CN102859033A - 用于气体输送系统的涂布的方法 - Google Patents

用于气体输送系统的涂布的方法 Download PDF

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CN102859033A
CN102859033A CN2011800201772A CN201180020177A CN102859033A CN 102859033 A CN102859033 A CN 102859033A CN 2011800201772 A CN2011800201772 A CN 2011800201772A CN 201180020177 A CN201180020177 A CN 201180020177A CN 102859033 A CN102859033 A CN 102859033A
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伊恩·肯沃西
杜安·奥特卡
郝方力
伦纳德·沙普利斯
杜义军
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Abstract

一种涂布用于等离子体工艺系统的气体输送系统的气体通道的内表面的方法，该等离子体处理系统诸如等离子体蚀刻系统，该方法包括（a）使耐腐蚀材料的流体前驱体流动通过气体通道，并沉积流体前驱体的层完全地覆盖该气体通道的内表面；（b）从内表面去除过量的流体前驱体；（c）固化该流体前驱体的沉积层，以形成耐腐蚀的材料涂层。

Description

用于气体输送系统的涂布的方法
背景技术
在衬底的处理中，例如，在半导体衬底或诸如在平板显示器制造中使用的玻璃面板，通常采用等离子体。例如，作为衬底处理的一部分（等离子体蚀刻，化学气相沉积，等离子体增强化学气相沉积，物理气相沉积，等），衬底被分成多个管芯或矩形区域，该多个管芯或矩形区域中的每个将成为集成电路。然后，该衬底在一系列的步骤中处理，其中，选择性地去除（蚀刻）和添加（沉积）材料，以形成其上的电气元件。
在示例性的等离子体工艺中，在蚀刻之前，衬底涂有硬化的感光乳液（即，如光致抗蚀剂掩模等）的薄膜。然后，选择性地去除硬化的感光乳液的区域，从而导致下伏衬底的一部分暴露。然后，在等离子处理系统的腔室中放置衬底在包括单极或双极型电极的被称为卡盘的衬底支撑结构上。然后使合适的工艺气体（如C4F8、C4F6、CHF3、CH2F2、CF4、CH3F、C2F4、N2、O2、HBr、Ar、Xe、He、H2、NH3、SF6、BCl3、Cl2，等等）通过气体输送系统的气体通道流入腔室，并使之电离形成等离子体以蚀刻衬底的暴露的区域。含卤素的工艺气体是高腐蚀性的，并且会损坏气体通道的内表面。
发明内容
公开了一种用于涂布气体输送系统的气体通道的内表面的方法，该气体输送系统被配置成输送气体进入等离子处理系统的腔室，该方法包括：(a)使耐腐蚀材料的流体前驱体流动通过气体通道，并沉积流体前驱体的层以完全覆盖气体通道的内表面;(b)从内表面去除过量的流体前驱体;(c)固化流体前驱体的所沉积的层，以形成耐腐蚀的材料涂层。
附图说明
图1是等离子体处理系统的简化横截面示意图。
图2示意了在波纹管的盘旋结构中耐腐蚀材料的流体前驱体的聚积。
具体实施方式
图1示出了等离子体处理系统100的简化的横截面视图。通常地，使一种或多种工艺气体从气体输送系统122通过入口108流入腔室102。这些工艺气体随后会被电离以形成等离子体110，以对衬底114的暴露的区域进行处理（例如，蚀刻或沉积等），衬底114诸如半导体衬底或玻璃面板等，其放置在静电卡盘116上。网状电极120，以及衬板112，有助于使等离子体110最优化地集中在衬底114上。
气体输送系统122可以包括一个或多个质量流量控制器，该控制器连接到含有等离子体处理气体（如C4F8、C4F6、CHF3、CH2F2、CF4、HBr、CH3F、C2F4、N2、O2、Ar、Xe、He、H2、NH3、SF6、BCl3、Cl2，等等）的压缩气体瓶124a-f。气瓶124a-f可通过外壳128得到进一步的保护，外壳128提供局部排气通风。质量流量控制器126可以是在半导体工业中使用的以便测量和调节到等离子体处理系统中的气体的质量流量的配套装置（由换能器、控制阀、和控制与处理信号的电子设备组成）。气体输送系统122包括工艺气体流过其中的气体通道。气体输送系统中的各个组成部分通过管材和波纹管区相互关联，其中，这些区容许诸如处理腔室门等某些组件的运动。
等离子体处理过程中，需要输送超纯的工艺气体，以最大限度地提高半导体工厂的生产效率和产量。然而，因为其高度腐蚀性和反应性，这类气体的输送产生了特殊的挑战。
特别地，在气体输送系统中产生的腐蚀可能会大幅降低衬底的产量。例如，在蚀刻衬底的工艺中，从在工艺气体中的材料（例如，碳，氟，氢，氮，氧，硅，硼，氯，等）中，从在衬底上的材料（如光致抗蚀剂，硅，氧，氮，铝，钛等）中，或从等离子体处理室或气体输送系统内的结构材料（例如，不锈钢，铝，石英等）中，可能会产生污染物。
在半导体生产中，具有被制造的器件特征尺寸的十分之一的颗粒可显著地损坏该器件。接着，与工艺气体接触的组件通常设计为以减少或消除系统污染的潜在来源。由于气体输送系统会是污染的重要来源，气体通道通常由一组选定的金属（例如，电抛光不锈钢，铜（Cu），铝（Al），金属合金等）组成。
例如，不锈钢是铁（Fe）系合金，具有众多铬（Cr）和镍（Ni）的合金化添加剂，其中，铬（Cr）给金属提供“不锈”或耐腐蚀的特性，以及镍（Ni）使奥氏体稳定并使金属无磁性和牢固。电解抛光通常可以改善部件的表面化学性质，增强钝化氧化膜，并从表面去除任何游离铁。
在一般情况下，不锈钢包括“钝化”膜涂层，该涂层可对进一步的“氧化”或生锈有抗性。当暴露在氧气中该膜可快速地形成。一旦该膜形成，金属变成“钝化的”时，氧化或“生锈”的速度将大大减慢。
尽管减少腐蚀做出的努力，诸如电解抛光、钝化、镜面光滑表面处理（粗糙度Ra<5密耳）等，但由于长期暴露于工艺气体，腐蚀仍然发生，特别是在某些区域，如靠近焊接接头的部分和周期性地暴露于湿气中的不锈钢气体通道的部分等。
腐蚀的程度和因此形成的污染物的量可取决于许多因素，如气体的浓度和纯度、含湿量、温度、气体通道材料的局部不均匀性、系统流速、曝露时间、和曝光频率等。例如，当含湿量超过百万分之几（ppm）时，诸如氯化氢或溴化氢等含卤素的气体可腐蚀不锈钢。
虽然湿气可以减少，但通常不能完全被去除。例如，虽然等离子体处理气体通常以纯净的形式存储在压缩气瓶中，但当气瓶被更换时或对处理腔室进行维护时，会引入湿气到气体输送系统中。
虽然在不锈钢中腐蚀的实际量往往是小的，但从腐蚀区域释放的铁和铬的量可以由不锈钢气体通道的气流携带到其中进行半导体衬底处理的等离子处理腔室中。结果在等离子体处理室中处理的半导体衬底会发生严重污染。在衬底上的铁或铬污染的典型容限小于5.0x1010原子/平方厘米。因此，为防止或大大减少不锈钢气体通道的腐蚀采取的措施是合乎需要的。减少气体输送系统中的腐蚀的途径之一，是防止不锈钢气体通道（例如管材和波纹管）接触腐蚀性气体。
根据此途径的一种方法是使用耐腐蚀管材（例如，聚乙烯管材、聚丙烯管材、弹性玻璃管材、金属涂布的塑料管材、陶瓷管材、具有传导屏蔽层夹在两层塑料之间的叠层管材、或阳极铝等）。
通过引用并入此处的普通转让的美国专利No.7,234,222，公开了将塑料套粘接或注射成型到不锈钢管材的内部表面上的方法。
本文描述了流动涂布法的实施方式，其中耐腐蚀材料的流体前驱体经过气体输送系统中的气体通道，以在气体通道的内表面上沉积流体前驱体的层，且使所沉积的该流体前驱体层固化以在气体通道的内表面上形成耐腐蚀材料的层。可以用焊接金属（如不锈钢）管材、波纹管，管接头，法兰，阀门等形成气体通道。流动涂布方法对涂布具有复杂的几何形状和/或小直径（例如，波纹管的内表面，或者具有0.25英寸或更小的外径的管材的内表面）的内表面是有效的。
流动涂布方法的实施方式包括以下步骤：（a）用合适的洗涤剂和/或合适的化学品（例如，用10至20wt.％的硝酸进行3分钟，并用去离子水冲洗内部表面至少5分钟）清洁气体输送系统的气体通道的内表面；（b）使内表面干燥（例如，通过吹入干燥氮气或干燥空气经过气体通道，并且在真空烘箱中以至少120℃的温度烘烤气体通道）；（c）使耐腐蚀材料流体前驱体（例如，PERMABOND生产的HL126液体聚合物前驱体或甲基丙烯酸酯）流动通过气体通道，并沉积流体前驱体的层以覆盖气体通道的内表面;（d）从内表面去除过量的流体前驱体（例如，通过吹入干燥氮气或干燥空气进入气体通道）；（e）固化流体前驱体的沉积层，以形成耐腐蚀的材料涂层（例如，通过在真空烘箱中在至少100℃的温度和1至10托的压强下烘烤气体通道，或保持气体通路在环境温度和压强下至少24小时）。可施加相同的第二涂层。生成的涂层可具有从0.0014至0.0034英寸厚的厚度，并且非脆性。
然而，如图2所示，如果气体通道包括焊接到气体通道的其他组件（如管材，配件，阀门，法兰等）的波纹管201，则流体前驱体会在波纹管201的内表面的盘旋结构202积聚，并在盘旋结构202上固化成过量的耐腐蚀材料，其可能会剥落并成为微粒污染物。
经过长时间暴露于腐蚀性气体之后，气体输送系统中的未涂布的不锈钢波纹管的检测展现波纹管的盘旋结构没有显示任何腐蚀迹象，而在该气体输送系统中的其他组件和组件之间的焊接接头存在严重的腐蚀。因此，选择性地涂布的方法可以消除在波纹管的盘旋结构中耐腐蚀材料的积聚的问题，其中，耐腐蚀材料的涂层被施加在气体输送系统中的气体通路的除了其中的波纹管的内表面以外的所有的内表面上。
选择性涂布方法的实施方式包括以下步骤：（a）在将波纹管焊接到气体通道的其余部分之前，用掩蔽剂涂布波纹管的内表面以防止流体前驱体的粘附，掩蔽剂如光致抗蚀剂、油、硅烷和/或烷氧基硅烷（硅烷和/或烷氧基硅烷可在波纹管的内表面上提供硅烷化的层）等;（b）将波纹管焊接到其他组件；（c）使流体前驱体（例如HL126液体聚合物前驱体或甲基丙烯酸酯）流动，通过气体通道，且沉积流体前驱体的层以覆盖除了波纹管的内表面的气体通道的内表面;（d）去除过量的流体前驱体（例如，通过吹入干燥氮气或干燥的空气进入气体通道）;（e）固化流体前驱体的沉积层（例如，在真空烘箱中在至少100℃的温度和在1至10托的压强下烘烤气体通道，或通过保持该气体通道在环境温度和压强下至少24小时）；（f）可选地，从波纹管的内表面去除掩蔽剂。
掩蔽剂可以是光致抗蚀剂、油、硅烷、烷氧基硅烷或其他适合的材料。流体前驱体可以是HL126聚合物或甲基丙烯酸酯或其它合适的材料。掩蔽剂可由丙酮、光致抗蚀剂去除剂或其它合适的材料去除（例如溶解、蚀刻，等）。
虽然参照其中特定的实施方式，对涂布气体输送系统的气体通道的内表面的方法已进行了详细描述，但对本领域技术人员而言，在不脱离所附的权利要求的范围下，可以做出各种变化和修改，以及使用等同方法是显而易见的。

Claims (17)

1.一种用于涂布气体输送系统的气体通道的内表面的方法，该气体输送系统被配置成输送气体进入等离子处理系统的腔室，所述方法包括：
(a)使耐腐蚀材料的流体前驱体流动通过所述气体通道，并沉积所述流体前驱体的层以覆盖所述气体通道的所述内表面;
(b)从所述内表面去除过量的流体前驱体;
(c)固化所述流体前驱体的所述沉积层，以形成耐腐蚀的材料涂层。
2.如权利要求1的方法，其中：
所述流体前体包括一种或多种甲基丙烯酸酯;
通过吹入干燥氮气或干燥空气到所述气体通道将过量的流体前驱体去除;
通过在真空烘箱中在至少100℃的温度和在1至10托的压强下烘烤所述气体通道，或通过保持所述气体通道在环境温度和压强下至少24小时，使所述流体前体的所述沉积层固化。
3.如权利要求1所述的方法，进一步包括在使所述流体前驱体流动之前，清洁所述内表面和干燥所述内表面。
4.如权利要求3所述的方法，其中：
用10至20wt.％的硝酸清洁所述内表面持续3分钟，并用去离子水冲洗所述内表面至少5分钟；以及，
通过吹入干燥的氮气或干燥的空气经过所述气体通道，并在真空烘箱中在至少120℃的温度下烘烤所述气体通道，使所述内部表面干燥。
5.如权利要求1所述的方法，其中，所述气体通道在具有0.25英寸或更小的外径的不锈钢管材中。
6.如权利要求5所述的方法，其中，至少一个不锈钢波纹管焊接到所述不锈钢管材中。
7.如权利要求6所述的方法，还包括：
在焊接所述波纹管到所述管材之前，用防止所述流体前驱体粘附的掩蔽剂涂布所述波纹管的所述内表面；以及可选地，在所述固化步骤后，从所述波纹管的所述内表面去除所述掩蔽剂。
8.如权利要求7所述方法，其中，所述掩模剂为光致抗蚀剂、油、硅烷和/或烷氧基硅烷。
9.如权利要求1所述的方法，其中，重复步骤(a)-(c)。
10.如权利要求1所述的方法，其中，所述涂层对含卤素的工艺气体有抗性。
11.如权利要求1所述的方法，其中，所述的耐腐蚀材料涂层具有0.0014至0.0034英寸的厚度。
12.一种配置成输送工艺气体到等离子体处理系统的腔室的气体输送系统，所述气体输送系统包括气体通道，其内表面涂布有通过将沉积在所述内表面的流体前驱体的层固化而形成的耐腐蚀材料涂层。
13.如权利要求12所述的气体输送系统，还包括焊接到其中具有所述气体通路的不锈钢管材的至少一个不锈钢波纹管，且所述波纹管的所述内表面未涂布所述涂层。
14.如权利要求12所述的气体输送系统，其中，所述气体通道是在具有0.25英寸或更小的外径的不锈钢管材中。
15.如权利要求12所述的气体输送系统，其中，所述涂层对含卤素的工艺气体有抗性。
16.一种包括如权利要求12所述的气体输送系统的等离子处理系统，其中，所述气体输送系统输送含卤素的工艺气体到所述等离子体处理系统的腔室中，并且激励所述工艺气体成等离子体以处理支架在所述腔室的单独半导体衬底。
17.如权利要求16所述的等离子体处理系统，其中，所述衬底由所述等离子体蚀刻。
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