CN110273144A - 化学水浴沉积方法和cigs光伏组件的制备方法 - Google Patents

化学水浴沉积方法和cigs光伏组件的制备方法 Download PDF

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CN110273144A
CN110273144A CN201810209148.4A CN201810209148A CN110273144A CN 110273144 A CN110273144 A CN 110273144A CN 201810209148 A CN201810209148 A CN 201810209148A CN 110273144 A CN110273144 A CN 110273144A
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layer
substrate
composite layer
deposition
cigs
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王磊
郭逦达
杨立红
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Beijing Apollo Ding Rong Solar Technology Co Ltd
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Beijing Apollo Ding Rong Solar Technology Co Ltd
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Priority to AU2018236863A priority patent/AU2018236863A1/en
Priority to JP2018184188A priority patent/JP2019161207A/ja
Priority to KR1020180126244A priority patent/KR20190108469A/ko
Priority to PCT/CN2019/078104 priority patent/WO2019174609A1/zh
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Abstract

本发明涉及化学水浴沉积方法和CIGS光伏组件的制备方法。所述化学水浴沉积方法包括以下步骤：提供一基板；在基板的相对侧面分别形成第一功能层和复合材料层，复合材料层包括高分子水凝胶和混合于高分子水凝胶中的磁性纳米粒子；将形成有第一功能层和复合材料层的基板置于沉积溶液中，在第一功能层上沉积形成第二功能层；将复合材料层和基板分离。所述CIGS光伏组件的制备方法采用上述化学水浴沉积方法。该方法在基板一侧面形成复合材料层作为保护层，使基板该侧面不被沉积溶液接触，同时利用复合材料层中的高分子水凝胶在反应液中溶胀，使该基板侧面的反应液的循环降低，避免了第二功能层在复合材料层的无效沉积，便于复合材料层的去除。

Description

化学水浴沉积方法和CIGS光伏组件的制备方法
技术领域
本发明涉及化学水浴沉积方法，特别是涉及改进的浸泡式化学水浴沉积方法和利用该方法制备CIGS光伏组件。
背景技术
化学水浴沉积方法，即chemical bath deposition(CBD)，具有成本低、成膜温度低、适合于制备大面积薄膜、易于实现连续生产、无污染、材料消耗量少等优越性，受到人们极大的关注。如：在高转换效率的CIGS薄膜太阳能电池结构中，采用化学水浴沉积方法制备的硫化镉(CdS)半导体薄膜作为缓冲层就具有重要作用。一般来说，CdS薄膜的化学水浴沉积法主要包括硫酸镉、氨水、纯水的预混合，硫脲加入，CdS在基板上生长，沉积结束后倾倒废液，取出基板，进入下一道工序。
现有技术中，CdS的化学水浴沉积法包括摇摆式和浸泡式。其中，摇摆式CBD工艺的镀膜均匀性明显高于浸泡式CBD工艺的镀膜均匀性，主要得益于较高的温度均匀性。以及，在摇摆式的CBD工艺中沉积CdS时，玻璃基板被率先加热，而化学反应液则以常温状态加入反应腔室。因此摇摆式的CBD工艺中，CdS会率先沉积在玻璃基板表面，而大大降低了化学液中形成的无规则CdS颗粒的浓度。但是在浸泡式CBD工艺中，化学预混合液(不含硫脲)会被率先加热至反应温度，之后加入硫脲，待混合液搅拌均匀后，冷基板进入反应腔室，开始CdS沉积。因此浸泡式CBD工艺的主要问题在于，在基板进入之前，反应液中已经开始了CdS颗粒的生成并在液体中悬浮，对镀膜工艺有负面影响。而未被预加热的基板则会缓慢的被溶液加热，CdS的沉积速率在初期较低，导致了较低的化学液利用率。另外，在浸泡式CBD工艺中，基板的正反面都会被CdS沉积，而最终只有正面的CdS是组件的有效膜层，背面的CdS膜层将不得不被清洗干净，而背面清洗机的设计也存在很多技术挑战，成为了浸泡式CBD产业化的瓶颈。
为了保证镀膜的均匀性，工业界常常倾向于使用摇摆式CBD，但是摇摆式CBD价格高昂。浸泡式CBD由于镀膜均匀度较低，但设备成本相比摇摆式CBD会大幅下降，也在不少产业上被使用。因此，提升浸泡式CBD基板温度均匀性，以及CdS在基板上的沉积速率，避免基板背面CdS沉积，是当前非常重要的研究课题。
发明内容
基于此，有必要针对上述问题，提供一种化学水浴沉积方法，该方法在基板一侧面形成复合材料层作为保护层，使基板该侧面不被沉积溶液接触，同时利用复合材料层中的高分子水凝胶在沉积溶液中的溶胀，使该基板侧面的沉积溶液的循环降低，避免了第二功能层在复合材料层的无效沉积，便于复合材料层的去除。
一种化学水浴沉积方法，所述方法包括以下步骤：
提供一基板；
在所述基板的相对侧面分别形成第一功能层和复合材料层，所述复合材料层包括高分子水凝胶和混合于所述高分子水凝胶中的磁性纳米粒子；
将形成有所述第一功能层和所述复合材料层的所述基板置于沉积溶液中，在所述第一功能层上沉积形成第二功能层；
将所述复合材料层和所述基板分离。
上述化学水浴沉积方法具有以下优点：
第一、在基板的一侧面形成复合材料层作为保护层，使基板该侧面不被沉积溶液接触，避免了第二功能层在基板该侧面的无效沉积；第二、复合材料层中的磁性纳米粒子的无接触式感应加热既可以保证基板加热的均匀性，又可以保证基板的温度高于沉积溶液的温度，使第二功能层的沉积更容易发生，提高了第二功能层在第一功能层上的沉积速率；第三、复合材料层中的高分子水凝胶作为磁性纳米粒子的有效载体，既可以保证磁性纳米粒子的均匀分布，又可以保证磁性纳米粒子不从复合材料中流失；第四、高分子水凝胶在反应液中溶胀，使该基板侧面的沉积溶液的循环降低，避免了第二功能层在复合材料层的无效沉积，便于复合材料层的去除；第五、复合材料的合成工艺成熟，可大批量产及购买、成本低廉，掺入的磁性纳米粒子可以重复利用。因此，上述化学水浴沉积方法对现有的浸泡式CBD工艺起到了有效地改善作用，解决了浸泡式CBD工艺中基板均匀加热的问题，提高了浸泡式CBD工艺的成膜效率和成膜均匀性。同时，可以保证第二功能层的沉积过程从基板的第一功能层面开始，降低了沉积溶液中快速生成的悬浮颗粒。此外，还可以完全避免第二功能层在基板上的无效沉积，免去了后续针对无效沉积的第二功能层的化学清洗过程。
本发明还提供一种CIGS光伏组件的制备方法，所述制备方法包括以下步骤：
提供一基板；
在所述基板的相对侧面分别形成CIGS层和复合材料层，所述复合材料层包括高分子水凝胶和混合于所述高分子水凝胶中的磁性纳米粒子；
将形成有所述CIGS层和所述复合材料层的所述基板置于沉积溶液中，在所述CIGS层上沉积形成CdS层；
将所述复合材料层和所述基板分离。
上述CIGS光伏组件的制备方法应用了上述化学水浴沉积方法，在制备过程中，以复合材料层作为基板一侧面的保护层，使基板该侧面不被沉积溶液接触并均匀加热基板，使CdS层的沉积在CIGS层上进行，避免了CdS层的无效沉积，免去了后续化学清洗的麻烦。
上述制备得到的CIGS光伏组件包括叠层设置的基板、CIGS层和CdS层，CdS层均匀、完整的覆盖在CIGS层表面形成紧密的p-n结界面，确保激子分离效率，保证光电转化率。使CIGS光伏组件具有光吸收能力强，发电稳定性好、转化效率高，白天发电时间长、发电量高，生产成本低以及能源回收周期短等优点。不仅可应用于光伏发电站，同时可应用于光伏建筑一体化(即BIPV)或光伏屋顶发电(光伏附着建筑，即BAPV)等领域。此外，柔性的CIGS光伏组件也可使其应用于便携式发电产品，如发电纸，发电背包等。
附图说明
图1为本发明化学水浴沉积方法的工艺流程图；
图2为本发明CIGS光伏组件的制备方法的工艺示意图；
图中：1、基板；2、CIGS层；3、复合材料层；4、CdS层；5、交变电流；6、溶剂。
具体实施方式
以下将对本发明提供的化学水浴沉积硫化镉薄膜的方法作进一步说明。
如图1所示，本发明提供一种化学水浴沉积方法，所述方法包括以下步骤：
a、提供一基板；
b、在所述基板的相对侧面分别形成第一功能层和复合材料层，所述复合材料层包括高分子水凝胶和混合于所述高分子水凝胶中的磁性纳米粒子；
c、将形成有所述第一功能层和所述复合材料层的所述基板置于沉积溶液中，在所述第一功能层上沉积形成第二功能层；
d、将所述复合材料层和所述基板分离。
在步骤a中，所述基板材料不限。
在步骤b中，所述第一功能层包括p-结材料层、发光层。所述p-结材料层是光伏组件的光吸收层，所述p-结材料层包括但不限于CIGS层(铜铟镓硒层)、单晶硅层、多晶硅层、砷化镓层、有机染料层。所述发光层是OLED的功能层，所述发光层包括但不限于有机发光半导体材料层。
在步骤b中，所述复合材料层采用丝网印刷的方式形成于基板的一侧面。复合材料层包括磁性纳米粒子和高分子水凝胶，具备两种材料的特性，既可以感应加热，也具备成膜性和溶胀特性。其中，作为载体的高分子水凝胶可丝网印刷，通过丝网印刷的方式将复合材料涂在基板的一侧面，可以保证复合材料层的均匀性。
在步骤b中，所述复合材料层中所述高分子水凝胶和所述磁性纳米粒子的质量百分比分别为80％～95％和5％～20％。所述高分子水凝胶包括聚丙烯酸树脂的共聚交联物、聚乙烯醇、聚丙烯酰胺、硅基水凝胶中的至少一种。所述磁性纳米粒子包括Fe3O4。通过使用不同的高分子水凝胶材料，使复合材料层的强度、溶胀等特性达到最佳。考虑到聚丙烯酸树脂的共聚交联物具有好的涂膜性、合成方法简单、成本低，同时水溶胀性好，溶胀比例可调节，因此，所述高分子水凝胶优选为聚丙烯酸树脂的共聚交联物。
在步骤c中，所述第二功能层包括n-结材料层。n-结材料层是光伏组件的缓冲层，与p-结材料层匹配形成p-n结，常见的n-结材料层为CdS层。可以理解，在其它领域，所述第二功能层为能够与第一功能层匹配使用的功能层。
在步骤c中，在所述沉积过程中利用交变磁场对所述基板进行感应加热，所述交变磁场的频率为450kHz～550kHz，所述加热温度根据沉积的第二功能层确定。通过交变磁场对基板进行感应加热，使基板先被加热，然后沉积溶液通过基板温度加热。因此，保证了基板温度高于沉积溶液的温度，使沉积更容易在基板上发生，避免了因沉积溶液温度高于基板温度而导致沉积溶液中有悬浮颗粒产生的负面影响。所述交变磁场优选由交变电流产生，所述交变磁场与复合材料层的感应加热功能匹配，使其达到最佳的工艺水平，所述复合材料层的感应加热功能可以通过调节上述磁性纳米粒子和高分子水凝胶的质量百分比达到。
在步骤c的所述沉积过程中，优选基板与容器/反应槽的侧壁平行设置，便于布置电路，使交变电流与基板基本垂直，产生的交变磁场感应加热效果最佳，以达到最佳工艺水平。
在步骤d中，将所述复合材料层和所述基板分离时，采用溶剂溶解所述复合材料层。溶剂包括但不限于二甲基亚砜(DMSO)溶液、二甲基甲酰胺(DMF)溶液中的至少一种。DMSO和DMF等溶剂都可以溶解高分子水凝胶，要分离复合材料层和基板时，只要将复合材料层浸泡于溶剂中进行溶解即可。溶剂将高分子水凝胶溶解后，复合材料层中的磁性纳米粒子也随之流入溶剂中，使复合材料层与基板有效分离。上述通过湿法工艺去除基板一侧面的复合材料层，不仅技术成本和技术门槛低，而且不会对基板造成伤害，同时，还可以回收再利用磁性纳米粒子。
上述化学水浴沉积方法具有以下优点：
第一、在基板的一侧面形成复合材料层作为保护层，使基板该侧面不被沉积溶液接触，避免了第二功能层在基板该侧面的无效沉积；第二、复合材料层中的磁性纳米粒子的无接触式感应加热既可以保证基板加热的均匀性，又可以保证基板的温度高于沉积溶液的温度，使第二功能层的沉积更容易发生，提高了第二功能层在第一功能层上的沉积速率；第三、复合材料层中的高分子水凝胶作为磁性纳米粒子的有效载体，既可以保证磁性纳米粒子的均匀分布，又可以保证磁性纳米粒子不从复合材料中流失；第四、高分子水凝胶在反应液中溶胀，使该基板侧面的沉积溶液的循环降低，避免了第二功能层在复合材料层的无效沉积，便于复合材料层的去除；第五、复合材料的合成工艺成熟，可大批量产及购买、成本低廉，掺入的磁性纳米粒子可以重复利用；第六、复合材料层的分离不仅技术成本和技术门槛低，而且不会对基板造成伤害；第七、磁性纳米粒子可以回收再利用。
因此，上述化学水浴沉积方法对现有的浸泡式CBD工艺起到了有效地改善作用，解决了浸泡式CBD工艺中基板均匀加热的问题，提高了浸泡式CBD工艺的成膜效率和成膜均匀性。同时，可以保证第二功能层的沉积过程从基板的第一功能层面开始，降低了沉积溶液中快速生成的悬浮颗粒。此外，还可以完全避免第二功能层在基板上的无效沉积，免去了后续针对无效沉积的第二功能层的化学清洗过程。
如图2所示，本发明还提供一种CIGS光伏组件的制备方法，所述方法包括以下步骤：
S1、提供一基板1；
S2、在所述基板1的相对侧面分别形成CIGS层2和复合材料层3，所述复合材料层3包括高分子水凝胶和混合于所述高分子水凝胶中的磁性纳米粒子；
S3、将形成有所述CIGS层2和所述复合材料层3的所述基板1置于沉积溶液中，在所述CIGS层2上沉积形成CdS层4；
S4、将所述复合材料层3和所述基板1分离。
在步骤S1中，所述基板1材料不限，常用的光伏组件的基板均可以，优选为玻璃基板。
在步骤S3中，在所述沉积过程中利用交变磁场对所述基板进行感应加热，所述感应加热的温度为60℃～70℃。所述沉积溶液包括硫酸镉、氨水、纯水的预混合溶液和硫脲溶液，所述基板先置于预混合溶液中，利用预混合溶液中的氨水对基板进行表面处理，基板经感应加热以后，再加入硫脲溶液，反应开始，CdS开始沉积。
上述CIGS光伏组件的制备方法应用了上述化学水浴沉积方法，在制备过程中，以复合材料层作为基板一侧面的保护层，使基板该侧面不被沉积溶液接触并均匀加热基板，使CdS层的沉积在CIGS层上进行，避免了CdS层的无效沉积，免去了后续化学清洗的麻烦。
上述制备得到的CIGS光伏组件包括叠层设置的基板、CIGS层和CdS层，CdS层均匀、完整的覆盖在CIGS层表面形成紧密的p-n结界面，确保激子分离效率，保证光电转化率。使CIGS光伏组件具有光吸收能力强，发电稳定性好、转化效率高，白天发电时间长、发电量高，生产成本低以及能源回收周期短等优点。不仅可应用于光伏发电站，同时可应用于光伏建筑一体化(即BIPV)或光伏屋顶发电(光伏附着建筑，即BAPV)等领域。此外，柔性的CIGS光伏组件也可使其应用于便携式发电产品，如发电纸，发电背包等。
以下，将通过以下具体实施例对所述CIGS光伏组件的制备方法做进一步的说明。
实施例1：
参照图1和图2，选择玻璃基板1并在玻璃基板1的一侧面镀上CIGS层2。
然后在玻璃基板1的另一侧面采用丝网印刷的方式涂上复合材料层3，复合材料层3包括聚丙烯酸树脂的共聚交联物和混合于聚丙烯酸树脂的共聚交联物中的Fe3O4颗粒，两者的质量百分比分别为90％和10％。
然后将形成有CIGS层2和复合材料层3的玻璃基板1竖直放置，浸泡在盛有硫酸镉、氨水、纯水的预混合溶液的反应槽中。之后开启交变电流5，其产生的频率为500kHz的交变磁场使得复合材料层3中的Fe3O4颗粒快速加热，从而使玻璃基板1均匀加热至65℃。此时加入硫脲溶液，CdS沉积开始在CIGS层2表面发生。
沉积结束后将玻璃基板1翻转至水平，复合材料层3浸泡在DMSO溶液6中，溶解聚丙烯酸树脂的共聚交联物材料，同时Fe3O4颗粒也随之流入DMSO溶液6，整个复合材料层3与玻璃基板1脱离，获得玻璃基板1、CIGS层2和CdS层4叠层设置的CIGS光伏组件，CIGS光伏组件中CdS层4均匀完整的覆盖在CIGS层2表面上。
经检验，CdS层4光透过率高、禁带宽度约为2.4eV，非常适合做CIGS薄膜太阳能电池的缓冲层。
实施例2：
参照图1和图2，选择玻璃基板1并在玻璃基板1的一侧面镀上CIGS层2。
然后在玻璃基板1的另一侧面采用丝网印刷的方式涂上复合材料层3，复合材料层3包括聚乙烯醇和混合于聚乙烯醇中的Fe3O4颗粒，两者的质量百分比分别为80％和20％。
然后将形成有CIGS层2和复合材料层3的玻璃基板1竖直放置，浸泡在盛有硫酸镉、氨水、纯水的预混合溶液的反应槽中。之后开启交变电流5，其产生的频率为550kHz的交变磁场使得复合材料层3中的Fe3O4颗粒快速加热，从而使玻璃基板1均匀加热至60℃。此时加入硫脲溶液，CdS沉积开始在CIGS层2表面发生。
沉积结束后将玻璃基板1翻转至水平，复合材料层3浸泡在DMF溶液6中，溶解聚乙烯醇材料，同时Fe3O4颗粒也随之流入DMF溶液6，整个复合材料层3与玻璃基板1脱离，获得玻璃基板1、CIGS层2和CdS层4叠层设置的CIGS光伏组件，CIGS光伏组件中CdS层4均匀完整的覆盖在CIGS层2表面上。
经检验，CdS层4光透过率高、禁带宽度约为2.4eV，非常适合做CIGS薄膜太阳能电池的缓冲层。
实施例3：
参照图1和图2，选择玻璃基板1并在玻璃基板1的一侧面镀上CIGS层2。
然后在玻璃基板1的另一侧面采用丝网印刷的方式涂上复合材料层3，复合材料层3包括聚丙烯酰胺和混合于聚丙烯酰胺中的Fe3O4颗粒，两者的质量百分比分别为85％和15％。
然后将形成有CIGS层2和复合材料层3的玻璃基板1竖直放置，浸泡在盛有硫酸镉、氨水、纯水的预混合溶液的反应槽中。之后开启交变电流5，其产生的频率为500kHz的交变磁场使得复合材料层3中的Fe3O4颗粒快速加热，从而使玻璃基板1均匀加热至68℃。此时加入硫脲溶液，CdS沉积开始在CIGS层2表面发生。
沉积结束后将玻璃基板1翻转至水平，复合材料层3浸泡在DMSO溶液6中，溶解聚丙烯酰胺材料，同时Fe3O4颗粒也随之流入DMSO溶液6，整个复合材料层3与玻璃基板1脱离，获得玻璃基板1、CIGS层2和CdS层4叠层设置的CIGS光伏组件，CIGS光伏组件中CdS层4均匀完整的覆盖在CIGS层2表面上。
经检验，CdS层4光透过率高、禁带宽度约为2.4eV，非常适合做CIGS薄膜太阳能电池的缓冲层。
实施例4：
参照图1和图2，选择玻璃基板1并在玻璃基板1的一侧面镀上CIGS层2。
然后在玻璃基板1的另一侧面采用丝网印刷的方式涂上复合材料层3，复合材料层3包括硅基水凝胶和混合于硅基水凝胶中的Fe3O4颗粒，两者的质量百分比分别为95％和5％。
然后将形成有CIGS层2和复合材料层3的玻璃基板1竖直放置，浸泡在盛有硫酸镉、氨水、纯水的预混合溶液的反应槽中。之后开启交变电流5，其产生的频率为450kHz的交变磁场使得复合材料层3中的Fe3O4颗粒快速加热，从而使玻璃基板1均匀加热至70℃。此时加入硫脲溶液，CdS沉积开始在CIGS层2表面发生。
沉积结束后将玻璃基板1翻转至水平，复合材料层3浸泡在DMSO溶液6中，溶解硅基水凝胶材料，同时Fe3O4颗粒也随之流入DMSO溶液6，整个复合材料层3与玻璃基板1脱离，获得玻璃基板1、CIGS层2和CdS层4叠层设置的CIGS光伏组件，CIGS光伏组件中CdS层4均匀完整的覆盖在CIGS层2表面上。
经检验，CdS层4光透过率高、禁带宽度约为2.4eV，非常适合做CIGS薄膜太阳能电池的缓冲层。
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (10)

1.一种化学水浴沉积方法，其特征在于，所述方法包括以下步骤：
提供一基板；
在所述基板的相对侧面分别形成第一功能层和复合材料层，所述复合材料层包括高分子水凝胶和混合于所述高分子水凝胶中的磁性纳米粒子；
将形成有所述第一功能层和所述复合材料层的所述基板置于沉积溶液中，在所述第一功能层上沉积形成第二功能层；
将所述复合材料层和所述基板分离。
2.根据权利要求1所述的化学水浴沉积方法，其特征在于，所述第一功能层包括p-结材料层、发光层。
3.根据权利要求1所述的化学水浴沉积方法，其特征在于，所述第二功能层包括n-结材料层。
4.根据权利要求1所述的化学水浴沉积方法，其特征在于，所述复合材料层中所述高分子水凝胶和所述磁性纳米粒子的质量百分比分别为80％～95％和5％～20％。
5.根据权利要求1所述的化学水浴沉积方法，其特征在于，所述高分子水凝胶包括聚丙烯酸树脂的共聚交联物、聚乙烯醇、聚丙烯酰胺、硅基水凝胶中的至少一种。
6.根据权利要求1所述的化学水浴沉积方法，其特征在于，所述磁性纳米粒子包括Fe3O4。
7.根据权利要求1所述的化学水浴沉积方法，其特征在于，在所述沉积过程中利用交变磁场对所述基板进行感应加热。
8.根据权利要求7所述的化学水浴沉积方法，其特征在于，所述交变磁场的频率为450kHz～550kHz。
9.根据权利要求1所述的化学水浴沉积方法，其特征在于，将所述复合材料层和所述基板分离时，采用溶剂溶解所述复合材料层。
10.一种CIGS光伏组件的制备方法，其特征在于，所述制备方法包括以下步骤：
提供一基板；
在所述基板的相对侧面分别形成CIGS层和复合材料层，所述复合材料层包括高分子水凝胶和混合于所述高分子水凝胶中的磁性纳米粒子；
将形成有所述CIGS层和所述复合材料层的所述基板置于沉积溶液中，在所述CIGS层上沉积形成CdS层；
将所述复合材料层和所述基板分离。
CN201810209148.4A 2018-03-14 2018-03-14 化学水浴沉积方法和cigs光伏组件的制备方法 Pending CN110273144A (zh)

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