CN103205807A - Ingot furnace for preparing quasi-monocrystalline silicon and method of preparing quasi-monocrystalline silicon - Google Patents
Ingot furnace for preparing quasi-monocrystalline silicon and method of preparing quasi-monocrystalline silicon Download PDFInfo
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Abstract
The invention provides an ingot furnace for preparing quasi-monocrystalline silicon, and further provides a method of preparing the quasi-monocrystalline silicon. According to the method, growth of the quasi-monocrystalline silicon is completed in the quasi-monocrystalline ingot furnace, a heat exchange device is employed, and heat exchange by gas is utilized to control temperature and adjust solid-liquid interface, so as to grow the quasi-monocrystalline. According to the invention, through using the special heat exchange device, a way of the heat change by gas is utilized to replace a way of heat exchange by a heat insulation cage, and a temperature of seed crystal can be accurately controlled, thereby solving problems of not flat solid-liquid interface, and increasing a proportion of the quasi-monocrystalline and a utilization rate of silicon materials.
Description
Technical field
The present invention relates to a kind of method for preparing the ingot furnace of quasi-monocrystalline silicon and prepare quasi-monocrystalline silicon.
Background technology
Accurate monocrystalline (Mono Like) is based on the technology of polycrystalline ingot casting, uses single crystal seed by part when long crystalline substance, obtains the polysilicon chip of outward appearance and the equal single crystal-like of electrical property.This mode by ingot casting forms the technology of silicon single crystal, and its power consumption only Duos 5% than common polysilicon, and the quality of the silicon single crystal of producing is near pulling of silicon single crystal.Briefly, this technology is exactly the cost with polysilicon, the technology of manufacture order crystal silicon.
In current fast-developing photovoltaic industry, high-level efficiency and low cost are the targets that the insider pursues always.Crystalline silicon is as current topmost solar cell material and widespread use, and silicon single crystal and polysilicon are occupied an leading position on the crystalline silicon market.Silicon single crystal generally adopts vertical pulling method (Cz) method to make, use specific to operation preparations such as single crystal seed processization material, seeding, shouldering, commentaries on classics shoulder, isometrical, ending, the gained crystal has advantages such as low defective, high-level efficiency, but this method is higher to raw material and operational requirement, and to throw the stove amount few at every turn, and cost is higher; Polysilicon generally adopts directional solidification method (DSS) to make, by operation preparations such as heating, thawing, long crystalline substance, annealing, coolings, the gained crystal has shortcomings such as polycrystalline circle, poor efficiency, but this method is not high to raw material and operational requirement, and to throw the stove amount big at every turn, and cost is lower.In order to pursue a kind of advantage that silicon single crystal efficiency of conversion height is lower with the polysilicon process cost, be easy to scale operation that has concurrently, industrial community is considered to come casting single crystal with the method that polycrystalline is cast, namely realize long brilliant with the silicon single-crystal seed crystal of reserving as the starting point of crystal growth, Yang Deren, the Yu Xuegong of Zhejiang University have launched a few thing at this, its patent CN 101654805A has mentioned a kind of method, but its operation is comparatively complicated and be difficult to control, and the accurate monocrystalline ratio that obtains is not high.
The accurate monocrystalline ingot casting of DSS ingot furnace process typical method: lay one deck seed crystal in crucible bottom, the silicon raw material is heated to gradually and begins more than 1410 ℃ to melt, this moment, heat-insulation cage moved to certain altitude from the bottom up, make the whole thawings of silicon raw material guarantee that for liquid the bottom seed crystal is not melted fully, after entering crystal growth, continue to promote heat-insulation cage, heat is derived from crucible bottom, form vertical thermograde, thereby the directional freeze of melt begins from the bottom up.Because melting and growing the movement that the brilliant stage all relates to heat-insulation cage, and seed temperature and solid-liquid interface can't be accurately controlled in the movement of heat-insulation cage, often the phenomenon that part seed crystal excessive melting occurs or do not have to melt causes forming the accurate monocrystalline of big area or does not have accurate monocrystalline; Open at long brilliant starting stage heat-insulation cage, temperature control is disorderly, enough condensate depression and smooth solid-liquid interface is not provided and causes silicon ingot bottom impurity to be concentrated at nucleation stage, causes silicon material utilization ratio to descend, and increases cost.
Summary of the invention
The invention provides a kind of ingot furnace for preparing quasi-monocrystalline silicon.Another technical scheme of the present invention has provided the preparation method of quasi-monocrystalline silicon.
The invention provides a kind of ingot furnace for preparing quasi-monocrystalline silicon, comprise body of heater, crucible, graphite post; The graphite post is installed in bottom of furnace body, and crucible is installed on the graphite post, and body of heater has guide shell to link to each other with crucible; Be provided with heat-proof device between body of heater and the crucible; The crucible outer setting has heating unit; Crucible bottom is provided with heat exchanger; There is refrigerator pipe to be connected with heat exchanger with heating pipe on the heat exchanger.
Wherein, cold air is entered by the middle part in the described heat exchanger (6), enters the diffluence pass of 5 * 5 matrixes or 6 * 6 matrixes, is flowed out by the edge.
The present invention also provides a kind of method for preparing quasi-monocrystalline silicon, and it is the growth of finishing quasi-monocrystalline silicon in above-mentioned ingot furnace.
Particularly, it comprises the steps:
A, charging: the raw material that will comprise seed crystal is put into crucible, and wherein seed crystal is tiled in crucible bottom, places primary polysilicon and doped element on seed crystal top, and resistivity is adjusted to 1.5 Ω .cm;
B, heating: in 9 hours, crucible temperature is risen to 1412-1550 ℃;
C, fusing: keep 1412-1550 ℃ of crucible head temperature, open the gas valve of heat exchanger, in 2 hours, gas flow is upgraded to 30SLM, and lasting supply gas, the crucible bottom temperature transfers to 1390-1410 ℃, and whole thaw process continues 8-10 hour;
D, long brilliant: keep 1412-1550 ℃ of crucible head temperature, the crucible bottom gas flow increases to 65SLM from 30SLM in half an hour, and bottom temp is reduced to 1356-1370 ℃ rapidly, lasting 23-25 hour of the brilliant process of whole length from 1390-1410 ℃;
E, close the gas valve of heat exchanger, crucible namely gets the quasi-monocrystalline silicon ingot in 1356-1370 ℃ of annealing, cooling.
Wherein the head temperature of crucible is normally measured the temperature of bath surface by infrared thermometer.The crucible bottom temperature is to measure the temperature of crucible and heat exchanger contact surface by thermopair.
Further preferably, the described doped element of step a is boron.
Further preferably, the described crucible temperature of step b is 1550 ℃.
Further preferably, the head temperature of the described crucible of c step is 1430 ℃; Described crucible bottom temperature is 1410 ℃.
Further preferably, described d step is: keep 1430 ℃ of head temperature, the bottom gas flow increases to 65SLM by 30SLM in half an hour, and this moment, bottom temp was reduced to 1356 ℃ rapidly by 1410 ℃, and the brilliant process of whole length continues 24 hours.
Further preferably, described e step is 1370 ℃ of annealing 2 hours and cool off and namely got the quasi-monocrystalline silicon ingot in 10 hours.
The present invention with the alternative traditional heat-insulation cage heat exchange of the mode of gas converting heat, has solved the problem that is difficult to accurately control seed temperature and solid-liquid interface unevennessization by using special heat exchanger, improves accurate monocrystalline ratio and promotes silicon material utilization ratio.
Description of drawings
Fig. 1 ingot furnace structural representation of the present invention
Fig. 2 ingot furnace heat exchanger sectional view
The quasi-monocrystalline silicon photo of Fig. 3 the present invention preparation
Embodiment
The preparation method of embodiment 1 quasi-monocrystalline silicon of the present invention
Adopt the structural representation of the described ingot furnace air cooling heat radiation of Fig. 1, concrete grammar is as follows:
A, charging: the raw material that will comprise seed crystal is put into crucible, and wherein seed crystal is tiled in crucible bottom, places primary polysilicon and doped element on seed crystal top, and resistivity is adjusted to 1.5 Ω .cm;
B, heating: in 9 hours crucible temperature is risen to 1550 ℃, this moment, raw material began to melt from the top;
C, fusing: the crucible head temperature is adjusted to 1430 ℃, bottom temp transfers to 1410 ℃, opens the bottom gas valve simultaneously, and in 2 hours gas flow is upgraded to 30SLM, and continue supply to guarantee that seed crystal is not all melted, whole thaw process can continue 8-10 hour;
D, long brilliant: keep 1430 ℃ of head temperature, the bottom gas flow increases to 65SLM to realize the demand of crystal growth condensate depression by 30SLM in half an hour, this moment, bottom temp was reduced to 1356 ℃ rapidly by 1410 ℃, realize the directed heat radiation in bottom, crystal begins growth, and the brilliant process of whole length can continue about 24 hours;
E, 1370 ℃ of annealing 2 hours and cool off and namely got the quasi-monocrystalline silicon ingot in 10 hours.
The present invention adopts special heat exchanger as shown in Figure 2, and gas is entered by the middle part, advances 5 * 5 diffluence pass, is flowed out by the edge.Because silicon ingot weight is about 420 kilograms in producing, 840 * 840 person of outstanding talent's rice are divided into 5 * 5=25 piece silico briquette through after the evolution, so as required, adopt 5x5 ventage in the heat exchanger design.25 ventilating pits evenly pass to cooling gas and accurately control temperature in thawing and the long brilliant process.
Wherein the diameter of ventilating pit and height design according to air flow, in general, the whole graphite block of DS-BLOCK in the ingot furnace thermal field can be transformed into the interchanger with ventilation device, open air outlet and the inlet mouth of appropriate size simultaneously as required in the body of heater bottom.
Main points of the present invention are shown in the table 1: open just entering thawing stage chassis flow, the silicon material melts downwards gradually from the top, and crucible bottom is owing to there is the existence of cooling gas, by setting the chassis temperature, PID regulates the chassis flow makes temperature be lower than the set point change of fusing point all the time, and isothermal curve is parallel with crucible bottom all the time, the local superheating phenomenon can not occur, this just can accurately control crucible bottom (seed crystal) temperature, the phenomenon that the seed crystal excessive melting can not occur or not have to melt.After melting end, remain bottom temp at 1410 ℃, one hour the abundant churning time of melt is arranged, after entering long crystalline substance, the bottom airshed strengthens and makes bottom temp descend to provide enough big condensate depression, melt is grown along the seed crystal direction fast, well inherited the crystalline structure of seed crystal, obtain complete single crystal structure, also accurately control of temperature provides uniform isothermal curve in the brilliant process of follow-up length, makes the solid-liquid interface planarization, impurity is well discharged, and has improved the quality of accurate single crystal rod.Heat-proof device is not opened in whole process, has avoided mechanical disturbance and thermal convection.
The accurate single crystal preparation part of table 1. technique initialization
Begin growth because realize quasi-monocrystalline silicon in about 1 square metre crucible bottom, the heat that need take out of is very big, be about 20-60kw, gas flow rate is fast in the circulation line, and gas consumption is big, based on cost consideration, the closed cycles of adopting gas more, high-temperature gas after the heat exchange is derived body of heater, carry out the outer water-cooled of stove, cryogenic gas reenters the thermal field cooling then.Technological process is as shown in Figure 1: body of heater connects a heat exchanger, makes the superthermal gas that brings out through heat exchange, becomes cryogenic gas, enters the thermal field circulation again.
This scheme uses gas converting heat to control temperature and adjusting solid-liquid interface by using special heat exchanger, has realized seed temperature control and the planarization of long crystal boundary face, thereby has improved accurate monocrystalline ratio and promote silicon material utilization ratio.Have experiment to show, by the accurate monocrystalline of this scheme growth, battery conversion efficiency exceeds 0.1-0.2% than conventional accurate single crystal battery efficiency of conversion, and the utilization ratio of polycrystal silicon ingot can improve 4-5%.
Fig. 3 is the quasi-monocrystalline silicon of the present invention's preparation, by naked-eye observation, and the no polycrystalline crystal boundary in quasi-monocrystalline silicon ingot middle part, and process the silicon chip height that its efficiency ratio is common by follow-up battery.
The preparation method of embodiment 2 quasi-monocrystalline silicons of the present invention
A, charging: the raw material that will comprise seed crystal is put into crucible, and wherein seed crystal is tiled in crucible bottom, places primary polysilicon and doped element on seed crystal top, and resistivity is adjusted to 1.5 Ω .cm;
B, heating: in 9 hours crucible temperature is risen to 1412 ℃, this moment, raw material began to melt from the top;
C, fusing: the heating unit head temperature is adjusted to 1412 ℃, bottom temp transfers to 1407 ℃, opens bottom gas simultaneously, and in 2 hours gas flow is upgraded to 30SLM, and continue supply to guarantee that seed crystal is not all melted, whole thaw process can continue 8 hours;
D, long brilliant: keep 1412 ℃ of head temperature, the bottom gas flow increases to 65SLM to realize the demand of crystal growth condensate depression by 30SLM in half an hour, this moment, bottom temp was reduced to 1356 ℃ rapidly by 1407 ℃, realize the directed heat radiation in bottom, crystal begins growth, and the brilliant process of whole length can continue about 24 hours;
E, 1370 ℃ of annealing 2 hours and cool off and namely got the quasi-monocrystalline silicon ingot in 10 hours.
The preparation method of embodiment 3 quasi-monocrystalline silicons of the present invention
A, charging: the raw material that will comprise seed crystal is put into crucible, and wherein seed crystal is tiled in crucible bottom, places primary polysilicon and doped element on seed crystal top, and resistivity is adjusted to 1.5 Ω .cm;
B, heating: in 9 hours crucible temperature is risen to 1550 ℃, this moment, raw material began to melt from the top;
C, fusing: the heating unit head temperature is adjusted to 1550 ℃, bottom temp transfers to 1410 ℃, opens bottom gas simultaneously, and in 2 hours gas flow is upgraded to 30SLM, and continue supply to guarantee that seed crystal is not all melted, whole thaw process can continue 10 hours;
D, long brilliant: keep 1550 ℃ of head temperature, the bottom gas flow increases to 65SLM to realize the demand of crystal growth condensate depression by 30SLM in half an hour, this moment, bottom temp was reduced to 1356 ℃ rapidly by 1410 ℃, realize the directed heat radiation in bottom, crystal begins growth, and the brilliant process of whole length can continue about 24 hours;
E, 1356 ℃ of annealing 2 hours and cool off and namely got the quasi-monocrystalline silicon ingot in 10 hours.
In sum, the preparation method's of quasi-monocrystalline silicon of the present invention technical essential is as follows:
1. the method for using the bottom ventilation to enter thermal field in polycrystalline silicon ingot or purifying furnace guarantees vertical thermograde, and guarantees that the inculating crystal layer of crucible bottom is not melted fully.
2. the gas that enters from the bottom for cooling is argon gas, the contour ratio of specific heats gas of nitrogen or helium.The gas heat dissipation capacity is consistent with the heat dissipation capacity that promotes heat-proof device, is about 20-60kw.
3. cooling gas adopts closed cycle control, and the hot gas of derivation enters ingot furnace thermal field bottom after cooling off through peripheral water-cooled heat-exchanger rig again, plays the effect of circulation heat radiation.
4, this air cooling circulation guarantees the nonfused design of ingot furnace inner bottom part seed crystal, can be used in G5, and the ingot furnace thermal field of G6 both can have been produced 5 * 5 about 840 * 840 square millimeters, also can produce 6 * 6 about 1000 * 1000 square millimeters square silicon ingots.
Claims (9)
1. an ingot furnace for preparing quasi-monocrystalline silicon is characterized in that: comprise body of heater (1), crucible (2), graphite post (3); Graphite post (3) is installed in body of heater (1) bottom, and crucible (2) is installed on the graphite post (3), and body of heater (1) has guide shell (8) to link to each other with crucible (2); Be provided with heat-proof device (4) between body of heater (1) and the crucible (2); Crucible (2) outer setting has heating unit (5); Crucible bottom is provided with heat exchanger (6); There is refrigerator pipe (61) to be connected with heat exchanger (7) with heating pipe (62) on the heat exchanger (6).
2. ingot furnace according to claim 1 is characterized in that: cold air is entered by the middle part in the described heat exchanger (6), enters the diffluence pass of 5 * 5 matrixes or 6 * 6 matrixes, is flowed out by the edge.
3. method for preparing quasi-monocrystalline silicon, it is the growth of finishing quasi-monocrystalline silicon in claim 1 or 2 described ingot furnaces.
4. the preparation method of quasi-monocrystalline silicon according to claim 1, it comprises the steps:
A, charging: the raw material that will comprise seed crystal is put into crucible, and wherein seed crystal is tiled in crucible bottom, places primary polysilicon and doped element on seed crystal top, and resistivity is adjusted to 1.5 Ω .cm;
B, heating: in 9 hours, crucible temperature is risen to 1412-1550 ℃;
C, fusing: keep 1412-1550 ℃ of crucible head temperature, open the gas valve of heat exchanger, in 2 hours, gas flow is upgraded to 30SLM, and lasting supply gas, the crucible bottom temperature transfers to 1390-1410 ℃, and whole thaw process continues 8-10 hour;
D, long brilliant: keep 1412-1550 ℃ of crucible head temperature, the crucible bottom gas flow increases to 65SLM from 30SLM in half an hour, and bottom temp is reduced to 1356-1370 ℃ rapidly, lasting 23-25 hour of the brilliant process of whole length from 1390-1410 ℃;
E, close the gas valve of heat exchanger, crucible namely gets the quasi-monocrystalline silicon ingot in 1356-1370 ℃ of annealing, cooling.
5. the preparation method of quasi-monocrystalline silicon according to claim 4, it is characterized in that: the described doped element of step a is boron.
6. the preparation method of quasi-monocrystalline silicon according to claim 4, it is characterized in that: the described crucible temperature of step b is 1550 ℃.
7. the preparation method of quasi-monocrystalline silicon according to claim 4, it is characterized in that: the described head temperature of c step is 1430 ℃; Described crucible bottom temperature is 1410 ℃.
8. the preparation method of quasi-monocrystalline silicon according to claim 4, it is characterized in that: described d step is: keep 1430 ℃ of head temperature, the bottom gas flow increases to 65SLM by 30SLM in half an hour, this moment, bottom temp was reduced to 1356 ℃ rapidly by 1410 ℃, and the brilliant process of whole length continues 24 hours.
9. the preparation method of quasi-monocrystalline silicon according to claim 4 is characterized in that: described e step was 1370 ℃ of annealing 2 hours and cool off and namely got the quasi-monocrystalline silicon ingot in 10 hours.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103628127A (en) * | 2013-11-26 | 2014-03-12 | 江苏大学 | DSS (directional solidification system) quasi-monocrystal silicon growth furnace and growth method of quasi-monocrystal silicon |
| CN104389017A (en) * | 2014-08-18 | 2015-03-04 | 吕铁铮 | Internal inlet gas gas-cooling device of coagulation enhancing block of polycrystalline silicon ingot furnace and polycrystalline silicon ingot furnace |
| CN104404619A (en) * | 2014-08-18 | 2015-03-11 | 吕铁铮 | Polysilicon ingot furnace and coagulation aid block external admission air cooling device thereof |
| CN105780108A (en) * | 2016-04-08 | 2016-07-20 | 江西旭阳雷迪高科技股份有限公司 | Method for modifying G5 polycrystal ingot furnace into G6 polycrstal ingot furnace |
| CN106222741A (en) * | 2016-08-31 | 2016-12-14 | 宜昌南玻硅材料有限公司 | One exempts from out heat-insulation cage ingot casting device and method |
| CN107723793A (en) * | 2017-11-21 | 2018-02-23 | 浙江师范大学 | Crucible bottom heat conducting device and method for high quality polycrystalline silicon growth |
| CN108950681A (en) * | 2017-05-27 | 2018-12-07 | 镇江仁德新能源科技有限公司 | The graphite chassis and polycrystalline ingot furnace of polycrystalline ingot furnace |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103628127A (en) * | 2013-11-26 | 2014-03-12 | 江苏大学 | DSS (directional solidification system) quasi-monocrystal silicon growth furnace and growth method of quasi-monocrystal silicon |
| CN104389017A (en) * | 2014-08-18 | 2015-03-04 | 吕铁铮 | Internal inlet gas gas-cooling device of coagulation enhancing block of polycrystalline silicon ingot furnace and polycrystalline silicon ingot furnace |
| CN104404619A (en) * | 2014-08-18 | 2015-03-11 | 吕铁铮 | Polysilicon ingot furnace and coagulation aid block external admission air cooling device thereof |
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| CN105780108B (en) * | 2016-04-08 | 2019-06-25 | 江西旭阳雷迪高科技股份有限公司 | A kind of method that G5 polycrystalline ingot furnace transform G6 polycrystalline ingot furnace as |
| CN106222741A (en) * | 2016-08-31 | 2016-12-14 | 宜昌南玻硅材料有限公司 | One exempts from out heat-insulation cage ingot casting device and method |
| CN108950681A (en) * | 2017-05-27 | 2018-12-07 | 镇江仁德新能源科技有限公司 | The graphite chassis and polycrystalline ingot furnace of polycrystalline ingot furnace |
| CN108950681B (en) * | 2017-05-27 | 2020-12-15 | 镇江仁德新能源科技有限公司 | Graphite chassis of polycrystal ingot furnace and polycrystal ingot furnace |
| CN107723793A (en) * | 2017-11-21 | 2018-02-23 | 浙江师范大学 | Crucible bottom heat conducting device and method for high quality polycrystalline silicon growth |
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Application publication date: 20130717 |