CN106854774A - One species monocrystal silicon and preparation method thereof and a species monocrystalline silicon cast ingot stove - Google Patents
One species monocrystal silicon and preparation method thereof and a species monocrystalline silicon cast ingot stove Download PDFInfo
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- CN106854774A CN106854774A CN201611269682.1A CN201611269682A CN106854774A CN 106854774 A CN106854774 A CN 106854774A CN 201611269682 A CN201611269682 A CN 201611269682A CN 106854774 A CN106854774 A CN 106854774A
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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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
-
- 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
Abstract
The invention discloses the preparation method of a species monocrystal silicon, including：Seed crystal is laid in crucible and forms inculating crystal layer；The silicon melt of molten condition, fusing point of the control crucible bottom temperature less than seed crystal so that inculating crystal layer is not completely melted are set above inculating crystal layer；Regulation thermal field forms supercooled state, silicon melt is started crystalline substance long on the basis of inculating crystal layer；During crystalline substance long, continued with 1 rev/min 60 revs/min of mixing speed or discontinuously stir silicon melt；After whole silicon melts have been crystallized, annealed cooling obtains class monocrystal silicon.The preparation method of the class monocrystal silicon that the present invention is provided, silicon melt is stirred by during crystalline substance long, strengthens the convection current of silicon melt, metal impurities can be so reduced to enter in class monocrystal silicon, the enrichment of impurity is reduced, the minority carrier life time of silicon ingot is improved, the monocrystalline area of casting class monocrystalline is also improved.Present invention also offers using class monocrystal silicon obtained in the preparation method, present invention also offers a species monocrystalline silicon cast ingot stove.
Description
Technical field
The present invention relates to field of semiconductor manufacture, more particularly to a species monocrystal silicon and preparation method thereof and a species list
Crystal silicon ingot furnace.
Background technology
At present, production casting class single crystal process is mainly in crucible bottom place mat single crystal seed, by taking G5 silicon ingots as an example, seed crystal
Size is that 156mm is long and 156mm is wide, is highly 30mm, by 25 pieces of seed crystals in the way of 5 × 5 place mat internal diameter 840mm it is long and
In crucible 840mm wide.Then silicon material is loaded above seed crystal, control temperature melts silicon material and forms silicon melt from top to bottom, when
After being melted to single crystal seed layer position, cooling enters crystal growing stage, and class list is grown on the single crystal seed layer of incomplete fusing
It is brilliant.
In existing casting class single crystal technology, silicon melt carries out free convection, causes during crystal growth, and impurity is easy
The accumulation of impurity occurs in solid liquid interface silicon melt side, one layer of impurity enriched layer is formed.Problems with can so be brought：
(1) metal impurities, particularly transition metal impurity are easily accessible in silicon crystal, can influence the minority carrier life time of silicon ingot, so that shadow
Ring the electrical property of silicon chip.(2) solid-state do not melt that impurity (silicon nitride, carborundum, silica etc.) is easily enriched at solid-liquid crystal face can be into
It is nucleating center, so as to produce the polycrystalline of other crystal orientation, can so influences to cast the monocrystalline area of class monocrystalline, so as to influence silicon
The quality of piece.
Therefore, it is necessary to provide a kind of preparation method of new class monocrystal silicon.
The content of the invention
In consideration of it, the invention provides the preparation method of a species crystal silicon ingot, the preparation method can strengthen the right of silicon melt
Stream, reduces the enrichment of impurity, the monocrystalline area of casting class monocrystalline is improved, while the method is simple to operation.The present invention is also simultaneously
Disclose a kind of class monocrystal silicon obtained by the preparation method, and a species monocrystalline silicon cast ingot stove.
Embodiment of the present invention first aspect provides the preparation method of a species monocrystal silicon, including：
Seed crystal is laid in crucible and forms inculating crystal layer；The silicon melt of molten condition, control are set above the inculating crystal layer
Fusing point of the crucible bottom temperature less than the seed crystal so that the inculating crystal layer is not completely melted；
Regulation thermal field forms supercooled state, the silicon melt is started crystalline substance long on the basis of the inculating crystal layer；The length
During crystalline substance, continued with 1 rev/min -60 revs/min of mixing speed or discontinuously stir the silicon melt；
After whole silicon melts have been crystallized, annealed cooling obtains class monocrystal silicon.
In embodiment of the present invention, during the crystalline substance long, the silicon melt is stirred, the convection current of silicon melt can be strengthened,
Metal impurities can so be reduced to enter in class monocrystal silicon, the enrichment of impurity is reduced, the minority carrier life time of silicon ingot is improved, also reduced
The probability that forming core is enriched with solid-liquid crystal face of impurity is not melted, improves the monocrystalline area of casting class monocrystalline.
Alternatively, the mixing speed is 20 revs/min -50 revs/min.
Alternatively, it is described discontinuously stir the silicon melt mode be：A silicon melt is stirred every 5min-1h, often
Secondary mixing time is 1min-1h.
Alternatively, the silicon melt is stirred using agitating device, during stirring, the agitating device is gradually increasing, it is described on
The speed for rising is more than or equal to the brilliant speed long.
Alternatively, in whipping process, the agitating device crystallizes the silicon wafer to be formed with the inculating crystal layer or the silicon melt
The vertical range of body is 2-6cm.
The preparation method of the class monocrystal silicon that first aspect present invention is provided, by when crystal growth, will stir
Device is stirred in extending into silicon melt, strengthens the convection current of silicon melt, can so reduce metal impurities into class monocrystalline silicon
In ingot, the enrichment of impurity is reduced, improve the minority carrier life time of silicon ingot, it is also possible to reduce the enrichment shape at solid-liquid crystal face for not melting impurity
The probability of core, improves the monocrystalline area of casting class monocrystalline.Meanwhile, the preparation side of class monocrystal silicon provided in an embodiment of the present invention
Method is simple to operation.
Embodiment of the present invention second aspect provides a species monocrystal silicon, and the class monocrystal silicon is according to such as first aspect
Described preparation method is obtained.
The class monocrystal silicon that embodiment of the present invention second aspect is provided, impurity is less, and minority carrier life time is higher, the list of class monocrystalline
Crystal face product is larger.
Refering to Fig. 1, the embodiment of the present invention third aspect provides a species monocrystalline silicon cast ingot stove, including ingot casting furnace body and
Agitating device, the ingot casting furnace body includes crucible, and the agitating device includes agitator and drives the agitator motion
Drive device, the agitator is stretched into for the silicon melt stirred in the crucible in the crucible, and the drive device is set
On ingot casting furnace body.
Alternatively, the agitator includes agitating paddle, and the length of the agitating paddle is 30cm-80cm.
Alternatively, the agitator is connected by a connecting rod with the drive device.
Alternatively, the agitator is pollution-free to silicon melt, and fusing point is more than silicon.
The class monocrystalline silicon cast ingot stove that third aspect present invention is provided, by increasing an agitating device on ingot furnace,
When crystal growth, agitator is extend into silicon melt and is stirred, strengthen the convection current of silicon melt, can so reduce gold
Category impurity enter class monocrystal silicon in, reduce impurity enrichment, improve silicon ingot minority carrier life time, do not reduce molten yet impurity admittedly
The probability of forming core is enriched with liquid crystal surface, the monocrystalline area of casting class monocrystalline is improve.Meanwhile, the agitating device simple structure, easily
In operation.
Implement the embodiment of the present invention, have the advantages that：
(1) preparation method of the class monocrystal silicon that the present invention is provided, when crystal growth, stirs silicon melt, enhancing
The convection current of silicon melt, reduce impurity enrichment, improve silicon ingot minority carrier life time, cannot not also reduce moltenly impurity at solid-liquid crystal face
The probability of forming core is enriched with, the monocrystalline area of casting class monocrystalline is improve；Meanwhile, the method is simple to operation；
(2) impurity of the class monocrystal silicon that the present invention is provided is less, and minority carrier life time is higher, the monocrystalline area of class monocrystalline compared with
Greatly；
(3) the class monocrystalline silicon cast ingot stove that the present invention is provided, by increasing an agitating device on ingot furnace, in crystal life
When long, agitator extend into silicon melt and is stirred, strengthen the convection current of silicon melt, reduce the enrichment of impurity, improved
The monocrystalline area of casting class monocrystalline.Meanwhile, the agitating device simple structure, it is easy to operate.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will to embodiment or
The accompanying drawing to be used needed for description of the prior art is briefly described, it should be apparent that, drawings in the following description are only
Some embodiments of the present invention, for those of ordinary skill in the art, without having to pay creative labor, also
Other accompanying drawings can be obtained according to these accompanying drawings.
The structural representation of the class monocrystalline silicon cast ingot stove that Fig. 1 is provided for an embodiment of the present invention；
Embodiment 2 and the minority carrier life time figure of class monocrystal silicon obtained in comparative example 1 that Fig. 2 is provided for comparative example of the present invention；
Embodiment 2 and the silicon chip outside drawing of class monocrystal silicon obtained in comparative example 1 that Fig. 3 is provided for comparative example of the present invention.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Embodiment of the present invention first aspect provides the preparation method of a species monocrystal silicon, including：
Seed crystal is laid in crucible and forms inculating crystal layer；The silicon melt of molten condition, control are set above the inculating crystal layer
Fusing point of the crucible bottom temperature less than the seed crystal so that the inculating crystal layer is not completely melted；
Regulation thermal field forms supercooled state, the silicon melt is started crystalline substance long on the basis of the inculating crystal layer；The length
During crystalline substance, continued with 1 rev/min -60 revs/min of mixing speed or discontinuously stir the silicon melt；
After whole silicon melts have been crystallized, annealed cooling obtains class monocrystal silicon.
In embodiment of the present invention, during into crystal growing stage, the silicon melt is stirred, the convection current of silicon melt can be strengthened,
Metal impurities can so be reduced to enter in class monocrystal silicon, the enrichment of impurity is reduced, the few sub- longevity of class monocrystal silicon is improve
Life, cannot not also reduce moltenly the probability that forming core is enriched with solid-liquid crystal face of impurity, improve the monocrystalline area of casting class monocrystalline.
In embodiment of the present invention, stirring can be started into crystal growing stage.Stirring silicon melt can be continued until long brilliant
Soon terminate, it is also possible to discontinuously stir silicon melt.
In embodiment of the present invention, crucible scribbles the crucible of silicon nitride coating for inwall.Specific set-up mode is that industry is normal
Rule selection, will not be described here.
In embodiment of the present invention, alternatively, seed crystal is seed of single crystal silicon.Alternatively, the thickness of inculating crystal layer is 10mm-
30mm。
In embodiment of the present invention, alternatively, mixing speed is 20 revs/min -50 revs/min.Alternatively, mixing speed
It is 1 rev/min -20 revs/min.Still optionally further, mixing speed is 30 revs/min -50 revs/min.Specifically, speed is stirred
Degree can for 1,2,3,4,5,6,7,8,9,10,11,12,13,14,15,16,17,18,19,20,21,22,23,24,25,26,
27、28、29、30、31、32、33、34、35、36、37、38、39、40、41、42、43、44、45、46、47、48、49、50、51、
52nd, 53,54,55,56,57,58,59,60 revs/min.
Under the mixing speed of the embodiment of the present invention, can both strengthen the convection current of silicon melt, reduce the enrichment of impurity.Again may be used
To avoid, stirring intensity is larger to cause that convection intensity is too big, cause coming off for crucible silicon nitride coating.
In embodiment of the present invention, alternatively, it is described discontinuously stir the silicon melt mode be：Every 5min-1h
Silicon melt of stirring, each mixing time is 1min-1h.Still optionally further, a silicon is stirred every 30min-50min to melt
Body, each mixing time is 1min-1h.Still optionally further, a silicon melt is stirred every 30min-50min, every time stirring
Time is 30min-50min.Specifically, every 5min, 10min, 15min, 20min, 25min, 30min, 35min, 40min,
45min, 50min, 55min, 1h stir a silicon melt.Specifically, each mixing time be 1min, 5min, 10min,
15min、20min、25min、30min、35min、40min、45min、50min、55min、1h。
In embodiment of the present invention, alternatively, the silicon melt is stirred using agitating device, during stirring, the stirring dress
Put and be gradually increasing, the speed of the rising is more than or equal to the brilliant speed long.Still optionally further, the agitating device
The rate of climb is 15mm/h.
In embodiment of the present invention, in whipping process, the agitating device is crystallized with the inculating crystal layer or the silicon melt
The vertical range of the crystal of formation is 2-6cm.It is further preferred that agitating device is crystallized with the inculating crystal layer or the silicon melt
The vertical range of the crystal of formation is 3-5cm, specifically, the agitating device and the inculating crystal layer or the silicon melt crystalline
Into crystal vertical range for 2,3,4,5,6cm.During crystalline substance long, silicon melt crystallizes the silicon crystal of the certain altitude to be formed,
A certain distance is left between agitating device and inculating crystal layer or silicon crystal.Stirring can so be avoided to inculating crystal layer or silicon melt
Crystallize the silicon crystal for being formed and produce influence, while it also avoid agitating device scratches the crystal for having grown.
In embodiment of the present invention, when the height of uncrystallized silicon melt is 3-5cm, stop stirring.To can now stir
Mix device and rise to crucible top, the crystallization of silicon melt is not interfered with so.
The preparation method of the class monocrystal silicon that first aspect present invention is provided, during crystalline substance long, stirs silicon melt, enhancing
The convection current of silicon melt, can so reduce metal impurities and enter in class monocrystal silicon, reduce the enrichment of impurity, improve lacking for silicon ingot
The sub- life-span.The probability that forming core is enriched with solid-liquid crystal face of impurity cannot not be reduced moltenly, the monocrystalline area of casting class monocrystalline is improved yet.Together
When, the preparation method of class monocrystal silicon provided in an embodiment of the present invention is simple to operation.
Embodiment of the present invention second aspect provides a species monocrystal silicon, and the class monocrystal silicon is according to such as first aspect
Described preparation method is obtained.
The class monocrystal silicon that embodiment of the present invention second aspect is provided improves silicon ingot, and impurity is less, and minority carrier life time is higher, class
The monocrystalline area of monocrystalline is larger.
Refering to Fig. 1, the structural representation of the class monocrystalline silicon cast ingot stove that Fig. 1 is provided for an embodiment of the present invention；The present invention
The embodiment third aspect provides a species monocrystalline silicon cast ingot stove, including ingot casting furnace body 10 and agitating device 20, the ingot casting
Furnace body 10 includes crucible 11, and the agitating device 20 includes agitator 21 and drives the drive device of the agitator motion,
The agitator 21 is stretched into for the silicon melt stirred in the crucible 11 in the crucible 11, and the drive device is arranged on casting
On ingot furnace body 10.
In embodiment of the present invention mode, alternatively, drive device can be fixed on ingot casting furnace body by conventional methods, such as
Bolt fixation etc..Alternatively, drive device includes motor.Alternatively, the agitator 21 passes through a connecting rod 22 and the drive
Dynamic device connection.Specifically, one end of connecting rod 22 is connected with agitator 21, and the other end is connected with drive device.Alternatively, institute
Stating agitator 21 includes agitating paddle, and the length of the agitating paddle is less than the width of crucible, and specifically, the length of agitating paddle is
30cm-80cm.Alternatively, agitating paddle can be straight leaf, curved leaf or oblique leaf agitating paddle.Alternatively, the agitator is to the silicon
Melt is pollution-free, and fusing point is more than silicon.Specific alternatively the agitating paddle is pollution-free to silicon melt, and fusing point is more than silicon.Enter one
Alternatively, fusing point is more than 1560 DEG C to step, and specifically alternatively, the material of agitating paddle includes graphite, silicon nitride or carborundum.It is optional
Ground, in whipping process, the vertical range that the agitating paddle crystallizes the crystal to be formed with the inculating crystal layer or the silicon melt is 3-
5cm.Alternatively, agitating paddle can clockwise be stirred or stirred counterclockwise.Arrow represents the mixing direction of agitating device in Fig. 1,
Alternatively, the mixing direction of agitating device can also with figure arrow it is in opposite direction.
In embodiment of the present invention mode, the connecting rod can stretch up and down.The concrete structure of connecting rod can be conventional structure,
When need not stir, connecting rod is shunk the position not reached up to silicon melt, when stirring is needed, will be even
Extension bar extends, and agitating paddle is stirred in extending silicon melt.Specifically, in the melting stage, agitating paddle can rise to heater
Near, when crystal growing stage, agitating paddle drops to and continuously stirred in silicon melt or be spaced stirring.Alternatively, the connection
Bar is pollution-free to silicon melt, and fusing point is more than silicon.Still optionally further, connecting rod fusing point is more than 1560 DEG C, specifically alternatively, even
The material of extension bar includes graphite, silicon nitride or carborundum.Alternatively, connecting rod can stretch into crucible by the gas port on ingot furnace
It is interior.
The class monocrystalline silicon cast ingot stove that third aspect present invention is provided, by increasing an agitating device on ingot furnace,
When crystal growth, agitator is extend into silicon melt and is stirred, strengthen the convection current of silicon melt, reduce the richness of impurity
Collection.Metal impurities can so be reduced to enter in class monocrystal silicon, the minority carrier life time of silicon ingot is improved, impurity cannot not be also reduced moltenly
The probability of forming core is enriched with solid-liquid crystal face, the monocrystalline area of casting class monocrystalline is improved.Meanwhile, the agitating device simple structure,
It is easily operated.
Embodiment 1
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, form the seed that thickness is 10mm
Crystal layer, then loads the silicon material of various bulks above inculating crystal layer.The above-mentioned crucible equipped with silicon material is fitted into ingot furnace, is started
Ingot casting program, vacuumizes and heats, and is heated to silicon melting temperature, silicon material is slowly fused into silicon melt.
(2) fusing point of the control crucible bottom temperature less than seed crystal so that inculating crystal layer is not completely melted；In control crucible
, along being gradually increasing to form thermograde perpendicular to crucible bottom upwardly direction, into crystal growing stage, silicon melt is in seed crystal for temperature
On the basis of start long brilliant to form crystal；During crystalline substance long, silicon melt persistently being stirred using agitating device, mixing speed is 1 turn/
Minute；In whipping process, the rate of climb of agitating device is 15mm/h, and agitating device crystallizes to be formed with inculating crystal layer or silicon melt
Silicon crystal vertical range be 2cm；
(3) after silicon melt residue 3-5cm is not crystallized, stop stirring, agitating device is risen to from head heater 3cm
Place.Continue long brilliant, after whole silicon melts have been crystallized, annealed cooling obtains class monocrystal silicon.
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, form the seed that thickness is 20mm
Crystal layer, then loads the silicon material of various bulks above inculating crystal layer.The above-mentioned crucible equipped with silicon material is fitted into ingot furnace, is started
Ingot casting program, vacuumizes and heats, and is heated to silicon melting temperature, silicon material is slowly fused into silicon melt.
(2) fusing point of the control crucible bottom temperature less than seed crystal so that inculating crystal layer is not completely melted；In control crucible
, along being gradually increasing to form thermograde perpendicular to crucible bottom upwardly direction, into crystal growing stage, silicon melt is in seed crystal for temperature
On the basis of start long brilliant to form crystal；During crystalline substance long, silicon melt persistently being stirred using agitating device, mixing speed is 20 turns/
Minute；In whipping process, the rate of climb of agitating device is 15mm/h, and agitating device crystallizes to be formed with inculating crystal layer or silicon melt
Silicon crystal vertical range be 4cm；
(3) after silicon melt residue 3-5cm is not crystallized, stop stirring, agitating device is risen to from head heater 3cm
Place.Continue long brilliant, after whole silicon melts have been crystallized, annealed cooling obtains class monocrystal silicon.
Embodiment 3
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, form the seed that thickness is 30mm
Crystal layer, then loads the silicon material of various bulks above inculating crystal layer.The above-mentioned crucible equipped with silicon material is fitted into ingot furnace, is started
Ingot casting program, vacuumizes and heats, and is heated to silicon melting temperature, silicon material is slowly fused into silicon melt.
(2) fusing point of the control crucible bottom temperature less than seed crystal so that inculating crystal layer is not completely melted；In control crucible
, along being gradually increasing to form thermograde perpendicular to crucible bottom upwardly direction, into crystal growing stage, silicon melt is in seed crystal for temperature
On the basis of start long brilliant to form crystal；During crystalline substance long, silicon melt persistently being stirred using agitating device, mixing speed is 50 turns/
Minute；In whipping process, the rate of climb of agitating device is 15mm/h, and agitating device crystallizes to be formed with inculating crystal layer or silicon melt
Silicon crystal vertical range be 6cm；
(3) after silicon melt residue 3-5cm is not crystallized, stop stirring, agitating device is risen to from head heater 3cm
Place.Continue long brilliant, after whole silicon melts have been crystallized, annealed cooling obtains class monocrystal silicon.
Embodiment 4
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, form the seed that thickness is 30mm
Crystal layer, then loads the silicon material of various bulks above inculating crystal layer.The above-mentioned crucible equipped with silicon material is fitted into ingot furnace, is started
Ingot casting program, vacuumizes and heats, and is heated to silicon melting temperature, silicon material is slowly fused into silicon melt.
(2) fusing point of the control crucible bottom temperature less than seed crystal so that inculating crystal layer is not completely melted；In control crucible
, along being gradually increasing to form thermograde perpendicular to crucible bottom upwardly direction, into crystal growing stage, silicon melt is in seed crystal for temperature
On the basis of start long brilliant to form crystal；During crystalline substance long, silicon melt is discontinuously stirred using agitating device, mixing speed is 60
Rev/min；A silicon melt is stirred every 5min, each mixing time is 1min.In whipping process, the rising of agitating device
Speed is 15mm/h, and the vertical range that agitating device crystallizes the silicon crystal to be formed with inculating crystal layer or silicon melt is 3cm；
(3) after silicon melt residue 3-5cm is not crystallized, stop stirring, agitating device is risen to from head heater 3cm
Place.Continue long brilliant, after whole silicon melts have been crystallized, annealed cooling obtains class monocrystal silicon.
Embodiment 5
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, form the seed that thickness is 30mm
Crystal layer, then loads the silicon material of various bulks above inculating crystal layer.The above-mentioned crucible equipped with silicon material is fitted into ingot furnace, is started
Ingot casting program, vacuumizes and heats, and is heated to silicon melting temperature, silicon material is slowly fused into silicon melt.
(2) fusing point of the control crucible bottom temperature less than seed crystal so that inculating crystal layer is not completely melted；In control crucible
, along being gradually increasing to form thermograde perpendicular to crucible bottom upwardly direction, into crystal growing stage, silicon melt is in seed crystal for temperature
On the basis of start long brilliant to form crystal；During crystalline substance long, silicon melt is discontinuously stirred using agitating device, mixing speed is 30
Rev/min；A silicon melt is stirred every 1h, each mixing time is 1h.In whipping process, the rate of climb of agitating device
It is 15mm/h, the vertical range that agitating device crystallizes the silicon crystal to be formed with inculating crystal layer or silicon melt is 2cm；
(3) after silicon melt residue 3-5cm is not crystallized, stop stirring, agitating device is risen to from head heater 3cm
Place.Continue long brilliant, after whole silicon melts have been crystallized, annealed cooling obtains class monocrystal silicon.
Embodiment 6
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, form the seed that thickness is 25mm
Crystal layer, then loads the silicon material of various bulks above inculating crystal layer.The above-mentioned crucible equipped with silicon material is fitted into ingot furnace, is started
Ingot casting program, vacuumizes and heats, and is heated to silicon melting temperature, silicon material is slowly fused into silicon melt.
(2) fusing point of the control crucible bottom temperature less than seed crystal so that inculating crystal layer is not completely melted；In control crucible
, along being gradually increasing to form thermograde perpendicular to crucible bottom upwardly direction, into crystal growing stage, silicon melt is in seed crystal for temperature
On the basis of start long brilliant to form crystal；During crystalline substance long, silicon melt is discontinuously stirred using agitating device, mixing speed is 20
Rev/min；A silicon melt is stirred every 30min, each mixing time is 30min.In whipping process, agitating device it is upper
Lifting speed is 15mm/h, and the vertical range that agitating device crystallizes the silicon crystal to be formed with inculating crystal layer or silicon melt is 4cm；
(3) after silicon melt residue 3-5cm is not crystallized, stop stirring, agitating device is risen to from head heater 3cm
Place.Continue long brilliant, after whole silicon melts have been crystallized, annealed cooling obtains class monocrystal silicon.
Comparative example
In order to verify beneficial effects of the present invention, the present invention is provided with comparative example, and comparative example is as follows：
The difference of comparative example 1 and embodiment 2 is that comparative example 1 is normal ingot casting process, not right during crystalline substance long
Silicon melt is stirred, and class monocrystal silicon is obtained.
To class monocrystal silicon obtained in embodiment 2 and class monocrystal silicon obtained in comparative example 1 carries out minority carrier lifetime, survey
As shown in Fig. 2 A figures are class monocrystal silicon obtained in comparative example 1 in Fig. 2, B figures are class monocrystalline silicon obtained in embodiment 2 to test result
Ingot.From figure 2 it can be seen that the minority carrier life time of the head (circled) of class monocrystal silicon obtained in comparative example 1 is relatively low (to be less than 4 μ
S), the minority carrier life time of class monocrystal silicon distributes very evenly obtained in embodiment 2, and low minority carrier life time region area is small, few sub- longevity
Life is about 6-8 μ s, illustrates, the embodiment of the present invention can strengthen the convection current of silicon melt by stirring, reduce the enrichment of impurity, obtain
The dislocation of the class monocrystal silicon for arriving is less, and minority carrier life time is higher.
To class monocrystal silicon obtained in embodiment 2 and obtained in comparative example 1, class monocrystal silicon centre position is cut into slices, and is obtained
To the outside drawing of silicon chip, as a result as shown in figure 3, C figures are the outer of the silicon chip that class monocrystal silicon obtained in comparative example 1 is obtained in Fig. 3
Figure is seen, D figures are the outside drawing of the silicon chip that class monocrystal silicon obtained in embodiment 2 is obtained, from figure 3, it can be seen that comparative example 1 is made
There is the crystal grain (as shown in circled in figure) of other crystal orientation in the silicon chip that the class monocrystal silicon for obtaining is obtained, the embodiment of the present invention is obtained
In the absence of the crystal grain of other crystal orientation, monocrystalline rate is 100% to silicon chip.Illustrate, the embodiment of the present invention cannot not reduced moltenly miscellaneous by stirring
The probability that forming core is enriched with solid-liquid crystal face of matter, improves the monocrystalline area of class monocrystal silicon.
To sum up, during crystalline substance long, by stirring silicon melt, the convection current of silicon melt can be strengthened, can so reduces gold
Category impurity enters in class monocrystal silicon, reduces the enrichment of impurity, improves the minority carrier life time of silicon ingot.Impurity cannot can not also be reduced moltenly
The probability of forming core is enriched with solid-liquid crystal face, the monocrystalline area of casting class monocrystalline is improved.Meanwhile, class provided in an embodiment of the present invention
The preparation method of monocrystal silicon is simple to operation.
The above 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.
Claims (10)
1. the preparation method of a species monocrystal silicon, it is characterised in that including：
Seed crystal is laid in crucible and forms inculating crystal layer；The silicon melt of molten condition is set above the inculating crystal layer, and control is described
Fusing point of the crucible bottom temperature less than the seed crystal so that the inculating crystal layer is not completely melted；
Regulation thermal field forms supercooled state, the silicon melt is started crystalline substance long on the basis of the inculating crystal layer；The crystalline substance mistake long
Cheng Zhong, is continued with 1 rev/min -60 revs/min of mixing speed or discontinuously stirs the silicon melt；
After whole silicon melts have been crystallized, annealed cooling obtains class monocrystal silicon.
2. the preparation method of class monocrystal silicon as claimed in claim 1, it is characterised in that the mixing speed is 20 revs/min
- 50 revs/min of clock.
3. the preparation method of class monocrystal silicon as claimed in claim 1, it is characterised in that described discontinuously to stir the silicon and melt
The mode of body is：The once silicon melt is stirred every 5min-1h, each mixing time is 1min-1h.
4. the preparation method of class monocrystal silicon as claimed in claim 1, it is characterised in that the silicon is stirred using agitating device
Melt, during stirring, the agitating device is gradually increasing, and the speed of the rising is more than or equal to the brilliant speed long.
5. the preparation method of class monocrystal silicon as claimed in claim 4, it is characterised in that in whipping process, the stirring dress
It is 2cm-6cm to put the vertical range for crystallizing the silicon crystal to be formed with the inculating crystal layer or the silicon melt.
6. a species monocrystal silicon, it is characterised in that the class monocrystal silicon is according to the system as described in claim any one of 1-5
Preparation Method is obtained.
7. a species monocrystalline silicon cast ingot stove, it is characterised in that including ingot casting furnace body and agitating device, the ingot casting furnace body bag
Crucible is included, the agitating device includes agitator and drives the drive device of the agitator motion, and the agitator stretches into institute
State for the silicon melt stirred in the crucible in crucible, the drive device is arranged on the ingot casting furnace body.
8. class monocrystalline silicon cast ingot stove as claimed in claim 7, it is characterised in that the agitator includes agitating paddle, described to stir
The length for mixing oar is 30cm-80cm.
9. class monocrystalline silicon cast ingot stove as claimed in claim 7, it is characterised in that the agitator by a connecting rod with it is described
Drive device is connected.
10. class monocrystalline silicon cast ingot stove as claimed in claim 7, it is characterised in that the agitator is to the silicon melt without dirt
Dye, and fusing point is more than silicon.
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