CN104319305A - 一种制备cigs薄膜的方法及cigs薄膜 - Google Patents
一种制备cigs薄膜的方法及cigs薄膜 Download PDFInfo
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Abstract
本发明涉及一种采用多靶材制备CIGS薄膜的方法，采用镀钼的玻璃、不锈钢或柔性高分子膜作为基底，纯金属Cu、In、Ga、Se作为四个溅射靶的靶材，以纯的氩气为溅射气体，在溅射设备内对靶材进行溅射，使基底上沉积CIGS薄膜，得到的CIGS薄膜其组分为CuxInyGa(1-y)Se，0≤x<1，0<y<1；其中，Cu、In、Ga与Se的溅射功率为W1、W2、W3与W4。可通过改变溅射靶的溅射功率，直接调节薄膜的元素比，无需更换靶材情况下制备出不同组分的膜层；所制备的薄膜具有与基底结合力高、均匀性好。
Description
技术领域
本发明属于CIGS薄膜制备技术领域，具体是涉及一种多靶材共溅射制备CIGS薄膜的方法。
背景技术
CIGS是太阳能薄膜电池CuInxGa(1-x)Se2的简写，铜铟镓硒薄膜太阳能电池由于具有高转换效率、高光吸收系数、高稳定性和良好的抗辐射能力等优点，被认为是第三代太阳能电池的主要材料，其最高转换效率已达到19％以上。CIGS薄膜太阳能电池是多层结构组件，主要结构包括：基底、背电极、吸收层、缓冲层、透明导电层和减反射层。目前的研究重点主要集中在吸收层的制备工艺开发上。制备CIGS吸收层的主要方法有共蒸发法和溅射法。
一般CIGS薄膜的制备采用三步共蒸发法，是在真空室内由蒸发源向基底政法金属，反应沉积CIGS薄膜。蒸发过程的控制是制备薄膜的关键，一般可通过控制蒸发速率和蒸发源温度来实现。控制蒸发速率通常采用原子吸收法或荧光光谱法，但设备造价高；蒸发源温度的控制比较简单，但可靠性和重现性差。且所制备的薄膜与基底的结合力低，存在易脱落的问题。另外，共蒸发法工艺难度大、成品率低、原料利用率也较低。
对于工业化应用，磁控溅射法更适用于薄膜的量化生产。不仅可大面积制备CIGS薄膜，原材料利用率高，且溅射法制备的前驱体薄膜致密性高，组分均匀性好。现有技术中，一般采用的磁控溅射方法是单一靶材直接溅射后硒化法，首先在基底上沉积Cu-In-Ga金属预制层，然后在H2Se或Se蒸汽氛围中进行后处理，得到满足化学计量比的CIGS薄膜。为将预置层彻底硒化，需进行较长时间的热处理，这增加了工艺的复杂性。且H2Se蒸汽有毒，不利于人体健康。同时，此方法对原材料靶材的质量要求很高，靶材的制备过程较复杂，且靶材组分一旦固定，薄膜成分即受其限制而不可调控。
研究发现，太阳能电池吸收层用CIGS薄膜通过改变Ga、In、Cu量，可调节太阳能电池的光电转换率，主要调节措施包括富Ga膜、富In膜、贫Cu膜等。制备工艺中所使用靶材为合金靶材，使得薄膜各元素之间比例受靶材元素成分的限制，不能在不更换靶材的情况下，人为任意调节各元素的量。若使用不用元素比的靶材制备不同的CIGS薄膜，需要制备大量合金靶材。且合金靶的制备工艺较复杂，增加了CIGS薄膜制备的成本。
发明内容
基于现有技术中CIGS薄膜制备中的问题，本发明的目的是提供了一种磁控溅射多靶材共溅射制备CIGS薄膜的方法，制备的薄膜具有与基底结合力高、均匀性好、组分可调节等优点。且所使用靶材为纯金属靶材，靶材易得，该方法可调节薄膜的元素比，制备出不同组分的膜层，而无需更换靶材。
为达到上述目的，本发明是通过以下的技术方案来实现的：
采用镀钼的玻璃、不锈钢或柔性高分子膜作为基底，纯金属Cu、In、Ga、Se作为四个溅射靶的靶材，以纯的氩气为溅射气体，在溅射设备内对靶材进行溅射，使基底上沉积CIGS薄膜，得到的CIGS薄膜其组分为CuxInyGa(1-y)Se，0≤x<1，0<y<1；其中，Cu、In、Ga与Se的溅射功率为W1、W2、W3与W4，溅射生长时各溅射靶离基底的距离为d，氩气的气压为Ps，溅射生长时的基底温度为Ts。
在上述的技术方案中，所述溅射为直流溅射、交流溅射、反应溅射或磁控溅射；所述溅射为对四种靶材同时进行溅射；其中，溅射功率W1、W2、W3、W4的取值范围为：0W≤W1≤500W，0W<W2≤500W、0W<W3≤500W、0W<W4≤500W。
在上述的技术方案中，所所述氩气的纯度大于99.9％，气压Ps的取值范围为：10-3Pa≤Ps≤10Pa。
在上述的技术方案中，基底温度Ts的取值范围为500K<Ts<1500K。
在上述的技术方案中，Cu、In、Ga、Se靶材的纯度大于99.9％。
在上述的技术方案中，溅射靶离基底的距离d的取值范围为：0cm<d≤30cm。
本发明还提供一种CIGS膜，采用上述所述的方法制备，其薄膜组分为CuxInyGa(1-y)Se，包括富Ga膜、富In膜和贫Cu膜。
在上述的CIGS膜中，其中富Ga膜中0<x<1，0<y<0.5；富In膜中，0<x<1，0<y<0.5；贫Cu膜中，0≤x<1。
本发明的技术方案，其有益效果是，使用靶材为多个纯金属靶材，靶材易得；可通过改变溅射靶的溅射功率，直接调节薄膜的元素比，无需更换靶材情况下制备出不同组分的膜层；所制备的薄膜具有与基底结合力高、均匀性好、组分可调节等优点。
具体实施方式
以下结合具体实施例对本发明的技方案作详细的说明。
以下实施例都用到的主要设备是磁控溅射仪，其至少具有四个电源和能安装四种靶材，每个电源接一个靶材，基压可达1.0×10-5Pa。
实施例1：CIGS薄膜的制备
以镀钼的玻璃为基底，将基底以及纯度大于99.99％的纯金属Cu、In、Ga、Se靶材装入磁控溅射仪内，进行抽真空至5.0×10-5Pa以下；调节每个溅射靶离基底的距离d为25cm，通入纯度大于99.9％的氩气体，调节流量为40sccm(体积流量单位)，调节沉积压力Ps为10Pa；对靶材进行预溅射，其Cu、In、Ga、Se靶材的溅射功率W1、W2、W3、W4分别为350W、350W、350W、350W，溅射时间为5min；加热基底温度Ts至1000K，同时打开Cu、In、Ga、Se靶材挡板进行溅射，基底上进行沉积生长CIGS薄膜，沉积时间t1为5小时。
停止加热，关闭挡板和关闭电源，停止通气；待基底温度冷却至20℃时，打开溅射仪取出基底，经检测本实施例的薄膜组分为CuxInyGa(1-y)Se，其中x＝0.6786,y＝0.5355。
本实施例制备的CIGS薄膜，其中In、Ga、Se的组分比例基本相等，膜具有与基底结合力高、均匀性好。
实施例2：富Ga的CIGS薄膜的制备：
以镀钼的玻璃为基底，将基底以及纯度大于99.99％的纯金属Cu、In、Ga、Se靶材装入磁控溅射仪内，进行抽真空至5.0×10-5Pa以下；调节每个溅射靶离基底的距离d为25cm，通入纯度大于99.9％的氩气体，调节流量为40sccm(体积流量单位)，调节沉积压力Ps为10Pa；对靶材进行预溅射，其Cu、In、Ga、Se靶材的溅射功率W1、W2、W3、W4分别为350W、350W、450W、350W，溅射时间为5min；加热基底温度Ts至1000K，同时打开Cu、In、Ga、Se靶材挡板进行溅射，基底上进行沉积生长CIGS薄膜，沉积时间t1为5小时。
停止加热，关闭挡板和关闭电源，停止通气；待基底温度冷却至20℃时，打开溅射仪取出基底，经检测本实施例的薄膜组分为CuxInyGa(1-y)Se，其中x＝0.5692,y＝0.3672。
本实施例制备的CIGS薄膜，膜具有与基底结合力高、均匀性好，Ga含量的适当增加，有利于提高薄膜的转换率。
实施例3：富In的CIGS薄膜的制备
以镀钼的玻璃为基底，将基底以及纯度大于99.99％的纯金属Cu、In、Ga、Se靶材装入磁控溅射仪内，进行抽真空至5.0×10-5Pa以下；调节每个溅射靶离基底的距离d为25cm，通入纯度大于99.9％的氩气体，调节流量为40sccm(体积流量单位)，调节沉积压力Ps为10Pa；对靶材进行预溅射，其Cu、In、Ga、Se靶材的溅射功率W1、W2、W3、W4分别为350W、450W、350W、350W，溅射时间为5min；加热基底温度Ts至1000K，同时打开Cu、In、Ga、Se靶材挡板进行溅射，基底上进行沉积生长CIGS薄膜，沉积时间t1为5小时。
停止加热，关闭挡板和关闭电源，停止通气；待基底温度冷却至20℃时，打开溅射仪取出基底，经检测本实施例的薄膜组分为CuxInyGa(1-y)Se，其中x＝0.6256,y＝0.7624。
本实施例制备的CIGS薄膜，膜具有与基底结合力高、均匀性好，In含量的适当增加，也可提高薄膜的转换率。
实施例4：贫Cu的CIGS薄膜的制备
以镀钼的玻璃为基底，将基底以及纯度大于99.99％的纯金属Cu、In、Ga、Se靶材装入磁控溅射仪内，进行抽真空至5.0×10-5Pa以下；调节每个溅射靶离基底的距离d为25cm，通入纯度大于99.9％的氩气体，调节流量为40sccm(体积流量单位)，调节沉积压力Ps为10Pa；对靶材进行预溅射，其Cu、In、Ga、Se靶材的溅射功率W1、W2、W3、W4分别为250W、350W、350W、350W，溅射时间为5min；加热基底温度Ts至1000K，同时打开Cu、In、Ga、Se靶材挡板进行溅射，基底上进行沉积生长CIGS薄膜，沉积时间t1为5小时。
停止加热，关闭挡板和关闭电源，停止通气；待基底温度冷却至20℃时，打开溅射仪取出基底，经检测本实施例的薄膜组分为CuxInyGa(1-y)Se，其中x＝0.3025,y＝0.5875。
本实施例制备的CIGS薄膜，膜具有与基底结合力高、均匀性好，Cu含量的适当减少，可提高薄膜的转换率。
以上描述了本发明的优选实施例，并非因此局限本发明的权利范围。本领域技术人员不脱离本发明的范围和实质内所作的任何修改、等同替换和改进，均应在本发明的权利范围之内。
Claims (10)
1.一种制备CIGS薄膜的方法，其特征在于，采用镀钼的玻璃、不锈钢或柔性高分子膜作为基底，纯金属Cu、In、Ga、Se作为四个溅射靶的靶材，以纯的氩气为溅射气体，在溅射设备内对靶材进行溅射，使基底上沉积CIGS薄膜，得到的CIGS薄膜其组分为CuxInyGa(1-y)Se，0≤x<1，0<y<1；其中，Cu、In、Ga与Se的溅射功率为W1、W2、W3与W4。
2.根据权利要求1所述的制备CIGS薄膜的方法，其特征在于，所述溅射为直流溅射、交流溅射、反应溅射或磁控溅射。
3.根据权利要求1或2所述的制备CIGS薄膜的方法，其特征在于，所述溅射为对靶材同时进行溅射。
4.根据权利要求1或2所述的制备CIGS薄膜的方法，其特征在于，所述溅射功率W1、W2、W3、W4的取值范围为：0W≤W1≤500W，0W<W2≤500W、0W<W3≤500W、0W<W4≤500W。
5.根据权利要求1所述的制备CIGS薄膜的方法，其特征在于，所述氩气的纯度大于99.9％，气压Ps的取值范围为：10-3Pa≤Ps≤10Pa。
6.根据权利要求1所述的制备CIGS薄膜的方法，其特征在于，基底温度Ts的取值范围为500K<Ts<1500K。
7.根据权利要求1所述的制备CIGS薄膜的方法，其特征在于，Cu、In、Ga、Se靶材的纯度大于99.9％。
8.根据权利要求1所述的制备CIGS薄膜的方法，其特征在于，溅射靶离基底的距离d的取值范围为：0cm<d≤30cm。
9.一种如权利要求1所述的方法制备的CIGS薄膜，其特征在于，薄膜组分为CuxInyGa(1-y)Se，包括富Ga膜、富In膜和贫Cu膜。
10.根据权利要求9所述的CIGS膜，其特征在于，其中富Ga膜中0<x<1，0<y<0.5；富In膜中，0<x<1，0<y<0.5；贫Cu膜中，0≤x<1。
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