CN103966660A - Growing method of pseudo-monocrystal silicon ingot - Google Patents
Growing method of pseudo-monocrystal silicon ingot Download PDFInfo
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- CN103966660A CN103966660A CN201410214862.4A CN201410214862A CN103966660A CN 103966660 A CN103966660 A CN 103966660A CN 201410214862 A CN201410214862 A CN 201410214862A CN 103966660 A CN103966660 A CN 103966660A
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Abstract
The invention discloses a growing method of a pseudo-monocrystal silicon ingot. The growing method comprises the following steps: a) heating a polycrystalline silicon material in a quartz crucible to be melted to form a silicon melt; b) after pre-heating seeds, movably immersing the seeds into the silicon melt from top to bottom; c) controlling the rotating speed of the seeds and slowly lifting the seeds and growing from the contact face of the seeds and the silicon melt downward and all around to form the pseudo-monocrystal silicon ingot; and d) when the growing proportion of the pseudo-monocrystal silicon ingot reaches the predetermined threshold valve, finishing growth of crystals, cooling to annealing temperature and cooling and discharging. According to the growing method of the pseudo-monocrystal silicon ingot provided by the invention, the seeds are immersed into the silicon melt from top to bottom and the seeds are control to rotate and lifted upward, so that liquid silicon exists between the pseudo-monocrystal silicon ingot and the wall of the quartz crucible during growth to effectively avoid direct contact of the pseudo-monocrystal silicon ingot and the quartz crucible, thereby having the advantages of high monocrystal rate and low dislocation rate. No crucible contact pollution is generated and the edge layer needs not to be removed.
Description
Technical field
The present invention relates to a kind of silicon ingot preparation method for solar cell, relate in particular to a kind of quasi-monocrystalline silicon ingot growth method.
Background technology
Along with the development of solar electrical energy generation industry, silicon solar cell is due to cheap, and technique is relatively ripe, becomes the main product of commercial market.Solar battery efficiency prepared by silicon single crystal is high, but general silicon single crystal adopts vertical pulling method (Czochralski) to make, and cost is higher, and polysilicon adopts the way of heat exchange to carry out ingot casting, and cost is lower, but its battery efficiency of making is relatively low.
As can be seen here, the way of development utilization polycrystalline silicon ingot casting is carried out a kind of emerging technology of being grown to serve as of accurate monocrystalline.Generally accurate monocrystalline ingot casting adopts bottom to lay the way of seed crystal, under the state of bottom seed crystal semi-melting, starts to carry out ingot casting.The accurate monocrystalline of this method growth, its monocrystalline rate only has 60% left and right, the high dislocation region that exists a large amount of polycrystalline and monocrystalline to coexist in the silicon ingot region contacting with sidewall of crucible, after this region section, the battery efficiency of preparation is still lower compared with common polycrystalline battery, causes the utilization ratio of accurate monocrystalline ingot casting to reduce.Existing quasi-monocrystalline silicon ingot casting technology does not show obvious advantage compared with polycrystalline silicon ingot casting.
Therefore, be necessary to provide a kind of method of novel accurate monocrystalline ingot casting, to reduce or to avoid existing of high dislocation region that in quasi-monocrystalline silicon ingot, polycrystalline and monocrystalline coexist, thereby accurate monocrystalline ingot casting odds for effectiveness can be kept, the cost of silicon solar cell can be further reduced again.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of quasi-monocrystalline silicon ingot growth method, and monocrystalline rate is high, and dislocation rate is low; And without crucible contact stain, without removing flaw-piece layer.
The present invention solves the problems of the technologies described above the technical scheme adopting to be to provide a kind of quasi-monocrystalline silicon ingot growth method, comprises the steps: a) in quartz crucible, polycrystalline silicon material heat fused to be formed to melted silicon; B) to after seed crystal preheating, by seed crystal mobile immersion in melted silicon from top to bottom; C) control the speed of rotation of seed crystal and slowly promote seed crystal, from the contact surface of seed crystal and melted silicon downwards and surrounding growth form accurate single crystal rod; D) in the time that the growth fraction of accurate single crystal rod weighs predetermined threshold value, finish crystal growth, be cooled to annealing temperature, cooling coming out of the stove.
Above-mentioned quasi-monocrystalline silicon ingot growth method, wherein, described step a) adopts the mode of surrounding side and bottom-heated that the polycrystalline silicon material in quartz crucible is heated to 1450 DEG C of fusings in foundry furnace, after silicon material melts completely, slowly melted silicon temperature is adjusted to 1420 DEG C of left and right.
Above-mentioned quasi-monocrystalline silicon ingot growth method, wherein, in described foundry furnace, temperature raises from top to bottom successively, and thermograde changing value is 1～2 DEG C/cm.
Above-mentioned quasi-monocrystalline silicon ingot growth method, wherein, the seed crystal of described step in b) is silicon single crystal bar, and the top of described silicon single crystal bar is connected with water cooler, and bottom is preheating to 1370～1390 DEG C.
Above-mentioned quasi-monocrystalline silicon ingot growth method, wherein, the crystal orientation of described silicon single crystal bar is [100], and diameter is 5～15cm, and length is 20cm.
Above-mentioned quasi-monocrystalline silicon ingot growth method, wherein, described step c) in the rotational velocity range of seed crystal be 0.5～2 rev/min, the lift height of described seed crystal is 1～5cm, and the height at the accurate single crystal rod top that forms of growth is not higher than the height of quartz crucible sidewall.
Above-mentioned quasi-monocrystalline silicon ingot growth method, wherein, described step b) middle seed crystal immerses the 5cm degree of depth in melted silicon, first controls seed crystal speed of rotation and remains on 1 rev/min; Along with the continuous growth of accurate single crystal rod, seed crystal is slowly upwards promoted to about 2cm, when after the more than 60% melted silicon directional freeze of gross weight, continue to reduce the temperature to 1405 DEG C of quartz crucible wall, and control the speed of rotation to 2 rev/min of accurate single crystal rod; Become after accurate monocrystalline when more than 80% melted silicon of gross weight continues long crystal solidification, finish crystal growth.
Above-mentioned quasi-monocrystalline silicon ingot growth method, wherein, described steps d) in after long crystalline substance finishes, first Heating temperature be slowly reduced to 1350 DEG C of annealing temperatures and be incubated 2 hours; Then with the rate of temperature fall higher than 150 DEG C/h not, slow cooling to 300 DEG C following tapping temperature, comes out of the stove after foundry furnace cavity pressure is adjusted to normal atmosphere.
The present invention contrasts prior art following beneficial effect: quasi-monocrystalline silicon ingot growth method provided by the invention, seed crystal is immersed in melted silicon from top to bottom, by controlling the rotation of seed crystal and upwards promoting, crystal is started from top to bottom and surrounding is grown by liquid level seed crystal place, in the time of growth and between quartz crucible wall, there is liquid-state silicon in accurate single crystal rod, effectively avoid quasi-monocrystalline silicon ingot directly to contact with sidewall of crucible, thereby it is high to have monocrystalline rate, the advantage that dislocation rate is low; And without crucible contact stain, without removing flaw-piece layer.
Brief description of the drawings
Fig. 1 is the structural representation of the single crystal silicon ingot furnace that uses of the present invention;
Fig. 2 is quasi-monocrystalline silicon ingot growth control schematic flow sheet of the present invention.
In figure:
1 water cooler 2 seed crystal 3 quartz crucibles
4 melted silicon 5 well heaters
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Fig. 1 is the structural representation of the single crystal silicon ingot furnace that uses of the present invention; Fig. 2 is quasi-monocrystalline silicon ingot growth control schematic flow sheet of the present invention.
Refer to Fig. 1 and Fig. 2, quasi-monocrystalline silicon ingot growth method provided by the invention, immerses melted silicon, the method for carrying out accurate single crystal growing with the seed crystal 2 of water cooler 1 from top.Heat is mainly taken away by seed crystal 2 and inert gas flow with water cooler 1; Seed crystal with water cooler is connected with actuating unit, can realize seed crystal rotation and promote.Polycrystalline silicon material is put into the quartz crucible 3 of silicon nitride coating and is melted, and adopts the well heater 5 of surrounding side and bottom to heat.Specifically comprise the steps:
Step S1: polycrystalline silicon material heat fused is formed melted silicon 4 by 3 in quartz crucible; As the polycrystalline silicon material in quartz crucible is heated to 1450 DEG C of fusings by the mode that adopts surrounding side and bottom-heated in foundry furnace, after silicon material melts completely, slowly melted silicon temperature is adjusted to 1420 DEG C of left and right; In foundry furnace, temperature raises from top to bottom successively, and thermograde changing value is 1～2 DEG C/cm;
Step S2: after seed crystal 2 preheatings, seed crystal bottom temperature range is 1370～1390 DEG C, by seed crystal mobile immersion in melted silicon 4 from top to bottom;
Step S3: control the speed of rotation of seed crystal 2 and slowly promote seed crystal, from the contact surface of seed crystal 2 and melted silicon 4 downwards and surrounding growth form accurate single crystal rod; The rotational velocity range of seed crystal 2 is preferably 0.5～2 rev/min, slowly promotes seed crystal, and ensures silicon ingot and the uniform contact surface of melted silicon, and the lift height of the accurate single crystal rod of growth is not higher than quartz crucible sidewall height, to ensure that accurate single crystal rod is in heating region;
Step S4: in the time that the growth fraction of accurate single crystal rod weighs predetermined threshold value, such as treating the growth fraction of accurate single crystal rod the more than 80% of former melted silicon that weighs, finish crystal growth, be cooled to annealing temperature, cooling coming out of the stove.
In the present invention, preferred seed crystal crystal orientation be [100], and when the thermograde of direction of controlling crystal growth is during at 1～1.5 DEG C/cm, the crystal profile of growing is square, and when thermograde is during at 3～4 DEG C/cm, crystal shape is cylindrical.The accurate monocrystalline of growing in the present invention, owing to there being melted silicon to exist between the accurate single crystal rod of growing and quartz crucible, does not directly contact, and thermal stresses is little, so accurate single crystal rod of this method growth, entirety monocrystalline rate is higher, and skin does not have polycrystalline region, and dislocation desity is lower.Meanwhile, due to the region not contacting with crucible, there is no the pollution of impurity in crucible, process without peeling, utilization ratio is high.Thereby solved after existing accurate monocrystalline ingot casting, monocrystalline rate is low, silicon ingot contacts the polycrystalline and the monocrystalline that cause and coexists with quartz crucible wall, the problem that dislocation desity is high.
Take crystal orientation as [100] below, diameter is 5～15cm, and the silicon single crystal bar of the about 20cm of length is as seed crystal 2, and top is connected with the water cooler 1 of well in advance.
Selecting a quartzy square crucible size is 550mm*550mm*550mm, with silicon nitride to crucible inside coating sintering, pack the about 150kg of polycrystalline silicon material into, in ingot furnace, adopt the mode of the heating of four sides, side and bottom-heated to be heated to 1450 DEG C of fusings, after silicon material melts completely, slowly melted silicon temperature is adjusted to 1420 DEG C of left and right (this sentences the fusing point of 1408 DEG C of silicon under normal pressure of detected temperatures), leaves standstill one hour.
Preheating is carried out in seed crystal top with water cooler, be heated to behind 1385 DEG C of left and right, immerse in the melted silicon face at crucible center, the degree of depth is 5cm.Heat is taken away by water cooler through seed crystal conduction.Quasi-monocrystalline silicon is downward by top, starts growth by middle mind-set surrounding, solves the problem that in common accurate monocrystalline ingot casting process, seed crystal need keep under semi-melting state.The initial speed of rotation of seed crystal remains on 1 rev/min, and along with the continuous growth of accurate single crystal rod, seed crystal evenly slowly upwards promotes about 2cm to be finished to crystal growth, the contact surface that guarantee melted silicon and silicon ingot are uniform and stable.
After accounting for more than 60% melted silicon of gross weight and solidifying, continue to reduce the temperature to 1405 DEG C of quartz crucible wall, the speed of rotation to 2 of accurate single crystal rod rev/min, continues to be longly brilliantly frozen into accurate monocrystalline to accounting for more than 80% melted silicon of gross weight, the long brilliant approximately 30 hours time.
After long crystalline substance, Heating temperature is slowly reduced to 1350 DEG C of annealing temperatures, by side and bottom surface well heater, quartz crucible is heated, accurate single crystal rod temperature was 1350 DEG C of insulations 2 hours.
Slow cooling is to tapping temperature below 300 DEG C, and rate of temperature fall is higher than 150 DEG C/h, comes out of the stove after furnace chamber internal pressure is adjusted to normal atmosphere.
Although the present invention discloses as above with preferred embodiment; so it is not in order to limit the present invention, any those skilled in the art, without departing from the spirit and scope of the present invention; when doing a little amendment and perfect, therefore protection scope of the present invention is worked as with being as the criterion that claims were defined.
Claims (8)
1. a quasi-monocrystalline silicon ingot growth method, is characterized in that, comprises the steps:
A) in quartz crucible, polycrystalline silicon material heat fused is formed to melted silicon;
B) to after seed crystal preheating, by seed crystal mobile immersion in melted silicon from top to bottom;
C) control the speed of rotation of seed crystal and slowly promote seed crystal, from the contact surface of seed crystal and melted silicon downwards and surrounding growth form accurate single crystal rod;
D) in the time that the growth fraction of accurate single crystal rod weighs predetermined threshold value, finish crystal growth, be cooled to annealing temperature, cooling coming out of the stove.
2. quasi-monocrystalline silicon ingot growth method as claimed in claim 1, it is characterized in that, described step a) adopts the mode of surrounding side and bottom-heated that the polycrystalline silicon material in quartz crucible is heated to 1450 DEG C of fusings in foundry furnace, after silicon material melts completely, slowly melted silicon temperature is adjusted to 1420 DEG C of left and right.
3. quasi-monocrystalline silicon ingot growth method as claimed in claim 2, is characterized in that, in described foundry furnace, temperature raises from top to bottom successively, and thermograde changing value is 1～2 DEG C/cm.
4. quasi-monocrystalline silicon ingot growth method as claimed in claim 1, is characterized in that, the seed crystal of described step in b) is silicon single crystal bar, and the top of described silicon single crystal bar is connected with water cooler, and bottom is preheating to 1370～1390 DEG C.
5. quasi-monocrystalline silicon ingot growth method as claimed in claim 4, is characterized in that, the crystal orientation of described silicon single crystal bar is [100], and diameter is 5～15cm, and length is 20cm.
6. quasi-monocrystalline silicon ingot growth method as claimed in claim 1, it is characterized in that, the described step c) rotational velocity range of middle seed crystal is 0.5～2 rev/min, the lift height of described seed crystal is 1～5cm, and the height at the accurate single crystal rod top that forms of growth is not higher than the height of quartz crucible sidewall.
7. quasi-monocrystalline silicon ingot growth method as claimed in claim 6, is characterized in that, described step b) middle seed crystal immerses the 5cm degree of depth in melted silicon, first controls seed crystal speed of rotation and remains on 1 rev/min; Along with the continuous growth of accurate single crystal rod, seed crystal is slowly upwards promoted to about 2cm, when after the more than 60% melted silicon directional freeze of gross weight, continue to reduce the temperature to 1405 DEG C of quartz crucible wall, and control the speed of rotation to 2 rev/min of accurate single crystal rod; Become after accurate monocrystalline when more than 80% melted silicon of gross weight continues long crystal solidification, finish crystal growth.
8. quasi-monocrystalline silicon ingot growth method as claimed in claim 2, is characterized in that described steps d) in after long crystalline substance finishes, first Heating temperature be slowly reduced to 1350 DEG C of annealing temperatures and be incubated 2 hours; Then with the rate of temperature fall higher than 150 DEG C/h not, slow cooling to 300 DEG C following tapping temperature, comes out of the stove after foundry furnace cavity pressure is adjusted to normal atmosphere.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105019022A (en) * | 2015-08-12 | 2015-11-04 | 常州天合光能有限公司 | Quasi mono-crystalline silicon co-doped with gallium, germanium and boron and preparing method thereof |
| CN111717919A (en) * | 2019-03-21 | 2020-09-29 | 新疆大全新能源股份有限公司 | A kind of manufacturing process of silicon core for polysilicon reduction furnace |
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| US20120067272A1 (en) * | 2010-09-16 | 2012-03-22 | Covalent Materials Corporation | Single crystal pulling-up apparatus and single crystal pulling-up method |
| CN101798704B (en) * | 2009-12-31 | 2012-05-23 | 峨嵋半导体材料研究所 | Process for growing phi 8'' solar-grade Czochralski silicon by using 18-inch thermal field |
| CN103160918A (en) * | 2013-02-26 | 2013-06-19 | 宏大中源太阳能股份有限公司 | Preparation furnace and preparation method of pseudo single crystal silicon |
| JP2013151385A (en) * | 2012-01-25 | 2013-08-08 | Shin Etsu Handotai Co Ltd | Method of manufacturing silicon single crystal |
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Patent Citations (4)
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| CN101798704B (en) * | 2009-12-31 | 2012-05-23 | 峨嵋半导体材料研究所 | Process for growing phi 8'' solar-grade Czochralski silicon by using 18-inch thermal field |
| US20120067272A1 (en) * | 2010-09-16 | 2012-03-22 | Covalent Materials Corporation | Single crystal pulling-up apparatus and single crystal pulling-up method |
| JP2013151385A (en) * | 2012-01-25 | 2013-08-08 | Shin Etsu Handotai Co Ltd | Method of manufacturing silicon single crystal |
| CN103160918A (en) * | 2013-02-26 | 2013-06-19 | 宏大中源太阳能股份有限公司 | Preparation furnace and preparation method of pseudo single crystal silicon |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105019022A (en) * | 2015-08-12 | 2015-11-04 | 常州天合光能有限公司 | Quasi mono-crystalline silicon co-doped with gallium, germanium and boron and preparing method thereof |
| CN111717919A (en) * | 2019-03-21 | 2020-09-29 | 新疆大全新能源股份有限公司 | A kind of manufacturing process of silicon core for polysilicon reduction furnace |
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