CN104593828A - Preparation method of low-boron-phosphorus metallurgical grade silicon - Google Patents
Preparation method of low-boron-phosphorus metallurgical grade silicon Download PDFInfo
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- CN104593828A CN104593828A CN201410852837.9A CN201410852837A CN104593828A CN 104593828 A CN104593828 A CN 104593828A CN 201410852837 A CN201410852837 A CN 201410852837A CN 104593828 A CN104593828 A CN 104593828A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/36—Alloys obtained by cathodic reduction of all their ions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
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Abstract
The invention discloses a preparation method of low-boron-phosphorus metallurgical grade silicon; aluminium-silicon alloy is prepared through electrolysis by taking a fused salt electrolysis method as the core technology, wherein an electrolyte system is a cryolite molten salt system; Al2O3, CaO, NaCl and raw SiO2 powder are added; a certain amount of aluminium blocks are added into fused salt; and the aluminium-silicon alloy is prepared through electrolysis by taking iron-nickel alloy as an inert anode and liquid metal aluminium as a cathode. According to the invention, the aluminium-silicon alloy is prepared through electrolysis by utilizing the iron-nickel inert anode; the difficulty in removing impurities out of silicon, which is caused when the impurities such as boron and phosphorus are brought in by a carbon sacrificial anode, can be avoided; the subsequent impurity-removing cost is saved; therefore, the preparation method has a certain economic benefit; gas generated by anode electrolysis is green gas, namely oxygen; the environmental pollution is greatly reduced; clean production can be realized; and thus, the preparation method has a certain social benefit.
Description
Technical field
The present invention relates to the technology that fused salt electrolysis process prepares metallurgical grade silicon, be specifically related to a kind of preparation method of low boron phosphorus metallurgical grade silicon.
Background technology
Polysilicon is refined by the metallurgical grade silicon that silicon purity is lower, and the traditional technology that production of polysilicon is main in the world at present has: improved Siemens, silane thermal decomposition process and fluidized bed process.Wherein improved Siemens is the production method of current main flow, and the polysilicon adopting this method to produce accounts for 85% of polysilicon whole world ultimate production.But because the Siemens Method complex process of improvement, large, the comprehensive power consumption of investment are high, the polysilicon of production is expensive.Metallurgy method, as the novel process from the direct synthesis solar energy level silicon of metallurgical grade silicon, demonstrates its superiority in every respect, and compared with improved Siemens, metallurgy method is produced polysilicon and wanted economy, low consumption and environmental protection many.From cost, metallurgy-prepared polysilicon production cost is 25 ~ 300,000 yuan per ton at present, and than improvement, siemens is low by 20% ~ 30%.
Metallurgy method is produced polysilicon and is similar to Metal smelting purification process, one of its feature is that silicon does not participate in any chemical reaction in purification process, from the chemical property of impurity, the different of physical properties, silicon is purified according to silicon in metalluragical silicon, as purification metalluragical silicons such as directional freeze, plasma removal of impurities, acidleach, vacuum distillings.Wherein, directional freeze is the difference of basis separation factor of impurity in liquid phase and solid phase thus the impurity in solid phase is removed.Directional freeze effectively can remove the little impurity element of separation factor in metallurgical grade silicon, but boron, the phosphorus removing poor effect larger to separation factor.
Have many research to adopt fused salt electrolysis process to prepare solar energy level silicon in recent years, in melting salt, electrolytic reduction silicate or silicon-dioxide directly prepare solar energy level silicon, the method have energy consumption low, pollute many advantages such as little.But be solid-state elemental silicon at electrolytic process cathode deposit, and the poorly conductive of silicon, the lasting lifting of electrolysis voltage will be caused, and regularly need stop groove taking-up silicon, affect the continuity of electrolysis.With traditional expendable carbon materials for anode carry out electrolysis time, anode consumption will produce a large amount of carbon dioxides, also can bring the impurity such as a certain amount of boron, phosphorus simultaneously into and enter ionogen, the boron caused in negative electrode silicon, phosphorus content are raised, for follow-up physics or chemical purification silicon add difficulty.
Summary of the invention
For solving the problem, the invention provides a kind of preparation method of low boron phosphorus metallurgical grade silicon, utilize iron nickel inert anode electrolytic preparation aluminum silicon alloy, thus avoid the difficulty that the impurity such as boron, phosphorus brought in carbon causes removal of impurities in follow-up silicon, save the cost of follow-up removal of impurities, there is certain economic benefit.
For achieving the above object, the technical scheme that the present invention takes is:
A preparation method for low boron phosphorus metallurgical grade silicon, comprises the steps:
S1, be 0.6 ~ 1.3 get iron and nickel prepares Fe-Ni alloy/C noble electrode in mass ratio;
S2, get appropriate cryolite fused salt, add Al by mass percentage
2o
31 ~ 3%, CaO 1 ~ 4%, NaCl1 ~ 5%, SiO
22.5 ~ 8.0% mix after, add the aluminium block of 5% by mass percentage; (additive A l in ionogen
2o
3, the content of CaO, NaCl is all within the specific limits, and addition is the quality proportion by subtraction accounting for mixed ionogen total amount)
S3, preparing the Fe-Ni alloy/C noble electrode of gained using step S1 as anode, take metallic aluminium as the cryolite fused salt of negative electrode, electrolysis step S2 gained;
S4, pass into electric current after, negative electrode separate out silicon, silicon forms aluminum silicon alloy after entering aluminium liquid;
S5, by the liquid aluminium silicon alloy sucking-off of step S4 gained, after carrying out directional freeze, eutectic, silicon in aluminum silicon alloy is separated out.
Wherein, the temperature of described electrolysis is 950 ~ 970 DEG C.
Wherein, described anodic current density is 0.4A/cm
2~ 1.3A/cm
2.
Wherein, the time of described electrolysis is 4 ~ 8h.
Wherein, described sodium aluminum fluoride molecular ratio is 2.2 ~ 2.4.
The present invention has following beneficial effect:
Utilize iron nickel inert anode electrolytic preparation aluminum silicon alloy, thus avoid the difficulty that the impurity such as boron, phosphorus brought in carbon causes removal of impurities in follow-up silicon, saved the cost of follow-up removal of impurities, there is certain economic benefit; The gas that anode electrolysis produces is green gases oxygen, greatly reduces the pollution to environment, can realize cleaner production thus have certain social benefit.
Accompanying drawing explanation
Fig. 1 is electrolyzer structural representation used in the embodiment of the present invention.
Embodiment
In order to make objects and advantages of the present invention clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment of the present invention electrolyzer used as shown in Figure 1, comprise electric furnace 3, iron crucible 4 is provided with in described electric furnace 3, plumbago crucible 5 is provided with in described iron crucible 4, corundum crucible 6 is provided with in described plumbago crucible 5, ionogen fused salt 7 is filled with in described corundum crucible 6, iron nickel inert anode 9 is provided with in described ionogen fused salt 7, described iron nickel inert anode 9 is connected with anode rod by alundum tube 2, outer wall upper end, described iron crucible 4 side is connected with cathode collector bar 10, is aluminium liquid 8 bottom described corundum crucible 6.
Embodiment 1
S1, be get iron and nickel prepare Fe-Ni alloy/C noble electrode at 3: 4 in mass ratio, the diameter of Fe-Ni alloy/C noble electrode is 3.Scm, and height is 2.7cm;
S2, get the sodium aluminum fluoride that 271.5g molecular ratio is 2.2,3g Al
2o
3, 3g CaO, 15g NaCl, 7.5gSiO
2after stirring, add the aluminium block of 15g;
S3, preparing the Fe-Ni alloy/C noble electrode of gained using step S1 as anode, take metallic aluminium as the cryolite fused salt of negative electrode, electrolysis step S2 gained;
S4, pass into electric current after, at temperature 950 DEG C, electrolysis 8h, negative electrode separate out silicon, silicon forms aluminum silicon alloy after entering aluminium liquid;
S5, by the liquid aluminium silicon alloy sucking-off of step S4 gained, after carrying out directional freeze, eutectic, silicon in aluminum silicon alloy is separated out.
Embodiment 2
S1, be get iron and nickel prepare Fe-Ni alloy/C noble electrode at 6: 10 in mass ratio;
S2, to get 252g molecular ratio be 2.3 sodium aluminum fluorides, 9g Al
2o
3, 12g CaO, 3g NaCl, 24g SiO
2after stirring, add the aluminium block of 15g;
S3, preparing the Fe-Ni alloy/C noble electrode of gained using step S1 as anode, take metallic aluminium as the cryolite fused salt of negative electrode, electrolysis step S2 gained;
S4, pass into electric current after, at temperature 960 DEG C, electrolysis 4h, negative electrode separate out silicon, silicon forms aluminum silicon alloy after entering aluminium liquid;
S5, by the liquid aluminium silicon alloy sucking-off of step S4 gained, after carrying out directional freeze, eutectic, silicon in aluminum silicon alloy is separated out.
Embodiment 3
S1, be get iron and nickel prepare Fe-Ni alloy/C noble electrode at 13: 10 in mass ratio;
S2, to get 263.75g molecular ratio be 2.4 sodium aluminum fluorides, 4g Al
2o
3, 7.5g CaO, 9g NaCl, 15.75g SiO
2after stirring, add the aluminium block of 15g;
S3, preparing the Fe-Ni alloy/C noble electrode of gained using step S1 as anode, take metallic aluminium as the cryolite fused salt of negative electrode, electrolysis step S2 gained;
S4, pass into electric current after, at temperature 970 DEG C, electrolysis 6h, negative electrode separate out silicon, silicon forms aluminum silicon alloy after entering aluminium liquid;
S5, by the liquid aluminium silicon alloy sucking-off of step S4 gained, after carrying out directional freeze, eutectic, silicon in aluminum silicon alloy is separated out.
After testing, in the product obtained after electrolysis in embodiment 1 ~ 3, the content of boron is 1 ~ 3ppmw; The content of phosphorus is 3 ~ 8ppmw.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. a preparation method for low boron phosphorus metallurgical grade silicon, is characterized in that, comprise the steps:
S1, be 0.6 ~ 1.3 get iron and nickel prepares Fe-Ni alloy/C noble electrode in mass ratio;
S2, get appropriate cryolite fused salt, add Al by mass percentage
2o
31 ~ 3%, CaO 1 ~ 4%, NaCl1 ~ 5%, SiO
22.5 ~ 8.0% mix after, add the aluminium block of 5% by mass percentage;
S3, preparing the Fe-Ni alloy/C noble electrode of gained using step S1 as anode, take metallic aluminium as the cryolite fused salt of negative electrode, electrolysis step S2 gained;
S4, pass into electric current after, negative electrode separate out silicon, silicon forms aluminum silicon alloy after entering aluminium liquid;
S5, by the liquid aluminium silicon alloy sucking-off of step S4 gained, after carrying out directional freeze, eutectic, silicon in aluminum silicon alloy is separated out.
2. the preparation method of a kind of low boron phosphorus metallurgical grade silicon according to claim 1, it is characterized in that, the temperature of described electrolysis is 950 ~ 970 DEG C.
3. the preparation method of a kind of low boron phosphorus metallurgical grade silicon according to claim 1, it is characterized in that, described anodic current density is 0.4A/cm
2~ 1.3A/cm
2.
4. the preparation method of a kind of low boron phosphorus metallurgical grade silicon according to claim 1, it is characterized in that, the time of described electrolysis is 4 ~ 8h.
5. the preparation method of a kind of low boron phosphorus metallurgical grade silicon according to claim 1, it is characterized in that, described sodium aluminum fluoride molecular ratio is 2.2 ~ 2.4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108823637A (en) * | 2018-07-30 | 2018-11-16 | 孟静 | The device of purifying polycrystalline silicon |
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Application publication date: 20150506 |