CN102549200A - 一种通过感应方法生产多晶硅锭的方法 - Google Patents
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Abstract
一种通过感应方法生产多晶硅锭的方法，包括将硅原料装入到被电感器包围的冷坩埚的熔化室内，形成熔体表面，以及熔化，其中，装入硅原料的质量速率和锭的拉出速度，设定至可以使熔体表面位置在电感器的上平面下，但是不低于其高度的1/3，且熔体表面保持在相同水平。通过保持电感器供给输出参数之一在预定的范围内，使熔体表面位置保持在相同水平上。该工艺提供的铸造多晶硅锭适用于太阳能电池的制作，重要的是其生产效率提高，能量的消耗降低。
Description
技术领域
本发明涉及多结晶硅的生产，特别是通过感应方法生产多晶硅，并且多晶硅可被用作制造太阳能电池。
晶体硅用作生产太阳能电池，将太阳能转化为电能。大晶体组成的多结晶硅，通常被称为多晶硅，其生产最近得到很多的关注，该种多晶硅提供的太阳能转化为电能的转化率接近于单晶硅的转化率。
背景技术
生产多晶硅锭的工艺在下列文献中公开了：美国专利号为4,572,812(国际专利分类号为B29D7/02，B22D27/02[1])，欧洲专利号为1254861(公开日为2002年11月06日(国际专利分类号为C01B33/02[2]))，欧洲专利号为：1754806(公开日为2007年02月21日(国际专利分类号为C30B11/00[3]))，以及该工艺包括将硅原料装入到被电感器包围的冷坩埚的熔化室内，形成熔体表面，熔化和拉出得到多晶硅锭。然而，这些工艺中都没有描述熔化条件和锭拉出的条件，这些条件正是提供熔融结晶化的持续条件。
一种通过感应方法生产多晶硅锭的工艺，该工艺与本发明的工艺密切相关，包括将硅原料装到被电感器包围的冷却坩埚的熔化室内，形成熔融表面，在监测电感器供给的输出参数的条件下熔化，和在控制的冷却条件下拉出多晶硅锭(欧洲专利号为1930483国际专利分类号为C30B35/00，C30B29/06，C01B33/02，公开日为2007年02月22日[4])。在现有技术的工艺中，熔化是通过监测电感器供给的输出功率控制的，其中测得的换流器频率与其预设的频率进行对比，而以热能方式供给的输出功率同时也被监测，其中测得的锭表面的温度与锭表面的预设温度进行对比。
然而，在这样的条件下，锭中硅的结晶化是不牢固的，因为在现有技术工艺中，电感器供给的输出功率的持续变化，会导致锭结晶化速度的持续变化从而对其质量产生不利影响。
另外，根据现有技术的工艺，熔体深度的增加要求电感器供给输出功率的降低。当通过提高熔体表面增加熔体深度，工作频率就会增加，电感器供给输出功率则会降低。一方面来说，这些依存关系导致熔体结晶化速率提高，另一方面来说，这些依赖导致了装入的原料熔化速率的降低，并且它能够使得熔体表面被原料完全填满并且使原料粘结在冷却坩埚壁上。因此，锭的拉出将被迫停止以进行连接坩埚的原料的熔化，规律的熔化过程被中断，熔化速率减慢，且生产效率将会降低。
本发明的目的在于针对通过感应方法生产多晶硅锭的工艺进行改进，其中硅结晶化会变得稳定，锭的质量会相对高，以及由于建议的工艺步骤使生产效率得到提高。
发明内容
为了完成上述的目标，提供了一种通过感应方法生产多晶硅锭的工艺，该工艺包括将硅原料装入到被电感器包围的冷坩埚的熔化室内，形成熔体表面，熔化的同时监测电感器供给的输出参数，以及在控制的冷却条件下拉出多晶硅锭，其中，在熔化过程中，装入硅原料的质量速率和锭的拉出速度设定至可以使熔体表面位置在电感器的上平面下但是不低于其高度的1/3，且熔体表面保持在相同水平。通过保持电感器供给输出参数之一在预定的范围内，特别是，工作频率、电压、电流，保持熔体表面位置在相同水平上。
在通过感应方法铸造多晶硅锭中，从实验上确定当熔体表面位置在电感器的上平面下的但是不低于其高度的1/3时，达到了最大的熔化速率，以及通过设定装入硅原料的质量速率，拉出锭的速度和电感器供给输出参数，例如，电感器的工作频率、电压或电流，使得熔体表面位置保持在这种水平时，硅稳定地结晶。
具体实施方式
为了熔化原料，热量被消耗用作原料的热焓和在固相与液相的界面吸收的熔化热。由于热量主要涉及液相，即，硅熔体，电磁能量的释放被限制在电感器关于熔体表面的吸收热量的位置之处。因此，熔化的速率得到提高，原因是熔体被混合，以及从感应电流区流向硅原料熔化区的过热熔体流，并且熔化稳定和迅速提供了硅结晶化的进一步的稳定性。因此生产的锭的颗粒截面大小达到太阳能电池生产商对晶片粒度的规格要求，所生产的锭适合用于制造太阳能电池。并且，锭的生产效率提高，能量的消耗降低。
本发明工作过程如下：
在控制的氩气氛围下的室内，移动可活动的底部而划定熔化室，将硅原料装入到熔化室内。通过包围冷却坩埚的电感器形成高频的电磁场。启动加热装置被插入到熔化室内，该熔化室内部通过电感器形成了高频电磁场。启动加热装置加热，硅原料在来自于启动加热装置和通过电感器形成的电磁场散发的热量的影响下被加热和熔化，启动加热装置从电磁场中移出，而在熔化室内，以熔化室截面的形式产生熔池。由于热量沿着熔池外围传递，熔体结晶并形成骨架以防止熔池从熔化室溢出。在熔池形成以后，硅原料被连续地提供到熔体表面上。在熔化过程中，装入硅原料的质量速率和锭的拉出速率设定至可以使熔体表面位置在电感器的上平面下，但是不低于其高度的1/3，且熔体表面保持在相同水平。例如，通过维持电感器的工作频率、电压或电流在一个预定的范围内，或者其他方法。
实施例
本发明通过如下实施例进一步描述。
实施例1
通过感应熔化技术使用一种带有正方形截面和边长为350mm的熔化室的装置获得多晶硅锭。在氩气氛围下的室内，移动可活动的底部而划定包围有120mm高的电感器的冷却坩埚的熔化室，块状的硅原料被装入到熔化室内。高频率的电磁场形成。启动加热装置插入到熔化室内，块状硅原料被加热和熔化，启动加热装置从电磁场中移出，以熔化室截面的形式产生熔池。熔体结晶并沿着熔池的外围形成骨架。颗粒大小在15-20mm范围内的硅原料被连续地提供到熔体表面上。电感器供给输出功率设定为300kW，装入硅原料的质量速率设定为每分钟0.4kg，拉出锭的速度设定为每分钟1.5mm，而熔体表面位置设定为在电感器的上平面下25mm。电感器供给的工作频率是16.7kHz。在熔化过程中，通过将电感器供给的工作频率维持在16.7±0.05kHz范围内，熔体表面保持在相同水平。通过调节装入硅原料的质量速率的方式保持频率在上述范围内，其中拉锭的速度也是恒定的。在熔化过程中，装入硅原料的质量速率被调节在每分钟0.40-0.45kg范围内，该数值依赖于原料可变参数的偶然变化，特别是颗粒大小还有进料器精度。为了消除锭生长的热应力，在退火室进行退火，以及在控制的条件下冷却。由于电感器供给稳定的输出功率和恒定拉锭速度，晶前面(crystallization front)变得稳定在单一水平上。由此，建立了在多晶硅锭中晶体生长的优选条件。并且，熔体表面的位置低于电感器上平面25mm，可以达到由给定的颗粒大小的原料生产的锭的拉锭最大速度。这是通过电感器和熔体表面区的电磁耦合实现的。接下来的退火和控制冷却，从退火室取出多晶硅锭和切成块状，该块状晶片随后被切割用于生产太阳能电池。
生产多晶硅锭的工艺的速率是每小时25.7kg。所生产的锭的颗粒截面大小达到太阳能电池生产商对晶片粒度的规格要求。
实施例2
通过感应熔化技术以实施例1中描述的相同的方法获得多晶硅锭。电感器供给的输出功率和硅原料的颗粒大小与实施例1中相似。装入硅原料的质量速率设定为每分钟0.3kg，拉锭的速度设定为每分钟1.2mm，而熔体表面位置设定为在电感器的上平面下5mm。电感器供给的工作频率是16.9kHz。在熔化过程中，通过将电感器供给的工作频率维持在16.9±0.05kHz范围内，使熔体表面保持在相同水平。通过调节装入硅原料的质量速率保持频率在上述范围内，其中拉锭的速度也是恒定的。在熔化过程中，装入硅原料的质量速率被调节在每分钟0.32-0.37kg范围内，该数值依赖于原料可变参数的偶然变化，特别是颗粒大小还有进料器精度。
生产多晶硅锭的工艺的速率是每小时20.6kg。所生产的锭的颗粒截面大小达到太阳能电池生产商对晶片粒度的规格要求。
实施例3
通过感应熔化技术以实施例1中描述的相同的方法获得多晶硅锭。电感器供给的输出功率和硅原料的颗粒大小与实施例1中相似。装入硅原料的质量速率设定为每分钟0.4kg，拉锭的速度设定为每分钟1.3mm，而熔体表面位置设定为在电感器的上平面下10mm。电感器供给的工作电流是4650A。在熔化过程中，通过将电感器供给的工作电流维持在4650±5A范围内，熔体表面保持在相同水平。通过调节装入硅原料的质量速率保持电流在上述范围内，其中拉锭的速度也是恒定的。在熔化过程中，装入硅原料的质量速率被调节在每分钟0.35-0.40kg范围内，该数值依赖于原料可变参数的偶然变化，特别是颗粒大小还有进料器精度。
生产多晶硅锭的工艺的速率是每小时22.3kg。所生产的锭的颗粒截面大小达到太阳能电池生产商对晶片粒度的规格要求。
本发明保证了多晶硅产量的提高和铸造的多晶硅锭的高质量，可以适用于太阳能电池的制作。
Claims (2)
1.一种通过感应方法生产多晶硅锭的方法，该方法包括将硅原料装入被电感器包围的冷却坩埚的熔化室内，形成熔体表面，熔化的同时监测电感器供给输出参数，以及在控制冷却条件下拉出多晶硅锭，其特征在于，在熔化过程中，装入硅原料的质量速率和锭的拉出速度，设定至使熔体表面位置在电感器的上平面以下，但是不低于其高度的1/3，且熔体表面保持在相同水平。
2.如权利要求1所述的方法，其特征在于，通过保持电感器供给输出参数之一在预定的范围内，特别是，工作频率、电压、电流，使熔体表面位置保持在相同水平上。
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| UAA200908864 | 2009-08-25 | ||
| UAA200908864A UA95131C2 (uk) | 2009-08-25 | 2009-08-25 | Спосіб одержання зливків мультикристалічного кремнію індукційним методом |
| PCT/UA2010/000053 WO2011025468A1 (en) | 2009-08-25 | 2010-08-20 | Process for production of multicrystalline silicon ingots by induction method |
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| CN102549200A true CN102549200A (zh) | 2012-07-04 |
| CN102549200B CN102549200B (zh) | 2014-05-14 |
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| US (1) | US9284661B2 (zh) |
| EP (1) | EP2470693B8 (zh) |
| JP (1) | JP5675814B2 (zh) |
| KR (1) | KR101511826B1 (zh) |
| CN (1) | CN102549200B (zh) |
| ES (1) | ES2442625T3 (zh) |
| UA (1) | UA95131C2 (zh) |
| WO (1) | WO2011025468A1 (zh) |
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| CN103194803B (zh) * | 2013-03-22 | 2015-11-04 | 中国科学院上海硅酸盐研究所 | 适用于高温氧化物晶体生长的辅助监测系统 |
| NO336720B1 (no) * | 2013-09-09 | 2015-10-26 | Elkem Solar As | Fremgangsmåte for forbedring av effektiviteten av solceller. |
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| JPS643027A (en) * | 1987-06-26 | 1989-01-06 | Nkk Corp | Production of silicic acid |
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| JP3000109B2 (ja) * | 1990-09-20 | 2000-01-17 | 株式会社住友シチックス尼崎 | 高純度シリコン鋳塊の製造方法 |
| JPH04338195A (ja) * | 1991-05-13 | 1992-11-25 | Osaka Titanium Co Ltd | シリコン鋳造方法 |
| DE4318184A1 (de) | 1993-06-01 | 1994-12-08 | Wacker Chemitronic | Verfahren und Vorrichtung zum Ziehen von Einkristallen |
| WO2006088037A1 (ja) * | 2005-02-17 | 2006-08-24 | Sumco Solar Corporation | シリコン鋳造装置およびシリコン基板の製造方法 |
| JP2007019209A (ja) * | 2005-07-07 | 2007-01-25 | Sumco Solar Corp | 太陽電池用多結晶シリコンおよびその製造方法 |
| JP2007051026A (ja) * | 2005-08-18 | 2007-03-01 | Sumco Solar Corp | シリコン多結晶の鋳造方法 |
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2009
- 2009-08-25 UA UAA200908864A patent/UA95131C2/uk unknown
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2010
- 2010-08-20 US US13/390,279 patent/US9284661B2/en not_active Expired - Fee Related
- 2010-08-20 ES ES10760133.8T patent/ES2442625T3/es active Active
- 2010-08-20 JP JP2012526694A patent/JP5675814B2/ja not_active Expired - Fee Related
- 2010-08-20 CN CN201080037571.2A patent/CN102549200B/zh not_active Expired - Fee Related
- 2010-08-20 EP EP10760133.8A patent/EP2470693B8/en not_active Not-in-force
- 2010-08-20 WO PCT/UA2010/000053 patent/WO2011025468A1/en active Application Filing
- 2010-08-20 KR KR20127005894A patent/KR101511826B1/ko not_active IP Right Cessation
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| US4572812A (en) * | 1984-08-13 | 1986-02-25 | The United States Of America As Represented By The Secretary Of Energy | Method and apparatus for casting conductive and semiconductive materials |
| US6027563A (en) * | 1996-02-24 | 2000-02-22 | Ald Vacuum Technologies Gmbh | Method and apparatus for the oriented solidification of molten silicon to form an ingot in a bottomless crystallization chamber |
| US20030150374A1 (en) * | 2000-12-28 | 2003-08-14 | Kenichi Sasatani | Silicon continuous casting method |
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Also Published As
| Publication number | Publication date |
|---|---|
| JP5675814B2 (ja) | 2015-02-25 |
| US9284661B2 (en) | 2016-03-15 |
| JP2013503100A (ja) | 2013-01-31 |
| US20120137473A1 (en) | 2012-06-07 |
| EP2470693A1 (en) | 2012-07-04 |
| KR101511826B1 (ko) | 2015-04-13 |
| ES2442625T3 (es) | 2014-02-12 |
| EP2470693B1 (en) | 2013-10-16 |
| UA95131C2 (uk) | 2011-07-11 |
| WO2011025468A1 (en) | 2011-03-03 |
| CN102549200B (zh) | 2014-05-14 |
| EP2470693B8 (en) | 2014-02-26 |
| KR20120059529A (ko) | 2012-06-08 |
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