冶金法制备太阳能级硅过程中氧化精炼除硼应用基础研究
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摘要
全球能源危机的日益加剧为新能源尤其是太阳能光伏产业的快速发展提供了机遇,由于太阳能发电的巨大优势,世界光伏产业以每年高于30%的增长率高速发展,2009年全球太阳能电池产量已增长至10.5GWp,我国达到4382MW,超过全球份额的40%。太阳能级硅(SoG-Si)是光伏产业发展的基础,2011年晶体硅太阳能电池产量已经占到全部太阳能电池的88%,因此硅材料的供给和生产成本成为太阳能电池发展的关键。目前,太阳能级硅的生产技术主要有改良西门子法和硅烷热分解法,高成本和高环境负荷已经严重制约了光伏产业的发展,而以冶金级硅(MG-Si)为原料,低成本、低能耗和环境友好的冶金法多晶硅制备新工艺正迈向产业化进程,但该新工艺的关键和难点是冶金级硅中杂质元素尤其是B、P的有效去除,并使太阳能级硅纯度达到6N及以上。
本文以硼含量为18ppmw的冶金级硅为原料,从多方面开展硅中杂质元素硼的氧化去除研究工作。研究发现,杂质在冶金级硅中呈深色、浅色和白色夹杂分布,深色夹杂分布在整个冶金级硅中,为熔渣型夹杂；浅色和白色夹杂位于硅的晶界处,为金属或金属间化合物。以Si-Me二元相图为基础,研究了冶金级硅中Fe、Al、Ca、Ti、Ni、Cu等金属杂质的存在形态,利用Si-B相图确定冶金级硅熔体中的物相形态为SiB6；通过Me-B、Si-Fe-B和Si-Al-B相图分析了B与Fe、Al、Ca间形成二元化合物FeB、Fe2B、AlB2、AlB12、CaB6及三元化合物Fe4.7Si2B、Fe5SiB2和Fe2Si0.4B0.6的可能性,研究发现,B与硅中其他元素间优先结合的顺序为TiB2>MnB2>AlB2>Co2B>NiB>Fe2B>MgB2>SiB3;实验表明,Si-B二元系中存在SiB4相,Si-Me-B相平衡实验也证明了FeSi2、CaB6和SiB6物相的存在,结果与二元相图吻合。
由02和H20-02吹气氧化精炼除硼热力学可知,向冶金级硅熔体中吹入02和H20-O2混合气体,杂质元素硼分别以气态硼氧化物(BxOy)和硼氢氧化物(BxHzOy)的形式挥发,并得到了1412-2230℃下杂质元素硼去除限度与硼化合物分压的热力学关系。研究表明,硼气态氢氧化物的平衡分压远高于硼气态氧化物,因此,利用H20-O2混合气体除硼效果应该更好。在1450℃时,各气态硼氢氧化物中,挥发性最大的是BH02和B3H306,当硼含量降低至5～10ppmw时,BH02平衡分压达到10SPa以上,降低至0.1ppm时为2500Pa,且各气态硼氢氧化物的平衡分压随温度的升高反而降低,在硅抬包中进行的02精炼实验表明,硅中Fe、Cu、V、C的去除率均低于20%,Al、Ca分别为98.2%和92.9%,B从35ppmw降低至18ppmw,去除率接近50%,P主要以P2的形式挥发,由184ppmw降低至112ppmw。在直流电弧炉中利用Ar-H2O-O2气氛进行除硼精炼实验表明,当精炼时间为10min时,硼含量可从18ppmw降低至2ppmw,由于受多方面动力学因素的影响和制约,硼的实验去除效果与热力学限度的理论计算值之间存在较大差距。
获得了平衡时硅中[%B]、熔渣中(%B)与aSiO2和acaO之间的热力学关系同时建立了CaO-SiO2熔渣与冶金级硅中杂质硼的电化学反应模型,该模型体现了硅中杂质硼与熔渣间的反应机理。熔渣精炼除硼实验表明,纯氧化物Si02基本起不到除硼的作用,这与热力学计算结果一致；采用CaO-SiO2熔渣时,当CaO/SiO2约为1.5时,硼的分配系数LB达到最大值1.58；当渣硅比为2.5、精炼时间3.0h时,硼含量可降低至1.8ppmw;向CaO-SiO2二元熔渣中添加MgO、Li2O、LiF和K20等形成CaO-SiO2-MeO三元熔渣精炼实验表明,添加MgO不利于除硼效率的提高,添加20%左右的Li20和LiF且当渣硅比为4：1时,硼含量可降低至1.3ppmw,硼的去除效率达到92.7%；添加30%K20时,硅中硼含量可降低至1.4ppmw;精炼后渣相的XRD结果表明,硅中杂质元素硼被氧化为B203并与加入的Li20形成Li2O·2B2O3。
提出和探讨了MeClx熔盐去除冶金级硅中杂质元素硼的方法和反应机理,得到了1550℃条件下CuCl2、FeCl3、MgCl2、NaCl、CaCl2和AICl3熔盐的除硼限度与BCly分压的热力学关系。实验发现,在冶金级硅中添加50%-60%的FeCl3时,可将硼含量由18ppmw降低至3.1ppmw,利用FeCl3-SiO2和MgCl2-SiO2混合体系除硼时,除硼效率随着熔盐含量的增加而增大。可以推测,采用FeCl3熔盐精炼除硼时,FeCl3被还原为金属Fe后与Si结合为金属间化合物FeSi2,而由于MgCl2的直接分解和Mg蒸汽的挥发,采用MgCl2熔盐时,渣样中没有发现金属Mg。
With the aggravation of global energy crisis, the rapid development of new energy materials especially for Photovoltaic industry is provided with chance of a lifetime. The Photovoltaic industry in the world has been rising at a speed of growth rate for30%annually. In2009, the production of solar cells had reached to10.5GWp on a global scale. It was4382MW in China and was more than40%for global totals. The solar grade silicon (SoG-Si) is base of Photovoltaic industry and the crystalline silicon solar cells had a share of88%in market in2009so the supply and cost of silicon materials is crucial for solar cells. Presently, the production of SoG-Si has mainly two methods:Siemens technology and thermal decompositon of SiH4, which have restricted the development of Photovoltaic industry for their high cost and heavy environmental load. To our inspiration, the new technology for SoG-Si preparation with metallurgical method, for its low cost, low energy consumption and friendly environment, has been growing up and applying. But the critical points and puzzled problems are the removal of impurities in metallurgical grade silicon (MG-Si) especially for B and P and the requirement for6N purity for SoG-Si.
In this paper, the features and removal of boron in MG-Si raw materials were systemically studied based on the MG-Si product with18ppmw for boron content. It was found that the impurities take on deep, light and white color inclusions in MG-Si. The deep inclusions confirmed as slag distribute in the whole MG-Si and the light and white ones that are thought to be metals or intermetallic compounds are lie in grain boundary of silicon. Based on binary phase diagrams between Si and impurity elements, the conformation of impurities Fe, Al, Ca, Ti, Ni, Cu etc in MG-Si raw materials was studied. The transformation among Si-B phases was analyzed and it was confirmed that SiB6is the form of Si-B phase in silicon melt. Based on Me-B, Si-Fe-B and Si-Al-B phase diagram systems, the probability of binary compounds FeB, Fe2B, AlB2, AlB12, CaB6and ternary compounds Fe4.7Si2B, Fe2Sio.4Bo.6were also analyzed. It was found that the preferential order for the combination between B and other elements is TiB2>MnB2>AlB2>Co2B>NiB>Fe2B>MgB2>SiB3. The phase equilibrium experiments indicated the existence of SiB4in Si-B binary system and also FeSi2, CaB6and SiB6in Si-Me-B systems, which was consistent with Si-Fe, Ca-B and Si-B phase diagrams.
The thermodynamic process of boron removal by O2and H2O-O2gas blowing was studied andit was found that the impurity boron is volatilized in forms of gaseous boron oxide species (BxOy)and gaseous boron hydrate species (BxHzOy) and the thermodynamic relationships betweenboron removal limitation and partial pressures of gaseous species at1412?2230°C wasobtained. It showed that the partial pressure of gaseous boron hydrate species is much higherthan that of gaseous boron oxide species so it is preferable to for boron removal with H2O-O2gasblowing. At1450°C, the volatilization of BHO2and B3H3O6is most among all gaseous boronhydrate species. The partial pressures of BHO2reach to105Pa and2500Pa when the boron levelis reduced to5ppmw and O.lppmw respectively and the thermodynamic relationships displaythat on the contrary the partial pressures of gaseous boron hydrate species will reduce with theincrease of temperature. The experimental results by O2gas blowing in ladle showed that theremoval rates of impurities Fe，Cu, V and C in MG-Si is lower than20%and it is98.2%and92.9%for A1and Ca. B is reduced from35ppmw to18ppmw which is close to50%and P isreduced from184ppmw to112ppmw which is volatilized in forms of gaseous P2. Theexperimental results by Ar-H20-02gas blowing in DC arc furnace showed the removal rate ofboron increased with the prolongation of refining time and it was reduced from18ppmw to2ppmw when the time reached to1Omin. But it has great difference between the boron removalresults in experiments and the calculated value for boron removal limitation in thermodynamicfor the effects and constraint for dynamic factors.
The thermodynamic relationships among boron level in silicon [%B], boron level in slag asi0and aCre obtained as
the same time, the electrochemical reactive model between Ca0-Si02slag and boron in MG-Siwas established, which displays the reactive mechanism between boron in silicon and molten slag. Theexperiments of slag refining in induction furnace showed it is not helpful to boron removal forpure Si2，which is accordant to thermodynamic results. The maximal value for partitioncoefficient of boron in silicon is1.58for Ca0-Si02slag when the composition of CaO/SiC>2is1.5. The boron level in silicon is reduced to1.8ppmw with the slag and silicon ratio2.5andrefining time3.Oh. The expeirmental results adding MgO, Li2，LiF and K2O to Ca0-Si02binary molten slag showed it is disadvantageous for boron removal with the addition of MgO.The boron level is respectively reduced to1.3ppmw and1,4ppmw when the slag and silicon ratio is4:1with the addition of20%LbO and30%K2O. The efficiency of boron removal is92.7%,The XRD spectrogram of refined slag showed that the experimental results with alloyed Si-Bsample are accordant to those of MG-Si refining and boron in MG-Si is oxidized into B2O3which combines into Li20*2B203with Li20.
The method of boron removal for MG-Si with molten salt MeClx refining was brought forward.The thermodynamic relation between boron level in silicon and equilibrium partial pressure ofBCly°with molten salt CuCb、FeCb、MgCh、NaCK CaCl2and AICI3at1550C was obtained.It was found by experiments the boron level in silicon is reduced from18ppmw to3.1ppmw withadding50%~60%FeCl3to MG-Si. The efficiency of boron removal increases with the higherratio of molten salt in mixed FeCl3-Si02and MgCb-Si02systems. It is presumed that FeCb isreduced to Fe, which combines into intermetallic compound FeSi: with Si when using FeCl3refining. However, Mg is not found in slag with MgCb refining maybe the decomposition ofMgCb and volatilization of Mg.
本文以硼含量为18ppmw的冶金级硅为原料,从多方面开展硅中杂质元素硼的氧化去除研究工作。研究发现,杂质在冶金级硅中呈深色、浅色和白色夹杂分布,深色夹杂分布在整个冶金级硅中,为熔渣型夹杂；浅色和白色夹杂位于硅的晶界处,为金属或金属间化合物。以Si-Me二元相图为基础,研究了冶金级硅中Fe、Al、Ca、Ti、Ni、Cu等金属杂质的存在形态,利用Si-B相图确定冶金级硅熔体中的物相形态为SiB6；通过Me-B、Si-Fe-B和Si-Al-B相图分析了B与Fe、Al、Ca间形成二元化合物FeB、Fe2B、AlB2、AlB12、CaB6及三元化合物Fe4.7Si2B、Fe5SiB2和Fe2Si0.4B0.6的可能性,研究发现,B与硅中其他元素间优先结合的顺序为TiB2>MnB2>AlB2>Co2B>NiB>Fe2B>MgB2>SiB3;实验表明,Si-B二元系中存在SiB4相,Si-Me-B相平衡实验也证明了FeSi2、CaB6和SiB6物相的存在,结果与二元相图吻合。
由02和H20-02吹气氧化精炼除硼热力学可知,向冶金级硅熔体中吹入02和H20-O2混合气体,杂质元素硼分别以气态硼氧化物(BxOy)和硼氢氧化物(BxHzOy)的形式挥发,并得到了1412-2230℃下杂质元素硼去除限度与硼化合物分压的热力学关系。研究表明,硼气态氢氧化物的平衡分压远高于硼气态氧化物,因此,利用H20-O2混合气体除硼效果应该更好。在1450℃时,各气态硼氢氧化物中,挥发性最大的是BH02和B3H306,当硼含量降低至5～10ppmw时,BH02平衡分压达到10SPa以上,降低至0.1ppm时为2500Pa,且各气态硼氢氧化物的平衡分压随温度的升高反而降低,在硅抬包中进行的02精炼实验表明,硅中Fe、Cu、V、C的去除率均低于20%,Al、Ca分别为98.2%和92.9%,B从35ppmw降低至18ppmw,去除率接近50%,P主要以P2的形式挥发,由184ppmw降低至112ppmw。在直流电弧炉中利用Ar-H2O-O2气氛进行除硼精炼实验表明,当精炼时间为10min时,硼含量可从18ppmw降低至2ppmw,由于受多方面动力学因素的影响和制约,硼的实验去除效果与热力学限度的理论计算值之间存在较大差距。
获得了平衡时硅中[%B]、熔渣中(%B)与aSiO2和acaO之间的热力学关系同时建立了CaO-SiO2熔渣与冶金级硅中杂质硼的电化学反应模型,该模型体现了硅中杂质硼与熔渣间的反应机理。熔渣精炼除硼实验表明,纯氧化物Si02基本起不到除硼的作用,这与热力学计算结果一致；采用CaO-SiO2熔渣时,当CaO/SiO2约为1.5时,硼的分配系数LB达到最大值1.58；当渣硅比为2.5、精炼时间3.0h时,硼含量可降低至1.8ppmw;向CaO-SiO2二元熔渣中添加MgO、Li2O、LiF和K20等形成CaO-SiO2-MeO三元熔渣精炼实验表明,添加MgO不利于除硼效率的提高,添加20%左右的Li20和LiF且当渣硅比为4：1时,硼含量可降低至1.3ppmw,硼的去除效率达到92.7%；添加30%K20时,硅中硼含量可降低至1.4ppmw;精炼后渣相的XRD结果表明,硅中杂质元素硼被氧化为B203并与加入的Li20形成Li2O·2B2O3。
提出和探讨了MeClx熔盐去除冶金级硅中杂质元素硼的方法和反应机理,得到了1550℃条件下CuCl2、FeCl3、MgCl2、NaCl、CaCl2和AICl3熔盐的除硼限度与BCly分压的热力学关系。实验发现,在冶金级硅中添加50%-60%的FeCl3时,可将硼含量由18ppmw降低至3.1ppmw,利用FeCl3-SiO2和MgCl2-SiO2混合体系除硼时,除硼效率随着熔盐含量的增加而增大。可以推测,采用FeCl3熔盐精炼除硼时,FeCl3被还原为金属Fe后与Si结合为金属间化合物FeSi2,而由于MgCl2的直接分解和Mg蒸汽的挥发,采用MgCl2熔盐时,渣样中没有发现金属Mg。
With the aggravation of global energy crisis, the rapid development of new energy materials especially for Photovoltaic industry is provided with chance of a lifetime. The Photovoltaic industry in the world has been rising at a speed of growth rate for30%annually. In2009, the production of solar cells had reached to10.5GWp on a global scale. It was4382MW in China and was more than40%for global totals. The solar grade silicon (SoG-Si) is base of Photovoltaic industry and the crystalline silicon solar cells had a share of88%in market in2009so the supply and cost of silicon materials is crucial for solar cells. Presently, the production of SoG-Si has mainly two methods:Siemens technology and thermal decompositon of SiH4, which have restricted the development of Photovoltaic industry for their high cost and heavy environmental load. To our inspiration, the new technology for SoG-Si preparation with metallurgical method, for its low cost, low energy consumption and friendly environment, has been growing up and applying. But the critical points and puzzled problems are the removal of impurities in metallurgical grade silicon (MG-Si) especially for B and P and the requirement for6N purity for SoG-Si.
In this paper, the features and removal of boron in MG-Si raw materials were systemically studied based on the MG-Si product with18ppmw for boron content. It was found that the impurities take on deep, light and white color inclusions in MG-Si. The deep inclusions confirmed as slag distribute in the whole MG-Si and the light and white ones that are thought to be metals or intermetallic compounds are lie in grain boundary of silicon. Based on binary phase diagrams between Si and impurity elements, the conformation of impurities Fe, Al, Ca, Ti, Ni, Cu etc in MG-Si raw materials was studied. The transformation among Si-B phases was analyzed and it was confirmed that SiB6is the form of Si-B phase in silicon melt. Based on Me-B, Si-Fe-B and Si-Al-B phase diagram systems, the probability of binary compounds FeB, Fe2B, AlB2, AlB12, CaB6and ternary compounds Fe4.7Si2B, Fe2Sio.4Bo.6were also analyzed. It was found that the preferential order for the combination between B and other elements is TiB2>MnB2>AlB2>Co2B>NiB>Fe2B>MgB2>SiB3. The phase equilibrium experiments indicated the existence of SiB4in Si-B binary system and also FeSi2, CaB6and SiB6in Si-Me-B systems, which was consistent with Si-Fe, Ca-B and Si-B phase diagrams.
The thermodynamic process of boron removal by O2and H2O-O2gas blowing was studied andit was found that the impurity boron is volatilized in forms of gaseous boron oxide species (BxOy)and gaseous boron hydrate species (BxHzOy) and the thermodynamic relationships betweenboron removal limitation and partial pressures of gaseous species at1412?2230°C wasobtained. It showed that the partial pressure of gaseous boron hydrate species is much higherthan that of gaseous boron oxide species so it is preferable to for boron removal with H2O-O2gasblowing. At1450°C, the volatilization of BHO2and B3H3O6is most among all gaseous boronhydrate species. The partial pressures of BHO2reach to105Pa and2500Pa when the boron levelis reduced to5ppmw and O.lppmw respectively and the thermodynamic relationships displaythat on the contrary the partial pressures of gaseous boron hydrate species will reduce with theincrease of temperature. The experimental results by O2gas blowing in ladle showed that theremoval rates of impurities Fe，Cu, V and C in MG-Si is lower than20%and it is98.2%and92.9%for A1and Ca. B is reduced from35ppmw to18ppmw which is close to50%and P isreduced from184ppmw to112ppmw which is volatilized in forms of gaseous P2. Theexperimental results by Ar-H20-02gas blowing in DC arc furnace showed the removal rate ofboron increased with the prolongation of refining time and it was reduced from18ppmw to2ppmw when the time reached to1Omin. But it has great difference between the boron removalresults in experiments and the calculated value for boron removal limitation in thermodynamicfor the effects and constraint for dynamic factors.
The thermodynamic relationships among boron level in silicon [%B], boron level in slag asi0and aCre obtained as
the same time, the electrochemical reactive model between Ca0-Si02slag and boron in MG-Siwas established, which displays the reactive mechanism between boron in silicon and molten slag. Theexperiments of slag refining in induction furnace showed it is not helpful to boron removal forpure Si2，which is accordant to thermodynamic results. The maximal value for partitioncoefficient of boron in silicon is1.58for Ca0-Si02slag when the composition of CaO/SiC>2is1.5. The boron level in silicon is reduced to1.8ppmw with the slag and silicon ratio2.5andrefining time3.Oh. The expeirmental results adding MgO, Li2，LiF and K2O to Ca0-Si02binary molten slag showed it is disadvantageous for boron removal with the addition of MgO.The boron level is respectively reduced to1.3ppmw and1,4ppmw when the slag and silicon ratio is4:1with the addition of20%LbO and30%K2O. The efficiency of boron removal is92.7%,The XRD spectrogram of refined slag showed that the experimental results with alloyed Si-Bsample are accordant to those of MG-Si refining and boron in MG-Si is oxidized into B2O3which combines into Li20*2B203with Li20.
The method of boron removal for MG-Si with molten salt MeClx refining was brought forward.The thermodynamic relation between boron level in silicon and equilibrium partial pressure ofBCly°with molten salt CuCb、FeCb、MgCh、NaCK CaCl2and AICI3at1550C was obtained.It was found by experiments the boron level in silicon is reduced from18ppmw to3.1ppmw withadding50%~60%FeCl3to MG-Si. The efficiency of boron removal increases with the higherratio of molten salt in mixed FeCl3-Si02and MgCb-Si02systems. It is presumed that FeCb isreduced to Fe, which combines into intermetallic compound FeSi: with Si when using FeCl3refining. However, Mg is not found in slag with MgCb refining maybe the decomposition ofMgCb and volatilization of Mg.
引文
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