CN110867383A - 一种三步硫化工艺制备铜锌锡硫薄膜吸收层的方法 - Google Patents
一种三步硫化工艺制备铜锌锡硫薄膜吸收层的方法 Download PDFInfo
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Abstract
本发明公开了一种三步硫化工艺制备铜锌锡硫薄膜吸收层的方法，属于高质量铜锌锡硫薄膜吸收层制备技术领域，其特征在于，包括如下步骤：S1、在真空退火炉中，放置热舟，在舟上方放置前驱体膜，热舟中放置5g硫粉，抽真空到10‑3Pa后，对热舟进行快速加热，使其20秒到达800℃，而前驱体膜不加热，膜温度低于50℃，保持10分钟，使得硫原子能够均匀扩散到前驱体膜中；S2、将前驱体膜取出放入管式炉中，通入氩气，使得气压保持在1.2个大气压，加热管式炉到540℃‑580℃，保持10分钟，降温；S3、将管式炉气压降至1个大气压，温度保持在250℃‑300℃，保持10分钟，去除残留的硫，然后降至室温。
Description
技术领域
本发明属于高质量铜锌锡硫薄膜吸收层制备技术领域，具体涉及一种三步硫化工艺制备铜锌锡硫薄膜吸收层的方法。
背景技术
由于化石能源通常伴随着严重的环境污染问题，人们对可再生能源的需求和重视程度不断增加。太阳电池具有清洁、可再生和能量用之不竭等诸多优点，已逐渐成为解决能源危机和环境危机的有效途径之一。
在众多种类的太阳电池中，薄膜太阳电池由于用料少、直接带隙材料具有超高光吸收系数、适合柔性衬底制备等诸多优点，成为当今的研究热点。其中，以铜铟镓硒(CIGS)和碲化镉(CdTe)材料最有代表性，发展的也最好。但是，CdTe和CIGS和CdTe太阳电池应用了稀有元素和毒性元素(主要是Cd)，这在很大程度上限制了此两种薄膜太阳电池的产业化进程。基于以上原因，科研工作者将研究目标放在了无毒且原料丰富的材料上，铜锌锡硫(Cu2ZnSnS4，CZTS)太阳电池成为新的研究热点。总结各种制备CZTS吸收层的方法，如溅射法、纳米涂覆法、溶胶凝胶法等，大致都可以分为两步。首先制备包含铜、锌、锡等元素的前驱体膜，然后在硫气氛中退火处理形成符合要求的CZTS吸收层膜。常用的硫元素来源有两种，一为高纯硫粉，另外一种为包含一定比例的硫化氢(H2S)混合气。由于硫化氢为毒性气体，对使用条件要求很高，存在环境污染的潜在危险，关于采用该工艺制备CZTS吸收层及薄膜电池的专利如：申请号为201210135807.7和申请号为201310277578.7的专利申请材料。采用高纯硫粉做为硫原料来源，由于硫低温下(200℃以下)就回升华，原料损失严重、原料利用率较低；此外，在硫原子向前驱体膜中扩散过程中，率先与前驱体表层膜反应形成大晶粒层，从而阻止硫原子向前驱体膜深处的进一步扩散，导致下层晶粒细碎，影响载流子输运、电池效率受限，代表性的如：申请号为201410326643.5和申请号为201510550954.4的专利申请材料。传统硫化方式制备CZTS膜典型扫描电镜断面图如图1所示。
发明内容
本发明为解决公知技术中存在的技术问题(下层晶粒细碎、原料利用率较低)而提供一种三步硫化工艺制备高质量铜锌锡硫吸收层薄膜的方法，该方法的目的是在提升原料利用率的基础上，制备得到高质量的铜锌锡硫吸收层薄膜。
本发明的目的是提供一种三步硫化工艺制备铜锌锡硫薄膜吸收层的方法，通过在双层Mo背电极上利用溅射或者涂覆的方法制备包含铜、锌、锡元素的前驱体膜，然后在硫气氛下进行退火，形成高质量铜锌锡硫吸收层薄膜；包括如下步骤：
S1、在真空退火炉中，放置热舟，在舟上方放置前驱体膜，热舟中放置5g硫粉，抽真空到10-3Pa后，对热舟进行快速加热，使其20秒到达800℃，而前驱体膜不加热，膜温度低于50℃，保持10分钟，使得硫原子能够均匀扩散到前驱体膜中；
S2、将前驱体膜取出放入管式炉中，通入氩气，使得气压保持在1.2个大气压，加热管式炉到540℃-580℃，保持10分钟，降温；
S3、将管式炉气压降至1个大气压，温度保持在250℃-300℃，保持10分钟，去除残留的硫，然后降至室温。
进一步，在所述S2中，加热管式炉到540℃。
进一步，在所述S2中，加热管式炉到580℃。
进一步，在所述S3中，温度保持在250℃。
进一步，在所述S3中，温度保持在300℃。
本发明具有的优点和积极效果是：
本发明通过三步硫化工艺来提升薄膜结晶质量，精确控制膜中各元素比例和提升原料利用率。本发明通过在双层Mo背电极上利用溅射或者涂覆的方法制备包含铜、锌、锡元素的前驱体膜，然后在硫气氛下进行退火，能够形成高质量铜锌锡硫吸收层薄膜。
附图说明
图1是传统硫化工艺制备CZTS吸收层薄膜扫描电镜断面图；
图2是本发明优选实施例的流程图；
图3是采用本发明方法后的CZTS吸收层膜扫描电镜断面图
具体实施方式
为能进一步了解本发明的发明内容、特点及功效，兹例举以下实施例，并配合附图详细说明如下：
本发明针对采用传统硫化方式易造成吸收层膜分为两层下层晶粒细碎、成分不可控制及原料利用率低的问题，设计开发了三步硫化工艺来提升薄膜结晶质量，精确控制膜中各元素比例和提升原料利用率。
请参阅图1至图3：
本发明通过在双层Mo背电极上利用溅射或者涂覆的方法制备包含铜、锌、锡元素的前驱体膜，然后在硫气氛下进行退火，形成高质量铜锌锡硫吸收层薄膜。
具体为：
第一步：在真空退火炉中，放置热舟，在舟上方放置前驱体膜，热舟中放置5g硫粉，抽真空到10-3Pa后，对热舟进行快速加热，使其20秒到达800℃，而前驱体膜不加热(膜温度低于50℃)，保持10分钟，使得硫原子能够均匀扩散到前驱体膜中；
第二步，将前驱体膜取出放入管式炉中，通入氩气，使得气压保持在1.2个大气压(正压可以抑制硫元素流失)，加热管式炉到540℃-580℃，保持10分钟，降温；
第三步，将管式炉气压降至1个大气压，温度保持在250℃-300℃，保持10分钟，去除残留的硫，然后降至室温，具体工艺流程图如图2所示。采用三步硫化工艺制备的CZTS吸收层薄膜扫描电镜断面图如图3所示。
实施例1：在钠钙玻璃衬底上应用直流磁控溅射的方法制备双层Mo背电极，然后采用多靶共溅射的方法制备1.5μm到2μm厚的CZTS前驱体膜，对前驱体膜采用上述三步硫化工艺进行硫化，形成高质量铜锌锡硫吸收层薄膜。
实施例2：在钠钙玻璃衬底上应用直流磁控溅射的方法制备双层Mo背电极，然后采用溶胶凝胶后涂覆的方法制备1.5μm到2μm厚的CZTS前驱体膜，对前驱体膜采用上述三步硫化工艺进行硫化，形成高质量铜锌锡硫吸收层薄膜。
实施例3：在不锈钢衬底上应用直流磁控溅射的方法制备双层Mo背电极，然后采用多靶共溅射的方法制备1.5μm到2μm厚的CZTS前驱体膜，对前驱体膜采用上述三步硫化工艺进行硫化，形成高质量铜锌锡硫吸收层薄膜。
实施例4：在不锈钢衬底上应用直流磁控溅射的方法制备双层Mo背电极，然后采用溶胶凝胶后涂覆的方法制备1.5μm到2μm厚的CZTS前驱体膜，对前驱体膜采用上述三步硫化工艺进行硫化，形成高质量铜锌锡硫吸收层薄膜。
以上所述仅是对本发明的较佳实施例而已，并非对本发明作任何形式上的限制，凡是依据本发明的技术实质对以上实施例所做的任何简单修改，等同变化与修饰，均属于本发明技术方案的范围内。
Claims (5)
1.一种三步硫化工艺制备铜锌锡硫薄膜吸收层的方法，其特征在于，通过在双层Mo背电极上利用溅射或者涂覆的方法制备包含铜、锌、锡元素的前驱体膜，然后在硫气氛下进行退火，形成高质量铜锌锡硫吸收层薄膜；包括如下步骤：
S1、在真空退火炉中，放置热舟，在舟上方放置前驱体膜，热舟中放置5g硫粉，抽真空到10-3Pa后，对热舟进行快速加热，使其20秒到达800℃，而前驱体膜不加热，膜温度低于50℃，保持10分钟，使得硫原子能够均匀扩散到前驱体膜中；
S2、将前驱体膜取出放入管式炉中，通入氩气，使得气压保持在1.2个大气压，加热管式炉到540℃-580℃，保持10分钟，降温；
S3、将管式炉气压降至1个大气压，温度保持在250℃-300℃，保持10分钟，去除残留的硫，然后降至室温。
2.根据权利要求1所述三步硫化工艺制备铜锌锡硫薄膜吸收层的方法，其特征在于，在所述S2中，加热管式炉到540℃。
3.根据权利要求1所述三步硫化工艺制备铜锌锡硫薄膜吸收层的方法，其特征在于，在所述S2中，加热管式炉到580℃。
4.根据权利要求1所述三步硫化工艺制备铜锌锡硫薄膜吸收层的方法，其特征在于，在所述S3中，温度保持在250℃。
5.根据权利要求1所述三步硫化工艺制备铜锌锡硫薄膜吸收层的方法，其特征在于，在所述S3中，温度保持在300℃。
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