CN108048822A - 化学浴沉积装置及其沉积方法、废液回收系统 - Google Patents

化学浴沉积装置及其沉积方法、废液回收系统 Download PDF

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CN108048822A
CN108048822A CN201711386486.7A CN201711386486A CN108048822A CN 108048822 A CN108048822 A CN 108048822A CN 201711386486 A CN201711386486 A CN 201711386486A CN 108048822 A CN108048822 A CN 108048822A
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accumulator tank
chemical liquids
waste liquid
chemical
inlet
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王磊
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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 CN201711386486.7A priority Critical patent/CN108048822A/zh
Publication of CN108048822A publication Critical patent/CN108048822A/zh
Priority to PCT/CN2018/105795 priority patent/WO2019119902A1/zh
Priority to CN201880002715.7A priority patent/CN110177900A/zh
Priority to AU2018236877A priority patent/AU2018236877A1/en
Priority to US16/145,687 priority patent/US20190189829A1/en
Priority to JP2018232861A priority patent/JP2019111526A/ja
Priority to EP18212999.9A priority patent/EP3502061A1/en
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Abstract

本发明提供了一种化学浴沉积装置及其沉积方法、废液回收系统，化学浴沉积装置包括硫化镉反应槽、废液储存槽、制冷装置、过滤装置、化学液储存槽和补充供药装置；废液储存槽的进液口与硫化镉反应槽的出液口相连；废液储存槽的出液口与制冷装置的进液口相连；制冷装置的出液口与过滤装置的进液口相连；过滤装置的出液口与化学液储存槽的进液口相连；补充供药装置用于向化学液储存槽补入化学品；化学液储存槽的出液口与硫化镉反应槽的进液口相连。本发明提供的化学浴沉积装置及其沉积方法、废液回收系统通过对废液进行制冷、过滤，在补充化学品原料，从而得到与原液浓度相同的化学液，相比于现有技术，大大地提高了废液的回收利用，降低了生产成本。

Description

化学浴沉积装置及其沉积方法、废液回收系统
技术领域
本发明涉及太阳能电池的生产技术，尤其涉及一种化学浴沉积装置及其沉积方法、废液回收系统。
背景技术
铜铟镓硒(CIGS)太阳能电池技术作为最先进的薄膜发电技术之一，具有非常广阔的产业化前景。其产品可以基于刚性玻璃的大尺寸基板，在光照强烈的地方建造光伏发电站，也可用于建筑幕墙，光伏建筑一体化(BIPV)等。同时，铜铟镓硒光伏组件也可做成柔性小尺寸产品，其轻柔薄的特性可以使其在便携式发电产品中脱颖而出，如薄膜发电纸，发电背包等。
在生产CIGS光伏组件的过程中，硫化镉(CdS)是迄今为止发现的最佳n结缓冲层材料。CdS层与CIGS层间的界面即为p-n结，用于光吸收后产生的激子的分离，因此CdS层沉积的效果，尤其是致密性对组件的效率影响很大。现有的CdS沉积过程主要包括化学品预混合，硫脲加入，化学品加热，基板CdS生长，取出基板，排放废液等几大步骤。
现有的CdS沉积技术主要基于化学水浴沉积方法，即Chemical Bath Deposition(CBD)(化学浴沉积装置)。在加入硫脲至硫酸镉和氨水的混合液后，便开始发生化学反应，即有硫化镉粒子生成。一般来说，基板必须在此之前加入到化学品溶液中，并保证化学液的流场及温度在基板的各个角落均匀且稳定。反应结束后，化学品随即排放至废液槽，进入废液处理系统，并最终排放。
由于CdS层的厚度仅为50nm左右，在反应结束后，化学液中除了已生成的漂浮在液体中的CdS粒子外，还有大量未反应的化学品，包括硫酸镉，硫脲及氨水。由于废液在排放时还处在反应温度(约60摄氏度)，化学反应还在持续进行，且较为快速，因此未反应的化学品也在迅速降低，且不易检测。由于没有快速控制废液中化学反应的方法，也没有提纯及回复利用未反应化学品的方式，通常废液会在CdS沉积之后全部排放。
全部排放的废液会造成很大浪费，同时导致后期废水处理系统负担过重。最终排放至环境中的废物也相当多，对环境产生一定压力。
发明内容
本发明的目的是提供一种化学浴沉积装置及其沉积方法、废液回收系统，以解决现有技术中的问题，提高废液的回收利用率，降低生产成本。
本发明提供了一种化学浴沉积装置，包括硫化镉反应槽，其中，所述装置还包括：
废液储存槽、制冷装置、过滤装置、化学液储存槽和补充供药装置；
所述废液储存槽的进液口与所述硫化镉反应槽的出液口相连；
所述废液储存槽的出液口与所述制冷装置的进液口相连；
所述制冷装置的出液口与所述过滤装置的进液口相连；
所述过滤装置的出液口与所述化学液储存槽的进液口相连；
所述补充供药装置用于向所述化学液储存槽补入化学品；
所述化学液储存槽的出液口与所述硫化镉反应槽的进液口相连。
如上所述的化学浴沉积装置，其中，优选的是，还包括：冷却装置，包覆在所述废液储存槽的外壁上。
如上所述的化学浴沉积装置，其中，优选的是，所述冷却装置中的冷却液为水。
如上所述的化学浴沉积装置，其中，优选的是，所述化学液储存槽的出液口与所述硫化镉反应槽的进液口之间设置有第一调节阀；
所述化学液储存槽的进液口与所述补充供药装置的出液口之间设置有第二调节阀。
如上所述的化学浴沉积装置，其中，优选的是，还包括电导率检测仪，设置在所述化学液储存槽中，用于测量所述化学液储存槽中的化学液的电导率。
如上所述的化学浴沉积装置，其中，优选的是，还包括控制装置，用于根据所述电导率检测仪测量得到的电导率控制所述第二调节阀的启闭。
如上所述的化学浴沉积装置，其中，优选的是，还包括低温维护装置，设置在所述化学液储存槽的外壁上，用于保持所述化学液储存槽内的温度处于设定的温度区间。
本发明还提供了一种本发明的化学浴沉积装置的沉积方法，其中，包括：
将硫化镉反应槽中的硫化镉废液通入到废液储存槽中；
将降温后的废液通入到制冷装置中进行制冷；
将制冷后的废液通入到过滤装置中进行过滤；
将过滤后的废液通入到化学液储存槽中；
利用补充供药装置向化学液储存槽中的化学液加入化学品；
将所述化学液储存槽中的化学液通入到所述硫化镉反应槽中；以此循环进行沉积。
如上所述的硫化镉层沉积方法，其中，优选的是，将所述化学液储存槽中的化学液通入到所述硫化镉反应槽中之前，所述方法还包括：
监测化学液储存槽中化学液的电导率，根据测得的电导率数据计算化学液中镉粒子的含量，从而得到化学品原料的浓度；
当所述化学品原料的浓度达到设定值时，控制第二调节阀关闭，从而停止向化学液储存槽中的化学液加入化学品。
本发明又提供了一种废液回收系统，其中，包括：废液储存槽、制冷装置、过滤装置和化学液储存槽；
所述废液储存槽的进液口用于与硫化镉反应槽的出液口相连；
所述废液储存槽的出液口与所述制冷装置的进液口相连；
所述制冷装置的出液口与所述过滤装置的进液口相连；
所述过滤装置的出液口与所述化学液储存槽的进液口相连。
本发明提供的化学浴沉积装置及其沉积方法、废液回收系统，通过对废液进行制冷、过滤，在补充化学品原料，从而得到与原液浓度相同的化学液，相比于现有技术，大大地提高了废液的回收利用，降低了生产成本。
附图说明
图1为本发明实施例提供的化学浴沉积装置的结构示意图；
图2为本发明实施例提供的硫化镉层沉积方法的流程图；
图3为本发明实施例提供的废液回收方法的流程图。
具体实施方式
下面详细描述本发明的实施例，所述实施例的示例在附图中示出，其中自始至终相同或类似的标号表示相同或类似的元件或具有相同或类似功能的元件。下面通过参考附图描述的实施例是示例性的，仅用于解释本发明，而不能解释为对本发明的限制。
本发明旨在解决CBD法沉积CdS缓冲层过程中废液的回收利用问题。由于废液中仍有超过80％的原材料化学品溶解在溶液中，且未发生反应。在采用适当方法，将化学品提纯并补加相应化学原料后，理论上仍可作为CdS沉积的化学液，供后续的基板使用。
图1为本发明实施例提供的化学浴沉积装置的结构示意图，如图1所示，本发明实施例提供了一种化学浴沉积装置100，包括硫化镉反应槽，还包括废液储存槽、制冷装置、过滤装置、化学液储存槽和补充供药装置。其中，废液储存槽、制冷装置、过滤装置和化学液储存槽构成了本发明实施例提供的废液回收系统200。
废液储存槽的进液口与硫化镉反应槽的出液口相连，废液储存槽的出液口与制冷装置的进液口相连，制冷装置的出液口与过滤装置的进液口相连，过滤装置的出液口与化学液储存槽的进液口相连，补充供药装置用于向化学液储存槽补入化学品，化学液储存槽的出液口与硫化镉反应槽的进液口相连。
在化学反应完全并取出基板后，硫化镉反应槽中的化学液将作为废液引入到废液储存槽中，优选地，硫化镉反应槽中的废液通过第一动力泵泵入到废液储存槽中。
本领域技术人员可以理解的是，本发明实施例提供的化学浴沉积装置还可以包括第二动力泵、第三动力泵、第四动力泵和第五动力泵，其中，第二动力泵用于将废液储存槽中的废液泵入到制冷装置中；第三动力泵用于将制冷装置中的废液泵入到过滤装置中；第四动力泵用于将过滤装置中的化学液泵入到化学液储存槽中；第五动力泵用于将化学液储存槽中的液体泵入到硫化镉反应槽中。
该回收系统优选地还包括冷却装置，冷却装置中的冷却液优选为水，该冷却装置包覆在废液储存槽的外壁上，用于对废液收集的过程中进行降温，初步降低CdS的生成速率。
从废液储存槽出来后，废液将会被泵入到制冷装置，对废液进行进一步降温，将温度降至室温以下(5摄氏度)，使CdS的生成进入停滞状态。
上述制冷装置的具体结构可以有多种，可以为物理制冷装置也可以为化学制冷装置，这里就不再一一赘述。
冷却后的废液将进入装有滤芯(约0.02um)的过滤装置，将废液中的CdS颗粒过滤干净，同时也过滤析出的化学品原料：硫酸镉和硫脲。
经过过滤装置后，CdS等固体粒子被滤出。此提纯后的化学液将会被泵入至化学液储存槽。该化学液储存槽的外壁上优选地设置有低温维护装置，用于保持化学液储存槽内的温度处于设定的温度区间，确保溶液保持在低温状态。
优选地，化学液储存槽的出液口与硫化镉反应槽的进液口之间设置有第一调节阀；化学液储存槽的进液口与补充供药装置的出液口之间设置有第二调节阀。通过阀的启闭，控制槽与槽之间的液体流通。本领域技术人员还可以理解的是，废液储存槽的进液口与硫化镉反应槽的出液口之间也可以设有第三调节阀；废液储存槽的出液口与制冷装置的进液口之间也可以设有第四调节阀；制冷装置的出液口与过滤装置的进液口之间还可以设有第五调节阀；过滤装置的出液口与化学液储存槽的进液口之间还可以设有第六调节阀，在此不作一一限定。
进一步地，该回收系统还包括电导率检测仪，设置在化学液储存槽中，用于测量化学液储存槽中的化学液的电导率，在上述实施例的基础上，本发明实施例提供的化学浴沉积装置还包括控制装置，用于根据所述电导率检测仪测量得到的电导率控制所述第二调节阀的启闭。
根据测得的电导率数据计算化学液中镉粒子的含量，从而得到化学品原料的浓度；当化学品原料的浓度达到设定值时，上述控制装置控制第二调节阀关闭，从而停止向化学液储存槽中的化学液加入化学品。如图2所示，本发明实施例还提供了一种化学浴沉积装置的沉积方法，，包括如下步骤：
步骤S1、将硫化镉反应槽中的硫化镉废液通入到废液储存槽中，优选的在废液储存槽中可以先进行第一次降温。
具体地，可通过第一动力泵将硫化镉反应槽中的硫化镉废液通入到废液储存槽中。
步骤S2、将降温后的废液通入到制冷装置中进行制冷。
优选地，将降温后的废液通入到制冷装置中，使制冷装置中的液体温度降低至5摄氏度以下。
步骤S3、将制冷后的废液通入到过滤装置中进行过滤。
具体地，将制冷后的废液通入到过滤装置中，将制冷后的废液中的硫化镉全部滤除，同时滤出硫酸镉和硫脲。
步骤S4、将过滤后的废液通入到化学液储存槽中。
此槽具有低温维护装置，确保溶液保持在低温状态。
步骤S5、利用补充供药装置向化学液储存槽中的化学液加入化学品；
步骤S6、将化学液储存槽中的化学液通入到硫化镉反应槽中，以此循环上述步骤S1～S6进行沉积。
化学液储存槽装有精密的电导率监测仪，可对溶液的电导率进行快速测量。
优选地，将化学液储存槽中的化学液通入到硫化镉反应槽中之前，该方法还包括：
监测化学液储存槽中化学液的电导率，根据测得的电导率数据计算化学液中镉粒子的含量，从而得到化学品原料的浓度；
当化学品原料的浓度达到设定值时，控制第二调节阀关闭，从而停止向化学液储存槽中的化学液加入化学品。
本发明实施例又提供了一种废液回收系统200，参照图1，该回收系统包括废液储存槽、制冷装置、过滤装置和化学液储存槽；废液储存槽的进液口用于与硫化镉反应槽的出液口相连；废液储存槽的出液口与制冷装置的进液口相连；制冷装置的出液口与过滤装置的进液口相连；过滤装置的出液口与化学液储存槽的进液口相连。
优选地，该回收系统还包括第一动力泵、第二动力泵、第三动力泵和第四动力泵。
其中，第一动力泵用于将硫化镉反应槽中的废液泵入到废液储存槽中；第二动力泵用于将废液储存槽中的废液泵入到制冷装置中；第三动力泵用于将制冷装置中的废液泵入到过滤装置中；第四动力泵用于将过滤装置中的化学液泵入到化学液储存槽中。
进一步地，该回收系统包括冷却装置，包覆在废液储存槽的外壁上。优选地，该冷却装置中的冷却液为水。
如图3所示，本发明实施例再提供了一种废液回收方法，包括：
步骤S10、将硫化镉反应槽中的硫化镉废液通入到废液储存槽中，优选的，可以在所述废液储存槽中进行降温。
步骤S20、将降温后的废液通入到制冷装置中进行制冷。
将降温后的废液通入到制冷装置中，使制冷装置中的液体温度降低至5摄氏度以下。
步骤S30、将制冷后的废液通入到过滤装置中进行过滤。
将制冷后的废液通入到过滤装置中，将制冷后的废液中的硫化镉全部滤除，同时滤出硫酸镉和硫脲。
步骤S40、将过滤后的废液通入到化学液储存槽中。
本发明实施例提供的化学浴沉积装置、硫化镉层沉积方法、废液回收系统及方法，与现有CBD技术相比有着显著的优势，化学品的利用率大大增加，由原有的15％增加至65％。此方案尤其对浸泡(dipping)方式的CBD设备最为有益，因为浸泡方式对化学品溶液的用量需求大，持续大规模生产过程中的OPEX较高。通常来说，摇摆(wobbling)方式CBD设备价格高昂，但化学品用量较少。此技术方案将使造价较低的浸泡式CBD设备占有优势，使CIGS生产线的整体生产运营成本大大降低。
通过对工艺的优化，制冷与冷却过程可持续提高化学液提纯的效率，使得化学液的回收利用次数增加，进一步提高化学品利用率从65％提升至90％。
以上依据图式所示的实施例详细说明了本发明的构造、特征及作用效果，以上所述仅为本发明的较佳实施例，但本发明不以图面所示限定实施范围，凡是依照本发明的构想所作的改变，或修改为等同变化的等效实施例，仍未超出说明书与图示所涵盖的精神时，均应在本发明的保护范围内。

Claims (10)

1.一种化学浴沉积装置，包括硫化镉反应槽，其特征在于，所述化学浴沉积装置还包括：
废液储存槽、制冷装置、过滤装置、化学液储存槽和补充供药装置；
所述废液储存槽的进液口与所述硫化镉反应槽的出液口相连；
所述废液储存槽的出液口与所述制冷装置的进液口相连；
所述制冷装置的出液口与所述过滤装置的进液口相连；
所述过滤装置的出液口与所述化学液储存槽的进液口相连；
所述补充供药装置用于向所述化学液储存槽补入化学品；
所述化学液储存槽的出液口与所述硫化镉反应槽的进液口相连。
2.根据权利要求1所述的化学浴沉积装置，其特征在于，还包括：冷却装置，包覆在所述废液储存槽的外壁上。
3.根据权利要求2所述的化学浴沉积装置，其特征在于，所述冷却装置中的冷却液为水。
4.根据权利要求1所述的化学浴沉积装置，其特征在于，所述化学液储存槽的出液口与所述硫化镉反应槽的进液口之间设置有第一调节阀；
所述化学液储存槽的进液口与所述补充供药装置的出液口之间设置有第二调节阀。
5.根据权利要求4所述的化学浴沉积装置，其特征在于，还包括电导率检测仪，设置在所述化学液储存槽中，用于测量所述化学液储存槽中的化学液的电导率。
6.根据权利要求5所述的化学浴沉积装置，其特征在于，还包括控制装置，用于根据所述电导率检测仪测量得到的电导率控制所述第二调节阀的启闭。
7.根据权利要求1所述的化学浴沉积装置，其特征在于，还包括低温维护装置，设置在所述化学液储存槽的外壁上，用于保持所述化学液储存槽内的温度处于设定的温度区间。
8.一种如权利要求1所述的化学浴沉积装置的沉积方法，其特征在于，包括：
将硫化镉反应槽中的硫化镉废液通入到废液储存槽中；
将降温后的废液通入到制冷装置中进行制冷；
将制冷后的废液通入到过滤装置中进行过滤；
将过滤后的废液通入到化学液储存槽中；
利用补充供药装置向化学液储存槽中的化学液加入化学品；
将所述化学液储存槽中的化学液通入到所述硫化镉反应槽中；以此循环进行沉积。
9.根据权利要求8所述的硫化镉层沉积方法，其特征在于，将所述化学液储存槽中的化学液通入到所述硫化镉反应槽中之前，所述方法还包括：
监测化学液储存槽中化学液的电导率，根据测得的电导率数据计算化学液中镉粒子的含量，从而得到化学品原料的浓度；
当所述化学品原料的浓度达到设定值时，控制第二调节阀关闭，从而停止向化学液储存槽中的化学液加入化学品。
10.一种废液回收系统，其特征在于，包括：废液储存槽、制冷装置、过滤装置和化学液储存槽；
所述废液储存槽的进液口用于与硫化镉反应槽的出液口相连；
所述废液储存槽的出液口与所述制冷装置的进液口相连；
所述制冷装置的出液口与所述过滤装置的进液口相连；
所述过滤装置的出液口与所述化学液储存槽的进液口相连。
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