CN110408891B - 一种叠层蒸发源装置 - Google Patents

一种叠层蒸发源装置 Download PDF

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CN110408891B
CN110408891B CN201910705565.2A CN201910705565A CN110408891B CN 110408891 B CN110408891 B CN 110408891B CN 201910705565 A CN201910705565 A CN 201910705565A CN 110408891 B CN110408891 B CN 110408891B
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李青霄
张心会
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Henan University of Urban Construction
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Abstract

本发明提供了一种叠层蒸发源装置，第一冷却盒和第二冷却盒之间安置硒蒸发层，第二冷却盒上方安置金属蒸发层，所述硒蒸发层的硒蒸气管道贯穿第二冷却盒和金属蒸发层，本发明能够采用精准释放硒蒸汽质量束流提高原料利用率、硒分子团高温裂解为硒原子释放硒活性，提高膜厚均匀性，简化蒸发源装置结构、降低设备维护成本，兼容柔性和刚性基底蒸镀沉积，以此实现Cu、In、Ga、Se四种元素在薄膜的纵向和横向上的分布均匀性，充分释放硒活性、兼容柔性和刚性基底生长优质铜铟镓硒薄膜。本发明结构简单，降低能耗，易于维护，减少腔室脏污，降低腔室维护成本，缩短生产周期，进而提高效益。

Description

一种叠层蒸发源装置
技术领域
本发明涉及蒸镀技术领域，具体涉及一种叠层蒸发源装置。
背景技术
近年来，随着传统能源的枯竭，绿色清洁能源—光伏电池需求增加。目前，晶硅光伏电池仍然是市场的主流产品，但是受工艺制程限制，已不能通过减薄硅片厚度降低生产成本。薄膜太阳能电池的功能层厚度可控制在几微米以内，又由于薄膜太阳能电池既可以做成刚性产品又可以做成柔性产品，生产工艺又简单易行，生产过程环境友好，致使薄膜太阳能电池的需求与日俱增。世界主要能源需求大的国家，都对薄膜太阳能电池投入大量资金进行研究开发。
当前，铜铟镓硒(Cu(InxGa1-x)Se2简称CIGS)已经是规模化量产的薄膜太阳能电池。在沉积CIGS功能层时，通常采用的技术路线之一是蒸镀技术。在工程实践过程中发现，沉积功能膜层时，蒸发源装置是影响CIGS薄膜太阳能电池性能的核心因素。蒸发源装置决定CIGS功能膜层厚度均匀性、元素分布、原料的利用率。另外，为提高CIGS薄膜太阳能电池性能，硒的活性决定膜质质量。然而，由于硒原子官能团易于团聚，降低硒活性，致使硒不能与其它元素充分反应，影响功能膜层膜质，造成CIGS薄膜太阳能电池性能下降。目前，尚无原料利用率高、硒活性高、膜厚均匀性好，并且兼容柔性和刚性基底的蒸发源。
US 2009258444A1描述了一种用于柔性衬底上生长铜铟镓硒薄膜太阳电池的蒸发源和蒸发设备。源采用独立控制的硒源和金属源方式，包括放置坩埚的石墨盒部分；坩埚和装料部分；坩埚加热丝部分。设备采用分腔室隔离方式，避免原料蒸发后相互交叉污染。该蒸发源装置的设计，考虑了镀膜膜厚分布均匀性问题。但是，存在的缺陷是，所设计硒蒸发源装置，使得硒蒸汽处于“大水漫灌式”地沉积，造成原料利用率低，致使腔室内严重脏污，维护成本高；硒蒸汽压波动较大，硒蒸汽压波动一个是造成硒活性降低，不易与金属Cu、In、Ga原子充分化合反应，所制备铜铟镓硒薄膜中有硒分子团聚，降低膜质；另一个是所制备的铜铟镓硒薄膜的厚度均匀性，偏离理论设计较多，降低产品良率。
CN 108425091 A描述了一种用于柔性衬底上低温生长铜铟镓硒薄膜太阳电池的高温裂解硒蒸发源，包括：坩埚加热蒸发部分；硒原子团的高温裂解部分；高温裂解硒蒸发源控制电路。通过对硒原子团的高温裂解，提高蒸发的硒原子在薄膜表面迁移速率和反应活性，使其更容易与金属Cu、In、Ga原子化合，更容易在薄膜表面和内部扩散，改善低温沉积CIGS薄膜的结晶质量，解决在柔性PI(聚酰亚胺)衬底上低温生长高质量CIGS薄膜的问题，促进柔性PI衬底CIGS薄膜太阳电池的工业化应用。
上述描述的概念复杂，仅适用柔性基底，另外描述的该装置结构复杂，设备成本高，维护困难。且由于硒蒸汽直接释放在真空沉积室内，造成了沉积室内非常脏污，增加了设备维护成本，制约CIGS规模化生产。
发明内容
本发明要解决的技术问题是未能提高原料利用率、充分释放硒活性、提高膜厚均匀性，不兼容柔性和刚性基底的蒸发源，设备结构复杂昂贵、维护成本高，为解决上述问题，本发明提供一种叠层蒸发源装置。
本发明的目的是以下述方式实现的：
一种叠层蒸发源装置，包括硒蒸发层、冷却层和金属蒸发层，冷却层包括第一冷却盒和第二冷却盒，第二冷却盒在第一冷却盒上方，所述第一冷却盒和第二冷却盒之间安置硒蒸发层，第二冷却盒上方安置金属蒸发层，所述硒蒸发层的硒蒸气管贯穿第二冷却盒和金属蒸发层。
冷却层包括第一冷却盒和第二冷却盒，所述第一冷却盒和第二冷却盒的结构相同，第一冷却盒和第二冷却盒两侧均设有进水管和出水管。
硒蒸发层包括第一坩埚、第一加热器、第一隔热层、第二隔热层和硒蒸气管，所述第一隔热层安置于第一冷水盒上方，第一隔热层上方安置第一坩埚，第一坩埚上方设置第一加热器，第一加热器上方设置有第二隔热层，所述硒蒸气管设置在第一坩埚中部，且硒蒸气管贯穿第一加热器和第二隔热层。
硒蒸气管至少有一个。
第一隔热层和第二隔热层均为石墨毡材质；第一加热器为铠装加热丝或有氮化硼涂层的石墨加热丝；硒蒸气管为氮化硼材质；第一坩埚为石墨或不锈钢材质。
金属蒸发层包括容纳盒、第三隔热层、第二坩埚、盖板、第四隔热层、第二加热器和蒸发管，所述容纳盒安置在第二冷却盒上方，在容纳盒内壁安置第三隔热层，在第三隔热层内侧安置第二坩埚，第二坩埚上部设置有盖板，所述盖板上方设置第二加热器，在第二加热器上方设置第四隔热层，所述蒸发管贯穿第四隔热层、第二加热器和盖板，且蒸发管延伸出第四隔热层。
蒸发管至少有一个。
容纳盒和盖板均为石墨材质，第三隔热层和第四隔热层均为石墨毡材质；第二加热器为涂有氮化硼涂层的石墨加热丝；第二坩埚为石墨或不锈钢材质，
蒸发管为氮化硼材质。
相对于现有技术，本发明能够采用精准释放硒蒸汽质量束流提高原料利用率、硒分子团高温裂解为硒原子释放硒活性，提高膜厚均匀性，简化蒸发源装置结构、降低设备维护成本，兼容柔性和刚性基底蒸镀沉积，实现硒蒸气压稳定控制和精准沉积在基底上指定区域，提高原料利用率和膜厚均匀性，以此实现Cu、In、Ga、Se四种元素在薄膜的纵向和横向上的分布均匀性，充分释放硒活性、兼容柔性和刚性基底生长优质铜铟镓硒薄膜。本发明结构简单，降低能耗，易于维护，减少腔室脏污，降低腔室维护成本，缩短生产周期，进而提高效益。
附图说明
图1是小平面源蒸发质量束流分布数学模型原理示意图。
图2是平行小平面源基底上的质量束流分布数学计算示意图。
图3是单个小平面源蒸汽释放口的质量束流空间分布计算结果。
图4是本发明叠层蒸发源剖面示意图。
图5是本发明蒸发源蒸镀的CIGS膜厚沿基底横向分布实际效果图。
图6是本发明蒸发源沉积生长的优质CIGS实际效果图。
其中，1.第一冷却盒，101.进水管，102.出水管，2.第一隔热层，3.第一坩埚，4.第一加热器，5.第二隔热层，6.第二冷却盒，7.容纳盒，8.第三隔热层，9.第二坩埚，10.硒蒸气管，11.盖板，12.第二加热器，13.第四隔热层，14.蒸发管，15.金属原料，16.硒原料。
具体实施方式
如附图1到6所示，一种叠层蒸发源装置，包括硒蒸发层、冷却层和金属蒸发层，冷却层包括第一冷却盒1和第二冷却盒6，第二冷却盒6在第一冷却盒1上方，所述第一冷却盒1和第二冷却盒6之间安置硒蒸发层，第二冷却盒6上方安置金属蒸发层，所述硒蒸发层的硒蒸气管10贯穿第二冷却盒6和金属蒸发层。
冷却层包括第一冷却盒1和第二冷却盒6，所述第一冷却盒1和第二冷却盒6的结构相同，第一冷却盒1和第二冷却盒6两侧均设有进水管101和出水管102，对硒蒸发层和金属蒸发层进行冷却。
硒蒸发层包括第一坩埚3、第一加热器4、第一隔热层2、第二隔热层5和硒蒸气管10，所述第一隔热层2安置于第一冷水盒上方，第一隔热层2上方安置第一坩埚3，第一坩埚3上方设置第一加热器4，第一加热器4上方设置有第二隔热层5，所述硒蒸气管10设置在第一坩埚3中部，且硒蒸气管10贯穿第一加热器4和第二隔热层5，硒蒸发层将硒原料16加热成液体蒸发，
硒蒸气管10至少有一个，使硒蒸气多个散发口，确保混合均匀。
第一隔热层2和第二隔热层5均为石墨毡材质；第一加热器4为铠装加热丝或有氮化硼涂层的石墨加热丝；硒蒸气管10为氮化硼材质；第一坩埚3为石墨或不锈钢材质，石墨毡材质、氮化硼材质和石墨或不锈钢材质耐高温。
金属蒸发层包括容纳盒7、第三隔热层8、第二坩埚9、盖板11、第四隔热层13、第二加热器12和蒸发管14，所述容纳盒7安置在第二冷却盒6上方，在容纳盒7内壁安置第三隔热层8，所述第三隔热层8的纵截面为U型状，在第三隔热层8内侧安置第二坩埚9，第二坩埚9上部设置有盖板11，所述盖板11上方设置第二加热器12，在第二加热器12上方设置第四隔热层13，所述蒸发管14贯穿第四隔热层13、第二加热器12和盖板11，且蒸发管14延伸出第四隔热层13，对金属原料15Cu、In和Ga进行加热蒸发，与硒蒸气混合。
蒸发管14至少有一个，多个散发口，确保金属蒸气充足。
容纳盒7和盖板11均为石墨材质，第三隔热层8和第四隔热层13均为石墨毡材质；第二加热器12为涂有氮化硼涂层的石墨加热丝；第二坩埚9为石墨或不锈钢材质，蒸发管14为氮化硼材质，石墨毡材质、氮化硼材质和石墨或不锈钢材质耐高温，盖板11为石墨材质，盖板11传递第二加热器12的热量，并且盖板11每个地方传递的热量相同，使金属原料15受热均匀，从蒸发管14散出的金属蒸气量相同。
本发明的工作原理：对此进行以下实验分析：在真空蒸发镀膜过程中，在平面或曲面基片上获得均匀膜厚，是制膜的关键。基片上任何种类的镀膜厚度，都决定于蒸发源蒸汽释放口的特点，基片和蒸发源的几何结构，相对位置以及膜材蒸速率。
首先，对膜厚及其膜厚分布进行理论计算，找出蒸镀膜厚的分布规律，对蒸发过程作如下假定：
(1)蒸发是在充分低的气压下进行的，以致可以忽略因蒸汽分子与气体分子之间的碰撞而引起的散射；
(2)蒸发强度较低，以致可以忽略蒸发源释放口附近蒸汽分子之间的碰撞；
(3)碰撞到基片表面上的每一个蒸汽分子，在第一次碰撞时就凝结到基片表面上。
上述假定的实质就是每一个蒸汽分子，在入射到基片表面上的过程中均不发生任何碰撞，而且到达基片后又全部凝结。因此它必然与实际的蒸发过程有所出入。但是，这些假定对于在10-2Pa或更低的气压下所进行的蒸镀过程而言，它与实际情况是非常接近的。CIGS薄膜电池的铜、铟、镓三种元素蒸镀气压落在10-2Pa附近，NaF(氟化钠)和KF(氟化钾)蒸镀气压小于10-2Pa，因此，CIGS薄膜电池沉积过程符合上述假设。
目前，蒸发源种类繁多，但大致可以分为两类：点蒸发源和小平面蒸发源。规模化制造铜铟镓硒薄膜太阳电池的蒸发源通常选择面源，限于该发明，在此仅涉及平行平面基底的小平面蒸发源的分析。
如图1所示，假设蒸发源是小平面源dA1，膜材从小平面上的表面以单位时间m克的速率进行蒸发时，则按余弦定律，膜材在单位时间内通过与该小平面法线成角度方向的立体角dω的束流质量为：
Figure BDA0002151656910000061
若蒸发材料到达与蒸发方向成θ角的小平面dA2的几何尺寸是已知的，则沉积在这个小平面上去的膜材的束流质量是：
Figure BDA0002151656910000062
假定膜材的密度为ρ，单位时间内凝结到dA2上的膜厚度为t，则沉积到dA2上的膜材体积为t﹒dA2。即：
dm＝tdA2 (3)
(3)式代入(2)式，得：
Figure BDA0002151656910000063
图2给出的是从一个小平面源dA1到与A平面相平行的基片上的蒸发情况。因为夹角
Figure BDA0002151656910000064
和夹角θ相等，式(4)可改写为：
Figure BDA0002151656910000065
由于蒸发源上面O点处δ＝0，故O点处的膜厚计算式可写成：
Figure BDA0002151656910000066
那么，从O点到R点的膜厚变化率为：
Figure BDA0002151656910000067
图3给出了单个小平面源蒸汽释放口的质量束流空间分布计算结果。
其次，释放Se的活性是沉积高品质CIGS薄膜的核心，也是提高原料利用率的关键。目前，用来提高薄膜沉积过程中的Se活性，增强CIGS薄膜材料中的Se含量，国际上主要存在以下两类技术：一种是等离子体辅助硒化技术(见文献：Takuro.Manufacture of ThinFilm Solar Battery.Japanese Patent.1993-05-03)；另一种射频等离子体活化硒源(见文献：S.Ishizuka,A.Yamada,H.Shibata et al,Large grain Cu(In,Ga)Se2thin filmgrowth using a Se-radical beam source,Solar Energy Materials and Solar Cells,93(2009)792-796.)。前一种技术可用于对大原子团的Se进行裂解，进而增强硒化反应；后一种技术表明等离子体促进了大原子团Sen(n≥5)的分解，提高了Se元素的活性。上述技术虽然有效释放了工艺过程中Se的活性，但是，等离子体加强、射频加强蒸发源等技术，都需在真空室内通入Ar或H2气。通入气体会降低薄膜的质量。高温裂解Se蒸发源工作过程中不需通入其它气体，直接在高真空下高温裂解Se大原子团，提高蒸发原子的活性，提高原材料的利用率(见文献：D.A.Cammack,K.Shahzad and T.Marshall,Low-temperature growthof ZnSe by molecular beam epitaxy using cracked selenium,Applied PhysicsLetters,1989,56:845-847.)，在600℃高温裂解下，Sen(n＞2)几乎全部转化为Se2甚至Se。
在装置安装时，先把底层带有进水管101和出水管102的第一冷却盒1放置在电阻蒸发镀膜设备的真空腔室内，第一隔热层2安置于第一冷水盒上方，第一隔热层2上方安置第一坩埚3，第一坩埚3上方设置第一加热器4，第一加热器4上方设置有第二隔热层5，硒蒸气管10设置在第一坩埚3中部，硒蒸气管10与第一坩埚3由螺丝固定在一起，带有进水管101和出水管102的第二冷却盒6放置在第二隔热层5上方，容纳盒7安置在第二冷却盒6上方，在容纳盒7内壁安置第三隔热层8，在第三隔热层8内侧安置第二坩埚9，第二坩埚9上部设置有盖板11，盖板11上方设置第二加热器12，在第二加热器12上方设置第四隔热层13，蒸发管14贯穿第四隔热层13、第二加热器12和盖板11，第二隔热层5、第一加热器4、第二冷却盒6、容纳盒7、第三隔热层8、第二坩埚9、盖板11、第二加热器12和第四隔热层13的中心位置均设有孔道，硒蒸气管10通过孔道贯穿第二冷却盒6和金属蒸发层，工作时第一加热器4和第二加热器12可以实现独立通电加热控制，根据实际工艺需要可以同时加热，也可以错时加热，提高工艺实施的灵活性，第一加热器4和第二加热器12通电后，第二坩埚9内的金属原料15蒸发熔化并维持在高温(600-1400℃)状态，形成液态和蒸气混合，第一坩埚3内的固态硒蒸发原料受热(260-300°)变成Se蒸汽，完成第一步裂解，形成Se分子和原子团，Se分子和原子团进入硒蒸气管10后，在经过金属蒸发层区域段，完成第二步裂解，形成Se小分子和原子，与金属蒸汽一起沉积在衬底上，生长为优质CIGS薄膜，金属蒸气为Cu、In和Ga蒸气。
以上所述的仅是本发明的优选实施方式，应当指出，对于本领域的技术人员来说，在不脱离本发明整体构思前提下，还可以作出若干改变和改进，这些也应该视为本发明的保护范围。

Claims (6)

1.一种叠层蒸发源装置，包括硒蒸发层、冷却层和金属蒸发层，其特征在于：冷却层包括第一冷却盒和第二冷却盒，第二冷却盒在第一冷却盒上方，所述第一冷却盒和第二冷却盒之间安置硒蒸发层，第二冷却盒上方安置金属蒸发层，所述硒蒸发层的硒蒸气管贯穿第二冷却盒和金属蒸发层；硒蒸发层包括第一坩埚、第一加热器、第一隔热层、第二隔热层和硒蒸气管，所述第一隔热层安置于第一冷却盒上方，第一隔热层上方安置第一坩埚，第一坩埚上方设置第一加热器，第一加热器上方设置有第二隔热层，所述硒蒸气管设置在第一坩埚中部，且硒蒸气管贯穿第一加热器和第二隔热层；金属蒸发层包括容纳盒、第三隔热层、第二坩埚、盖板、第四隔热层、第二加热器和蒸发管，所述容纳盒安置在第二冷却盒上方，在容纳盒内壁安置第三隔热层，在第三隔热层内侧安置第二坩埚，第二坩埚上部设置有盖板，所述盖板上方设置第二加热器，在第二加热器上方设置第四隔热层，所述蒸发管贯穿第四隔热层、第二加热器和盖板，且蒸发管延伸出第四隔热层。
2.根据权利要求1所述的叠层蒸发源装置，其特征在于：所述第一冷却盒和第二冷却盒的结构相同，第一冷却盒1和第二冷却盒两侧均设有进水管和出水管。
3.根据权利要求1所述的叠层蒸发源装置，其特征在于：硒蒸气管至少有一个。
4.根据权利要求1所述的叠层蒸发源装置，其特征在于：第一隔热层和第二隔热层均为石墨毡材质；第一加热器为铠装加热丝或有氮化硼涂层的石墨加热丝；硒蒸气管为氮化硼材质；第一坩埚为石墨或不锈钢材质。
5.根据权利要求1所述的叠层蒸发源装置，其特征在于：蒸发管至少有一个。
6.根据权利要求1所述的叠层蒸发源装置，其特征在于：容纳盒和盖板均为石墨材质，第三隔热层和第四隔热层均为石墨毡材质；第二加热器为涂有氮化硼涂层的石墨加热丝；第二坩埚为石墨或不锈钢材质，蒸发管为氮化硼材质。
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Assignee: Luoyang Kemiler Intelligent Technology Co.,Ltd.

Assignor: Henan University of Urban Construction

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Denomination of invention: A stacked evaporation source device

Granted publication date: 20210907

License type: Common License

Record date: 20240105

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