CN207398068U - 一种制备铜铟镓硒化合物的装置 - Google Patents

一种制备铜铟镓硒化合物的装置 Download PDF

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CN207398068U
CN207398068U CN201721463168.1U CN201721463168U CN207398068U CN 207398068 U CN207398068 U CN 207398068U CN 201721463168 U CN201721463168 U CN 201721463168U CN 207398068 U CN207398068 U CN 207398068U
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陈腾
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Hongyi Technology Co.,Ltd.
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Beijing Hina Film Power Technology Co Ltd
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Priority to EP18195753.1A priority patent/EP3480857A1/en
Priority to PCT/CN2018/107005 priority patent/WO2019085679A1/zh
Priority to US16/139,111 priority patent/US20190136345A1/en
Priority to CA3018689A priority patent/CA3018689A1/en
Priority to JP2018003730U priority patent/JP3219221U/ja
Priority to KR2020180004447U priority patent/KR20190001161U/ko
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Abstract

本实用新型公开一种制备铜铟镓硒化合物的装置，所述装置包括L型石英管(1)，高温合成区(3)、低温蒸发区(2)，加热装置(5)，封泡(4)，其中：所述高温合成区(3)和低温蒸发区(2)分别设置在L型石英管(1)的两端;所述加热装置(5)间隔设置在L型石英管(1)的周围，用于对L型石英管(1)加热，并形成梯度温度；所述L型石英管一端封闭，另一端开放并设置有缩口，通过封泡(4)进行密封。利用本实用新型的装置制备的铜铟镓硒合金工艺流程简单，成分均匀，易于控制。

Description

一种制备铜铟镓硒化合物的装置
技术领域
本发明涉及一种合金制备反应装置，具体涉及一种制备铜铟镓硒化合物的装置。
背景技术
众所周知，CIGS薄膜电池是最具潜力的一种薄膜太阳能电池， 目前产业上制备CIGS的主流方法为共蒸发法和磁控溅射法，基于前两种方法的高真空性，无论从设备还是工艺角度，成本都比较高，因此，类似印刷等非真空低成本制备CIGS的技术被业界不断推动。
当前非真空印刷CIGS涂布浆料或胶体的制备主要有两种方法，第一，采用化学合成方法制备CIGS纳米材料并进一步调制成浆料，但是化学合成CIGS纯度低，制备的CIGS薄膜少子寿命低，因此目前采用该种吸收层的电池效率比较低；第二，采用四种单质粉末或几种二三元化合物粉末调配涂布原材料，这种浆料在成膜进一步反应形成四元化合物时反应难于控制，不充分的反应会造成组分失配，同时，较高的反应温度也易于造成硒组分的大量流失，从而制备的CIGS薄膜质量差。
另外，制备渐变带隙的CIGS薄膜有利于提高薄膜光吸收层的转化效率，而当前印刷制备CIGS薄膜局限于CIGS材料的制备方法，多为单一固定组分CIGS，不利于高效电池的制备。
发明内容
针对上述问题，本发明提供一种能够精准控制CIGS合金成分的铜铟镓硒化合物的制备装置。
为达到上述目的，本发明提供一种制备铜铟镓硒化合物的装置，所述装置包括L型石英管(1)，高温合成区(3)、低温蒸发区(2)，加热装置(5)，封泡(4)，其中：
所述高温合成区(3)和低温蒸发区(2)分别设置在L型石英管(1)的两端;
所述加热装置(5)间隔设置在L型石英管(1)的周围，用于对L型石英管(1)加热，并形成梯度温度；
所述L型石英管一端封闭，另一端开放并设置有缩口，通过封泡(4)进行密封。
进一步地，所述高温合成区(3)和低温蒸发区(2)均为石英舟。
进一步地，所述高温合成区(3)和低温蒸发区(2)均为坩埚。
进一步地，所述高温合成区(3)和低温蒸发区(2)均为凹坑，所述凹坑设置在L型石英管(1)上。
进一步地，所述高温合成区(3)位于L型石英管(1)的长边的一端，所述低温蒸发区(2)位于L型石英管(1)的短边的一端。
进一步地，所述L型石英管(1)的长边长度为1100-1600mm，短边长度为400-700mm，L型石英管(1)的直径为60-80mm，所述封泡长度为200mm，直径为50mm。
进一步地，加热装置(5)为电加热线圈，其环绕在L型石英管(1)外表面，并且间隔设置。
进一步地，所述缩口在L型石英管(1)的长边的一端，所述封泡(4)与缩口匹配能够将开口密封。
进一步地，所述石英舟直径为66mm，长为300mm的半管。
通过L型管的设置和温度梯度的设置，避免了Se蒸汽的沉降在管臂上，保证了Se和CuInGa的充分化合反应，由于油墨的铜铟镓硒含量可控，实现了制作不同铟镓比的铜铟镓硒化合物的，制备出的化合物更加均匀，更加可控。
附图说明
图1是本发明制备铜铟镓硒化合物的装置示意图。
图2是本发明实施例4中涂布完第一层油墨后的示意图；
图3为本发明实施例4中第一层油墨烘干后的示意图；
图4是本发明实施例4中涂布完第二层油墨后的示意图；
图5是本发明实施例4中退火后形成铜铟镓硒光吸收层薄膜的示意图。
具体实施方式
下面结合说明书附图对本发明做进一步的描述。
以下，仅为本发明的较佳实施例，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求所界定的保护范围为准。
实施例1
为一种制备铜铟镓硒化合物的装置，所述装置包括L型石英管(1)，高温合成区(3)、低温蒸发区(2)，加热装置(5)，封泡(4)，其中：所述高温合成区(3)和低温蒸发区(2)分别设置在L型石英管(1)的两端;所述加热装置(5)间隔设置在L型石英管(1)的周围，用于对L型石英管(1)加热，并形成梯度温度；所述L型石英管一端封闭，另一端开放并设置有缩口，通过封泡(4)进行密封。
所述高温合成区(3)和低温蒸发区(2)均为石英舟。
所述高温合成区(3)位于L型石英管(1)的长边的一端，所述低温蒸发区(2)位于L型石英管(1)的短边的一端。
所述L型石英管(1)的长边长度为1500mm，短边长度为500mm，L型石英管(1)的直径为75mm，所述封泡长度为200mm，直径为50mm。
加热装置(5)为电加热线圈，其环绕在L型石英管(1)外表面，并且间隔设置。
所述缩口在L型石英管(1)的长边的一端，所述封泡(4)与缩口匹配能够将开口密封。
所述石英舟直径为66mm，长为300mm的半管。
所述电加热线圈对应石英舟半管位置的长度为300mm，两个对应石英舟位置的电加热线圈之间间隔设置长度为200mm的电加热线圈，电加热线圈之间的间隔为100mm。
本实施例提供利用上述装置制备铜铟镓硒化合物的制备方法，步骤如下：
S1提供一真空容器，真空容器包括间隔设置的高温合成区1和低温蒸发区2；
S2将铜、铟、镓单质放置在高温合成区1，将硒单质放置在低温蒸发区2；
S3将高温合成区1的铜、铟、镓加热至熔融状态，将低温蒸发区2的硒加热至气态状态；低温蒸发区2的硒开始转变为气态的时间不早于铜铟镓熔融的时间；
S4将高温合成区1和低温蒸发区2保温；
S5将高温合成区1温度降至不低于铜铟镓硒合金的熔融温度并进行保温，然后将高温合成区1和低温蒸发区2降温至100℃以下；
在上述步骤中，始终保持低温蒸发区2与高温合成区1之间存在正向温度梯度。
在S1中，提供一种容器，该容器可以为石英管、陶瓷管等采用耐高温材质制备的具有一定刚性的容器。将真空容器中具有一定间隔的部分分别作为高温合成区1和低温蒸发区2。当物料放入上述的容器中后，将容器内的气压抽至10-1Pa或者以下就成为真空容器。真空容器内的气压可以为10-1Pa、10-2Pa、10-3Pa或者10-4Pa。
在S2中，使用纯度大于5N的Cu、In、Ga和Se单质为原材料，各单质质量按照组分CuIn0.7Ga0.3Se2.05去称配，将Se单质置于L型石英管短端的石英舟内，将Cu、In、Ga单质置于L型石英管长端的石英舟内，将石英管抽真空至10-2Pa以下封管放入电热炉中，盛有Se单质的石英舟对应炉中低温蒸发区2，盛有CuInGa单质的石英舟对应高温合成区1。当然，也可以不采用石英舟盛放物料而采用其他耐高温的容器盛放，例如采用坩埚盛放物料。如果在容器的高温合成区1和低温蒸发区2具有凹坑，可以不采用其他容器盛放物料，直接将物料置于凹坑内。
上述铜铟镓硒化合物的成分并不对本发明的制备的铜铟镓硒化合物的成分形成限定，例如，还可以制备以下组分的铜铟镓硒化合物CuIn0.85Ga0.15Se2.05，CuIn0.9Ga0.1Se2，CuIn0.8Ga0.2Se2，CuIn0.75Ga0.25Se2；在上述铜铟镓硒化合物的制备过程中，称量时应当按照铟和镓的摩尔分数之和应当与铜的摩尔分数基本相等进行计算，而硒的摩尔分数应当大于铜的摩尔分数的两倍进行计算；例如硒的摩尔分数可以为铜的2.1倍、2.2倍、2.3倍、2.4倍或者2.5倍。采用过量的硒放置在低温蒸发区2，这样，在整个反应过程中，由于硒是过量的，能够始终保持在硒蒸汽的氛围中进行反应。
在S3中，调整高温合成区和低温合成区之间的温控功率，形成从低温到高温的线性温度梯度区间。高温合成区1设定85min-90min升温至1100℃-1150℃，当高温合成区1启动升温55min-60min时，高温合成区1的温度升至700℃-750℃，此时启动低温蒸发区2升温，设定55min-60min升温至550℃-600℃。
在S4中，待低温蒸发区2达到最高温度后保持6h。保温时间可以根据物料的数量、反应类型等条件进行计算。
在S5中，将高温合成区设定为15min降温至950-1000℃，再保持1.5h-2h，之后关闭所有温区加热装置随炉冷却至100℃以下，在高温合成区1端石英舟内得到CIGS四元化合物，合成的CIGS化合物组分为CuIn0.7Ga0.3Se2。
为了保证硒蒸汽在输运过程中不会凝结在石英管的内壁上，需要保证有低温蒸发区2道高温合成区1之间具有正向的温度梯度，为了保证蒸汽输运速率的稳定性，最好控制整个石英管的低温蒸发区2到高温合成区1之间具有线性的温度梯度。
本实施例的铜铟镓硒化合物制备方法中，首先将铜铟镓加热至熔融状态，使铜铟镓首先开始反应，然后将硒加热升华为气态，使真空容器中形成硒氛围，从而将铜铟镓进行硒化。为了使铜铟镓在硒化过程中能够均匀硒化，本发明需要保证铜铟镓的熔融时间不晚于硒开始升华的时间。另外，为了保证硒蒸汽的能够以稳定的速率向高温合成区1输送，需要保证低温蒸发区2向高温合成区1始终具有一个正向的温度梯度。
实施例2
本实施例提供一种制备CIGS油墨的方法，包括以下步骤：
S1将上述实施例1制备的铜铟镓硒化合物研磨成粉末状；
S2向所述粉末中加入溶剂、粘结剂和分散剂并搅拌均匀形成；
S3将混合物经过加热蒸发或静置挥发，除去溶剂形成浆料。
在S1中，可以使用氧化锆行星球磨机将实施例1制备的CIGS化合物研磨成纳米粉末，当然，粉碎CIGS化合物的方法并不限于氧化锆行星球磨机，也可以采用其他方式，只要能够将CIGS粉碎成纳米粉末即可。
在S2中，将铜铟镓硒化合物粉末与溶剂、粘结剂以及分散剂进行混合；将上述的混合物进行搅拌超声形成均匀的混合物。溶剂可以采用乙醇、甲醇或者两者的混合物；粘结剂采用乙基纤维素、纤维素衍生物或者两者的混合物；分散剂采用萜品醇、特丁醇或者两者的混合物。
在S3中，用旋转蒸发仪蒸发掉上述预调浆料中的无水乙醇能够得到CIGS的印刷浆料。在超声搅拌过程中，乙基纤维素、纤维素衍生物或者两者的混合物溶于萜品醇、特丁醇或者两者的混合物中形成液态的粘合相，而无水乙醇则用来将粘合相的粘度调节至合适的范围，便于铜铟镓硒合金的均匀分布，分布完成后，将其中的无水乙醇蒸发掉，最终铜铟镓硒合金的粉末均匀的悬浮于上述的液态物中，形成铜铟镓硒油墨。
蒸发掉无水乙醇的方法是采用旋转蒸发仪进行蒸发，该方式并不对本发明中蒸发乙醇的方法形成限制，例如，还可以采用降压蒸发的方法去除无水乙醇，或者对混合物进行加热蒸发掉其中的无水乙醇，甚至可以将混合物置于室温下待无水乙醇自然蒸发。
实施例3
本实施例提供一种制备铜铟镓硒光吸收层的制备方法，将实施例3制备的铜铟镓硒油墨利用丝网印刷在镀Mo的钠钙玻璃或者不锈钢衬底上进行浆料的涂布，涂布方式可根据薄膜电池整体工艺要求进行间断涂布或者连续涂布。将涂布浆料的衬底转移进入连续烧结炉进行浆料烘干和退火，烘干温度150℃-250℃，烘干时间3min-5min，退火温度450℃-550℃，退火时间10min-15min，最终得到具有CIGS薄膜吸收层。
在本实施例中，实施例3制备的油墨在镀Mo的钠钙玻璃或者不锈钢衬底上，然后对浆料进行烘干，烘干过程中能够将液态的粘合相蒸发掉或者分解掉，而铜铟镓硒粉末则会留在衬底上，然后将铜铟镓硒粉末进行退火，退火的过程中，铜铟镓硒粉末会生长形成铜铟镓硒的光吸收层，制备油墨采用的是铜铟镓硒合金，因此，在退火过程中不需要将其加热到铜铟镓硒的反应温度，只需要加热到退火温度使粉末生长成膜。
由于本发明的铜铟镓硒合金的制备方法在制备过程中能够精准的控制铜铟镓硒合金的成分，因此，采用本实施例的铜铟镓硒光吸收层的制备方法制备的薄膜同样可以控制光吸收层的成分，从而能够控制光吸收层的带隙宽度。
实施例4
如图2-5所示，本实施例提供一种铜铟镓硒光吸收层的制备方法，利用丝网印刷在镀Mo的钠钙玻璃或者不锈钢衬底上先进行浆料一的涂布，如图2所示，涂布方式可根据薄膜电池整体工艺要求进行间断涂布或者连续涂布。将涂布浆料一的衬底转移进入烧结炉进行浆料烘干，烘干温度150℃-250℃，烘干时间2min-3min，如图3所示。选用浆料二在附着有烘干的浆料一的衬底上进行二次印刷，如图4所示，涂布方式可根据薄膜电池整体工艺要求进行间断涂布或者连续涂布。将涂布浆料二的衬底转移进入连续烧结炉进行浆料烘干和退火，烘干温度150℃-250℃，烘干时间3min-5min，退火温度450℃-550℃，退火时间10min-15min，最终得到具有双带隙的CIGS薄膜吸收层， 如图5所示。
在本实施例中，浆料一是将实施例2中制备的铜铟镓硒合金按照实施例3的制备方法制备的浆料，浆料二是将实施例1中制备的铜铟镓硒合金按照实施例3的制备方法制备的浆料。
当然，上述浆料中采用的浆料并不对本实施例的浆料选用形成限定，并且，上述的浆料印刷次数也不能对本发明的浆料印刷次数形成限定。
例如，还可以采用CuIn0.9Ga0.1Se2，CuIn0.8Ga0.2Se2，CuIn0.75Ga0.25Se2等成分的铜铟镓硒合金制备的浆料进行三次或者三次以上的印刷，但是，在印刷过程中要始终注意，相邻两层油墨中靠近向阳面的一层油墨的铟镓含量比值低于远离向阳面的一层油墨的铟镓含量比值；这样，能够保证渐进带隙的光吸收层由向阳面向背阳面的带隙逐渐变窄，从而，长波长的光能够通过前一吸收层而被后一吸收层吸收。这样，各个波长的光被由向阳面向背阳面排列的各吸收层逐层吸收，能够提高光吸收率。
实施例5
首先制备铜铟镓硒化合物，步骤如下：
S1提供一真空容器，真空容器包括间隔设置的高温合成区1和低温蒸发区2；
S2将铜、铟、镓单质放置在高温合成区1，将硒单质放置在低温蒸发区2；
S3将高温合成区1的铜、铟、镓加热至熔融状态，将低温蒸发区2的硒加热至气态状态；低温蒸发区2的硒开始转变为气态的时间不早于铜铟镓熔融的时间；
S4将高温合成区1和低温蒸发区2保温；
S5将高温合成区1温度降至不低于铜铟镓硒合金的熔融温度并进行保温，然后将高温合成区1和低温蒸发区2降温至100℃以下；
在上述步骤中，始终保持低温蒸发区2与高温合成区1之间存在正向温度梯度。
S1，提供一真空容器，所述真空容器为L型石英管，真空容器包括高温合成区和低温蒸发区，将真空容器中具有一定间隔的部分分别作为高温合成区1和低温蒸发区2，所述L型石英管的两端分别为高温合成区和低温蒸发区，高温合成区放置盛有铜铟硒单质的石英舟，在低温蒸发区放置盛有硒单质的石英舟；
S2，使用纯度大于5N的Cu、In、Ga和Se单质为原材料，各单质质量按照组分CuIn0.8Ga0.2Se2.05去称配，将Se单质置于L型石英管短端的石英舟内，将Cu、In、Ga单质置于L型石英管长端的石英舟内，将石英管抽真空至10-3Pa以下封管放入电热炉中，盛有Se单质的石英舟对应炉中低温蒸发区2，盛有CuInGa单质的石英舟对应高温合成区1。
在S3中，调整高温合成区和低温合成区之间的温控功率，形成从低温到高温的线性温度梯度区间。高温合成区1设定88min升温至1125℃，当高温合成区1启动升温55min时，高温合成区1的温度升至725℃，此时启动低温蒸发区2升温，设定56min升温至575℃。
在S4中，待低温蒸发区2达到575℃后，将高温合成区温度和低温蒸发区温度保持6h。在S5中，将高温合成区设定为15min降温至960℃，再保持2h，之后关闭所有温区加热装置随炉冷却至100℃以下，在高温合成区1端石英舟内得到CIGS四元化合物，合成的CIGS化合物组分为CuIn0.8Ga0.2Se2。
为了保证硒蒸汽在输运过程中不会凝结在石英管的内壁上，需要保证有低温蒸发区2道高温合成区1之间具有正向的温度梯度，为了保证蒸汽输运速率的稳定性，最好控制整个石英管的低温蒸发区2到高温合成区1之间具有线性的温度梯度。
接着利用上述CIGS四元化合物制备CIGS油墨，包括以下步骤：
S1，用氧化锆行星球磨机将制备的CIGS化合物研磨成纳米粉末。
S2，将铜铟镓硒化合物粉末与溶剂、粘结剂以及分散剂进行混合；将上述的混合物进行搅拌超声形成均匀的混合物。溶剂为乙醇；粘结剂为乙基纤维素；分散剂为萜品醇。
S3，用旋转蒸发仪蒸发掉上述预调浆料中的无水乙醇能够得到CIGS的印刷浆料。在超声搅拌过程中，乙基纤维素溶于萜品醇中形成液态的粘合相，而无水乙醇则用来将粘合相的粘度调节至合适的范围，便于铜铟镓硒合金的均匀分布，分布完成后，将其中的无水乙醇蒸发掉，最终铜铟镓硒合金的粉末均匀的悬浮于上述的液态物中，形成铜铟镓硒油墨。
利用上述制备得到的铜铟镓硒油墨制备铜铟镓硒光吸收层的制备方法，将制备的铜铟镓硒油墨利用丝网印刷在镀Mo的钠钙玻璃或者不锈钢衬底上进行浆料的涂布，涂布方式可根据薄膜电池整体工艺要求进行间断涂布或者连续涂布。将涂布浆料的衬底转移进入连续烧结炉进行浆料烘干和退火，烘干温度180℃，烘干时间4min，退火温度500℃，退火时间13min，最终得到具有CIGS薄膜吸收层。
另一种利用上述铜铟镓硒油墨的制备铜铟镓硒光吸收层的方法，利用丝网印刷在镀Mo的钠钙玻璃或者不锈钢衬底上先进行浆料一的涂布，如图2所示，涂布方式可根据薄膜电池整体工艺要求进行间断涂布或者连续涂布。将涂布浆料一的衬底转移进入烧结炉进行浆料烘干，烘干温度160℃，烘干时间3min，如图3所示。选用浆料二在附着有烘干的浆料一的衬底上进行二次印刷，如图4所示，涂布方式可根据薄膜电池整体工艺要求进行间断涂布或者连续涂布。将涂布浆料二的衬底转移进入连续烧结炉进行浆料烘干和退火，烘干温度200℃，烘干时间4min，退火温度525℃，退火时间13min，最终得到具有双带隙的CIGS薄膜吸收层， 如图5所示。
由于本发明的铜铟镓硒合金制备方法在制备过程中能够精准的控制铜铟镓硒合金的成分，因此，在制备渐进带隙的光吸收层时，能够控制各个吸收层的铜铟镓硒的成分，也就能够控制各个吸收层的带隙宽度，从而，使印刷的方法制备渐进带隙的光吸收层能够实现。
以上实施例仅用于对本发明进行具体说明，其并不对本发明的保护范围起到任何限定作用，本发明的保护范围由权利要求确定。根据本领域的公知技术和本发明所公开的技术方案，可以推导或联想出许多变型方案，所有这些变型方案，也应认为是本发明的保护范围。

Claims (9)

1.一种制备铜铟镓硒化合物的装置，其特征在于：所述装置包括L型石英管(1)，高温合成区(3)、低温蒸发区(2)，加热装置(5)，封泡(4)，其中：
所述高温合成区(3)和低温蒸发区(2)分别设置在L型石英管(1)的两端；
所述加热装置(5)间隔设置在L型石英管(1)的周围，用于对L型石英管(1)加热，并形成梯度温度；
所述L型石英管一端封闭，另一端开放并设置有缩口，通过封泡(4)进行密封。
2.如权利要求1所述的制备铜铟镓硒化合物的装置，其特征在于，所述高温合成区(3)和低温蒸发区(2)均为石英舟。
3.如权利要求1所述的制备铜铟镓硒化合物的装置，其特征在于，所述高温合成区(3)和低温蒸发区(2)均为坩埚。
4.如权利要求1所述的制备铜铟镓硒化合物的装置，其特征在于，所述高温合成区(3)和低温蒸发区(2)均为凹坑，所述凹坑设置在L型石英管(1)上。
5.如权利要求1-4之一所述的制备铜铟镓硒化合物的装置，其特征在于，所述高温合成区(3)位于L型石英管(1)的长边的一端，所述低温蒸发区(2)位于L型石英管(1)的短边的一端。
6.如权利要求5所述的制备铜铟镓硒化合物的装置，其特征在于，所述L型石英管(1)的长边长度为1100-1600mm，短边长度为400-700mm，L型石英管(1)的直径为60-80mm，所述封泡长度为200mm，直径为50mm。
7.如权利要求1-4之一所述的制备铜铟镓硒化合物的装置，其特征在于，加热装置(5)为电加热线圈，其环绕在L型石英管(1)外表面，并且间隔设置。
8.如权利要求1-4、6之一所述的制备铜铟镓硒化合物的装置，其特征在于，所述缩口在L型石英管(1)的长边的一端，所述封泡(4)与缩口匹配能够将开口密封。
9.如权利要求2所述的制备铜铟镓硒化合物的装置，其特征在于，所述石英舟直径为66mm，长为300mm的半管。
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CN112680781B (zh) * 2020-12-09 2023-10-03 清远先导材料有限公司 碲化镉晶体生长装置及其生长方法

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