CN102583389A - 一种炉外精炼提纯工业硅的方法 - Google Patents
一种炉外精炼提纯工业硅的方法 Download PDFInfo
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- CN102583389A CN102583389A CN2012100546524A CN201210054652A CN102583389A CN 102583389 A CN102583389 A CN 102583389A CN 2012100546524 A CN2012100546524 A CN 2012100546524A CN 201210054652 A CN201210054652 A CN 201210054652A CN 102583389 A CN102583389 A CN 102583389A
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- silicon
- refining
- ladle
- external refining
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 95
- 239000010703 silicon Substances 0.000 title claims abstract description 95
- 238000007670 refining Methods 0.000 title claims abstract description 90
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound 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[Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 94
- 239000002893 slag Substances 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 22
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- 229910004261 CaF 2 Inorganic materials 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials 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- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
本发明涉及一种炉外精炼提纯工业硅的方法，在矿热炉释放硅熔体到抬包之前，向抬包中持续通入精炼气体，接着释放硅熔体到抬包中，并在抬包中进行加热，控制熔体温度在一定范围内，再向抬包中加入精炼剂进行造渣精炼，随着抬包内硅熔体量的不断增加，调整精炼气体的通入流量、压力等进行炉外精炼；待炉外精炼完毕后，进行渣硅分离，再进行浇注，即完成炉外精炼提纯工业硅。通过上述炉外精炼过程，可以去除工业硅熔体中包括Al、Ca、Ti、Na在内的大部分金属杂质和部分B、P、S、C等非金属杂质，同时可以为后续的工业硅提纯控制有效的成分，为冶金法制备太阳能级硅提供高品质的原料。本发明具备充分利用和节约能源、生产效率高、基建投资较少、环境无污染等特点。
Description
一种炉外精炼提纯工业硅的方法
技术领域
[0001] 本发明涉及一种炉外精炼提纯工业硅的方法，尤其是涉及一种在带自带加热系统的抬包中对刚从矿热炉放出的硅水进行造渣、吹气精炼来提纯工业硅的方法，属于冶金法提纯工业硅制备太阳能级硅的技术领域。
背景技术
[0002] 根据“十二五”规划，我国要达到“‘十二五’末非化石能源在一次能源消费中的比重达到11.4%”这一目标，未来数年必将掀起太阳能等新兴能源产业的投资浪潮。目前，我国只能依靠引进国外改良Siemens法工艺技术进行小批量的生产，在产业化方面同国际先进水平差距主要表现在多晶硅的产能低，供需矛盾突出；生产规模小；工艺设备落后，物料和电力消耗过大，三废问题多。采用传统的氯化提纯工艺生产太阳能级硅，虽然技术成熟， 但成本过高，不能满足太阳能电池工业发展的需求。因此，研究和开发生产廉价的太阳能级多晶硅的新技术成为当务之急。
[0003] 多晶硅是制备单晶硅和太阳能硅电池的原料，是全球电子工业及光伏产业的基石。因此，世界各国竞相开发低成本、低能耗的太阳能级硅信制备技术与工艺，并趋向于把制备高纯度的太阳能级硅(纯度>99. 9999wt%)工艺与制备高纯度的电子级硅(纯度 >99. 9999999wt%)工艺区别开来，以进一步降低成本。
[0004] 冶金法提纯多晶硅，是指提纯过程中硅没有发生化学变化，未通过化学反应转化为其它化合物来达到提纯的目的。在提纯过程中主要利用不同元素物理性质的差异来使之分离，其中包括湿法冶金、吹气、造渣、定向凝固、真空条件下的电子束、等离子体、太阳聚光及感应熔炼等。冶金法生产太阳能级硅与传统的生产方法具有环境压力小、成本低等优点。
发明内容
[0005] 为克服生产效率低、生产成本高、规模小等问题，本发明目的在于提供一种炉外精炼提纯工业硅的方法，该方法直接在自带加热系统的抬包中对刚从矿热炉中流出的熔融硅水进行炉外精炼。在精炼过程中，先吹压缩空气，再吹混合精炼气体和以SiO2-CaO为基础渣的复合渣系的气固混合物，实现出硅、加热、精炼同步进行。通过上述炉外精炼之后，使硅中的大部分金属杂质得到去除，同时部分非金属杂质B、P、C等也被去除。
[0006] 一种炉外精炼提纯工业硅的方法，经过下列步骤：
在矿热炉释放硅熔体之前，向抬包中持续通入精炼气体，接着释放硅熔体到抬包中，并在抬包中进行加热、保温，使硅熔体的炉外精炼温度控制在1450〜1700°C，实现边加热、边出娃水、边精炼冋步进彳丁 ；再向抬包中加入精炼剂进彳丁造潘精炼，使潘娃比控制在10 . I〜
I ： 10，随着抬包中硅熔体量的不断增加，调整精炼气体的通入流量为I〜10m3/h，压力为 2〜8atm，进行炉外精炼I〜6h ;该过程可以实现出硅水、抬包加热、炉外精炼(包括吹气和造渣精炼）同时进行；然后进行渣硅分离，再进行浇注，即完成炉外精炼提纯工业硅。
[0007] 所述精炼剂的主要成分包括Ca0、Si02、CaF2、Al203、Na20、Ba0等中的一种或多种的任一比例混合物，但不限于上述组分。
[0008] 所述精炼气体包括空气、氧气、水蒸气、氩气、氮气等中的一种或多种气体的任一比例混合，但不限于上述气体。
[0009] 所述精炼剂的加入是通过抬包炉口直接加入和通气管道加入，利用精炼气体的压力和流量将精炼剂以气固混合物的形式带入抬包中，实现精炼剂和硅熔体的成分接触和反应，提高炉外精炼的效果。
[0010] 根据专利号：ZL200910094078. 3利用向熔融硅中吹入压缩空气和SiO2-CaO熔渣氧化物粉末的气固混合物进行氧化精炼，之后吹入氧化性气体H2O蒸汽，最终去除大部分金属杂质Al、Ca、Ti等以及少部分非金属杂质B、P等,达到娃中金属杂质减低至I. Oppmw以下，非金属杂质B、P分别降低至O. 2ppmw和O. 5ppmw以下，电阻率达到2. 5 Ω *cm以上的目的。与上述发明相比，本发明与其有着明显的区别，在充分研究工业硅的生产工艺和特点之后，本发明直接对抬包进行改进，使抬包具有保温和加热能力，一方面可以有效利用刚出炉硅熔体的热量，节约能源消耗，另一方面可以保障硅熔体在进行炉外精炼时温度不会降低， 有效提升硅熔体的炉外精炼效果。极大程度上利用熔融硅的热量和减少了熔融的热量损失，缩短了生产时间，提高了生产效率，不需要使用石墨坩埚，很大程度上降低了生产成本， 同时提高了所生产工业硅的品质。根据冶金法制备太阳能级硅的工艺要求，可以在炉外精炼过程中加入一定量的辅助材料，控制工业硅产品的成分，为后续冶金法提纯工艺做足铺垫，进一步降低冶金法制备太阳能级硅的生产成本，提高生产效率。在进行炉外精炼(包括吹气和造渣精炼）时，可以根据熔体量的多少和精炼气体的通入量以及精炼时间长短等因素，综合考虑调节抬包自带加热系统的工作温度、功率和电流等参数，达到尽可能低的综合电耗。
[0011] 本发明的有益效果是：
I、充分利用和节约能源：根据工业硅生产的特点，采用抬包炉外精炼能够充分利用熔融硅的自身热量，与其他火法精炼工业硅相比能够节约70%的能耗。
[0012] 2、生产效率高：本方法采用在抬包中进行炉外精炼，将工业硅的造渣、吹起精炼联合交叉进行，适应性强、精炼效果好、操作方便，大大提高了生产效率，并实现大规模工业化生产。
[0013] 3、基建投资较少：本发明只要对抬包进行改造，安装自带的加热装置，其基建投资相对于相同生产规模的其他火法精炼方法可减少50%。
[0014] 4、环境无污染：由于此过程利用的原料和副产品均不会污染环境，因此该发明对环境压力小，能实现清洁生产，符合绿色冶金的要求。
具体实施方式
[0015] 下面结合和实施例对本发明作进一步详细说明。
[0016] 实施例I
在矿热炉释放硅熔体之前，向抬包中持续通入空气和氧气的混合气，接着释放纯度为 98%的2吨工业硅熔体到抬包中，并在抬包中进行加热、保温，使硅熔体的炉外精炼温度控制在1700°C，实现边加热、边出硅水、边精炼同步进行；再通过抬包炉口直接加入和通气管道向抬包中加入按45%Si02+45%Ca0+10%CaF2混合的精炼剂进行造渣精炼，使渣硅比控制在10 ： 1，随着抬包中硅熔体量的不断增加，调整精炼气体的通入流量为60m3/h，压力为 5atm,进行炉外精炼Ih ；除去硅中的大部分Al、Ca、Ti、Na等金属杂质和部分C、B、P、S等非金属杂质；该过程可以实现出硅水、抬包加热、炉外精炼(包括吹气和造渣精炼）同时进行； 然后进行渣硅分离，再进行浇注，即完成炉外精炼提纯工业硅。工业硅的纯度达到2. 5N，其中B、P的含量< 3ppmw。
[0017] 实施例2
在矿热炉释放硅熔体之前，向抬包中持续通入水蒸气、氩气和氮气的混合气体，接着释放硅熔体到抬包中，并在抬包中进行加热、保温，使硅熔体的炉外精炼温度控制在1450°C， 实现边加热、边出硅水、边精炼同步进行；再通过抬包炉口直接加入和通气管道向抬包中加入按30%CaF2+60%Al203+10%Na20混合的精炼剂进行造渣精炼，使渣硅比控制在I : 10，随着抬包中硅熔体量的不断增加，调整精炼气体的通入流量为10m3/h，压力为2atm，进行炉外精炼4h ;除去硅中的大部分Al、Ca、Ti、Na等金属杂质和部分C、B、P、S等非金属杂质，该过程可以实现出硅水、抬包加热、炉外精炼(包括吹气和造渣精炼）同时进行；然后进行渣硅分离，再进行浇注，即完成炉外精炼提纯工业硅。工业硅的纯度达到2. 5N，其中Al的含量 <IOOppmw, Ca 的含量 <30ppmw, B 的含量〈lppmw。
[0018] 实施例3
在矿热炉释放硅熔体之前，向抬包中持续通入精炼气体水蒸气，接着释放硅熔体到抬包中，并在抬包中进行加热、保温，使硅熔体的炉外精炼温度控制在1600°C，实现边加热、边出硅水、边精炼同步进行；再通过抬包炉口直接加入和通气管道向抬包中加入精炼剂BaO 进行造渣精炼，使渣硅比控制在5 ： 1，随着抬包中硅熔体量的不断增加，调整精炼气体的通入流量为lm3/h，压力为8atm，进行炉外精炼6h ;除去硅中的大部分Al、Ca、Ti、Na等金属杂质和部分C、B、P、S等非金属杂质，该过程可以实现出硅水、抬包加热、炉外精炼(包括吹气和造渣精炼)同时进行；然后进行渣硅分离，再进行浇注，即完成炉外精炼提纯工业硅。工业娃的纯度达到2· 5N,其中Al的含量〈lOOppmw, Ca的含量<20ppmw, B的含量〈lppmw。
Claims (4)
1. 一种炉外精炼提纯工业硅的方法，其特征在于经过下列步骤：在矿热炉释放硅熔体之前，向抬包中持续通入精炼气体，接着释放硅熔体到抬包中，并在抬包中进行加热、保温，使硅熔体的炉外精炼温度控制在1450〜1700°C，再向抬包中加入精炼剂进行造渣精炼，使渣硅比控制在10 : I〜I : 10，随着抬包中硅熔体量的不断增加，调整精炼气体的通入流量为I〜10m3/h，压力为2〜8atm，进行炉外精炼I〜6h ;然后进行渣硅分离，再进行浇注，即完成炉外精炼提纯工业硅。
2.根据权利要求I所述的炉外精炼提纯工业硅的方法，其特征在于：所述精炼剂的主要成分包括CaO、SiO2, CaF2, Al2O3> Na2O, BaO中的一种或多种的任一比例混合物。
3.根据权利要求I所述的炉外精炼提纯工业硅的方法，其特征在于：所述精炼气体包括空气、氧气、水蒸气、氩气、氮气中的一种或多种气体的任一比例混合。
4.根据权利要求I所述的炉外精炼提纯工业硅的方法，其特征在于：所述精炼剂的加入是通过抬包炉口直接加入和通气管道加入。
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