CN103409808A - 多晶硅片制绒添加剂及其使用方法 - Google Patents

多晶硅片制绒添加剂及其使用方法 Download PDF

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CN103409808A
CN103409808A CN2013103947032A CN201310394703A CN103409808A CN 103409808 A CN103409808 A CN 103409808A CN 2013103947032 A CN2013103947032 A CN 2013103947032A CN 201310394703 A CN201310394703 A CN 201310394703A CN 103409808 A CN103409808 A CN 103409808A
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polycrystalline silicon
additive
wool
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CN103409808B (zh
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符黎明
章圆圆
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Jiangsu Jieyang Energy Equipment Co ltd
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Changzhou Shichuang Energy Technology Co Ltd
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Priority to PCT/CN2013/089693 priority patent/WO2015032154A1/zh
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Abstract

本发明提供一种多晶硅片制绒添加剂。本发明还提供一种用于多晶硅片制绒的制绒液，其含有酸溶液和上述多晶硅片制绒添加剂。本发明还提供一种多晶硅片的制绒方法，利用上述制绒液对多晶硅片进行表面制绒。该多晶硅片制绒添加剂应用于多晶硅片的绒面制作，可以得到均匀性好、晶粒间无明显色差的微洞型的微结构绒面，从而降低反射率，有效减少黑线产生数量；该多晶硅片制绒添加剂改变反应机理，控制反应速度，使制绒可以在接近室温的条件下进行，大大降低温度控制成本；还能有效去除滚轮印，使硅片更清洁，与后道工艺更匹配，电池性能更稳定。

Description

多晶硅片制绒添加剂及其使用方法
技术领域
本发明涉及多晶硅片制绒添加剂及其使用方法。
背景技术
在多晶硅太阳电池制造过程中，硅片表面制绒是关键的环节。制绒的效果直接影响了最终电池片的转换效率和成品率。由于多晶硅片由不同晶向的晶粒组成，并且各个晶粒的晶向随意分布，因此，在一般制绒工艺中多采用酸性溶液的湿化学腐蚀方法对多晶硅片表面进行制绒。该制绒工艺基于酸性溶液对硅的各向同性腐蚀原理，在硅片不同晶粒表面形成相似的凹坑状绒面，绒面的形貌与晶粒取向性无关。
目前，工业生产中常用的酸溶液由硝酸、氢氟酸和去离子水等组成。这种酸溶液的制绒效果并不是十分理想，存在的问题包括：绒面尺寸较大且均匀性不佳，不同晶粒之间色差比较明显，存在宏观形貌如黑线状的深腐蚀坑，表面反射率较高，制绒稳定性不好。因此，如果可以通过在酸溶液中加入制绒添加剂，来解决上述问题，将具有重要的意义。
发明内容
本发明的目的在于提供一种多晶硅片制绒添加剂及其使用方法，该多晶硅片制绒添加剂应用于多晶硅片的绒面制作，可以得到均匀性好、晶粒间无明显色差的微洞型的微结构绒面，从而降低反射率，有效减少黑线产生数量；该多晶硅片制绒添加剂改变反应机理，控制反应速度，使制绒可以在接近室温的条件下进行，大大降低温度控制成本；还能有效去除滚轮印，使硅片更清洁，与后道工艺更匹配，电池性能更稳定。
为实现上述目的，本发明提供一种多晶硅片制绒添加剂，其组分包括：柠檬酸三胺、聚乙烯吡咯烷酮、聚乙烯醇、柠檬酸和余量的水。
优选的，所述多晶硅片制绒添加剂中各组分的质量百分含量为：柠檬酸三胺0.2%～0.5%，聚乙烯吡咯烷酮0.1%～1%，聚乙烯醇0.1%～0.2%，柠檬酸2%～2.5%，余量为水。
优选的，所述水为去离子水。
本发明还提供一种用于多晶硅片制绒的制绒液，其含有酸溶液和上述多晶硅片制绒添加剂，所述多晶硅片制绒添加剂与酸溶液的质量比为0.1～0.6:100；所述酸溶液中配入了7%～14%的HF水溶液和25%～50%的HNO3水溶液；所述HF水溶液中含有49%的HF，所述HNO3水溶液中含有69%的HNO3;其中，所述百分比为质量百分比。
本发明还提供一种多晶硅片的制绒方法，利用上述制绒液对多晶硅片进行表面制绒。
优选的，所述表面制绒的制绒温度为5～25℃，制绒时间为45～180s。
上述多晶硅片的制绒方法的具体步骤包括：
1）配置制绒添加剂：将质量百分比为0.2%～0.5%的柠檬酸三胺、0.1%～1%的聚乙烯吡咯烷酮、0.1%～0.2%的聚乙烯醇、2%～2.5%的柠檬酸加入到余量的水中，混合均匀配成制绒添加剂；其中水优选为去离子水；
2）配置制绒液：将步骤1）制成的制绒添加剂加到酸溶液中，混合均匀配成制绒液；所述制绒添加剂与酸溶液的质量比为0.1～0.6:100；所述酸溶液中配入了7%～14%的HF水溶液和25%～50%的HNO3水溶液；所述HF水溶液中含有49%的HF，所述HNO3水溶液中含有69%的HNO3;其中，所述百分比为质量百分比；
3）将多晶硅片浸入步骤2）制得的制绒液中进行表面制绒，制绒温度为5～25℃，制绒时间为45～180s。
本发明的优点和有益效果在于：提供一种多晶硅片制绒添加剂及其使用方法，该多晶硅片制绒添加剂应用于多晶硅片的绒面制作，可以得到均匀性好、晶粒间无明显色差的微洞型的微结构绒面，从而降低反射率，有效减少黑线产生数量；该多晶硅片制绒添加剂改变反应机理，控制反应速度，使制绒可以在接近室温的条件下进行，大大降低温度控制成本；还能有效去除滚轮印，使硅片更清洁，与后道工艺更匹配，电池性能更稳定。
附图说明
图1是本发明实施例3的多晶硅片表面绒面的扫描电镜平面图。
具体实施方式
下面结合附图和实施例，对本发明的具体实施方式作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。
本发明具体实施的技术方案是：
实施例1
一种多晶硅片的制绒方法，采取如下工艺步骤：
1）配制制绒添加剂：将0.2g柠檬酸三胺、0.1g聚乙烯吡咯烷酮、0.1g聚乙烯醇、2g柠檬酸溶解于去离子水中，得到100g制绒添加剂；
2）配置制绒液：将7kg的HF水溶液(HF水溶液中HF的质量百分含量为49%)和25kg的HNO3水溶液(HNO3水溶液中HNO3的质量百分含量为69%)溶于去离子水中，得到100kg酸溶液；然后在该酸溶液中加入步骤1）制成的100g制绒添加剂得到制绒液；
3）制绒：将多晶硅电池片浸入制绒液中进行表面制绒，制绒温度为5℃，制绒时间为180s。
实施例2
一种多晶硅片的制绒方法，采取如下工艺步骤：
1）配制制绒添加剂：以去离子水为溶剂，将3g柠檬酸三胺、6g聚乙烯吡咯烷酮、1.2g聚乙烯醇、15g柠檬酸溶解于去离子水中，得到600g制绒添加剂；
2）配置制绒液：将14kg的HF水溶液(HF水溶液中HF的质量百分含量为49%)和50kg的HNO3水溶液(HNO3水溶液中HNO3的质量百分含量为69%)混合，得到100kg的酸溶液；然后在该酸溶液中加入步骤1）制成的600g制绒添加剂得到制绒液；
3）制绒：将多晶硅电池片浸入制绒液中进行表面制绒，制绒温度为25℃，制绒时间为45s。
实施例3
一种多晶硅片的制绒方法，采取如下工艺步骤：
1）配制制绒添加剂：以去离子水为溶剂，将1.2g柠檬酸三胺、1.5g聚乙烯吡咯烷酮、0.45g聚乙烯醇、6.9g柠檬酸溶解于去离子水中，得到300g制绒添加剂；
2）配置制绒液：将10kg的HF水溶液(HF水溶液中HF的质量百分含量为49%)和40kg的HNO3水溶液(HNO3水溶液中HNO3的质量百分含量为69%)溶于去离子水中，得到100kg的酸溶液；然后在该酸溶液中加入步骤1）制成的300g制绒添加剂得到制绒液；
3）制绒：将多晶硅电池片浸入制绒液中进行表面制绒，制绒温度为12℃，制绒时间为100s。
图1给出了本实施例3得到的多晶硅片表面绒面的扫描电镜平面照片，从图中可以看到制绒后在多晶硅片表面形成了微洞型的微结构绒面，绒面分布比较均匀。
 
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (7)

1.多晶硅片制绒添加剂，其特征在于，其组分包括：柠檬酸三胺、聚乙烯吡咯烷酮、聚乙烯醇、柠檬酸和余量的水。
2.根据权利要求1所述的多晶硅片制绒添加剂，其特征在于，所述多晶硅片制绒添加剂中各组分的质量百分含量为：柠檬酸三胺0.2%～0.5%，聚乙烯吡咯烷酮0.1%～1%，聚乙烯醇0.1%～0.2%，柠檬酸2%～2.5%，余量为水。
3.根据权利要求1或2所述的多晶硅片制绒添加剂，其特征在于，所述水为去离子水。
4.用于多晶硅片制绒的制绒液，其特征在于，其含有酸溶液和权利要求1-3中任意一项的多晶硅片制绒添加剂，所述多晶硅片制绒添加剂与酸溶液的质量比为0.1～0.6:100；所述酸溶液中配入了7%～14%的HF水溶液和25%～50%的HNO3水溶液；所述HF水溶液中含有49%的HF，所述HNO3水溶液中含有69%的HNO3;其中，所述百分比为质量百分比。
5.多晶硅片的制绒方法，其特征在于，利用权利要求4所述的制绒液对多晶硅片进行表面制绒。
6.根据权利要求5所述多晶硅片的制绒方法，其特征在于，所述表面制绒的制绒温度为5～25℃，制绒时间为45～180s。
7.根据权利要求6所述多晶硅片的制绒方法，其特征在于，其具体步骤包括：
1）配置制绒添加剂：将质量百分比为0.2%～0.5%的柠檬酸三胺、0.1%～1%的聚乙烯吡咯烷酮、0.1%～0.2%的聚乙烯醇、2%～2.5%的柠檬酸加入到余量的水中，混合均匀配成制绒添加剂；
2）配置制绒液：将步骤1）制成的制绒添加剂加到酸溶液中，混合均匀配成制绒液；所述制绒添加剂与酸溶液的质量比为0.1～0.6:100；所述酸溶液中配入了7%～14%的HF水溶液和25%～50%的HNO3水溶液；所述HF水溶液中含有49%的HF，所述HNO3水溶液中含有69%的HNO3;其中，所述百分比为质量百分比；
3）将多晶硅片浸入步骤2）制得的制绒液中进行表面制绒，制绒温度为5～25℃，制绒时间为45～180s。
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