CN101665253B - Polysilicon purification method and crucible and purification device used for polysilicon purification - Google Patents
Polysilicon purification method and crucible and purification device used for polysilicon purification Download PDFInfo
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- CN101665253B CN101665253B CN200910177448XA CN200910177448A CN101665253B CN 101665253 B CN101665253 B CN 101665253B CN 200910177448X A CN200910177448X A CN 200910177448XA CN 200910177448 A CN200910177448 A CN 200910177448A CN 101665253 B CN101665253 B CN 101665253B
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Abstract
A polysilicon purification method includes the following steps: impurity containing low purity polysilicon is maintained to be fusion state for a period of time in a crucible; the polysilicon liquid in fusion state is gradually cooled and solidified from the bottom to the top through relative move of the crucible and an induction coil arranged at the periphery of the crucible in a surrounding way; and the solidified polysilicon after cooling is taken out from the crucible and is purified by mechanical cutting. The invention also discloses a crucible used for polysilicon purification and a purification device provided with the crucible. The invention has the advantages that the polysilicon purification method and device has strong operability, low cost, no secondary pollution in purification process and the like.
Description
Technical field
The present invention relates to the purify production technique of (or refining) of polysilicon, especially with a kind of polysilicon purification method and a kind ofly be used for the crucible that polysilicon purifies and the equipment for purifying with this crucible is relevant.
Background technology
In the last few years, for the energy and environment problem, caused showing great attention to of the whole world as environmental problems such as traditional fossil energy mass consumption and Global warmings.Under this background, global photovoltaic industry fast development, the silicon demand of silicon solar cell material increases sharply.Caused the shortage of silicon materials thus, price is higher, becomes the bottleneck of photovoltaic industry development.Improving polysilicon output and quality, reducing cost is the direction of polysilicon industry development.
The scale operation polysilicon mainly adopts the chlorination purification techniques both at home and abroad at present, and this technology is that metallurgical grade silicon and anhydrous hydrogen chloride are reacted generation trichlorosilane (SiHCI
3), adopt distillation to purify then and obtain high-purity SiHCI
3, under 1100 ℃ temperature condition, reduce again with high-purity hydrogen, obtain the above polysilicon of purity 9N.This technological investment scale is big and space that reduce is limited, will produce a large amount of obnoxious flavoures in the production process, needs very complicated Technology to carry out the vent gas treatment utilization.Purity requirement is generally about 6N silicon solar cell to silicon, and the silicon of 6N purity can reach the commercial transformation efficiency that requires.Therefore industry is thirsted for a kind of technology that can prepare the silicon raw material that is used for solar cell cheaply of exploitation, in recent years by oxidation-reduction reaction with solidify/and the metallurgical technology of segregation produces high-purity solar-grade polysilicon and is subject to the people's attention and develops.
Unidirectional solidification/segregation purification techniques extensively is used in the purification aspect of semiconductor material.The ratio of the impurity concentration in the impurity concentration in the solid and the melt is called segregation coefficient.Therefore, in the melt crystallization process, equilibrium segregation coefficient constantly segregates to the melt from solid-liquid interface much smaller than 1 impurity, form conveying and the enrichment of impurity to melt, treat that the whole crystallizations of melt finish, final set partly is the enrichment region of impurity, the polycrystalline semiconductor material that adopts mechanically cutting to obtain to purify.This technology is used to silicon equally and purifies.How much content of impurity element B, P can determine the conduction type of silicon in the silicon, must strict control.These elements have very large segregation coefficient, are about 0.8,0.35 respectively.Utilize above-mentioned unidirectional solidification/segregation DeGrain in fact of purifying.Removal about B, P in the silicon has various other ways.
Say various single crystal growth apparatus widely, comprise the single crystal growing furnace or the zone melting furnace of vertical pulling method, and casting solidification equipment can be called as unidirectional solidification/segregation equipment.But utilize these equipment purification counter investments higher, be embodied in following two aspects: one, the investment of equipment itself and support equipment is bigger; Two, single crystal growing furnace and ingot furnace consumptive material expense in process of production is higher, and promptly production cost is higher, and as high purity quartz or the plumbago crucible that uses in the production process, its price is all very expensive.And be not easy to improve single furnace output, because the required internal volume of quartz or plumbago crucible is when increasing, the cost of making this quartz or plumbago crucible just is geometricprogression and rises.Though in the zone melting furnace purification process without consumptive materials such as crucibles, its single furnace output is low, production efficiency is low.Three, these production processes are all kept away unavoidable meeting HIGH-PURITY SILICON are produced secondary pollution, and traditional technology is when for example using plumbago crucible, because the volatilization of graphite easily causes secondary pollution to metalluragical silicon.
A large amount of work is being done by Japan JFE company aspect the Pure Silicon Metal purification, a lot of patents have been applied for simultaneously, its main technique route is: with the Pure Silicon Metal of buying is raw material, at first with Pure Silicon Metal heat fused under vacuum environment, utilizes beam bombardment to get rid of phosphorus (P).Boron (B) is removed with plasma gun (Plasma Torch) winding-up in the fusing back in argon (Ar) gas then, then by extracting the polysilicon of 6 nine (6N) after the directional freeze.Using plain metal refinement operation can reduce to the concentration of metallic impurity below the 0.1ppmw.This process need repeatedly melts-process of setting, and production efficiency and cost are all very high.
Publication number is CN1569629A, name is called the Chinese invention patent of " manufacture method of photovoltaic silicon ", 1), in the negative pressure of vacuum chamber its disclosed silicon method of purification is:, heat up 〉=1850 ℃ with medium-frequency induction furnace, the fusion of raw material chemical grade silicon, remove aluminium, boron, phosphorus, sulphur, carbon and other impurity; 2), adopt protection of inert gas in melted silicon, to feed 1: (1.1～1.5) hydrogen and water vapor, stir refining 〉=2 hour, pour coagulator into after making other element high-temperature evaporation; 3), carry out directional freeze from the bottom up in the negative pressure of vacuum chamber, remove de-iron and other heavy metal; 4) be cooled to normal temperature, at a slow speed, get photovoltaic silicon.This method treatment time is long, must fall stove in technological process, has increased contamination of heavy.
Publication number is that the Japanese Patent of JP3205352 has related to the technology of using plasma body in the silicon refining.Day JP2001-58811 of the present invention has spoken of and has used in the silicon refining in argon gas with addition of a certain proportion of water vapour, feeds then in the fused silicon liquid.What these were all only considered is the B element of how removing in the silicon, in process of production once after the fusing, will not make silicon liquid take off B, take off the consideration that combines of P and this several links of unidirectional solidification/segregation.
Summary of the invention
Unresolved problems of the prior art, the invention provides a kind of technology simply, polysilicon purification method cheaply.
The present invention also provides a kind of crucible that polysilicon is purified that is used for.
The present invention also provides a kind of equipment for purifying that polysilicon is purified that is used for.
Technical scheme of the present invention is as follows:
Polysilicon purification method of the present invention comprises step:
Step S1: in crucible, make polysilicon keep the molten state certain hour than low-purity;
Step S2: by beginning from the bottom to top cooled and solidified gradually around being arranged on polysilicon liquid that relatively moving of ruhmkorff coil around the crucible arm and crucible make described molten state;
Step S3: from crucible, extract the described polysilicon after the cooled and solidified, reach described polysilicon after flaw-piece obtains to purify end to end by mechanically cutting.
Method of purification of the present invention, preferred, described crucible comprises the stool of bottom and is arranged on sidewall of crucible on the stool, and described sidewall of crucible is made up of water-cooled copper, and the material of stool has the copper or the stainless material of water-cooling channel in being.
Method of purification of the present invention, preferred, step S2 can repeat certain number of times as required.
Method of purification of the present invention, preferred, in step S1, liquid metalluragical silicon remained in 1450 ℃ of-1850 ℃ of scopes more than 30 minutes, and furnace atmosphere is rare gas element or high vacuum, and furnace pressure can be adjusted according to process requirements, and its variation range is 1 * 10
-3Pa-1.5 * 10
5In the Pa scope.。
Method of purification of the present invention, preferred, in step S1, can be by auxiliary thermal source or directly described polysilicon is heated or refining, can in described metalluragical silicon liquid, feed hydrogen or moisture when carrying out refining with the enhancing refining effect.
Method of purification of the present invention, preferred, the relatively moving of described ruhmkorff coil and crucible body can comprise ruhmkorff coil fixedly crucible move, or the crucible fixed inductor moves, or ruhmkorff coil and crucible are all mobile.
Method of purification of the present invention, preferred, in step S1, the purifying polycrystalline silicon form for the treatment of that contains impurity that drops into described crucible can be powder or piece material, and its temperature can be normal temperature or high temperature, or the liquid of the polysilicon of molten state is directly poured in the crucible.When described polysilicon is powdery or bulk, can also can heat and fusing it by auxiliary thermal source as the case may be directly to its heating and fusing, described auxiliary thermal source can be plasma arc or adds easy induction thermal objects etc.
Of the present inventionly be used for the crucible that polysilicon is purified, comprise the stool of bottom and be arranged on sidewall of crucible on the stool, described sidewall of crucible is made up of water-cooled copper, and the material of stool has the copper or the stainless material of water-cooling channel in being.
Equipment for purifying of the present invention is used for metalluragical silicon and purifies, and has crucible of the present invention.
Equipment for purifying of the present invention, preferably, described equipment for purifying comprises furnace shell and is arranged at described crucible in the furnace shell, also comprise ruhmkorff coil around described crucible setting, be used for the ruhmkorff coil lifting jacking system, be used for crucible lifting the crucible lifting system, be used for the metalluragical silicon in the crucible is heated or purified auxiliary thermal source and be used for the inflation system of inflating and be used to make the vacuum system that becomes and keep vacuum in the described furnace shell in described furnace shell.
Beneficial effect of the present invention is the following aspects, and crucible of the present invention can be described as cold-crucible or induction cold-crucible.The present invention is the easy control the water-cooled inductive crucible, organically is combined togather with the link of air blowing, vacuum refinement and unidirectional solidification/segregation.Concrete comprise following some:
1, water-cooled inductive crucible of the present invention is compared with single crystal growing furnace, ingot furnace and zone melting furnace, and is workable.
2, use water-cooled inductive crucible of the present invention and polysilicon purification method of the present invention and equipment and carry out the silicon purification, avoided polysilicon secondary pollution purifying; Heat with the purified process in because the water-cooled effect of sidewall of crucible, the part in the periphery of silicon liquid near the crucible inwall forms a silicon shell, this silicon shell has effectively prevented to use in the prior art quartz crucible or the easily secondary pollution of generation of plumbago crucible institute.
3, use water-cooled inductive crucible of the present invention and polysilicon purification method of the present invention and equipment and carry out the silicon purification, single furnace output is big, can accomplish 500kg or more very easily; And quartz crucible or the plumbago crucible used in the existing purification techniques, if the crucible volume is done greatly, required cost can increase greatly.
4, use the water-cooled inductive crucible and carry out the silicon purification, equipment is simple, very easily expands output.
5, use water-cooled inductive crucible of the present invention and polysilicon purification method of the present invention and equipment and carry out the silicon purification, equipment cost is low.
6, use water-cooled inductive crucible of the present invention and polysilicon purification method of the present invention and equipment, the production process cost is low.Because purification process does not re-use other crucible, as quartz or plumbago crucible, cold-crucible can also be reused simultaneously.
7, use water-cooled inductive crucible of the present invention and polysilicon purification method of the present invention and equipment, production process only needs once just can realize taking off B after the fusing, take off P and this several links of unidirectional solidification/segregation, and technology compactness, efficient height, cost are low.
Description of drawings
Fig. 1 is the synoptic diagram of the equipment for purifying of the preferred embodiment of the present invention.
Embodiment
In order to make technical problem to be solved by this invention, technical scheme and beneficial effect clearer,, the present invention is further elaborated below in conjunction with specific embodiment.Should be pointed out that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
Introduce the crucible and the equipment for purifying of the embodiment of the invention earlier.
As shown in Figure 1, the crucible that is used for the polysilicon purification of the embodiment of the invention, the stool 12 and the sidewall of crucible 5 that is arranged on the stool that comprise the bottom, the internal space that sidewall of crucible 5 surrounds is used for the polysilicon after polysilicon purification process polycrystalline silicon raw material, polysilicon liquid (molten state liquid) or cooled and solidified successively ccontaining to be purified, described sidewall of crucible is made up of a plurality of water-cooled coppers, can be provided with the water entry and the backwater channel that are connected in the water-cooled copper; The material of stool has the copper or the stainless material of water-cooling channel in being.Therefore, crucible of the present invention can be called cold-crucible.As shown in Figure 1, be provided with cooling water intake 7 and cooling water outlet 8 in crucible bottom, last aquaporin in each water-cooled copper all links to each other with cooling water intake 7 by certain pipeline of the water-cooling channel in the stool, and the backwater channel in each water-cooled copper all links to each other with cooling water outlet 8 by certain pipeline of the water-cooling channel in the stool.Sidewall of crucible and stool must have enough water-cooled abilities, will guarantee that at least the water in the water-cooling channel does not gasify, and promptly need to have suitable discharge and water pressure.Can ensure the water-cooled ability by detecting water temp, inflow temperature is 20 degrees centigrade usually, and leaving water temperature(LWT) is 30 degrees centigrade.If detecting leaving water temperature(LWT) is higher than 30 degrees centigrade, can consider to increase flooding quantity or intake pressure to keep the water-cooled ability of cold-crucible.
As shown in Figure 1, the equipment for purifying of the preferred embodiment of the present invention comprises the crucible of the preferred embodiment of the present invention.
As shown in Figure 1, the equipment for purifying of the preferred embodiment of the present invention comprises furnace shell 1 and the described crucible that is arranged in the furnace shell 1, and this furnace shell 1 is provided with the crucible access way.Equipment for purifying also comprises ruhmkorff coil 2 around described crucible setting, be used for the ruhmkorff coil jacking system (not shown) of ruhmkorff coil 2 oscilaltions, be used for crucible lifting crucible lifting system (not shown), be used for the polysilicon in the crucible is heated or purified auxiliary thermal source 6 and be used for the inflation system 9 of inflation in described furnace shell 1 and be used to make the vacuum system 10 (or air-bleed system) that becomes in the described furnace shell 1 and keep vacuum.For crucible lifting system and ruhmkorff coil jacking system, can on furnace shell 1 inwall, install the fluctuating orbit of above-below direction, connecting arm is set, connecting arm one end is connected with crucible or ruhmkorff coil 2, the other end is connected in this fluctuating orbit, drives crucible or ruhmkorff coil 2 carries out lifting by connecting arm along the lifting of fluctuating orbit.
Energy required in the heating of described polysilicon, fusing, constant temperature and the directional freeze process is converted into heat energy to electric energy and is applied on the described polysilicon by the electromagnetic induction between the polysilicon in described ruhmkorff coil 2 and the crucible.
Introduce the concrete steps and the embodiment of the method for purification of polysilicon of the present invention below again.
Polysilicon purification method of the present invention, at first the purifying polycrystalline silicon (claiming raw silicon again) for the treatment of that blocky or powdered contains impurity low-purity is put into cold-crucible of the present invention, can also directly inject when raw silicon is high-temperature liquid state.The raw silicon of non high temperature liquid state, need by ruhmkorff coil 2 induction heating, raw silicon is maintained under the liquid state, the silicon liquid temp can remain in 1450 ℃ of-1850 ℃ of scopes, soaking time can be determined according to arts demand, purpose is that raw silicon is thoroughly melted, and has good flowability, is beneficial to the directed fractional condensation of subsequent step.But blanketing with inert gas in the stove also can be kept higher vacuum, and the furnace pressure variation range is bigger, 1 * 10
-3Pa-1.5 * 10
5In the Pa scope.Equipment for purifying inside is provided with auxiliary thermal source 6, and this auxiliary thermal source can be and adds easy induction thermal objects or plasma arc etc., uses in induction initial stage or insulating process, can wait other means liquid towards metalluragical silicons to carry out refining by air blowing in the insulating process.Relatively move by ruhmkorff coil 2 and cold-crucible speed in accordance with regulations then, the polysilicon liquid in the crucible is begun to top cooled and solidified gradually from crucible bottom.Utilize the impurity element dephlegmation in the process of cooling again, in process of cooling Impurity removal to reach the purpose of purifying polycrystalline silicon.
Specifically can may further comprise the steps:
Step 1: blocky or powdered raw silicon is put into cold-crucible low-purity.
Step 2: start vacuum system 10, make the vacuum tightness that reaches certain in the furnace shell 1 of equipment for purifying after, close vacuum system 10, open inflation system 9 again, in stove, charge into high-purity rare gas element, the argon gas as 99.99% is to the pressure of regulation.Charge into rare gas element and can prevent oxidation polysilicon.
Step 3: as the temperature of raw silicon less than 800 ℃, look the particular case of raw silicon, can directly heat by electromagnetic induction raw silicon, also can start auxiliary thermal source 6 and be preheating to 800 ℃ for raw silicon, starting ruhmkorff coil 2 afterwards is heated to the temperature of regulation to raw silicon and makes it fusing, the silicon liquid temp can remain in 1450 ℃ of-1850 ℃ of scopes, and soaking time can be determined according to arts demand.Auxiliary thermal source 6 can be turned off also and can work on according to arts demand after ruhmkorff coil 2 starts.
Step 4: the metalluragical silicon liquid to molten state carries out can carrying out refining between soak, as slag making or to operations such as metalluragical silicon liquid air blowings.Can be blown into hydrogen or moisture (contain the argon gas of hydrogen or contain the argon gas of water vapour).
Step 5: start crucible lifting system or ruhmkorff coil jacking system after insulation or the refining, relatively move, the metalluragical silicon liquid in the crucible is begun to top directional freeze gradually from crucible bottom by coil and cold-crucible speed in accordance with regulations.In process of cooling, utilize the fractional condensation characteristic of impurity in silicon water cooling process of setting, make the two ends of accumulation of impurities, truncate to reach the effect of removal of impurities through crop at last polycrystalline rod at polycrystalline rod.
Introduce the preferred embodiment of a metallurgical silicon purification method of the present invention below.
As shown in Figure 1, open fire door, installing the blocky raw silicon of 200kg, the crucible of purity about 2N put into furnace shell 1, and material piece size is in the 100-150mm scope, and temperature is a room temperature.The crucible size is: diameter of phi 500mm, high 600mm.Close fire door.By vacuum system 10, vacuumize and make furnace shell 1 interior vacuum tightness reach 5Pa, close vacuum system 10 and in stove, feed high-purity argon gas to a normal atmosphere again, and then open vacuum system 10 (or air-bleed system) and make that vacuum tightness reaches 5Pa in the stove, fill high-purity argon gas to a normal atmosphere again, triplicate makes furnace pressure keep a barometric point at last altogether, and keeping the flow of high-purity argon gas is the flow of 1 Liter Per Minute, and promptly furnace pressure is running balance.Energising begins by the raw silicon induction heating in 2 pairs of crucibles of ruhmkorff coil, up to blocky raw silicon fusing, kept this molten state 30 minutes, begin to start crucible lifting system or coil jacking system, relatively move by coil 2 and cold-crucible speed (this fixing speed for example can be 5 millimeters/hour) in accordance with regulations, the raw silicon that makes molten state begins to top cooled and solidified gradually from crucible bottom.Utilize the impurity segregation characteristic, make accumulation of impurities at the solid two ends.Treat to open furnace shell 1 after the furnace charge cooling in the crucible, take out crucible, obtain the furnace charge after the cooled and solidified, the polysilicon after the furnace charge that reaches surrounded surface end to end of excision furnace charge promptly obtains purifying.
Its composition analysis result is shown in table 1, table 2 and table 3 before and after the purification of the embodiment of the invention, analytical procedure is ICP-OES (Inductively Coupled Plasma Optical Emission Spectrometer, the inductive coupling plasma emission spectrograph method), the ppmw of unit.Shown in table 1, table 2 and table 3, after purifying with metallurgical silicon purification method of the present invention, each foreign matter content in the raw silicon all has tangible reduction.Negative representative in the table does not detect this composition.
Table 1
| The composition title | Fe | Al | Ca | Ti | Ni | B | P |
| Before the processing | 1280 | 510 | 980 | 182 | 46 | 21 | 32 |
| After the processing | 113 | 30 | 54 | 1.5 | 0.7 | 19 | 15 |
Table 2
| Dopant species | Content in the raw silicon | Content in the polysilicon after the purification |
| Fe | 2760.335491 | 171.2637782 |
| Dopant species | Content in the raw silicon | Content in the polysilicon after the purification |
| Al | 289.0571641 | 25.04043029 |
| Ca | 273.3547744 | 49.0528471 |
| B | 6.223315145 | 7.095652715 |
| P | 39.72106152 | 20.14056969 |
| K | 0.296260025 | 0.306010017 |
| Na | 1.92130295 | 2.68200791 |
| Mg | -8.740393245 | 3.911143195 |
| Mn | 35.16326299 | -0.206000182 |
| Ni | 136.0662479 | 3.698595563 |
| Ti | 99.68788567 | 4.587921742 |
| Cu | 35.30182322 | 0.777484276 |
| Co | 2.450454806 | -2.054470922 |
| Cr | 57.65849263 | 4.783011435 |
| V | 24.7078472 | 0.801076785 |
| Zn | -56.30143808 | -2.89429236 |
Table 3
| Dopant species | Content in the raw silicon | Content in the polysilicon after the purification |
| Fe | 2545.004233 | 132.963298 |
| Al | 268.9096149 | 15.49397483 |
| Ca | 237.825662 | -19.15773874 |
| Dopant species | Content in the raw silicon | Content in the polysilicon after the purification |
| B | 5.975040805 | 7.779196935 |
| P | 40.93609287 | 16.19473972 |
| K | 0.258479283 | 0.315136426 |
| Na | 3.25726887 | 2.08493925 |
| Mg | -8.507276595 | -6.531443245 |
| Mn | 30.78143608 | -0.607872074 |
| Ni | 105.0922565 | 1.817715096 |
| Ti | 95.99995754 | 4.220282263 |
| Cu | 33.98035777 | 0.514740053 |
| Co | 2.311090248 | -2.435383727 |
| Cr | 6.04874815 | -1.850399722 |
| V | 22.72041541 | 0.876972093 |
| Zn | -56.30143808 | -2.89429236 |
Among other embodiment of the present invention, sidewall of crucible can be made up of and there is water-cooling channel copper pipe inside copper pipe.
Among other embodiment of the present invention, the relatively moving of ruhmkorff coil and crucible body can be that coil stationary is motionless and crucible moves, and also can be that crucible maintains static and coil moves, or the two all moves.In the embodiment that has only ruhmkorff coil to move, the ruhmkorff coil jacking system can only be set, and save the crucible lifting system.Otherwise, in the embodiment that has only crucible to move, the crucible lifting system can only be set, and save the ruhmkorff coil jacking system.The relative moving speed of ruhmkorff coil and crucible body is determined according to concrete processing requirement.
In different embodiments of the invention, ruhmkorff coil both can be one ruhmkorff coil, also can be ruhmkorff coil in groups.
In other embodiments of the invention, the cooled and solidified process of the molten state metalluragical silicon liquid in the crucible can be one time also can be multipass, as carry out multipass, can further strengthen refining effect.
In other embodiments of the invention, raw silicon can be removed volatile impurity or some compounds in the silicon by the way that keeps high vacuum in the stove in liquid insulating process, as P or some oxide compounds and halogenide etc.
So far it is explanation of the invention that embodiment as herein described is construed as, but not limitation of the present invention.Scope of the present invention is not to be illustrated by above specification sheets, but is limited by the claim of patent, this invention is intended to comprise all corrections that meaning and scope with this patent claim are equal to.
Claims (10)
1. metallurgical silicon purification method comprises step:
Step S1: make polysilicon to be purified keep the molten state certain hour in crucible, described crucible comprises the stool and the sidewall of crucible that is arranged on the stool of bottom, and described sidewall of crucible is made up of water-cooled copper;
Step S2: by beginning from the bottom to top cooled and solidified gradually around being arranged on polysilicon liquid that relatively moving of ruhmkorff coil around the crucible arm and crucible make described molten state;
Step S3: the described metalluragical silicon from crucible after the extraction cooled and solidified, by the described polysilicon after the mechanically cutting acquisition purification.
2. method of purification as claimed in claim 1 is characterized in that, the material of stool has the copper or the stainless material of water-cooling channel in being.
3. method of purification as claimed in claim 1 or 2 is characterized in that step S2 repeats certain number of times.
4. method of purification as claimed in claim 1 is characterized in that, in step S1, liquid polysilicon remained in 1450 ℃ of-1850 ℃ of scopes more than 30 minutes, and furnace atmosphere is rare gas element or high vacuum, and the furnace pressure variation range is 1 * 10
-3Pa-1.5 * 10
5In the Pa scope.
5. method of purification as claimed in claim 1, it is characterized in that, in step S1, energy required in the heating of described polysilicon, fusing, constant temperature and the directional freeze process is converted into heat energy to electric energy and is applied on the described polysilicon by the electromagnetic induction between the polysilicon in described ruhmkorff coil and the crucible.
6. method of purification as claimed in claim 1 is characterized in that, the relatively moving of described ruhmkorff coil and crucible body comprise ruhmkorff coil fixedly crucible move, or the crucible fixed inductor moves, or ruhmkorff coil and crucible all move.
7. method of purification as claimed in claim 1, it is characterized in that, in step S1, the purifying polycrystalline silicon form for the treatment of that contains impurity that drops into described crucible is powder or piece material, its temperature is normal temperature or high temperature, or the liquid of the polysilicon of molten state directly pours in the crucible, and described polysilicon is a powdery or when block, directly its heating is heated and fusing it with fusing or by auxiliary thermal source, described auxiliary thermal source is plasma arc or adds easy induction thermal objects.
8. one kind is used for the crucible that polysilicon is purified, it is characterized in that, described crucible comprises the stool of bottom and is arranged on sidewall of crucible on the stool, and described sidewall of crucible is made up of water-cooled copper, and the material of stool has the copper or the stainless material of water-cooling channel in being.
9. an equipment for purifying is used for polysilicon and purifies, and it is characterized in that described equipment for purifying has the described crucible of claim 8.
10. equipment for purifying as claimed in claim 9, it is characterized in that, described equipment for purifying comprises furnace shell and is arranged at described crucible in the furnace shell, also comprise ruhmkorff coil around described crucible setting, be used for the ruhmkorff coil lifting jacking system, be used for crucible lifting the crucible lifting system, be used for the polysilicon in the crucible is heated or purified auxiliary thermal source and be used for the inflation system of inflating and be used to make the vacuum system that becomes and keep vacuum in the described furnace shell in described furnace shell.
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| CN102275929A (en) * | 2010-06-10 | 2011-12-14 | 上海华巨硅材料有限公司 | Method for improving purity of metallurgical silicon and apparatus for realizing method |
| CN102452837B (en) * | 2010-10-28 | 2013-11-06 | 上海普罗新能源有限公司 | Crucible for external refining for preparation of solar grade polysilicon as well as preparation method of crucible |
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| CN101377010A (en) * | 2007-08-30 | 2009-03-04 | 上海太阳能工程技术研究中心有限公司 | Device and method for manufacturing solar grade polysilicon |
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