CN1326255C - 在衬底上淀积氧化物膜的方法 - Google Patents
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Abstract
本发明涉及一种在放置在腔室(26)中的钢化玻璃衬底(10)上淀积透明导电氧化物层(12)的方法。本发明方法这样构成：提供原料源(32，34，36)，其中分别装有一种氧基液态化合物，一种想要形成氧化物的液态金属化合物和一种气态或液态的掺杂物；将腔室中的温度设定在130-300℃之间，压力设定在0.01-2mbar之间；将原料源与上述腔室相连通。这样，这些液体在其表面蒸发，无需任何的载体气体即可吸入腔室中，并与掺杂物反应，从而在衬底上形成氧化物层。
Description
本发明涉及一种在衬底上淀积透明氧化物膜的方法，特别是用在光伏电池，又叫太阳能电池的制造中。本发明也涉及到这样的一种电池，其中的透明氧化物膜是采用本方法淀积的。
目前，技术上最先进的太阳能电池包括衬底，淀积在衬底上的TCO(透明导电氧化物)膜以及淀积在该氧化物膜上的光伏有源膜。有利地，这种光敏膜由无定形的，微晶的或者纳米晶氢合硅的三个亚层组成，构成一个p-i-n结。更精确的，两个外部亚层分别是正掺杂和负掺杂的，然而，中间的亚层是本征的。
例如，在申请EP 96934294.8中的一些实施方案里面就详细描述了这种类型的电池。
在现有的技术状况下，光伏电池通常采用熟知的CVD(化学气相淀积)方法将一种由二氧化锡(SnO2)或氧化锌(ZnO)制成的透明导电氧化物膜淀积在玻璃衬底上，采用的温度通常在400-550℃之间。
然而，能够在更低的温度下淀积氧化物膜是特别有益的，因为这样就可以使用比如像钢化玻璃的衬底，这可以满足户外应用所需的安全标准。
不幸的是，上述温度会对由钢化处理得到的衬底性能造成有害影响。
专利US 5252140中公开了一种钢化玻璃上的太阳能电池，其中在制备了氧化物膜之后才进行韧化。为了防止膜的退化，热处理的最高温度为650℃，持续时间小于2分钟，然后在空气中迅速冷却。然而，这些预防措施使得该方法更加昂贵，而且不能保证韧化的质量。
所以，目前的制造商必然满足于在没有韧化的玻璃制成的太阳能电池，这种玻璃相对较脆，当碎成尖锐的碎片时有很大的潜在危险。因而它们在居室内的应用受到限制，甚至禁止在有窗帘的墙上使用。
在专利US 4751149和5002796中公开了在气相中淀积氧化物膜的方法，其中将用化学化合物饱和的载体气体喷射到腔室中，从而将要在反应中沉淀的这些化合物带入到腔室中。
公认地，这种方法确实意味着反应条件更加温和，因为其没有损害到衬底的性能，因此，特别是可以用来在钢化玻璃上制造太阳能电池。然而，该方法不能合适的控制所包含的反应物的量，因为决定载体气体的饱和阈值的热力学平衡强烈的依赖于温度和这种气体的流速。由于在整个过程中保持精确的温度是存在问题的，所以在该装置的较冷点处存在不可控的反应物凝结的危险。结果，要保证膜的均匀性和可重复性是相当困难的。
本发明的一个目的就是提供一种淀积方法，其不但允许采用由钢化玻璃或者其它耐高温(300℃以上)很差的材料制成的衬底，而且能够精确控制所包含的反应物的量，因为供给线路中的实验条件足以避免任何不合适的凝结。
更具体的，本发明涉及一种在放置在腔室中的衬底上淀积透明导电氧化物膜的方法。其特征在于这种方法这样构成：
-提供原料源，其中分别装有一种氧基液态化合物，一种想要形成氧化物的金属的液态化合物和一种气态或者液态的掺杂物；
-将腔室中的温度设定在130-300℃之间，压力设定在0.01-2mbar之间；然后
-将原料源与上述腔室连通，该腔室能够使液体在它们的表面上蒸发，不用载体气体即可将它们引入到腔室中，并能够使它们在其中与掺杂物反应，从而在衬底上形成氧化物层。
依据本发明，当上面提到的温度太低，以致不能让形成氧化物的化学反应发生时，优选采用一种本领域技术人员熟知的叫做PECVD(等离子体增强化学气相淀积)的技术，化学蒸发发生在在腔室中形成的淀积气体的等离子体中。
本发明还涉及到一种光伏电池，其特征在于这种电池包括：
-衬底；
-用上述方法在衬底上淀积的透明导电氧化物膜；以及
-淀积在该氧化物膜上的光伏有源膜。
有利地，这种电池的有源膜包括无定形的，微晶的或者纳米晶的氢合硅的三个亚层，构成一个p-i-n结，两个外部亚层分别是正掺杂和负掺杂的。
有利地，衬底由玻璃制成，优选的是钢化玻璃，但也可以由不锈钢，铝或者聚合物制成。
下面，结合附图进行的描述将使本发明的其它特征变得明显。附图包括：
-图1：依据本发明的电池截面图；以及
-图2：制造这种电池的设备示意图。
图1中所示的电池采用了一个钢化玻璃薄板作衬底10，其厚度在大约1-8mm，并在上面淀积了透明导电氧化物(TCO)膜12，一般的，该膜厚度在0.2-4μm。
有利地，层12由二氧化锡(SnO2)，氧化锌(ZnO)或者一种锡锌氧化物制成，通过化学气相淀积(CVD)进行淀积，其所用的工艺将在后面描述。
在氧化膜12上淀积光伏有源膜14，其厚度在大约0.2-10μm。该层由无定形的，微晶的或者纳米晶的氢合硅的三个亚层16，18，20组成，构成一个p-i-n结。两个外部亚层分别是正掺杂和负掺杂的。
最后，这种电池还包括一个淀积在有源膜14上的例如由氧化锌制成的背接触膜22，以及一个淀积在膜22上的例如由银或铝制成的反射膜24。
其它的尤其是采用了一个n-i-p结的电池结构，也可以在相同的钢化玻璃衬底和相同的透明氧化物膜上制造。在上面提到的EP资料中对它们进行了详细描述。
现在参照图2，其中所示的是在钢化玻璃板10上CVD淀积氧化锌膜12的设备。如图所示，在密封的腔室26中有一个加热支座28，钢化玻璃板就放在这个支座上面。腔室26是与真空泵30和三个容器32，34和36相连的，这些容器依次装着水，二乙基锌(C2H5)2Zn和有利的形式是乙硼烷(B2H6)的掺杂物，当然，也可以使用本领域技术人员熟知的其它的锌基化合物和其它的掺杂物。32和34两个容器中装的是液体，而容器36中装的是用一种比如氮气，氩气或者氢气的气体稀释的乙硼烷含量在0.5-2％的气体混和物。应该注意，容器32和34直接与腔室相连的。容器36是先连接到容器34的导管上的，但它也可以直接连接到腔室上。
在操作中，用加热支座28将腔室26加热到大约180℃的温度，但可以在130-300℃之间，同时用泵30将压力降低到0.3-0.5mbar，但可以在0.01-20mbar之间。然后将连接容器32，34，36和腔室26的可调阀门(没有标出)打开。由于在腔室中的压力非常低，所以，在这些容器中装着的液态的二乙基锌和水会在它们的表面蒸发，得到的气体被引入到腔室中，并与掺杂气体(B2H6)一起按照已知的反应式在衬底温度下进行反应，这样就在钢化玻璃板10上淀积了所要得到的氧化锌膜12。
由于该操作是在一个相对较低的温度下进行的，钢化玻璃的性能没有受到破坏。而且，由于在该装置中的均匀的低压力，蒸发的气体在它们进入腔室之前没有凝结的危险。
上述方法非常适合于淀积乙硼烷掺杂的氧化锌，因为在所述温度下，所包含的化学反应没有任何问题。相反，当采用更稳定的掺杂物，比如四氟化碳(CF4)通过CVD来淀积二氧化锡或者氧化锌时，这些温度就太低了，以致于这些反应不能正常发生。
依据本发明，接下来用等离子体增强气相淀积或PECVD方法来淀积氧化物膜。此时，腔室26中，在加热支座28上，例如以栅电极38那样的形式，装备一个电极，并且有一个发电机40连接在这个电极和支座之间。
这样，在操作中，尽管温度和压力保持在上面提到的数值，引入到腔室26中的气体可以在电极38和支座28之间形成等离子体。通过等离子体产生活性的游离基，使得形成氧化物涂层膜的反应可以在一个基本上比通常必须的温度低的温度下发生，这样，就可以保留住衬底的性能。
有利地，为了得到所希望的SnO2层，容器34和36中分别装有比如四甲基锡(CH3)4Sn和作为掺杂物的四氟化碳(CF4)。也可以采用本领域熟知的这里没有提到的其它化合物。
应该注意，装在容器32中的水可用任何的含氧化合物(N2O，CH3OH，C2H5OH......)代替，并且，装在容器36中的掺杂物也可以是液态的。
通过参照一个钢化玻璃衬底对本发明进行了描述，其作为一个在窗帘墙壁方面的应用是特别有益的，但在本发明的内容中，同样可以采用这里没有提到的其它的衬底，比如普通玻璃，不锈钢，铝或者聚合物等等。
Claims (5)
1.一种在放置在腔室(26)中的衬底(10)上淀积透明导电氧化物膜(12)的方法，其特征在于该方法包括：
-提供原料源(32，34，36)，其中分别装有一种氧基液态化合物，一种想要形成所述氧化物的金属的液态化合物和一种气态或者液态的掺杂物；
-将所述腔室中的温度设定在130-300℃之间，压力设定在0.01-2mbar之间；然后
-将所述原料源与上述腔室连通，该腔室能够使所述液体在它们的表面蒸发，能够不用载体气体即可将它们引入到腔室中，并能够使它们在其中与掺杂物反应，从而在衬底上形成所述氧化物层。
2.权利要求1中的方法，用于淀积氧化锌膜，其特征在于所述原料源(32，34，36)中分别装有水，液态的二乙基锌和一种基于乙硼烷的气体混和物。
3.权利要求1中的方法，其特征在于，该方法还在于在腔室中形成被蒸发液体的等离子体。
4.权利要求3中的方法，用于淀积氧化锡膜，其特征在于所述原料源(32，34，36)中分别装有水，液态的四甲基锡和一种基于四氟化碳的气体混和物。
5.权利要求3中的方法，用于淀积氧化锌膜，其特征在于所述原料源(32，34，36)中分别装有水，液态的二乙基锌和一种基于四氟化碳的气体混和物。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP01810840A EP1289025A1 (fr) | 2001-08-30 | 2001-08-30 | Procédé de dépot d'une couche d'oxyde sur un substrat et cellule photovoltaique utilisant ce substrat |
| EP01810840.7 | 2001-08-30 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1550045A CN1550045A (zh) | 2004-11-24 |
| CN1326255C true CN1326255C (zh) | 2007-07-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB028170067A Expired - Fee Related CN1326255C (zh) | 2001-08-30 | 2002-08-23 | 在衬底上淀积氧化物膜的方法 |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US7390731B2 (zh) |
| EP (2) | EP1289025A1 (zh) |
| JP (1) | JP4491233B2 (zh) |
| CN (1) | CN1326255C (zh) |
| AU (1) | AU2002322952A1 (zh) |
| DE (1) | DE60215523T2 (zh) |
| ES (1) | ES2274069T3 (zh) |
| WO (1) | WO2003021690A2 (zh) |
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|---|---|---|---|---|
| EP1714309B1 (de) * | 2004-02-13 | 2007-06-13 | Shell Solar GmbH | Einrichtung zum aufbringen einer flüssigen dotierungsstofflösung auf einem wafer |
| EP1717341B1 (en) * | 2004-02-16 | 2015-04-15 | Kaneka Corporation | Process for producing transparent conductive film and process for producing tandem thin-film photoelectric converter |
| JP4918224B2 (ja) * | 2005-01-21 | 2012-04-18 | 昭和シェル石油株式会社 | 透明導電膜製膜装置及び多層透明導電膜連続製膜装置 |
| US8197914B2 (en) | 2005-11-21 | 2012-06-12 | Air Products And Chemicals, Inc. | Method for depositing zinc oxide at low temperatures and products formed thereby |
| EP1840966A1 (fr) * | 2006-03-30 | 2007-10-03 | Universite De Neuchatel | Couche conductrice transparente et texturée et son procédé de réalisation |
| WO2008027086A1 (en) * | 2006-08-29 | 2008-03-06 | Pilkington Group Limited | Method of making a low-resistivity, doped zinc oxide coated glass article and the coated glass article made thereby |
| US20080128022A1 (en) * | 2006-11-15 | 2008-06-05 | First Solar, Inc. | Photovoltaic device including a tin oxide protective layer |
| DE102006062019A1 (de) * | 2006-12-29 | 2008-07-03 | Näbauer, Anton, Dr. | Verfahren zur Herstellung von mechanisch stabilen Dünnschicht Photovoltaik Solarmodulen unter Verwendung von Glas |
| US8203071B2 (en) | 2007-01-18 | 2012-06-19 | Applied Materials, Inc. | Multi-junction solar cells and methods and apparatuses for forming the same |
| KR20100095426A (ko) | 2007-11-02 | 2010-08-30 | 어플라이드 머티어리얼스, 인코포레이티드 | 증착 공정들 간의 플라즈마 처리 |
| US20100264035A1 (en) * | 2009-04-15 | 2010-10-21 | Solopower, Inc. | Reel-to-reel plating of conductive grids for flexible thin film solar cells |
| US9528182B2 (en) | 2009-06-22 | 2016-12-27 | Arkema Inc. | Chemical vapor deposition using N,O polydentate ligand complexes of metals |
| JP5508800B2 (ja) * | 2009-09-30 | 2014-06-04 | 株式会社カネカ | 薄膜の製造方法、並びに、太陽電池の製造方法 |
| US8525019B2 (en) | 2010-07-01 | 2013-09-03 | Primestar Solar, Inc. | Thin film article and method for forming a reduced conductive area in transparent conductive films for photovoltaic modules |
| WO2012031102A2 (en) | 2010-09-03 | 2012-03-08 | Corning Incorporated | Thin film silicon solar cell in multi-junction configuration on textured glass |
| US8906732B2 (en) * | 2010-10-01 | 2014-12-09 | Stion Corporation | Method and device for cadmium-free solar cells |
| US8628997B2 (en) * | 2010-10-01 | 2014-01-14 | Stion Corporation | Method and device for cadmium-free solar cells |
| DE102015215434A1 (de) * | 2015-08-13 | 2017-02-16 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verfahren zur Abscheidung dünner Schichten |
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- 2001-08-30 EP EP01810840A patent/EP1289025A1/fr not_active Withdrawn
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2002
- 2002-08-23 US US10/488,174 patent/US7390731B2/en not_active Expired - Lifetime
- 2002-08-23 ES ES02754092T patent/ES2274069T3/es not_active Expired - Lifetime
- 2002-08-23 EP EP02754092A patent/EP1421630B1/fr not_active Expired - Lifetime
- 2002-08-23 AU AU2002322952A patent/AU2002322952A1/en not_active Abandoned
- 2002-08-23 DE DE60215523T patent/DE60215523T2/de not_active Expired - Lifetime
- 2002-08-23 WO PCT/CH2002/000458 patent/WO2003021690A2/fr active IP Right Grant
- 2002-08-23 CN CNB028170067A patent/CN1326255C/zh not_active Expired - Fee Related
- 2002-08-23 JP JP2003525919A patent/JP4491233B2/ja not_active Expired - Lifetime
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| US4751149A (en) * | 1985-06-04 | 1988-06-14 | Atlantic Richfield Company | Chemical vapor deposition of zinc oxide films and products |
| US5002796A (en) * | 1988-05-25 | 1991-03-26 | Canon Kabushiki Kaisha | Process for forming functional zinc oxide films using alkyl zinc compound and oxygen-containing gas |
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Also Published As
| Publication number | Publication date |
|---|---|
| JP2005501182A (ja) | 2005-01-13 |
| WO2003021690A3 (fr) | 2003-11-06 |
| ES2274069T3 (es) | 2007-05-16 |
| EP1421630B1 (fr) | 2006-10-18 |
| AU2002322952A1 (en) | 2003-03-18 |
| US20040235286A1 (en) | 2004-11-25 |
| DE60215523D1 (de) | 2006-11-30 |
| DE60215523T2 (de) | 2007-06-21 |
| CN1550045A (zh) | 2004-11-24 |
| US7390731B2 (en) | 2008-06-24 |
| WO2003021690A2 (fr) | 2003-03-13 |
| EP1289025A1 (fr) | 2003-03-05 |
| JP4491233B2 (ja) | 2010-06-30 |
| EP1421630A2 (fr) | 2004-05-26 |
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