent bond, barrier Si and other metals or it is nonmetallic it
Between reaction.Reduce the high concentration defect generated in crystal growing process and impurity, improves the uniformity of the growth of crystal, carry
Polycrystalline minority carrier life time is risen, few sub- overall distribution uniformity, crystal quality in silicon ingot is improved and is promoted, therefore polysilicon chip turns
Efficiency is changed to be obviously improved.The preparation method of polycrystalline silicon ingot casting proposed by the present invention, the overall distribution that few son in silicon ingot can be improved are equal
Even property promotes crystal quality and transfer efficiency.
The preparation method of the polycrystalline silicon ingot casting, wherein first preset time is 0.5~1h, and described first is default
Air pressure is less than 0.1mbar, and temperature when being vacuumized in the ingot furnace is less than 300 DEG C.
The preparation method of the polycrystalline silicon ingot casting, wherein second preset time is 4~8h, the described first default temperature
Degree is 1100 DEG C~1300 DEG C.
The preparation method of the polycrystalline silicon ingot casting, wherein second preset temperature is 1400 DEG C~1600 DEG C, described the
Two preset pressures are 400~600mbar, and the third preset time is 12~18h.
The preparation method of the polycrystalline silicon ingot casting, wherein the hydrogeneous purified is in hydrogen, silane, alkane or ammonia
At least one.
The preparation method of the polycrystalline silicon ingot casting, wherein the third preset temperature is 1400 DEG C~1420 DEG C, described the
Four preset times are 30~40h.
The preparation method of the polycrystalline silicon ingot casting, wherein the 4th preset temperature is 1300 DEG C~1370 DEG C, described the
Five preset times are 2~4h.
The preparation method of the polycrystalline silicon ingot casting, wherein the 5th preset temperature is 300 DEG C~500 DEG C, the third
Preset pressure is 950~1000mbar.
The preparation method of the polycrystalline silicon ingot casting, wherein described to include by the method that air pressure is gone up to the second preset pressure
Following steps：
Inert gas is passed through into the ingot furnace, the inert gas includes at least argon gas.
The preparation method of the polycrystalline silicon ingot casting, wherein the volume ratio of the hydrogeneous purified and the argon gas that are passed through
It is 1：550~650.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obviously, or practice through the invention is recognized.
Description of the drawings
Fig. 1 is the flow chart of the preparation method for the polycrystalline silicon ingot casting that first embodiment of the invention proposes；
Fig. 2 is the application effect figure of the preparation method for the polycrystalline silicon ingot casting that first embodiment of the invention proposes.
Specific implementation mode
To facilitate the understanding of the present invention, below with reference to relevant drawings to invention is more fully described.In attached drawing
Give the preferred embodiment of the present invention.But the present invention can realize in many different forms, however it is not limited to this paper institutes
The embodiment of description.On the contrary, purpose of providing these embodiments is make it is more thorough and comprehensive to the disclosure.
Unless otherwise defined, all of technologies and scientific terms used here by the article and belong to the technical field of the present invention
The normally understood meaning of technical staff is identical.Used term is intended merely to description tool in the description of the invention herein
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term " and or " used herein includes one or more phases
Any and all combinations of the Listed Items of pass.
In solar cells, polysilicon chip is one of those very important building block, wherein polysilicon chip
Total quality directly affects the transfer efficiency of solar cell.However, in existing polysilicon chip, there are still higher concentrations
Defect and impurity, defect itself and the impurity in fault location aggregation can form the complex centre of electron-hole, cause polycrystalline few
The problem of sub- service life reduction, few sub- distributing homogeneity is poor, bulk crystal mass deviation.
Embodiment one
In order to solve this technical problem, referring to Fig. 1, the present invention proposes a kind of preparation method of polycrystalline silicon ingot casting, institute
The method of stating includes the following steps：
S101 persistently vacuumizes the first preset time after silicon raw material is added into ingot furnace, until the air pressure in stove is the
One preset pressure.
Vacuumize operation：Specifically, the silicon raw material being passed through is pure silicon.The first preset time vacuumized be 0.5~
1h, vacuumizing the air pressure in rear ingot furnace should control in the first preset pressure.Wherein first preset pressure is less than
0.1mbar, the air pressure are similar to vacuum state.Herein it may also be noted that when being vacuumized, in the ingot furnace not into
Row heating, and the temperature in the ingot furnace need to be controlled and be less than 300 DEG C.
S102 continues to heat the second preset time, until in-furnace temperature is the first preset temperature.
Heating operation：Wherein, in this step, the vacuum state in above-mentioned ingot furnace need to be maintained, then proceed to heating 4~
8h, until the temperature in ingot furnace reaches 1100 DEG C~1300 DEG C.
In-furnace temperature is increased to the second preset temperature by S103, and air pressure is gone up to the second preset pressure, and fusing operation is carried out
Third preset time.
Melt operation：Ingot furnace is continued to heat so that the temperature in stove is increased to after 1400 DEG C~1600 DEG C, to this
Inert gas is passed through in ingot furnace.In the present embodiment, the inert gas being passed through is argon gas.It is passed through after argon gas so that the ingot furnace
Interior air pressure is gone up to 400~600mbar, so that the silicon raw material in the ingot furnace is melted.Wherein, melted when
Between be 12~18h.
S104 is passed through hydrogeneous purified into stove, and the temperature in stove is set as third preset temperature, carries out long brilliant operation
4th preset time.
Long crystalline substance operation：In long brilliant operation, hydrogeneous purified is passed through into ingot furnace, wherein the hydrogeneous purified can be
One kind in hydrogen, silane, alkane or ammonia.At the same time, it is 1400 DEG C~1420 DEG C to control the temperature in ingot furnace, then
Carry out 30~40h of long brilliant operation.In this respect it is to be noted that when being passed through above-mentioned hydrogeneous purified, it can be with inert gas
Argon gas is passed through together, it is only necessary to control the volume ratio between hydrogeneous purified and argon gas.In the present embodiment, it is passed through
The volume ratio of hydrogeneous purified and argon gas is 1：550~650.Herein it may also be noted that in this step, in ingot furnace
Air pressure is also required to control between 400~600mbar.
S105 continues to be passed through the hydrogeneous purified, and the temperature in stove is set as the 4th preset temperature, carries out annealing operation
5th preset time.
Annealing operation：In this step, continue to be passed through above-mentioned hydrogeneous purified.Wherein, the temperature in ingot furnace is controlled
It it is 1300 DEG C~1370 DEG C, compared in above-mentioned long brilliant operation, the temperature in this step in ingot furnace has occurred to a certain degree
Decline.Temperature control after preset temperature, is being subjected to 2~4h of annealing operation.Herein it may also be noted that in this step
In rapid, the air pressure in ingot furnace is also required to control between 400~600mbar.
In-furnace temperature is cooled to the 5th preset temperature, furnace pressure is gone up to third preset pressure by S106, is taken out
Finished product is to obtain the polycrystalline silicon ingot casting in stove.
Cooling operations：In this step, it needs the temperature in ingot furnace being cooled to 300 DEG C~500 DEG C, then to ingot casting
Argon gas is passed through in stove so that the air pressure in the ingot furnace is gone up to 950~1000mbar.It is normal to wait for that the air pressure in ingot furnace is gone up
Afterwards, just polycrystalline silicon ingot casting is taken out from the ingot furnace.
Referring to Fig. 2, Fig. 2 is the polycrystalline silicon ingot casting applied obtained by the preparation method of polycrystalline silicon ingot casting proposed by the present invention
Performance characterization figure, in conjunction in Fig. 2 it can be seen that：H and Si is chemically reacted under high temperature environment, polycrystalline minority carrier life time by
6.86-6.88 μ s are promoted to 7.00-7.02 μ s, and the PL defective values in silicon chip drop to 1.19 by 1.79, the conversion of polysilicon chip
Efficiency is promoted to 18.72% by 18.69%.
In conclusion by it was verified that minority carrier life time promotes 0.1 μ s or more, Defect value reduces by 32%, and silicon chip turns
Change 0.03% or more improved efficiency, hence it is evident that improve the quality of polysilicon chip.
Hydrogeneous purified is added in polycrystalline cast ingot process, in high temperature in the preparation method of polycrystalline silicon ingot casting proposed by the present invention
Under environment, the H and Si in hydrogeneous purified is chemically reacted, and forms covalent bond, barrier Si and other metals or it is nonmetallic it
Between reaction.Reduce the high concentration defect generated in crystal growing process and impurity, improves the uniformity of the growth of crystal, carry
Polycrystalline minority carrier life time is risen, few sub- overall distribution uniformity, crystal quality in silicon ingot is improved and is promoted, therefore polysilicon chip turns
Efficiency is changed to be obviously improved.The preparation method of polycrystalline silicon ingot casting proposed by the present invention, the overall distribution that few son in silicon ingot can be improved are equal
Even property promotes crystal quality and transfer efficiency.
Embodiment two
Second embodiment of the invention proposes that a kind of preparation method of polycrystalline silicon ingot casting, the preparation method include the following steps：
(1) operation is vacuumized：After silicon raw material is added into ingot furnace, 0.5h is persistently vacuumized, until the air pressure in stove is small
In 0.1mbar.
Herein it may also be noted that when being vacuumized, without heating in the ingot furnace, and the ingot casting need to be controlled
Temperature in stove is less than 300 DEG C.
(2) heating operation：The vacuum state in ingot furnace is maintained, ingot furnace is continued to heat 4h, until in ingot furnace
Temperature is 1100 DEG C.
(3) operation is melted：Ingot casting in-furnace temperature is increased to 1400 DEG C, and is passed through argon gas and so that air pressure is gone up in ingot furnace
To 400mbar, fusing operation 12h is carried out.
(4) long brilliant operation：It is passed through hydrogen into ingot furnace, and the temperature in ingot furnace is regulated to 1400 DEG C, is grown
Brilliant operation 30h.
In this respect it is to be noted that when being passed through hydrogen, can be passed through together with inert gas argon gas, it is only necessary to control
Volume ratio between hydrogeneous purified and argon gas.In the present embodiment, the volume ratio of the hydrogeneous purified and argon gas that are passed through
It is 1：550.Herein it may also be noted that in this step, the air pressure in ingot furnace is also required to control in 400mbar.
(5) annealing operation：Continue to be passed through hydrogen, the temperature in ingot furnace is set as 1300 DEG C, carries out annealing operation 2h.
Herein it may also be noted that in this step, the air pressure in ingot furnace is also required to control in 400mbar.
(6) cooling operations：Temperature in ingot furnace is cooled to 300 DEG C, continues to be passed through argon gas into ingot furnace, it will be in stove
Pressure is gone up to 950mbar, takes out in ingot furnace finished product to obtain polycrystalline silicon ingot casting.
Polycrystalline silicon ingot casting made from the present embodiment, polycrystalline minority carrier life time are promoted to 7.00 μ s, the PL in silicon chip by 6.86 μ s
Defective value drops to 1.19 by 1.79, and the transfer efficiency of polysilicon chip is promoted to 18.73% by 18.68%
Embodiment three
Third embodiment of the invention proposes that a kind of preparation method of polycrystalline silicon ingot casting, the preparation method include the following steps：
(1) operation is vacuumized：After silicon raw material is added into ingot furnace, 1h is persistently vacuumized, until the air pressure in stove is less than
0.1mbar。
Herein it may also be noted that when being vacuumized, without heating in the ingot furnace, and the ingot casting need to be controlled
Temperature in stove is less than 300 DEG C.
(2) heating operation：The vacuum state in ingot furnace is maintained, ingot furnace is continued to heat 8h, until in ingot furnace
Temperature is 1300 DEG C.
(3) operation is melted：Ingot casting in-furnace temperature is increased to 1600 DEG C, and is passed through argon gas and so that air pressure is gone up in ingot furnace
To 600mbar, fusing operation 18h is carried out.
(4) long brilliant operation：It is passed through hydrogen into ingot furnace, and the temperature in ingot furnace is regulated to 1420 DEG C, is grown
Brilliant operation 40h.
In this respect it is to be noted that when being passed through hydrogen, can be passed through together with inert gas argon gas, it is only necessary to control
Volume ratio between hydrogeneous purified and argon gas.In the present embodiment, the volume ratio of the hydrogen and argon gas that are passed through is 1：
650.Herein it may also be noted that in this step, the air pressure in ingot furnace is also required to control in 600mbar.
(5) annealing operation：Continue to be passed through hydrogen, the temperature in ingot furnace is set as 1370 DEG C, carries out annealing operation 4h.
Herein it may also be noted that in this step, the air pressure in ingot furnace is also required to control in 600mbar.
(6) cooling operations：Temperature in ingot furnace is cooled to 500 DEG C, continues to be passed through argon gas into ingot furnace, it will be in stove
Pressure is gone up to 1000mbar, takes out in ingot furnace finished product to obtain polycrystalline silicon ingot casting.
Polycrystalline silicon ingot casting made from the present embodiment, polycrystalline minority carrier life time are promoted to 7.01 μ s, the PL in silicon chip by 6.87 μ s
Defective value drops to 1.20 by 1.78, and the transfer efficiency of polysilicon chip is promoted to 18.73% by 18.68%.
Example IV
Fourth embodiment of the invention proposes that a kind of preparation method of polycrystalline silicon ingot casting, the preparation method include the following steps：
(1) operation is vacuumized：After silicon raw material is added into ingot furnace, 0.75h is persistently vacuumized, until the air pressure in stove is small
In 0.1mbar.
Herein it may also be noted that when being vacuumized, without heating in the ingot furnace, and the ingot casting need to be controlled
Temperature in stove is less than 300 DEG C.
(2) heating operation：The vacuum state in ingot furnace is maintained, ingot furnace is continued to heat 6h, until in ingot furnace
Temperature is 1200 DEG C.
(3) operation is melted：Ingot casting in-furnace temperature is increased to 1500 DEG C, and is passed through argon gas and so that air pressure is gone up in ingot furnace
To 500mbar, fusing operation 15h is carried out.
(4) long brilliant operation：It is passed through hydrogen into ingot furnace, and the temperature in ingot furnace is regulated to 1410 DEG C, is grown
Brilliant operation 35h.
In this respect it is to be noted that when being passed through hydrogen, can be passed through together with inert gas argon gas, it is only necessary to control
Volume ratio between hydrogeneous purified and argon gas.In the present embodiment, the volume ratio of the hydrogen and argon gas that are passed through is 1：
575.Herein it may also be noted that in this step, the air pressure in ingot furnace is also required to control in 500mbar.
(5) annealing operation：Continue to be passed through hydrogen, the temperature in ingot furnace is set as 1335 DEG C, carries out annealing operation 3h.
Herein it may also be noted that in this step, the air pressure in ingot furnace is also required to control in 500mbar.
(6) cooling operations：Temperature in ingot furnace is cooled to 400 DEG C, continues to be passed through argon gas into ingot furnace, it will be in stove
Pressure is gone up to 1000mbar, takes out in ingot furnace finished product to obtain polycrystalline silicon ingot casting.
Polycrystalline silicon ingot casting made from the present embodiment, polycrystalline minority carrier life time are promoted to 7.02 μ s, the PL in silicon chip by 6.88 μ s
Defective value drops to 1.19 by 1.78, and the transfer efficiency of polysilicon chip is promoted to 18.75% by 18.66%.
Embodiment five
Fifth embodiment of the invention proposes that a kind of preparation method of polycrystalline silicon ingot casting, the preparation method include the following steps：
(1) operation is vacuumized：After silicon raw material is added into ingot furnace, 0.75h is persistently vacuumized, until the air pressure in stove is small
In 0.1mbar.
Herein it may also be noted that when being vacuumized, without heating in the ingot furnace, and the ingot casting need to be controlled
Temperature in stove is less than 300 DEG C.
(2) heating operation：The vacuum state in ingot furnace is maintained, ingot furnace is continued to heat 6h, until in ingot furnace
Temperature is 1200 DEG C.
(3) operation is melted：Ingot casting in-furnace temperature is increased to 1500 DEG C, and is passed through argon gas and so that air pressure is gone up in ingot furnace
To 500mbar, fusing operation 15h is carried out.
(4) long brilliant operation：It is passed through ammonia into ingot furnace, and the temperature in ingot furnace is regulated to 1410 DEG C, is grown
Brilliant operation 35h.
In this respect it is to be noted that when being passed through ammonia, can be passed through together with inert gas argon gas, it is only necessary to control
Volume ratio between ammonia and argon gas.In the present embodiment, the volume ratio of the ammonia and argon gas that are passed through is 1：575.Herein
It may also be noted that in this step, the air pressure in ingot furnace is also required to control in 500mbar.
(5) annealing operation：Continue to be passed through ammonia, the temperature in ingot furnace is set as 1335 DEG C, carries out annealing operation 3h.
Herein it may also be noted that in this step, the air pressure in ingot furnace is also required to control in 500mbar.
(6) cooling operations：Temperature in ingot furnace is cooled to 400 DEG C, continues to be passed through argon gas into ingot furnace, it will be in stove
Pressure is gone up to 1000mbar, takes out in ingot furnace finished product to obtain polycrystalline silicon ingot casting.
Polycrystalline silicon ingot casting made from the present embodiment, polycrystalline minority carrier life time are promoted to 7.01 μ s, the PL in silicon chip by 6.87 μ s
Defective value drops to 1.19 by 1.79, and the transfer efficiency of polysilicon chip is promoted to 18.74% by 18.68%.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore 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, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.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 polycrystalline silicon ingot casting, which is characterized in that include the following steps：
After silicon raw material is added into ingot furnace, the first preset time is persistently vacuumized, until the air pressure in stove is the first default gas
Pressure；
Continue to heat the second preset time, until in-furnace temperature is the first preset temperature；
In-furnace temperature is increased to the second preset temperature, air pressure is gone up to the second preset pressure, and it is default to carry out fusing operation third
Time；
It is passed through hydrogeneous purified into stove, and the temperature in stove is set as third preset temperature, it is default to carry out long brilliant operation the 4th
Time；
Continue to be passed through the hydrogeneous purified, the temperature in stove is set as the 4th preset temperature, it is default to carry out annealing operation the 5th
Time；
In-furnace temperature is cooled to the 5th preset temperature, furnace pressure is gone up to third preset pressure, takes out finished product in stove
To obtain the polycrystalline silicon ingot casting.
2. the preparation method of polycrystalline silicon ingot casting according to claim 1, which is characterized in that first preset time is
0.5~1h, first preset pressure are less than 0.1mbar, and temperature when being vacuumized in the ingot furnace is less than 300 DEG C.
3. the preparation method of polycrystalline silicon ingot casting according to claim 2, which is characterized in that second preset time is 4
~8h, first preset temperature are 1100 DEG C~1300 DEG C.
4. the preparation method of polycrystalline silicon ingot casting according to claim 3, which is characterized in that second preset temperature is
1400 DEG C~1600 DEG C, second preset pressure is 400~600mbar, and the third preset time is 12~18h.
5. the preparation method of polycrystalline silicon ingot casting according to claim 1, which is characterized in that the hydrogeneous purified is hydrogen
At least one of gas, silane, alkane or ammonia.
6. the preparation method of polycrystalline silicon ingot casting according to claim 5, which is characterized in that the third preset temperature is
1400 DEG C~1420 DEG C, the 4th preset time is 30~40h.
7. the preparation method of polycrystalline silicon ingot casting according to claim 1, which is characterized in that the 4th preset temperature is
1300 DEG C~1370 DEG C, the 5th preset time is 2~4h.
8. the preparation method of polycrystalline silicon ingot casting according to claim 1, which is characterized in that the 5th preset temperature is
300 DEG C~500 DEG C, the third preset pressure is 950~1000mbar.
9. the preparation method of polycrystalline silicon ingot casting according to claim 1, which is characterized in that described that air pressure is gone up to second
The method of preset pressure includes the following steps：
Inert gas is passed through into the ingot furnace, the inert gas includes at least argon gas.
10. the preparation method of polycrystalline silicon ingot casting according to claim 9, which is characterized in that the hydrogeneous purifying being passed through
The volume ratio of object and the argon gas is 1：550~650.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN109750354A (en) * | 2019-03-28 | 2019-05-14 | 浙江晶科能源有限公司 | A kind of silicon wafer casting ingot method, silicon ingot and polysilicon chip |
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