CN103833038A - Method for purifying silicon through semi-continuous crystallization in silicon alloy melt - Google Patents
Method for purifying silicon through semi-continuous crystallization in silicon alloy melt Download PDFInfo
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- CN103833038A CN103833038A CN201410084115.3A CN201410084115A CN103833038A CN 103833038 A CN103833038 A CN 103833038A CN 201410084115 A CN201410084115 A CN 201410084115A CN 103833038 A CN103833038 A CN 103833038A
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Abstract
The invention discloses a method for purifying silicon through semi-continuous crystallization in silicon alloy melt. The method comprises the steps of heating and melting silicon and Al or Al alloy to form an Al-Si base alloy melt, inserting an air-cooled revolving crystallizing rod in the melt so that silicon crystal is separated out of the alloy melt while such major impurities as B and P are kept in the alloy melt, thus achieving an effect of removing impurities. The air-cooled continuous rotating crystallizing rod is inserted in the melt and relatively high cooling speed is adopted to improve crystal growth speed, so as to realize semi-continuous crystallizing growth in the silicon alloy melt. The method disclosed by the invention has the advantages of being low in energy consumption, free from pollution, high in production efficiency, capable of realizing semi-continuous production, small in investment scale, and simple in production process and equipment operation.
Description
Technical field
The present invention relates to silicon purification field, be specially a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon.
Background technology
Traditional energy is as oil, and the sign of coal exhaustion is day by day obvious, and seriously polluted, and for example at present Chinese " gray haze " PM2.5 emission source 50% is from fuel combustion.Photovoltaic generation has clean, safety, the plurality of advantages such as sustainable use, become one of main new forms of energy, obtained in recent years fostering energetically of multinational government of the world, the output of solar cell and market all present rapid growth, and rate of increase is every year on average all more than 30%.Due to the technical maturity of silicon materials, abundant raw material, price is relatively low, and environment is not had to toxic side effect, in solar cell, occupies an important position.The main raw material of manufacturing solar cell is high-purity solar-grade silicon.In the production of solar cell, the cost of solar-grade silicon material is once up to the more than 50% of total cost, and silicon material is purified the accounting of energy consumption and carbon emission in solar cell manufacturing processed still up to more than 50% at present.Therefore, exploitation has less energy-consumption, low emission, and silicon material purification techniques has great importance cheaply.In traditional silicon purification techniques, chemical method is main flow always, and the silicon material purity that chemical method is purified is high, and quality is good, technology maturation, but chemical method purifying technique is complicated and more difficult control, and seriously polluted, investment is large, and cost is high.The purity limit of metallurgy method purified silicon can only arrive 7N(99.99999%), although can not meet the 9N(99.9999999% of semiconducter device requirement) purity, can meet the desired 6N(99.9999% of solar-grade silicon material completely) purity.And metallurgy method purifies and have less investment, floor space is little, founds the factory fast, and energy consumption is low, pollutes littlely, and the advantage that cost is low, is therefore a kind of up-and-coming purification techniques.
The Major Difficulties of metallurgy method purifying technique is the removal of critical impurities element B and P.Mainly contain now slag making air blast, vacuum beam metallurgy method, silicon alloy method etc.Slag making air blast is to utilize B to be easily oxidized compared with silicon, and the higher feature of the vapour pressure of its oxide compound, in melt, pass into the gas of oxidisability as the slag of steam or oxidisability, make B oxidation enter bubble or slag mutually in and reach removal object, but slag making air blast is as undesirable in the removal effect of P for some impurity element.In vacuum beam metallurgy method, utilize the high-vapor-pressure of P to use in a vacuum beam bombardment silicon liquid, P is vapored away, owing to adopting vacuum technique, after melting melt amount increases, refining effect declines, can only be each port one port melting, production efficiency is low, be difficult to realize scale operation, and energy consumption is quite high.These two kinds of methods all need to utilize different processing steps to remove respectively B and P, and smelting temperature is high, and the time is long.It is by silicon and Al, Sn, Ga that silicon alloy method is purified, Cu, the melting of Fe equal solvent metal mixed, forms uniform alloy melt, then the processing such as slag making air blowing in addition, crystallisation by cooling again, in process of cooling, silicon can be with sheet or the growth of stratiform form from melt, form the silicon of higher degree, the Eutectic Silicon in Al-Si Cast Alloys of impurity element and part remains in solvent metal, finally will, by the silicon growing and base solvent metal separation, obtain the silicon of purifying.The method smelting temperature is low, time is short, can significantly reduce the energy consumption of melting, and can remove B simultaneously, all other impurity elements beyond P and alloy substrate element, technique is relatively simple, and after melting melt amount increases, refining effect can not decline, extremely be conducive to scale operation, become in recent years people's study hotspot.
At present, silicon alloy method method of purification has discontinuous crystalline growth and continuous crystallisation to grow two kinds.
US Patent No. 42567117A(R.K.Dawless, Silicon purification method) in, Si and Al are formed after alloy, cooling makes the growth of Si sheet, then with a block pressur plate, the Si sheet growing is pressed onto to crucible bottom, again unnecessary alloy melt is poured out to crucible, collect remaining Si sheet, realized discrete Si sheet crystalline growth, but the method speed of growth is slow, production efficiency is low, the separation method complexity of Si sheet and melt, operational difficulty.
World patent WO2010098676A1(H.Tathgar, Method for the production of solar grade silicon) in, adopt the stove of two molten Si alloys, higher stove of temperature is used for adding and melts Si raw material, then the Si alloy melt of high temperature is pumped to second stove that temperature is lower after filtering, in this stove, Si grows up to larger crystal and is regularly taken out, remaining Al-Si melt is withdrawn in first stove by a filtering net again, realize the continuous purification of Si, but the method Si crystalline growth velocity is slow, equipment and operating process are very complicated, be difficult to realize accurate control.
US Patent No. 3933981(G.F.Wakefield, H.S.Nagaraja Setty, Tin-Lead purification of silicon) in, a crucible is divided into high temperature and two parts of low temperature with thermal baffle, melt raw material Si in high-temperature part, in low temperature part, with upwards pulling growth Si rod of a Si seed crystal rod, realized the continuous purification growth of Si, but the method Si crystalline growth velocity is slow, equipment and operating process are all very complicated, are difficult to realize accurate control.
Chinese patent CN101798705A(Jiang Jun is auspicious, Hu Jianfeng, Xu's Jing jade, Dai Ning, Chu Junhao, a kind of method and special purpose device that from low-temperature melt, continuous crystallisation is purified) in, aforesaid method is improved, in low temperature part, with upwards pull growth Si rod of a water-cooled crystallization head, realize the continuous purification of Si, its growth pull rate is than increasing with Si seed pulling crystal bar, but be still that equipment and operating process are all very complicated, be difficult to realize accurate control.
Summary of the invention
The object of this invention is to provide a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon, the problem existing to solve prior art.
In order to achieve the above object, the technical solution adopted in the present invention is:
A kind of from silicon alloy melt the device of semicontinuous crystallization and purification silicon, it is characterized in that: include supporting seat, supporting seat one side is provided with airtight process furnace, in process furnace, be provided with crucible, described supporting seat top is vertically connected with support bar, supporting bar top is supported with drive-motor seat, on drive-motor seat, drive-motor is installed, drive-motor output shaft passes straight down drive-motor seat and is connected with vertical linear guide, on described linear guide, be fixed with brilliant rotating motor seat, on brilliant rotating motor seat, brilliant rotating motor is installed, brilliant rotating motor seat seat end is suspended from process furnace top, and brilliant rotating motor seat seat end is rotatablely equipped with belt pulley, described brilliant rotating motor output shaft is in transmission connection by belt and belt pulley, described belt pulley center is fixed with the crystallizatio pole of vertical inner hollow, the sealing of described crystallizatio pole bottom, crystallizatio pole bottom is stretched in crucible through process furnace straight down, in crystallizatio pole, be vertically inserted with cooling tracheae.
Described a kind of from silicon alloy melt the device of semicontinuous crystallization and purification silicon, it is characterized in that: described crystallizatio pole material is high temperature material preferably stainless steel, or vitrified pipe, or silica tube.
Described a kind of from silicon alloy melt the device of semicontinuous crystallization and purification silicon, it is characterized in that: described cold gas tube material is high temperature material preferably stainless steel, or vitrified pipe, or silica tube.
A method for semicontinuous crystallization and purification silicon from silicon alloy melt, is characterized in that: comprise the following steps:
(1) batching: industrial silicon and flux metal mixed are put into crucible, and the ratio of industrial silicon accounts for 20%～60% of gross weight;
(2) add hot smelting: crucible is put into process furnace and heat, until industrial silicon and flux metal are molten into well-mixed alloy melt completely, heat fused temperature is 600～1500 DEG C, then alloy melt is cooled to the temperature slightly higher than alloying constituent liquidus line;
(3) crystallization: undertaken in the crystallizatio pole insertion alloy melt of air cooling pass into cooling gas by cooling tracheae, and drive crystallizatio pole to keep the rotating speed of 5r/min～200r/min by brilliant rotating motor, cooling gas flow is 0.1～10m
3/ hr, starts to be cooled to 600 DEG C～700 DEG C from liquidus temperature with the speed of cooling of 0.1 DEG C/min to 10 DEG C/min, crystallizatio pole is proposed from alloy melt can obtain silicon xln.
Described a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon, it is characterized in that: in step (1), flux metal is Al, or the alloy of Al and Sn, or the alloy of Al and Ga, or the alloy of Al and Cu, or the alloy of Al and Fe.
Described a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon, it is characterized in that: in step (2), the type of heating of process furnace is resistive heating, or gas heating, or induction heating.
Described a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon, it is characterized in that: in step (3), the alloy melt forming after fusing can be blown or slag making processing.
Described a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon, it is characterized in that: the preferred air of cooling gas passing into crystallizatio pole by cooling tracheae can be also nitrogen, or argon gas.
Described a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon, it is characterized in that: in crystallisation process, furnace temperature of heating furnace declines according to the rate of temperature fall of setting.
Advantage of the present invention is:
1) can remove various impurity, particularly B and the P in metallurgical grade silicon simultaneously,
2) less energy-consumption, service temperature is far below the fusing point of silicon.
3) pollution-free, in purification process, there is no the generations such as waste gas, waste water, waste residue.
4) production efficiency is high, and silicon xln fast growth, can realize semicontinuous production, compares Discontinuous manufacture, and the speed of growth improves more than 3 times,
5) scale of investment is little, and operation of equipment and technique are simple, compares continuous production, and investment will reduce by half, and production process cost of labor will reduce by half above.
Brief description of the drawings
Fig. 1 is device schematic diagram of the present invention.
Embodiment
As shown in Figure 1.A kind of from silicon alloy melt the device of semicontinuous crystallization and purification silicon, include supporting seat 3, supporting seat 3 one sides are provided with airtight process furnace 9, in process furnace 9, be provided with crucible 8, supporting seat 3 tops are vertically connected with support bar 11, support bar 11 apical support have drive-motor seat 12, drive-motor 1 is installed on drive-motor seat 12, drive-motor 1 output shaft passes straight down drive-motor seat 12 and is connected with vertical linear guide 2, on linear guide 2, be fixed with brilliant rotating motor seat 10, on brilliant rotating motor seat 10, brilliant rotating motor 4 is installed, 10 ends of brilliant rotating motor seat are suspended from process furnace 9 tops, and 13 ends of brilliant rotating motor seat are rotatablely equipped with belt pulley 5, brilliant rotating motor 4 output shafts are in transmission connection by belt and belt pulley 5, belt pulley 5 centers are fixed with the crystallizatio pole 7 of vertical inner hollow, crystallizatio pole 7 bottom sealings, crystallizatio pole 7 bottoms are stretched in crucible 8 through process furnace 9 straight down, in crystallizatio pole 7, be vertically inserted with cooling tracheae 6.
A method for semicontinuous crystallization and purification silicon from silicon alloy melt, comprises the following steps:
(1) batching: industrial silicon and flux metal mixed are put into crucible, and the ratio of industrial silicon accounts for 20%～60% of gross weight;
(2) add hot smelting: crucible is put into process furnace and heat, until industrial silicon and flux metal are molten into well-mixed alloy melt completely, heat fused temperature is 600～1500 DEG C, then alloy melt is cooled to the temperature slightly higher than alloying constituent liquidus line;
(3) crystallization: undertaken in the crystallizatio pole insertion alloy melt of air cooling pass into cooling gas by cooling tracheae, and drive crystallizatio pole to keep the rotating speed of 5r/min～200r/min by brilliant rotating motor, cooling gas flow is 0.1～10m
3/ hr, starts to be cooled to 600 DEG C～700 DEG C from liquidus temperature with the speed of cooling of 0.1 DEG C/min to 10 DEG C/min, crystallizatio pole is proposed from alloy melt can obtain B the silicon xln that P and other impurity contents are lower.
In step (1), flux metal is Al, or the alloy of Al and Sn, or the alloy of Al and Ga, or the alloy of Al and Cu, or the alloy of Al and Fe.
In step (2), the type of heating of process furnace is resistive heating, or gas heating, or induction heating.
In step (3), the alloy melt forming after fusing can be blown or slag making processing.
The preferred air of cooling gas passing into crystallizatio pole by cooling tracheae, can be also nitrogen, or argon gas.
In crystallisation process, furnace temperature of heating furnace declines according to the rate of temperature fall of setting.
Specific embodiment 1:
Starting material 358.7g metalluragical silicon (trade mark 3303) is mixed with 1076.1g metallic aluminium (purity 96.5%), the exemplary impurity content of silicon and aluminium is heated to 950 DEG C in table 1. by mixture and melts and be incubated half hour, then stir melt with quartz pushrod and mix rear insertion crystallizatio pole completely, adopt the stainless steel tube of diameter 25.4mm to do crystallizatio pole, rotating speed is 130r/min, adopt the stainless steel tube of diameter 8mm to do cooling tracheae to the air that passes into room temperature in crystallizatio pole, Ventilation Rate is 0.8m
3/ hr, meanwhile, reduces furnace, and rate of cooling is 1.7 DEG C/min, is cooled to 616 DEG C, and crystallizatio pole is proposed to melt, and crystallizatio pole surface, with the silicon xln of growth, is knocked silicon xln is separated with crystallizatio pole with hammer, obtains 90.84g silicon xln.After silicon xln is soaked and removes the Al that adheres to dilute hydrochloric acid, carry out ICP-OES test, gained the results are shown in Table 2.
Exemplary impurity content (ppmw) in table 1. starting material
| Impurity element | B | P | Fe | Ti |
| Raw material Si | 7 | 11 | 1357 | 79 |
| Raw material A l | 7 | 35 | 9279 | 262 |
Exemplary impurity content (ppmw) in the silicon xln that table 2. is grown
| Impurity element | B | P | Fe | Ti |
| Purification Si | 2.7 | 5.1 | 501 | 11 |
Specific embodiment 2:
Starting material 622.5g metalluragical silicon (trade mark 3303) is mixed with 1228g metallic aluminium (purity 96.5%), the exemplary impurity content of silicon and aluminium is heated to 1050 DEG C in table 1. by mixture and melts and be incubated half hour, then stir melt with quartz pushrod and mix rear insertion crystallizatio pole completely, adopt the stainless steel tube of diameter 25.4mm to do crystallizatio pole, rotating speed is 130r/min, adopt the stainless steel tube of diameter 8mm to do cooling tracheae to the air that passes into room temperature in crystallizatio pole, Ventilation Rate is 0.1m
3/ hr, meanwhile, reduces furnace, and rate of cooling is 0.12 DEG C/min, is cooled to 602 DEG C, and crystallizatio pole is proposed to melt, and crystallizatio pole surface, with the silicon xln of growth, is knocked silicon xln is separated with crystallizatio pole with hammer, obtains 78.4g silicon xln.After silicon xln is soaked and removes the Al that adheres to dilute hydrochloric acid, carry out ICP-OES test, gained the results are shown in Table 3.
Exemplary impurity content (ppmw) in the silicon xln that table 3. is grown
| Impurity element | B | P | Fe | Ti |
| Purification Si | 2.7 | 6.5 | 480 | 21 |
Specific embodiment 3:
Starting material 642.8g metalluragical silicon (trade mark 3303) is mixed with 1499.8g metallic aluminium (purity 96.5%), the exemplary impurity content of silicon and aluminium is heated to 1050 DEG C in table 1. by mixture and melts and be incubated half hour, then stir melt with quartz pushrod and mix rear insertion crystallizatio pole completely, adopt the alumina tube of diameter 25.4mm to do crystallizatio pole, rotating speed is 25r/min, adopt the stainless steel tube of diameter 8mm to do cooling tracheae to the air that passes into room temperature in crystallizatio pole, Ventilation Rate is 0.1m
3/ hr, meanwhile, reduces furnace, and rate of cooling is 0.2 DEG C/min, is cooled to 600 DEG C, and crystallizatio pole is proposed to melt, and crystallizatio pole surface, with the silicon xln of growth, is knocked silicon xln is separated with crystallizatio pole with hammer, obtains 186g silicon xln.After silicon xln is soaked and removes the Al that adheres to dilute hydrochloric acid, carry out ICP-OES test, gained the results are shown in Table 4.
Exemplary impurity content (ppmw) in the silicon xln that table 4. is grown
| Impurity element | B | P | Fe | Ti |
| Purification Si | 2.1 | 6.6 | 483 | 18 |
Claims (9)
1. the device of a semicontinuous crystallization and purification silicon from silicon alloy melt, it is characterized in that: include supporting seat, supporting seat one side is provided with airtight process furnace, in process furnace, be provided with crucible, described supporting seat top is vertically connected with support bar, supporting bar top is supported with drive-motor seat, on drive-motor seat, drive-motor is installed, drive-motor output shaft passes straight down drive-motor seat and is connected with vertical linear guide, on described linear guide, be fixed with brilliant rotating motor seat, on brilliant rotating motor seat, brilliant rotating motor is installed, brilliant rotating motor seat seat end is suspended from process furnace top, and brilliant rotating motor seat seat end is rotatablely equipped with belt pulley, described brilliant rotating motor output shaft is in transmission connection by belt and belt pulley, described belt pulley center is fixed with the crystallizatio pole of vertical inner hollow, the sealing of described crystallizatio pole bottom, crystallizatio pole bottom is stretched in crucible through process furnace straight down, in crystallizatio pole, be vertically inserted with cooling tracheae.
According to claim 1 a kind of from silicon alloy melt the device of semicontinuous crystallization and purification silicon, it is characterized in that: described crystallizatio pole material is high temperature material preferably stainless steel, or vitrified pipe, or silica tube.
According to claim 1 a kind of from silicon alloy melt the device of semicontinuous crystallization and purification silicon, it is characterized in that: described cold gas tube material is high temperature material preferably stainless steel, or vitrified pipe, or silica tube.
4. a method for semicontinuous crystallization and purification silicon from silicon alloy melt, is characterized in that: comprise the following steps:
(1) batching: industrial silicon and flux metal mixed are put into crucible, and the ratio of industrial silicon accounts for 20% ~ 60% of gross weight;
(2) add hot smelting: crucible is put into process furnace and heat, until industrial silicon and flux metal are molten into well-mixed alloy melt completely, heat fused temperature is 600～1500 DEG C, then alloy melt is cooled to the temperature slightly higher than alloying constituent liquidus line;
(3) crystallization: undertaken in the crystallizatio pole insertion alloy melt of air cooling passing into cooling gas, and drive crystallizatio pole to keep the rotating speed of 5r/min～200 r/min by brilliant rotating motor, cooling gas flow is 0.1～10m
3/ hr, starts to be cooled to 600 DEG C～700 DEG C from liquidus temperature with the speed of cooling of 0.1 DEG C/min to 10 DEG C/min, crystallizatio pole is proposed from alloy melt can obtain silicon xln.
According to claim 4 a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon, it is characterized in that: in step (1), flux metal is Al, or the alloy of Al and Sn, or the alloy of Al and Ga, or the alloy of Al and Cu, or the alloy of Al and Fe.
According to claim 4 a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon, it is characterized in that: in step (2), the type of heating of process furnace is resistive heating, or gas heating, or induction heating.
According to claim 4 a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon, it is characterized in that: in step (3), the alloy melt forming after fusing can be blown or slag making processing.
According to claim 4 a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon, it is characterized in that: the preferred air of cooling gas passing into crystallizatio pole by cooling tracheae can be also nitrogen, or argon gas.
According to claim 4 a kind of from silicon alloy melt the method for semicontinuous crystallization and purification silicon, it is characterized in that: in crystallisation process, furnace temperature of heating furnace declines according to the rate of temperature fall of setting.
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| CN104556044A (en) * | 2014-12-10 | 2015-04-29 | 中国科学院等离子体物理研究所 | Method for quickly removing boron from silicon by introducing gas to Al-Si alloy |
| CN107557582A (en) * | 2017-07-25 | 2018-01-09 | 昆明理工大学 | A kind of selective extraction and the method for being enriched with valuable metal in more metals resources |
| CN110592667A (en) * | 2019-10-18 | 2019-12-20 | 衡水学院 | Method for purifying silicon |
| CN113026109A (en) * | 2021-03-08 | 2021-06-25 | 中国科学院过程工程研究所 | Device and method for preparing high-purity metal through rotary segregation purification |
| CN115261970A (en) * | 2022-06-17 | 2022-11-01 | 柳州市智甲金属科技有限公司 | Lifting mechanism, aluminum purification device applying same and method |
| CN115747515A (en) * | 2022-11-25 | 2023-03-07 | 宁波锦越新材料有限公司 | Continuous purification equipment of high-purity aluminium |
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| CN115261970A (en) * | 2022-06-17 | 2022-11-01 | 柳州市智甲金属科技有限公司 | Lifting mechanism, aluminum purification device applying same and method |
| CN115747515A (en) * | 2022-11-25 | 2023-03-07 | 宁波锦越新材料有限公司 | Continuous purification equipment of high-purity aluminium |
| CN115747515B (en) * | 2022-11-25 | 2023-07-14 | 宁波锦越新材料有限公司 | High-purity aluminum continuous purification equipment |
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