CN101268213B - 在常压下连续化学气相沉积的设备和方法及其用途 - Google Patents
在常压下连续化学气相沉积的设备和方法及其用途 Download PDFInfo
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Abstract
本发明涉及用于在常压下在基材上连续化学沉积的设备和方法。所述设备基于反应室,沿所述反应室的开口侧引导基材,因此可以在基材面向室内部的侧面进行相应的涂覆。
Description
技术领域
本发明涉及在常压下在基材上连续气相沉积的设备和方法。所述设备基于反应室,沿所述反应室的开口侧引导基材,因此可以在基材面向室内部的侧面上进行相应的涂覆。
背景技术
可以用多种技术方案由气态原材料(所谓的前体)制备薄层。对于所有方法共同的是将气态前体或成为气相的前体导入反应室,在该反应室中该前体通过结合能量而分解,所述气体的组分沉积在待涂覆的部件上。这些方法中的一种是常压化学气相沉积(称为APCVD,根据英文atmospheric pressure chemical vapor deposition)。其特征在于,所述前体和处理室均几乎在常压下。APCVD的一个实例是由氯硅烷制成的硅层的APCVD外延。在这种情况下,通常与氢混合的氯硅烷在温度为约1000至1200℃的反应室中分解,硅以相同的晶体取向沉积在晶体硅基材上。这个方法用于包括薄的晶体Si层的太阳能电池等。对于这种用途尤其需要硅沉积反应器,这种反应器可以非常廉价(低于30欧元/m2)并且高生产能力(>20m2/h)地沉积约10至20μm厚的Si层。因为现有技术的反应器a)生产能力太低(例如ASM Epsilon 3000:1m2/h)和b)只是非常不完整地(百分之几)利用前体中包含的硅,所以现有技术中的反应器不能满足这些要求。一项新的发展涉及用于硅的化学气相沉积/外延的高生产能力反应器的制造(Hurrle,S.Reber,N.Schillinger,J.Haase,J.G.Reichart,“High Throughput Continuous CVD Reactorfor silicon Deposition”,In Proc.19th European Conference onPhotovoltaic Energy Conversion,(WIP-Munich,ETA-Florence 2004,p.459)。除了沉积硅之外,原则上在该反应器中可生产在常压下可沉积的所有其它的层。
所述反应器体现下列原理(见图1):通过气封将两行平行的基材1、1’移动到管2中。管内部存在左右开口的室3。所述室的开口在下面也 称为“沉积区”。一行基材在所述室的一个开口侧上移动通过,封闭所述开口并从而密封相对于管体积的室体积。通过气体入口4从前端(即入口气封的侧)将前体引入室内,并且在所述室的后部区域通过气体出口5抽出前体。沉积室的特殊特征是,相对于位于室外的体积保持小的低压。这防止大量的处理气体从室中逸出。在上述温度下,前体(在此:SiHCl3/H2)分解,硅主要沉积在连续向后移动的基材行的内侧。优选选择处理气体混合物,使得气体在室后端全部消耗,不再发生另外的沉积。结果,自然形成的沉积分布(即不同沉积厚度的分布),然而通过基材的移动完全得到弥补。基材在管的后端再次通过气封离开设备。反应器的另一个特性是,基材可以在均匀的推进速率下连续涂布,即不需要控制复杂的循环操作。
在由石墨制成的室的部分6以及也在其它表面上产生不期望的“寄生”沉积。为了保持所有的横截面并因此不形成干扰薄片,必须定期除去这种沉积。除了室表面之外,寄生沉积还影响例如进气喷嘴或出气开口。
对于适用于生产太阳能电池的设备必须将上述原则在生产能力上按比例放大,并且还必须尽可能地最佳化所述设备的操作时间,即尽可能保证没有间断的持续操作。本发明考虑了这些需求。
发明内容
由此出发,本发明的目的是提供用于化学气相沉积的沉积设备,相对于现有技术中已知的方法,利用所述沉积设备可以明显提高生产能力。
通过具有权利要求1的特征的一类设备、具有权利要求12的特征的化学气相沉积反应器和具有权利要求14的特征的方法来实现该目的。其它的从属权利要求表明了有利的发展。
根据本发明,提供在常压下在基材上连续化学气相沉积的设备,所述设备具有在两个相对设置的侧面上开口的反应室。沿着所述开口侧可以传送待涂覆的基材,结果密封了反应室。由此构建所述反应室,使得其分别具有相对于基材传送方向的前侧壁和后侧壁或其它密封装置,它们通过两个相对设置的侧壁连接。现在对于本发明必要的是,本发明设备的侧壁分别具有至少两个处理气体的入口和出口,所述入口和出口在基材的传送方向上至少局部交替布置。由于气体入口和气体出口的交替布置,所以气流以逆流方式穿过所述设备。结果,可以最小化或完全避免所述设备中寄生涂层的形成(即在不意欲涂覆的位置)。与现有技术相反,为此目的不需要中断连续操作,结果可实现明显更高的生产能力。
本发明中的原理基于以下的方案(Ansaetzen):
·可以增加平行传送通过所述设备的基材的行的数目。
·增加沉积区的长度。
·在进行的沉积操作中可以防止寄生涂层的形成,或者可以在连续操作期间清洁寄生涂覆的表面。
通过下列方法可以实现这些方案:
·通过灵活布置气体入口和气体出口以及相关的气流。
·通过灵活调节在反应混合物中存在的反应平衡。
·气体入口和气体出口优选以喷嘴形式布置在侧壁上。
在这个变化方案中,将气体入口布置在第一侧壁上,而气体出口布置在相对设置的侧壁上。因此,结果是形成了基本上垂直于传送方向移动的气流。如果现在交替布置,则因为连续的气体入口或气体出口的气流在相对方向上移动所以结果是利用逆流原理。
所述设备优选具有至少一个气体入口,用来引入用于在基材上沉积的前体。在本发明设备的另一个优选实施方案中,所述设备同样具有至少一个气体入口,用来引入用于清除寄生沉积的蚀刻气体。
本发明设备的第二变化方案基于以下事实,所述气体入口和气体出口配置为管的形式,所述管垂直于所述传送方向延伸并具有多个分散在管的长度上的喷嘴。因此,本发明使用具有至少一个进气管和一个排气管的系统。从而优选以区块形式布置各个管。从而优选的变化方案提供包括设置在其间的两个进气管和排气管的一个区块,并且排气管位于所述进气管之 间。从而所述设备可以总共具有大量的这类在传送方向上连续布置的区块。同样可能的是,在区块中还另外布置用于蚀刻气体的进气管。
优选使用硅、陶瓷、玻璃和/或其复合物或层体系作为待涂覆的基材。
根据本发明还提供了化学气相沉积反应器,其包含加热炉,其中布置了至少两个互相平行的根据前述权利要求之一的设备。另一个化学气相沉积反应器同样包括加热炉,然而其中连续地布置本发明的设备。
根据本发明同样提供了在常压下在基材上连续化学气相沉积的方法,其中使用本发明的设备。在所述方法中控制气体供应,使得在基材上沉积期间,同时防止和/或除去寄生沉积。
优选通过至少一个气体入口供应至少一种前体,其随后在涂覆工艺期间沉积在基材上。从而通过至少一个气体出口从该设备抽出气体。可优选通过泵进行所述抽出。
本发明方法的一个优选变化方案提供:通过周期性改变至少一种供应的气体的组成,可以在沉积工艺期间防止和/或除去设备中的寄生沉积。如果要除去寄生沉积,那么优选供应至少一种蚀刻气体来除去这些寄生沉积。通过用于至少一种蚀刻气体的气体入口来进行所述至少一种蚀刻气体的供应。本发明中,既能够通过单独的气体入口供应蚀刻气体,也能够通过相同的气体入口供应蚀刻气体和前体,其在时间上循环进行。
在本发明的方法中,尤其优选通过不同的气体入口周期性交替地将至少一种前体和至少一种蚀刻气体供应到设备中。另外,优选至少一种蚀刻气体和至少一种前体化学上彼此相容。
优选气体入口应该设置侧壁中的气体入口或气体入口中的喷嘴,使得它们指向基材,以便可以在基材方向上产生气流。与此相反,用于至少一种蚀刻气体的气体入口或进气管中的喷嘴应该指向具有寄生沉积的设备表面,以便可以蚀刻掉设备的这些部件上的寄生沉积。
另外,优选在前述区块式构造中,将不同的处理气体供应到设备内,使得可以在基材传送期间在基材上沉积不同的层或层组成。
可以根据两个不同的变化方案实施本发明的方法。第一变化方案中,在处理室的边界和基材之间存在间隙,该间隙的尺寸基本上不随时间变化。因此,使得能够通过所述设备来连续传送基材(即基材在任何时间都不处于静止状态)和循环传送基材(包括传送循环和静止循环)。通过适当的吹入气体控制来防止处理气体排出。作为另外的选择,还可以使用滑动密封,以实现基材和处理室之间的密封。然而,在高温和高纯度要求下,这类密封可能出现问题。
第二优选方案提供:在工艺期间所述间隙的宽度周期性改变,基材以脉冲方式传送穿过所述设备。在沉积循环期间,基材停留在处理室的边界上,并且以足够气密的方式密封处理室。在短的传送循环期间,基材从该室升起,继续传送并再次放下。通过适当的吹入气体控制来防止气体在传送循环期间产生的间隙中逸出。由于室中的压力相对于环境压力降低,直到可能形成足够的吹入气流,或者至少防止了向外的流动,所以这与上述变化方案同样有效。该第二变化方案的优点在于,一方面对压力波动或流动波动具有较高的耐受性,另一方面是较低污染物的沉积量,例如关于吹入气体和其中夹带的污染物。
附图说明
参考下列实施例更详细说明本发明的主题,不希望将本发明限制在所述的具体实施方案中。
图1示出现有技术中已知的化学气相沉积反应器。
图2示出本发明设备的优选实施方案,所述设备包括在传送方向交替布置的气体入口和气体出口。
图3示出本发明设备的一个实施方案,其中使用布置在区块中的进气管和排气管。
图4示出图3所表示实施方案的平面图。
图5示出本发明设备的另一个实施方案,所述设备具有区块式布置的进气管和排气管以及额外的回蚀管(Rueckaetzrohren)。
图6示出根据本发明的布置,其中互相平行地布置了多个根据图5 的本发明的设备。
具体实施方式
实施例1
在第一优选实施方案中,前体通过位于沉积室纵向侧的入口喷嘴输送到沉积室1,所述沉积室不是由基材形成的(见图2)。一个气体入口2和一个气体出口3大致相互相对地布置,两个连续的对(例如图2的对1和对2)以镜像的方式布置。那么连续对的气流以逆流方式运动。根据本发明,如此操作所述系统,使得以理论上可能的高百分比的值来利用从一个对的气体入口到气体出口的前体,也就是说,形成图案,其中由于气体的消耗在一些点上几乎不再发生沉积。通过在一个或多个入口对中使用化学相容的蚀刻气体,而其它的对仍处于沉积操作中,进行寄生层的回蚀。或者,可以通过改变前体的气体组成来实现回蚀(例如提高氯硅烷中的Cl/H比)。在回蚀期间改变气流,使得优先侵蚀寄生涂覆的表面,并且尽可能保留待随后使用的层。必须有效回蚀至少归属于一对喷嘴的寄生涂覆的表面。回蚀完成之后,该对喷嘴再次供应用于沉积的前体,并对其它对喷嘴重新开始回蚀。周期性继续进行该工艺。
如果对所述工艺有利,可以周期性交换气体入口和气体出口的作用。
每m个对形成一个沉积室。
实施例2
本发明第二种形式的特征如下:代替在沉积室侧面的进气喷嘴/排气喷嘴,具有多个分布在管长度上的进气喷嘴/排气喷嘴的进气管垂直于移动方向横穿沉积室。进气管分别布置在一个排气管之前或之后(见图3和4)。气体优选在基材方向从进气管吹出。下面将这种布置称为“区块”。在沉积操作期间,将前体引入两个进气管,通过两个进气管之间的排气管抽出用过的气体。在沉积室中,连续布置任意数目的这些区块。为了回蚀,用蚀刻气体操作一个或多个区块,选择蚀刻气体的流动,使得气体优选供应到寄生涂覆的表面,并因此回蚀。如下扩展形式2:代替每个回蚀管分别2个进气管,在排气管之前或之后给区块补充额外的 进气管(“扩展区块”)。每m个区块(扩展区块)形成一个沉积室。
实施例3
在第三形式中,用前置的分离的回蚀管补充形式2的区块(见图5)。该回蚀管可以供应有蚀刻气体,并且分别回蚀相邻的进气管和排气管。选择蚀刻气流的方向,使得优先蚀刻寄生沉积的位置。所述回蚀既可以与形式1和2一样循环进行(即在回蚀期间中断前体向相邻进气管的供应),也可以在所有进气管的进行的沉积操作中进行。这种操作的基本特征是,通过所述蚀刻气体改变进气管和排气管位置处的气体组成,使得反应平衡从沉积移向蚀刻。通过蚀刻气体的方向和量,最大程度地防止蚀刻发生在基材自身上。与形式2一样,也可以通过额外的进气管来扩展形式3的区块。对于一个沉积室,串联地连续布置每m个区块,第m个区块之后的回蚀管密封沉积室。
Claims (29)
1.一种用于在基材上在常压下连续化学气相沉积的设备,所述设备包括具有在两个相对的侧的开口的反应室,沿着所述开口侧可以在密封所述反应室的同时传送待涂覆的基材,所述反应室分别具有相对于所述基材传送方向的前侧壁和后侧壁,所述前侧壁和后侧壁通过两个相对设置的侧壁连接,
其特征在于,
所述侧壁至少分别具有两个处理气体入口和两个处理气体出口,所述处理气体入口和处理气体出口至少局部交替地布置在所述传送方向上。
2.根据权利要求1的设备,其特征在于,所述基材由硅、陶瓷、玻璃和/或其复合物或层体系组成。
3.根据权利要求1的设备,其特征在于,在侧壁上的气体入口对应于在相对侧壁上的气体出口,形成基本垂直于传送方向移动的气流。
4.根据权利要求1至3中任一项的设备,其特征在于,所述设备具有用于引入前体以沉积在基材上的至少一个气体入口。
5.根据权利要求1至3中任一项的设备,其特征在于,所述设备具有用于引入蚀刻气体以清除寄生沉积的至少一个气体入口。
6.根据权利要求1至3中任一项的设备,其特征在于,所述气体入口和气体出口以喷嘴形式布置在所述侧壁上。
7.根据权利要求1的设备,其特征在于,所述气体入口和气体出口配置为管的形式,所述管垂直于所述传送方向延伸并具有多个分散在管的长度上的喷嘴。
8.根据权利要求7的设备,其特征在于,以区块形式布置所述多个管。
9.根据权利要求8的设备,其特征在于,一个区块包括两个进气管和位于所述进气管之间的排气管。
10.根据权利要求8的设备,其特征在于,所述设备具有在所述传送方向上连续布置的大量的区块。
11.根据权利要求8至10中任一项的设备,其特征在于,所述区块还具有用于蚀刻气体的进气管。
12.一种化学气相沉积反应器,包括加热炉,在所述加热炉中布置了互相平行的根据权利要求1至11中任一项的至少两个设备。
13.一种化学气相沉积反应器,包括加热炉,在所述加热炉中设置了至少两个连续布置的根据权利要求1至11中任一项的设备。
14.一种利用权利要求1至11中任一项的设备在常压下在基材上连续化学气相沉积的方法,在所述方法中控制气体供应,使得在所述基材上的沉积期间,同时防止和/或除去所述设备中的寄生沉积,其中通过周期性改变至少一种供应气体的组成,防止和/或除去所述设备上的寄生沉积。
15.根据权利要求14的方法,其特征在于,在每个区块中供应不同的处理气体,从而沉积不同的层或层组成。
16.根据权利要求14的方法,其特征在于,在所述处理室的边界和所述基材之间存在间隙,其中在所述处理室边界和所述基材之间的间隙的尺寸基本上不随时间变化。
17.根据权利要求14的方法,其特征在于,在所述处理室的边界和所述基材之间存在间隙,其中所述处理室的边界和所述基材之间的间隙的尺寸周期性变化。
18.根据权利要求14的方法,其特征在于,通过至少一个气体入口供应至少一种前体。
19.根据权利要求18的方法,其特征在于,所述至少一种前体的进气管的喷嘴指向基材,从而在所述基材的方向上产生气流。
20.根据权利要求14的方法,其特征在于,通过至少一个气体出口从所述设备中抽出气体。
21.根据权利要求20的方法,其特征在于,通过泵进行所述抽出。
22.一种利用权利要求1至11中任一项的设备在常压下在基材上连续化学气相沉积的方法,在所述方法中控制气体供应,使得在所述基材上的沉积期间,同时防止和/或除去所述设备中的寄生沉积,其中通过供应至少一种蚀刻气体除去所述设备中的寄生沉积。
23.根据权利要求22的方法,其特征在于,通过至少一个气体入口供应用于除去寄生沉积的至少一种蚀刻气体。
24.根据权利要求23的方法,其特征在于,通过至少一个气体入口供应所述至少一种蚀刻气体。
25.根据权利要求22的方法,其特征在于,所述至少一种蚀刻气体的进气管的喷嘴指向具有寄生沉积的设备表面,从而回蚀所述寄生沉积。
26.根据权利要求18至19和22至25中任一项的方法,其特征在于,通过相同的气体入口供应所述至少一种前体和所述至少一种蚀刻气体。
27.根据权利要求18至19和22至25中任一项的方法,其特征在于,通过不同的气体入口将所述至少一种前体和所述至少一种蚀刻气体周期性交替地供应给所述设备。
28.根据权利要求18至19和22至25中任一项的方法,其特征在于,所述至少一种前体和所述至少一种蚀刻气体化学上互相相容。
29.根据权利要求14至25中任一项的方法,其特征在于,第一气流和第二气流以逆流原理流动,所述第一气流从所述第一侧壁中的气体入口导向位于所述第二侧壁中的气体出口,第二气流与所述第一气流平行地从位于所述第二侧壁中的气体入口导向在所述第一侧壁中的气体出口。
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DE102005045582B3 (de) * | 2005-09-23 | 2007-03-29 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Vorrichtung und Verfahren zur kontinuierlichen Gasphasenabscheidung unter Atmosphärendruck und deren Verwendung |
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2005
- 2005-09-23 DE DE102005045582A patent/DE102005045582B3/de not_active Expired - Fee Related
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2006
- 2006-09-22 ES ES06792230T patent/ES2327568T3/es active Active
- 2006-09-22 WO PCT/EP2006/009228 patent/WO2007033832A2/de active Application Filing
- 2006-09-22 JP JP2008531617A patent/JP5138594B2/ja active Active
- 2006-09-22 US US12/067,233 patent/US8900368B2/en active Active
- 2006-09-22 AT AT06792230T patent/ATE438748T1/de active
- 2006-09-22 DE DE502006004463T patent/DE502006004463D1/de active Active
- 2006-09-22 CN CN2006800345443A patent/CN101268213B/zh active Active
- 2006-09-22 EP EP06792230A patent/EP1929066B1/de active Active
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2014
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Patent Citations (2)
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GB1328390A (en) * | 1970-01-02 | 1973-08-30 | Ibm | Vapour processing of semiconductor material |
CN1375575A (zh) * | 2001-03-19 | 2002-10-23 | 株式会社Apex | 化学气相沉积设备 |
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ES2327568T3 (es) | 2009-10-30 |
US9683289B2 (en) | 2017-06-20 |
US8900368B2 (en) | 2014-12-02 |
ATE438748T1 (de) | 2009-08-15 |
CN101268213A (zh) | 2008-09-17 |
WO2007033832A3 (de) | 2007-06-14 |
WO2007033832A2 (de) | 2007-03-29 |
DE502006004463D1 (de) | 2009-09-17 |
DE102005045582B3 (de) | 2007-03-29 |
EP1929066A2 (de) | 2008-06-11 |
JP2009509042A (ja) | 2009-03-05 |
JP5138594B2 (ja) | 2013-02-06 |
US20150037500A1 (en) | 2015-02-05 |
EP1929066B1 (de) | 2009-08-05 |
US20080317956A1 (en) | 2008-12-25 |
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