CN103147118B - 一种利用直拉区熔法制备太阳能级硅单晶的方法 - Google Patents

一种利用直拉区熔法制备太阳能级硅单晶的方法 Download PDF

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CN103147118B
CN103147118B CN201310057877.XA CN201310057877A CN103147118B CN 103147118 B CN103147118 B CN 103147118B CN 201310057877 A CN201310057877 A CN 201310057877A CN 103147118 B CN103147118 B CN 103147118B
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乔柳
王彦君
张雪囡
刘嘉
孙健
王遵义
涂颂昊
刘铮
冯啸桐
孙昊
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Zhonghuan Leading Semiconductor Technology Co ltd
Tianjin Zhonghuan Advanced Material Technology Co Ltd
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Abstract

本发明提供一种利用直拉区熔法制备太阳能级硅单晶的方法：在区熔阶段的等径生长工艺中，在区熔硅单晶炉电气控制系统的控制下，使下转电机正向、反向交替转动，所述下转电机带动硅单晶按照设定的正向角度和反向角度转动。本发明提高了太阳能级硅单晶的径向均匀性，解决了太阳能级硅单晶的黑心问题，能够提高由该太阳能级硅单晶制得的太阳能电池片的转换效率。

Description

一种利用直拉区熔法制备太阳能级硅单晶的方法
技术领域
本发明属于硅单晶的制备技术领域，尤其是涉及一种利用直拉区熔法制备太阳能级硅单晶的方法。
背景技术
直拉区熔硅单晶生产技术克服了传统直拉法和区熔法生产工艺中的固有缺陷，易于规模化生产。由直拉区熔法制得的硅单晶具有良好的性能价格比，且具有易于掺入特殊固态杂质元素的特性，所以在半导体材料领域具有广阔的市场和应用前景。但目前用于太阳能领域的直拉区熔硅单晶，在其制备工艺中的区熔阶段单晶是单方向旋转的，所以气相掺杂过程中，掺杂剂和氧碳等分布不均，仍然会出现直拉硅单晶常见的黑心现象，且其径向均匀性差，影响由其制得的太阳能电池片的转换效率。
发明内容
本发明要解决的问题是提供一种利用直拉区熔法制备太阳能级硅单晶的方法，尤其适合用于改善太阳能级硅单晶的光伏性能。
为解决上述技术问题，本发明采用的技术方案是：一种利用直拉区熔法制备太阳能级硅单晶的方法：在区熔阶段的等径生长工艺中，在区熔硅单晶炉电气控制系统的控制下，使下转电机正向、反向交替转动，所述下转电机带动硅单晶按照设定的正向角度和反向角度转动。
进一步，所述正向角度和所述反向角度的比值为一预设值。
进一步，所述正向角度和所述反向角度之比为380：620。
进一步，所述正向角度为100°-800°，所述反向角度为50°-750°。
本发明具有的优点和积极效果是：本发明在制备太阳能级硅单晶的等径生长工艺中引入双向旋转工艺，使太阳能级硅单晶的径向电阻率的均匀性有了很大改善，解决了太阳能级硅单晶的黑心问题，能够提高由该太阳能级硅单晶制得的太阳能电池片的转换效率。
附图说明
图1是利用现有技术制得的太阳能级硅单晶
图2是利用实施例所述的技术方案制得的太阳能级硅单晶
具体实施方式
本发明提供一种利用直拉区熔法制备太阳能级硅单晶的方法：在区熔阶段的等径生长工艺中，在区熔硅单晶炉电气控制系统的控制下，使下转电机正向、反向交替转动，下转电机带动硅单晶按照设定的正向角度和反向角度转动，正向角度和反向角度的比值为一预设值。正向角度的优选范围为100°-800°，反向角度优选为50°-750°。正向角度和反向角度的比值优选为380：620。
在整个太阳能级硅单晶的制备过程中，正向角度和反向角度的数值一直不变。在不同的太阳能级硅单晶的制备工艺中，根据制备需求，可以预设不同的正向角度和反向角度的比值。
具体实施例：
在本实施例中，首先用直拉法拉制硅单晶，然后进行锭型加工，清洗腐蚀，然后在区熔阶段的等径生长工艺中，采用双向旋转工艺进行太阳能级硅单晶的拉制，具体步骤如下：
1.将80公斤腐蚀清洗干净的块状硅多晶料装入直拉炉中的石英干锅内，然后抽真空、充氩气，经30-60分钟抽真空到压力≤100毫乇时充氩气至真空压力≤14乇；
2.加热前通冷却水，启动加热按钮，加热至1500-1600℃，块状硅多晶全部熔化后，开动籽晶旋转机构，下降籽晶熔接籽晶；
3.液面稳定后拉细颈，通过籽晶从融熔状多晶料中拉出一段直径约8mm、长为20mm的细颈；
4.下降籽晶升速，设定升速为0.5mm/min左右进行放肩，60分钟左右将直径从细颈的8mm扩大至140mm-150mm；
5.调节直径传感器，控制拉晶速度进行等径拉晶，等径生长时间为20小时；
6.降低晶体拉速进行收尾，收尾时间为2小时；
7.提高晶体使其离开液面，按下停炉按钮进行停炉操作，待功率表回零后切断电源，2小时后停止主真空泵抽空，将多晶棒料出炉；
8.将出炉后的多晶棒进行锭型加工，清洗腐蚀后装入区熔炉内晶体夹持器上，将<100>籽晶装入籽晶固定夹头上；
9.将预热片放在籽晶周围，关闭炉门抽真空充氩气后，对多晶棒进行加热；同时设置掺杂气体的掺杂值和电机旋转的正向角度和反向角度比值，正向角度和反向角度的比值设定为380：620；
10.预热结束后进行化料，待多晶料熔化后，将籽晶与熔硅进行熔接，熔接后对熔区进行整形和引晶；
11.引晶结束后，进行细颈生长，细颈直径为3-6mm，长度为20-100mm；
12.降低下部晶体速度，控制扩肩角度在50-70°(开始扩肩时打开掺杂气，掺杂气通过流量计按照设定值进入炉室)，扩肩至要求直径后，进行等径生长，此时按下电机控制按钮，使电机按设定程序进行正向和反向的交替旋转，正向角度为380°，反向角度为620°，直至单晶等径生长阶段结束，关闭程序，使电机开始带动单晶单向旋转；
13.上料不足时，开始进行收尾，收尾后停止掺杂气体充入，当收尾至单晶直径达到需要值时，将熔区拉开，下轴带动单晶继续向下，上轴带动多晶料改向上运动，并关闭氩气；
14.10-60分钟后，晶体尾部由红色逐渐变成黑色后，进行拆炉清炉工作，将单晶取出。
利用现有技术中的直拉区熔法制得的太阳能级硅单晶的径向均匀性(RRV值)为30％-40％，如图1所示，利用现有技术制得的硅单晶片存在黑心现象，后期制得的太阳能电池片的转换效率为21％，且存在一定的效率衰减效应。
本实施例制得的太阳能级硅单晶的径向均匀性(RRV值)为10％，如图2所示，没有黑心现象产生，后期制得的太阳能电池片的转换效率达到24％，电池效率基本不衰减。
以上对本发明的一个实施例进行了详细说明，但所述内容仅为本发明的较佳实施例，不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的均等变化与改进等，均应仍归属于本发明的专利涵盖范围之内。

Claims (1)

1.一种利用直拉区熔法制备太阳能级硅单晶的方法，其特征在于：在区熔阶段的等径生长工艺中，在区熔硅单晶炉电气控制系统的控制下，使下转电机正向、反向交替转动，所述下转电机带动硅单晶按照设定的正向角度和反向角度转动；
所述正向角度和所述反向角度的比值为一预设值；
所述正向角度和所述反向角度之比为380：620；
所述正向角度为100°-800°，所述反向角度为50°-750°。
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US14/769,627 US20160002819A1 (en) 2013-02-25 2013-11-01 Method for preparing solar grade silicon single crystal using czochralski zone melting method
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CN109440183B (zh) * 2018-12-20 2020-11-13 天津中环领先材料技术有限公司 一种优化型大直径区熔硅单晶收尾方法
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US20160002819A1 (en) 2016-01-07

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