CN103966660B - A kind of mono-like silicon ingot growing method - Google Patents
A kind of mono-like silicon ingot growing method Download PDFInfo
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- CN103966660B CN103966660B CN201410214862.4A CN201410214862A CN103966660B CN 103966660 B CN103966660 B CN 103966660B CN 201410214862 A CN201410214862 A CN 201410214862A CN 103966660 B CN103966660 B CN 103966660B
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Abstract
The invention discloses a kind of mono-like silicon ingot growing method, comprise the steps: that polycrystalline silicon material a) adds in silica crucible heat fusing forms melted silicon；B), after seed crystal being preheated, immerse mobile from top to bottom for seed crystal in melted silicon；C) controlling the rotary speed of seed crystal and slowly promote seed crystal, from the contact surface of seed crystal and melted silicon, downwards and surrounding growth forms quasi-single crystal rod；D) when the growth fraction of quasi-single crystal rod weighs predetermined threshold value, terminating crystal growth, be cooled to annealing temperature, cooling is come out of the stove.The mono-like silicon ingot growing method that the present invention provides, seed crystal is immersed in melted silicon from top to bottom, by controlling the rotation of seed crystal and being lifted up, quasi-single crystal rod is made to there is liquid-state silicon when growth and between silica crucible wall, it is prevented effectively from mono-like silicon ingot directly to contact with sidewall of crucible, thus it is high to have monocrystalline rate, the advantage that dislocation rate is low；And without crucible contact stain, it is not necessary to remove flaw-piece layer.
Description
Technical field
The present invention relates to a kind of silicon ingot preparation method for solaode, particularly relate to a kind of mono-like silicon ingot growth
Method.
Background technology
Along with the development of solar electrical energy generation industry, silicon solar cell due to cheap, technique relative maturity,
Become the main product of commercial market.Solar battery efficiency prepared by monocrystal silicon is high, but general monocrystal silicon uses
Vertical pulling method (Czochralski) prepares, relatively costly, and the way that polysilicon uses heat exchange carries out ingot casting, cost
Relatively low, but its battery efficiency made is relatively low.
As can be seen here, what the way of development utilization polycrystalline silicon ingot casting carried out quasi-monocrystalline is grown to serve as a kind of emerging technology.
Lay the way of seed crystal bottom the employing of the most quasi-monocrystalline ingot casting, when bottom seed crystal semi-molten, open
Begin to carry out ingot casting.The quasi-monocrystalline of the method growth, its monocrystalline rate only has about 60%, at the silicon contacted with sidewall of crucible
There is the high dislocation region that a large amount of polycrystalline coexists with monocrystalline in ingot region, after the section of this region, the battery efficiency of preparation is with general
Logical polycrystalline battery is compared the most relatively low, causes the utilization rate of quasi-monocrystalline ingot casting to reduce.Existing quasi-monocrystalline silicon ingot casting technology with
Polycrystalline silicon ingot casting is compared and is not shown obvious advantage.
Therefore, it is necessary to a kind of method that novel quasi-monocrystalline ingot casting is provided, to be reduced or avoided in mono-like silicon ingot
The existence in the high dislocation region that polycrystalline and monocrystalline coexist, thus quasi-monocrystalline ingot casting odds for effectiveness can be kept, can enter again
One step reduces the cost of silicon solar cell.
Summary of the invention
The technical problem to be solved is to provide a kind of mono-like silicon ingot growing method, and monocrystalline rate is high, dislocation
Rate is low；And without crucible contact stain, it is not necessary to remove flaw-piece layer.
The present invention solves that above-mentioned technical problem employed technical scheme comprise that a kind of mono-like silicon ingot growth side of offer
Method, comprises the steps: that polycrystalline silicon material a) adds in silica crucible heat fusing forms melted silicon；B) to seed crystal
After preheating, immerse mobile from top to bottom for seed crystal in melted silicon；C) control the rotary speed of seed crystal and slowly promote seed
Crystalline substance, from the contact surface of seed crystal and melted silicon, downwards and surrounding growth forms quasi-single crystal rod；D) when the growth of quasi-single crystal rod
When proportion reaches predetermined threshold value, terminating crystal growth, be cooled to annealing temperature, cooling is come out of the stove.
Above-mentioned mono-like silicon ingot growing method, wherein, described step a) uses surrounding side and the end in foundry furnace
Polycrystalline silicon material in silica crucible is heated to 1450 DEG C of fusings by the mode of portion's heating, after silicon material is completely melt, slow
Slowly melted silicon temperature is adjusted to about 1420 DEG C.
Above-mentioned mono-like silicon ingot growing method, wherein, described casting in-furnace temperature raises the most successively, temperature
Degree graded value is 1～2 DEG C/cm.
Above-mentioned mono-like silicon ingot growing method, wherein, the seed crystal in described step b) is silicon single crystal bar, described silicon
The top of monocrystal rod is connected with cooler, and bottom is preheating to 1370～1390 DEG C.
Above-mentioned mono-like silicon ingot growing method, wherein, the crystal orientation of described silicon single crystal bar is [100], a diameter of 5～
15cm, a length of 20cm.
Above-mentioned mono-like silicon ingot growing method, wherein, in described step c) rotational velocity range of seed crystal be 0.5～
2 revs/min, the hoisting depth of described seed crystal is 1～5cm, and the height at the quasi-single crystal rod top of growth formation is not higher than
The height of Quartz crucible lateral wall.
Above-mentioned mono-like silicon ingot growing method, wherein, the 5cm degree of depth in seed crystal immerses melted silicon in described step b),
First control seed crystal rotary speed and be maintained at 1 rev/min；Along with the continuous growth of quasi-single crystal rod, seed crystal is the most upwards carried
Rise about 2cm, when, after the melted silicon directional solidification of gross weight more than 60%, persistently reducing the temperature of silica crucible wall extremely
1405 DEG C, and control the rotary speed of quasi-single crystal rod to 2 revs/min；When the melted silicon of gross weight more than 80% is the longest
After crystal solidification becomes quasi-monocrystalline, terminate crystal growth.
Above-mentioned mono-like silicon ingot growing method, wherein, after in described step d), long crystalline substance terminates, first by heating-up temperature
It is slowly lowered to annealing temperature 1350 DEG C and is incubated 2 hours；Then with the rate of temperature fall of not higher than 150 DEG C/h,
The tapping temperature of slow cooling to less than 300 DEG C, adjusts foundry furnace cavity pressure and comes out of the stove to atmospheric pressure.
The present invention contrasts prior art a following beneficial effect: the mono-like silicon ingot growing method that the present invention provides,
Seed crystal is immersed in melted silicon from top to bottom, by controlling the rotation of seed crystal and being lifted up so that crystal is by liquid level
Starting at seed crystal from top to bottom and surrounding grows, there is liquid-state silicon when growth and between silica crucible wall in quasi-single crystal rod,
It is prevented effectively from mono-like silicon ingot directly to contact with sidewall of crucible, thus it is high to have monocrystalline rate, the advantage that dislocation rate is low；And
Contact stain without crucible, it is not necessary to remove flaw-piece layer.
Accompanying drawing explanation
Fig. 1 is the structural representation of the single crystal silicon ingot furnace that the present invention uses；
Fig. 2 is mono-like silicon ingot Growth Control schematic flow sheet of the present invention.
In figure:
1 cooler 2 seed crystal 3 silica crucible
4 melted silicon 5 heaters
Detailed description of the invention
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
Fig. 1 is the structural representation of the single crystal silicon ingot furnace that the present invention uses；Fig. 2 is mono-like silicon ingot of the present invention
Growth Control schematic flow sheet.
Referring to Fig. 1 and Fig. 2, the mono-like silicon ingot growing method that the present invention provides, with the seed crystal 2 of cooler 1
Melted silicon, the method carrying out quasi-crystal growth is immersed from top.Heat is mainly by seed crystal 2 He with cooler 1
Inert gas flow is taken away；Seed crystal with cooler connects dynamic mechanism, it is possible to realizes seed crystal and rotates and promote.
Polycrystalline silicon material is put in the silica crucible 3 with silicon nitride coating and is melted, and uses adding of surrounding side and bottom
Hot device 5 heats.Specifically include following steps:
Step S1: polycrystalline silicon material is added heat fusing and forms melted silicon 4 by 3 in silica crucible；As adopted in foundry furnace
By the mode of surrounding side and bottom-heated, the polycrystalline silicon material in silica crucible is heated to 1450 DEG C of fusings, treats silicon material
After being completely melt, slowly melted silicon temperature is adjusted to about 1420 DEG C；Casting in-furnace temperature rises the most successively
Height, thermograde changing value is 1～2 DEG C/cm；
Step S2: to seed crystal 2 preheat after, seed crystal bottom temperature range is 1370～1390 DEG C, by seed crystal by to
In lower mobile immersion melted silicon 4；
Step S3: control the rotary speed of seed crystal 2 and slowly promote seed crystal, from seed crystal 2 and the contact of melted silicon 4
Face down and surrounding growth forms quasi-single crystal rod；The rotational velocity range of seed crystal 2 is preferably 0.5～2 rev/min, slow
Slowly promoting seed crystal, and ensure silicon ingot and the uniform contact surface of melted silicon, the hoisting depth of the quasi-single crystal rod of growth is the highest
In Quartz crucible lateral wall height, to ensure that quasi-single crystal rod is in heating region；
Step S4: when the growth fraction of quasi-single crystal rod weighs predetermined threshold value, such as treat the growth proportion of quasi-single crystal rod
Reaching more than the 80% of former melted silicon, terminate crystal growth, be cooled to annealing temperature, cooling is come out of the stove.
In the present invention, preferred seed crystal crystal orientation is [100], when control the thermograde in direction of crystal growth 1～
During 1.5 DEG C/cm, crystal growth profile is square, and when thermograde is at 3～4 DEG C/cm, crystal shape is cylinder
Shape.In the present invention growth quasi-monocrystalline due to growth quasi-single crystal rod and silica crucible between with the presence of melted silicon, no
Directly contact, thermal stress is little, the quasi-single crystal rod grown in this approach, and overall monocrystalline rate is higher, and outer layer is the most
Territory, crystalline region exists, and dislocation density is relatively low.Simultaneously as the region not contacted with crucible, there is no impurity in crucible
Pollution, it is not necessary to peeling processes, and utilization rate is high.Thus after solving existing quasi-monocrystalline ingot casting, monocrystalline rate is low, silicon
Ingot contacts, with silica crucible wall, the polycrystalline caused and coexists with monocrystalline, the problem that dislocation density is high.
Below with crystal orientation for [100], a diameter of 5～15cm, the silicon single crystal bar of length about 20cm is as seed crystal 2, top
Portion is connected with the cooler 1 of well in advance.
Selecting a quartz square crucible size is 550mm*550mm*550mm, with silicon nitride to crucible internal walls coating also
Sintering, loads polycrystalline silicon material about 150kg, uses the mode of the heating of four sides, side and bottom-heated to heat in ingot furnace
To 1450 DEG C of fusings, after silicon material is completely melt, slowly melted silicon temperature is adjusted to about 1420 DEG C (this sentences
Detection temperature 1408 DEG C is as the fusing point of silicon under normal pressure), stand one hour.
Seed crystal top with cooler is preheated, after being heated to about 1385 DEG C, immerses the silicon at crucible center
In liquation face, the degree of depth is 5cm.Heat is taken away by cooler through seed crystal conduction.Quasi-monocrystalline silicon by top down, by
The heart starts growth to surrounding, solves the problem that seed crystal during common quasi-monocrystalline ingot casting need to keep under semi-molten state.
Seed crystal initial rotation speed is maintained at 1 rev/min, and along with the continuous growth of quasi-single crystal rod, seed crystal uniformly slowly upwards carries
Rise about 2cm to terminate to crystal growth, it is ensured that the contact surface that melted silicon is uniform and stable with silicon ingot.
After the melted silicon accounting for gross weight more than 60% solidifies, persistently the temperature of reduction silica crucible wall is to 1405 DEG C,
The rotary speed of quasi-single crystal rod is to 2 revs/min, and persistently long crystalline substance to the melted silicon accounting for gross weight more than 80% is frozen into accurate single
Crystalline substance, the long brilliant about 30 hours time.
After long crystalline substance, heating-up temperature is slowly lowered to annealing temperature 1350 DEG C, by side and bottom surface heater
Heating silica crucible, quasi-single crystal rod temperature is incubated 2 hours at 1350 DEG C.
Slow cooling is to tapping temperature less than 300 DEG C, and rate of temperature fall is not higher than 150 DEG C/h, by stove cavity pressure
Adjust and come out of the stove to atmospheric pressure.
Although the present invention discloses as above with preferred embodiment, so it is not limited to the present invention, any this area
Technical staff, without departing from the spirit and scope of the present invention, when a little amendment and perfect can be made, therefore this
Bright protection domain is when with being as the criterion that claims are defined.
Claims (7)
1. a mono-like silicon ingot growing method, it is characterised in that comprise the steps:
A) in silica crucible, polycrystalline silicon material is added heat fusing and forms melted silicon；
B), after seed crystal being preheated, immerse mobile from top to bottom for seed crystal in melted silicon；
C) control the rotary speed of seed crystal and slowly promote seed crystal, downward from the contact surface of seed crystal and melted silicon and four
Zhousheng length forms quasi-single crystal rod；The rotational velocity range of described seed crystal is 0.5～2 rev/min, the lifting of described seed crystal
It is highly 1～5cm, and the height at the quasi-single crystal rod top of growth formation is not higher than the height of Quartz crucible lateral wall；
D) when the growth fraction of quasi-single crystal rod weighs predetermined threshold value, terminate crystal growth, be cooled to annealing temperature,
Cooling is come out of the stove.
2. mono-like silicon ingot growing method as claimed in claim 1, it is characterised in that described step a) is in casting
Use the mode of surrounding side and bottom-heated that the polycrystalline silicon material in silica crucible is heated to 1450 DEG C in making stove to melt
Change, after silicon material is completely melt, slowly melted silicon temperature is adjusted to about 1420 DEG C.
3. mono-like silicon ingot growing method as claimed in claim 2, it is characterised in that described casting in-furnace temperature
Raising the most successively, thermograde changing value is 1～2 DEG C/cm.
4. mono-like silicon ingot growing method as claimed in claim 1, it is characterised in that the seed in described step b)
Crystalline substance is silicon single crystal bar, and the top of described silicon single crystal bar is connected with cooler, and bottom is preheating to 1370～1390 DEG C.
5. mono-like silicon ingot growing method as claimed in claim 4, it is characterised in that the crystalline substance of described silicon single crystal bar
To for [100], a diameter of 5～15cm, a length of 20cm.
6. mono-like silicon ingot growing method as claimed in claim 1, it is characterised in that seed crystal in described step b)
Immerse the 5cm degree of depth in melted silicon, first control seed crystal rotary speed and be maintained at 1 rev/min；Continuous along with quasi-single crystal rod
Growth, is slowly lifted up seed crystal about 2cm, when after the melted silicon directional solidification of gross weight more than 60%, persistently drops
The temperature of low quartz sidewall of crucible is to 1405 DEG C, and controls the rotary speed of quasi-single crystal rod to 2 revs/min；Work as gross weight
After the longest crystal solidification of melted silicon of more than 80% becomes quasi-monocrystalline, terminate crystal growth.
7. mono-like silicon ingot growing method as claimed in claim 2, it is characterised in that long crystalline substance in described step d)
After end, first heating-up temperature is slowly lowered to annealing temperature 1350 DEG C and is incubated 2 hours；Then with not higher than
The rate of temperature fall of 150 DEG C/h, the tapping temperature below slow cooling to 300 DEG C, foundry furnace cavity pressure is adjusted
Come out of the stove to atmospheric pressure.
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