CN101432457B - 大气压化学气相淀积 - Google Patents

大气压化学气相淀积 Download PDF

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CN101432457B
CN101432457B CN2005800282420A CN200580028242A CN101432457B CN 101432457 B CN101432457 B CN 101432457B CN 2005800282420 A CN2005800282420 A CN 2005800282420A CN 200580028242 A CN200580028242 A CN 200580028242A CN 101432457 B CN101432457 B CN 101432457B
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N·W·约翰斯顿
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Abstract

一种用于在大气压下涂覆衬底的方法，该方法包含下列步骤：在加热的惰性气流中在基本上大气压下蒸发可控质量的半导体材料，以产生具有高于该半导体材料凝结温度的温度的流体混合物；在基本上大气压下将该流体混合物引导到具有低于该半导体材料凝结温度的温度的衬底上；并且在该衬底的表面上淀积一层该半导体材料。

Description

大气压化学气相淀积
相关申请交叉引用
本申请要求2004年8月18日提出的临时专利申请序号No.60/602,405的权益。
技术领域
本发明一般性地涉及在衬底上的气相化学材料的淀积，并且更特别地，涉及一种用于在大气压下在衬底上淀积气相化学材料的方法。
背景技术
诸如热解工艺和水解工艺的化学气相淀积方法在涂覆衬底的技术中是公知的。在这种工艺中利用的涂覆反应物的物理特性可以是液体、气体、分散在气体混合物中的液体或固体、气溶胶或分散在气体混合物中的被蒸发的或蒸气状的涂覆反应物。
在制造光电器件中的玻璃衬底上的被蒸发的化学化合物的淀积方法中，典型地，在真空环境中淀积被蒸发的化学化合物。用于进行这种工艺的系统典型地包括具有较下部分和具有彼此水平连接的较上部分形成的密封淀积腔的外壳。密封配件插入到较下和较上外壳之间的连接处。提供传送装置以在腔内传输玻璃薄片衬底。化学气相分配器设置在淀积腔内，以在衬底通过腔时对玻璃衬底上提供涂覆。
系统包括用于在淀积腔内抽真空的真空源。典型地，淀积腔包括用于当玻璃薄片在系统中传送时对其进行加热的延长加热器。玻璃薄片从真空加热炉通过淀积腔，到真空淀积腔，真空淀积腔保持在近似于加热炉的真空和温度设置。将粉末状的硫化镉和粉末的碲化镉输入到气相淀积腔。然后，接着在先前被涂覆和加热的玻璃衬底上依次淀积膜。接着，涂覆的衬底通过一装载机构(load lock)被转移，之后进入一通过压缩的氮来制冷的冷却腔，并且最后通过出口装载机构到达一个为降低到环境温度的风冷部件中而被传送到大气压下。碲化镉薄膜材料需要下面的工艺步骤以对其多晶的结构进行重结晶，以便由薄膜层叠制造有效的光电器件。典型地，该步骤通过将氯化镉溶液施加到冷却的涂覆玻璃的碲化镉表面并且重新加热玻璃到约390℃至420℃的温度达约1 5到20分钟的一段时间而实现。必须小心，慢慢地加热和冷却玻璃以避免在该处理期间出现破损，这样的处理延长了该必要步骤的整个工艺时间。
众所周知，可再生的能源变得日益重要，因此相信用于产生电能的光电器件的商业生产对于满足可再生能源的需要是十分重要的。在玻璃衬底上的薄膜涂覆半导体材料的利用被认为是一种在基于光电的电能产生系统的领域中的可行的机制。
已经发现，基于上述参考技术的薄膜涂覆系统能在真空中在商业可获取的碱石灰玻璃衬底上淀积硫化镉/碲化镉光电材料的薄膜。接着处理光电材料以重结晶碲化镉表面，制造薄膜层叠为进一步处理成光电器件作准备。尽管上述系统能够制造适用于电能产生的光电面板，期待降低这种生产的成本而使得该系统变得商业可行。
发明内容
本发明的目的是在大气压下在衬底上通过由化学气相淀积半导体材料的薄膜而制造一种光电面板。
本发明的另一目的是在大气压下通过由蒸发硫化镉和碲化镉并将其淀积在加热的衬底的表面上以形成第一硫化镉薄膜和第二碲化镉薄膜而制造一种光电面板。
本发明的另一目的是通过快速高温重结晶薄膜碲化镉多晶硅材料以产生高效率的光电器件而制造一种光电面板。
已经惊讶地发现，上述目的可以通过在大气压下涂覆衬底的方法而实现，该方法包含下列步骤：(1)提供诸如硫化镉或碲化镉的半导体材料源；(2)在基本上大气压下，加热和蒸发半导体材料并且保持该蒸发材料处于高于它们的凝结温度的温度；并且(3)接着在基本上大气压下在诸如玻璃的衬底的热表面上淀积该蒸发材料以形成层状结构。任选地，尽管该层状结构仍然基本上处于淀积的温度并且在基本上大气压下，碲化镉层可以由反应性气体处理以实现碲化镉的重结晶。进行层状薄膜层叠的接下来的工艺可以制造有源(active)薄膜光电器件。
附图的简要说明
参考附图，从阅读本发明的优选实施方案的下文详细描述中，本发明上述和其它目的和优点对于本领域技术人员将变得显而易见，其中：
图1是用于在衬底上沉积半导体的方法的示意图。
图2a是用于在衬底上沉积半导体层的系统的示意说明，使用图1中所示的方法，其中衬底是水平的并且垂直于出口喷嘴。
图2b是用于在衬底上沉积半导体层的另一个系统的示意说明，使用图1中所示的方法，其中衬底是直立的并且垂直于出口喷嘴。
优选实施方案的详细说明
参考图1，图示出在大气压下利用碲化镉膜涂覆衬底10的表面的方法的步骤。
单独计量的半导体材料团，优选地硫化镉(CdS)或碲化镉(CdTe)以粉末状形式被导入由惰性气体流连续地净化的区域，优选氮气，该惰性气体在大约大气压下在入口和出口间流动。该粉末被以受控速率流动的惰性气体从入口带入到由加热的压缩的基座(bed)构成的蒸发器12中，其中，该粉末随着其通过压缩的基座的介质的填隙空位(void)时被蒸发。正如在图2a和2b中所示的那样，使加热的压缩基座的出口与加热区14的内部相通以向衬底10分布蒸发的材料。可选地，可以利用粉末蒸发方法，通过其加热计量的粉末团和载体惰性气体，用来产生蒸发的材料流体流。该可选的方法可包括，但不一定局限于，该载体惰性气体被加热和该粉末被蒸发的加热的流体化的基座、加热载体惰性气体和蒸发粉末的热“闪”蒸发器，和加热载体惰性气体和蒸发粉末的大气压热喷射单元。
该流体，优选包括硫化镉或碲化镉粉末和载体惰性气体，是一种在高于其凝结温度的温度下包含载体惰性气体和蒸发材料的高温流动混合物。典型地，流体混合物的温度在从约800℃到约1100℃的范围。然后，在基本大气压下，加热的流体混合物被引导到用于在沿着衬底10表面产生恒定速度的层状流的装置16内。典型地，衬底10是一种碱石灰玻璃，优选地具有透明的和电导性的低E涂覆。这种玻璃的一种例子是由Pilkington Glass Co.制造并且指定为TEC-15。衬底10的表面保持在从约585℃到约650℃的温度。
用于产生理想的流体混合物的层状流的装置16包含：一系列的单独的通道，其适用于当流体流经该通道时导致在瞬变流体中一系列的速度的变化。该装置16保持在高于硫化镉或碲化镉的蒸发的温度，以阻止在通道内的材料的凝结。这种流体流均匀向伸长的出口喷嘴18分布流体混合物，并且使恒定质量流分布的均匀层状流正切于衬底10地流动并提供给衬底10的表面，正如箭头A所指出的那样。以上动作使得流体混合物的分子均匀地分布到该伸长的出口喷嘴18的整个长度，并且使得该分子在通常的平行路径中并且以恒定的速度从出口喷嘴流出，直接朝着衬底10产生恒定速度和质量分布的层状流。
流出出口喷嘴18的流体混合物的速度可以通过控制导入入口的流体混合物的质量流速率而被调节。
为了控制从正在被施加到衬底10的装置喷出的流体内的蒸发材料的薄膜淀积速率，在控制低于蒸发材料的凝结点的衬底10的温度的同时，控制流体混合物的质量流速率和衬底10的速率。当加热的流体混合物碰撞到较冷的衬底10，其会冷却到低于蒸发材料的凝结温度的温度。该材料由该流体混合物以多晶形式凝结在衬底10上面成为连续薄膜层，该衬底10在传送装置20上移动。流体抽取装置22被设置在出口喷嘴18的上游和下游，以使得能够将对着衬底10表面的流体混合物的非膜(non-film)产生成分的可控制的回收，正如通过箭头B所指出的那样。
尽管有多种用于在瞬变玻璃衬底的表面上均匀地分布蒸发的硫化镉或碲化镉的不同的系统，但是估计在Hofer等人的US专利4,509,526中说明和描述的装置可以提供满意的结果。
可以根据本发明设想到，通过上述装置的硫化镉和/或碲化镉的任何数量的连续层的淀积，来制备层状结构。
在碲化镉多晶薄膜的淀积之后，需要重结晶步骤以由层状薄膜层叠实现光电器件的生产。已经发现，该步骤可以在不到一分钟内，在基本上一个大气压下，通过将热碲化镉膜施加到在氮中稀释的氯化氢的热气体气氛中而完成。在重结晶步骤的过程中，在保持衬底10的温度的同时控制碲化镉重结晶的能力消除了衬底/膜层叠组件的冷却和再加热。“干法”重结晶步骤的使用消除了有毒的氯化镉溶液及其应用装置的使用。典型地，退出该线上的重结晶工艺的玻璃衬底具有从约620℃到约630℃的温度。该温度范围允许当衬底/膜层叠离开该工艺线时该玻璃被冷却焠火气体流热回火。
上述方法涉及一种用于在碱石灰玻璃衬底的表面上产生一种薄膜硫化镉/碲化镉光电材料以提供大面积的光电面板的方法。然而，应当清楚，大气压气相淀积的概念可以延伸到包括在真空中正常地淀积的其他薄膜材料。
薄膜光电材料可以认为是CIGS(铜-铟-镓-联硒化物)、CdS/CIS合金(硫化镉/铜-铟-硒合金)、无定形硅或薄膜多晶硅，和Zn(O、S、OH)x/CIGS(锌氧化物硫化物氢氧化物/铜-铟-镓-联硒化物)。
其它的可以考虑应用到玻璃衬底的薄膜材料是光学涂层，诸如用于超低发射率膜和抗反射膜的多层层叠。其它的增值特征，诸如改善的耐用膜、自清洁膜、光学拍照(photo-optic)和电子光学(electro-optic)膜可以通过使用本发明的大气压淀积概念而被发展。
薄膜材料的大气压淀积方法可以应用到各种用于增强其表面特性的衬底材料中。可以考虑的衬底包括：聚合材料、陶瓷、金属、木材和其它材料。

Claims (13)

1.一种用于在大气压下涂覆加热到低于半导体材料的凝结温度的温度的衬底的方法，该方法包含下列步骤：
将可控质量的半导体材料和惰性气体流混合；
蒸发在惰性气体流中的半导体材料，以产生具有高于该半导体材料凝结温度的温度的流体混合物；
引导该流体混合物到衬底，其中所述衬底在基本上大气压下；和
在该衬底的表面上淀积一层该半导体材料。
2.根据权利要求1的方法，其中，该半导体材料是硫化镉和碲化镉之一。
3.根据权利要求1的方法，其中，该惰性气体是氮。
4.根据权利要求1的方法，其中，该流体混合物的温度范围是从800摄氏度到1100摄氏度。
5.根据权利要求1的方法，其中，该衬底包含玻璃。
6.根据权利要求5的方法，其中，该玻璃包括透明的、电导性的涂层。
7.根据权利要求1的方法，其中，该衬底具有从585摄氏度到650摄氏度的温度范围。
8.根据权利要求1的方法，其中，蒸发、引导和淀积步骤重复至少一次，以在该衬底上淀积至少另外的一层半导体材料。
9.根据权利要求1的方法，其中半导体材料是CIGS(铜-铟-镓-联硒化物)、CdS/CIS合金(硫化镉/铜-铟-硒合金)、无定形硅或薄膜多晶硅，和锌氧化物、锌硫化物、锌氢氧化物、或这些化合物的混合物/CIGS(铜-铟-镓-联硒化物)之一。
10.根据权利要求1的方法，其进一步包括提供衬底相对于流体混合物源的移动的步骤。
11.根据权利要求1的方法，其进一步包括选择性控制流体混合物的质量流速率，以控制半导体材料在衬底上的沉积速度的步骤。
12.一种用于在大气压下涂覆加热到低于半导体材料的凝结温度的温度的衬底的方法，该方法包含下列步骤：
将可控质量的半导体材料和惰性气体流混合；
蒸发在惰性气体流中的半导体材料，以产生具有从800摄氏度到1100摄氏度的温度范围的流体混合物；
在基本上大气压下引导该流体混合物到具有透明的、电导性的涂层并且具有从585摄氏度到650摄氏度的温度范围的衬底；和
在该衬底的表面上淀积一层该半导体材料。
13.根据权利要求12的方法，其中，蒸发、引导和淀积步骤重复至少一次，以在该衬底上淀积至少另外的一层半导体材料。
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