CN1130472C - 低蒸汽压化合物的等离子体增强化学沉积方法 - Google Patents

低蒸汽压化合物的等离子体增强化学沉积方法 Download PDF

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CN1130472C
CN1130472C CN98809599.8A CN98809599A CN1130472C CN 1130472 C CN1130472 C CN 1130472C CN 98809599 A CN98809599 A CN 98809599A CN 1130472 C CN1130472 C CN 1130472C
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J·D·阿菲尼托
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Abstract

本发明的设备通常为(a)闪蒸壳体(116)，该壳体带有一单体雾化器(120)，用于制备单体颗粒(122)、加热蒸发表面(124)，用于从单体颗粒制备蒸发物、和蒸发物出口(128)，联接于(b)辉光放电电极(204)，该电极从蒸发物产生辉光放电等离子体，其中(c)衬底(104)靠近辉光放电等离子体，以便在其上接受和冷凝辉光放电等离子体。本发明的方法具有下列步骤：(a)闪蒸液体单体，在蒸发物出口形成蒸发物；(b)使蒸发物通过辉光放电电极，从蒸发物产生辉光放电单体等离子体；以及(c)将辉光放电单体等离子体低温冷凝于衬底上，并使辉光放电等离子体交联其上，其中由辉光放电等离子体中产生的自由基导致交联，并达到自固化。

Description

低蒸汽压化合物的等离子体 增强化学沉积方法
发明领域
本发明总的涉及一种制造等离子体聚合膜的方法。具体而言，本发明涉及用闪蒸的低蒸汽压化合物的原料源经等离子体增强化学沉积以制造等离子体聚合膜。本文所用术语“(甲基)丙烯酸的”系指“丙烯酸的或甲基丙烯酸的”。本文所用术语“低温冷凝”及其形态系指当气体与温度低于气体露点的表面接触时气相转变为液相的相变物理现象。
发明背景
等离子体增强化学蒸汽沉积(PECVD)的基本方法叙述于“薄膜过程”，由J.L.Vossen，W.Kern编，Academie Press，1978，部分IV，章IV-1无机化合物的等离子体沉积，章IV-2辉光放电聚合，本文引为参考。大致说来，辉光放电等离子体产生在平滑的或有尖突物的电极上。按照传统，气体入口将高蒸汽压单体气体引入等离子体区，在其中形成自由基，致使其随后与衬底撞击，单体中的一些自由基在衬底上发生化学键合或交联(固化)。高蒸汽压单体气体包括CH4、SiH4、C2H6、C2H2或从高蒸汽压液体中产生的气体，例如苯乙烯(87.4°F(30.8℃)下为10乇)，环己环(60.4°F(15.8℃)下为100乇)，四甲基二硅氧烷(82.9°F(28.3℃)下的1，3二氯四甲基二硅氧烷为10乇)和它们的组合，它们能用温和的可控加热蒸发。由于这些高蒸汽压单体气体不易在室温或升温下低温冷凝，依靠自由基对相关表面的化学键合代替低温冷凝会使沉积速度低(最大只有零点几微米/分)。由于相关衬底被等离子体蚀刻对此问题的缓解使之可与低温冷凝相竞争。较低蒸汽压物质不能用于PECVD，因为将较高分子量的单体加热到足以使其蒸发的温度时通常会在蒸发之前引起反应或者使气体的计量难于控制，这二者都是不可行的。
闪蒸方法叙述于美国专利4,954,371中，本文引为参考。这种基本方法亦称为聚合物多层(PML)闪蒸。大体上，一种可辐射聚合和/或可交联的材料在低于该材料的分解温度和聚合温度的温度下供入。该材料雾化为微滴，该微滴尺寸界于1-50微米。通常采用超声雾化器。微滴然后在真空下与其温度高于该材料沸点但其温度又低于引起热解的加热表面接触以被闪蒸。蒸汽低温冷凝在衬底上，然后辐射聚合或交联为很薄的聚合物层。
该材料可包括基本单体或其混合物、交联剂和/或引发剂。闪蒸的缺点在于要求两个相连的步骤，低温冷凝后紧接固化或交联，而且两者在空间和时间上是分开的。
根据等离子体聚合膜制造的技术现状，PECVD和闪蒸或辉光放电等离子体沉积和闪蒸都未组合使用。但是据J.D.Affinito、M.E.Gross、C.A.Coronado和P.M.Martin在“聚合物电解质在柔性衬底上的真空沉积”中的报导，无机化合物辉光放电等离子体发生器已与低压气氛下(真空)的闪蒸组合用于衬底的等离子加工。文章发表于“第九届国际真空丝网涂复会议论文集”的全会报告中，1995.11.R.Baskin编，Baskin出版社1995，20-36页，并示于图1。在这个系统中，等离子体发生器100用于蚀刻移动衬底104的表面102，以便接受来自闪蒸106的单体气体流出物，单体气体在被蚀刻的表面102上低温冷凝，然后经过第一固化装置(末示)，例如电子束或紫外辐射，以引发交联和固化。等离子体发生器100具有壳体108、气体入口110。气体可以是氧、氮、水或惰性气体如氩、或它们的组合。在其内部，电极112是平滑的或具有一个或多个尖突物114，电极112产生辉光放电并使气体形成等离子体，等离子体蚀刻表面102。闪蒸器106具有壳体116、单体入口118和雾化喷嘴120，例如超声雾化器。流经喷嘴120的物流被雾化为颗粒或微滴122，它们撞击加热表面124，颗粒或微滴122在其上闪蒸为气体，该气体流经一系列挡板126(可任选用)至出口128并在表面102上低温冷凝。虽然采用过其它的气流分布装置，但发现挡板126能够提供适宜的气流分布或均匀度，同时可使表面102易于放大。固化装置(未示)位于闪蒸器106的下游。
因此，这里需要一种制造等离子体聚合层的设备和方法，其速度快且能自固化，无需固化装置。这种设备和方法将特别有利于制造PML聚合物层。
发明简述
本发明可从两方面来看，其(1)低蒸汽压单体材料用等离子体增强化学蒸汽沉积在衬底上的设备和方法，其(2)制造自固化聚合物层，特别是自固化PML聚合物层的设备和方法。从两方面来看，本发明是闪蒸和等离子体增强化学蒸汽沉积(PECVD)的组合，这种组合提供了一些出人意料的优点，它能在PECVD方法中应用低蒸汽压单体材料，并提供来自闪蒸方法的自固化，其沉积速率令人吃惊地快于标准PECVD的沉积速率。
一般说来，本发明的设备为(a)闪蒸壳体，其内部有用于制备单体颗粒的单体雾化器，用于将单体颗粒制成蒸汽的加热蒸发表面及蒸发物出口，(b)辉光放电电极，位于蒸发物出口下游，用于从蒸发物制备辉光放电等离子体，其中(c)衬底，它靠近辉光放电等离子体，用于接受辉光放电等离子体并使其衬底上低温冷凝。全部部件宜置于低压(真空)室中。
本发明的方法具有如下步骤：(a)闪蒸液体单体，在蒸发物出口形成蒸发物；(b)使蒸发物通至辉光放电电极，将蒸发物制成辉光放电单体等离子体；和(c)辉光放电单体等离子体在衬底上低温冷凝，并使辉光放电等离子体在其上交联，其中辉光放电等离子体中产生的自由基导致交联，并达到自固化。
本发明的一个目的在于提供一种组合闪蒸与辉光放电等离子体沉积的设备和方法。
本发明的一个目的在于提供一种制备自固化聚合物层的设备和方法。
本发明的另一目的在于提供一种制备自固化PML聚合物层的设备和方法。
本发明的还一目的在于提供一种低蒸汽压单体的PECVD沉积的设备和方法。
本发明的优点在于，它对衬底的移动方向是不敏感的，因为沉积的单体层是自固化的。在现有技术中，沉积的单体层需要辐射固化设备，以致衬底的移动应必须从沉积位置移向辐射设备。本发明的另一优点在于，可组合多层材料，例如，本文引作参考的美国专利5,547,508和5,396,644、5,260,095所列的多聚合物层、聚合物和金属的交替层和其它的层皆可用本发明在真空环境中制备。
本说明书结论部分具体和明确地对本发明的主题提出了权利要求，但是操作和编排方法两者及其其它优点和目的最好参阅下面的详细叙述结合附图来理解，其中相似的代码系指类似部件。
附图描述
图1是现有技术中无机化合物辉光发电等离子体发生器与闪蒸相组合的剖面图。
图2是本发明的闪蒸发和辉光放电等离子体沉积相组合的设备的剖面图。
图2a是本发明的设备的剖面端视图。
图3是本发明的以衬底作电极的剖面图。
优选实施方案描述
本发明的设备示于图2。本发明的设备和方法宜于在低压(真空)环境或室中实施。压力宜界于10-1乇-10-6乇。闪蒸器106拥有壳体116、单体入口118和雾化喷嘴120。经喷嘴120的物流雾化为颗粒或微滴122，颗粒或微滴122撞击加热表面124，并在其上颗粒或微滴闪蒸为气体或蒸发物，后者流经一系列挡板126至蒸发物出口128并低温冷凝在表面102上。防止在挡板126和其它内部构件表面上的低温冷凝的措施是将挡板126和其它内部构件表面加热到超过蒸发物的低温冷凝温度或其露点。虽然采用过其它的气流分布装置，但发现挡板126能提供适宜的气流分布和均匀度，同时易使表面102放大。蒸发物出口128将气体导向辉光放电电极204，使蒸发物生成辉光放电等离子体。在图2所示的实施方案中，辉光放电电极204置于辉光放电壳体200之中，壳体有蒸发物入口202，它靠近蒸发物出口128。在这个实施方案中，辉光放电壳体200和辉光放电电极204的温度保持在蒸发物露点以上。辉光放电等离子体流出辉光放电壳体200并在衬底104的表面102上低温冷凝。衬底104的温度宜保持在蒸发物露点以下，宜为室温或冷却至室温以下，以便提高低温冷凝速率。在这个实施方案中，衬底104是在移动，并可以是不导电的、导电的或经外加电压加上偏压，以便将带电粒子从辉光放电等离子体中引出。如果衬底104带偏压，它甚至可取代电极204，本身成为使单体气形成辉光放电等离子体的电极。基本上无偏压意味着未施加外电压，虽然可由于静电或由于与等离子体的相互作用会积累电荷。
辉光放电电极的一种优选形状示于图2a。在这个实施方案中，辉光放电电极204与衬底104是分开的，而且其形状使从蒸发物入口202来的物流基本上流经电极开口206。任何一种电极形状皆可用于形成辉光放电，但是电极204的优选形状不遮挡从出口202流出的蒸发物形成的等离子体，并且它相对于单体出口缝202和衬底104的对称关系提供在衬底宽度上蒸发物蒸汽流对等离子体的均匀性，同时横向宽度均匀性由衬底的移动来得到。
电极204与衬底材104形成的空间是能使等离子体撞击在衬底上的间隙或距离。等离子体从电极延伸出的这段距离将取决于蒸发的物质、电极204/底材104的几何、电压和频率以及压力，其标准方式详细叙述于“气体中的放电”，F.M.Penning，Gordon and Breach Seience出版社，1965，并摘要载于“薄膜方法”，J.L.Vossen、W.Kern编，科学出版社，1978，Part II，Chapter II-1，“辉光放电溅射沉积”，本文将两者均引此为参考。
一种适于间歇操作的设备示于图3。在这个实施方案中，辉光放电电极204与部件300(衬底)足够靠近，以致部件300成了电极204的延伸或组成部分。此外，该部件温度低于露点，以使辉光放电等离子体在部件300上低温冷凝，从而以单体冷凝物涂复部件300并自固化为聚合物层。足够靠近可以是与之连接、靠在其上直接接触或用能使等离子体撞击衬底的间隙或距离。等离子体从电极延伸出的这段距离将取决于蒸发的物质、电极204/底材104的几何、电压和频率以及压力，其标准方式叙述于“气体中的放电”，F.M.Penning，Cordon and Breach出版社，1965，本文引为参考。衬底300在低温冷凝过程中可处于静止或移动中。移动包括旋转和平移，并可以用于控制其上低温冷凝的单体层的厚度和均匀度。由于低温冷凝发生很快，在毫秒和秒之间发生，部件可在涂复之后和在超过涂复温度限值之前卸出。
操作中，不管是作为在衬底上进行低蒸汽压单体材料的等离子体增强化学蒸汽沉积方法，或者是作为形成自固化聚合物层(特别是PML)方法，本发明的方法具有下列步骤：(a)闪蒸液体单体，在蒸发物出口形成蒸发物；(b)使蒸发物通过辉光放电电极使蒸发物形成辉光放电单体等离子体；和(c)将辉光放电单体等离子体低温冷凝在衬底上，并将辉光放电等离子体交联其上。辉光放电等离子体中产生的自由基导致交联，从而能实现自固化。
闪蒸具有下列步骤：单体液体流入入口；单体液体经喷嘴雾化；和喷雾形成大量单体液体的单体颗粒。喷雾朝向在其上蒸发的加热蒸发表面，并通过蒸发物出口流出。
该液体单体可以是任何液体单体。但是，优选的单体材料或液体在室温下具有低蒸汽压，以致它易于低温冷凝。单体材料的蒸汽压在83°F(28.3℃)下宜小于10乇，优选在83°F(28.3℃)下低于1乇，最优选在83°F(28.3℃)下低于10毫乇。对于同一化学族的单体，低蒸汽压的单体通常亦具有较高的分子量，并比较高蒸汽压、较低分子量的单体易于低温冷凝。液体单体包括但不限于丙烯酸单体例如三丙二醇二丙烯酸酯、四甘醇二丙烯酸酯、三丙二醇单丙烯酸酯、己内酯丙烯酸酯及其组合；甲基丙烯酸单体；及其组合。(甲基)丙烯酸单体特别适于制造分子掺杂聚合物(MDP)，光发射聚合物(LEP)和光发射电化学电池(LEC)。
借助于采用闪蒸，单体很快蒸发，以致通常在从加热液体单体到蒸发温度之间发生的反应不再发生。此外，蒸发物供给速率严格地用进入闪蒸器106的进口118的液体单体的进料速率控制。
除了从液体单体产生的蒸发物外，在闪蒸器106中可以加入附加气体，该气体通过蒸发物出口128上游的气体入口130加入，优选在加热表面124和最靠近加热表面124的第一块挡板126之间加入。附加气体可以是有机的或无机的，其目的包括但不限于镇流、反应及其组合。镇流系指提供足够的分子，以便在低蒸发流量下保持等离子体点火。反应系指生成不同于蒸发物的化合物的化学反应。镇流气体包括但不限于周期表VIII族元素，氢、氧、氮、氯、溴、多原子气体包括例如二氢化碳、一氧化碳、水蒸气及它们的组合。一个示例性的反应是将氧添加到六甲基二硅氧烷中以得到二氧化硅。
实施例1
曾经进行了一个实验，以论证示于图2和上面所述的本发明。采用四甘醇二丙烯酸酯作液体单体。加热表面的温度设定在约650°F(343℃)。液体单体经内径为0.032英寸的毛细管引入入口。超声雾化器喷嘴的内径为0.051英寸。聚合物层的沉积速率对25微米厚聚合物层而言为0.5m/min，对1微米厚的聚合物层而言为100m/min。目检固化的聚合物层未发现任何针孔或裂痕。
结束语
尽管给出和叙述了本发明的优选实施方案，但对本专业技术人员来说，在不偏离本发明较宽的范围的前提下可作很多变更和修改。因此附录的权利要求试图概括在本发明的实质和范围内的所有这些变化和修改。

Claims (13)

1.一种用于在真空室中制造自固化聚合物层的设备，包括：
(a)闪蒸壳体，该壳体带有单体入口、单体雾化器，用于从该单体入口接受液体单体并制成单体颗粒、加热的蒸发表面，用于从该单体颗粒制备蒸发物、以及蒸发物出口；和
(b)辉光放电电极，该电极位于蒸发物出口25的下游，并从蒸发物制备辉光放电等离子体；以及
(c)衬底，用于在其上接受低温冷凝和交联辉光放电等离子体，辉光放电等离子体中产生的自由基导致交联，使其自固化。
2.权利要求1的设备，其中衬底靠近辉光放电电极，并由外加电压施加偏压。
3.权利要求1的设备，其中该辉光放电电极置于辉光放电壳体内部，该壳体具有靠近蒸发物出口的蒸发物入口，该辉光放电壳体和该辉光放电电极的温度保持在该蒸发物的露点以上。
4.权利要求1的设备，其中该闪蒸壳体具有置于加热表面和蒸汽出口之间的对立置放的挡板。
5.权利要求1的设备，还包括气体入口。
6.一种在真空室中用于制备自固化聚合物层的方法，包括：
(a)闪蒸低蒸汽压的液体单体为蒸发物；
(b)使蒸发物通过辉光放电电极，并从蒸发物制备辉光放电单体等离子体；和
(c)将该辉光放电单体等离子体低温冷凝在衬底上，作为低温冷凝单体，并使该低温冷凝单体交联于衬底上，该辉光放电等离子体中产生的自由基导致交联，使其自固化。
7.权利要求6的方法，其中衬底靠近辉光放电电极，并被外加电压施加偏压，接受冷凝其上的单体等离子体。
8.权利要求6的方法，其中该辉光放电电极置于辉光放电壳体内部，该壳体有靠近蒸发物出口的蒸发物入口，该辉光放电壳体和该辉光放电电极的温度保持在该蒸发物的露点以上，衬底位于该单体等离子体的下游，未施加外电压，虽然可由于静电或由于与等离子体的相互作用会积累电荷，用于接受冷凝其上的单体等离子体。
9.权利要求6的方法，其中该单体选自丙烯酸单体、甲基丙烯酸单体及其组合。
10.权利要求9的方法，其中该丙烯酸单体选自三丙二醇二丙烯酸酯、四甘醇二丙烯酸酯、三丙二醇单丙烯酸酯、己内酯丙烯酸酯及其组合。
11.权利要求6的方法，其中该衬底是经冷却的。
12.权利要求6的方法，其中，该低蒸汽压是在83°F(28.3℃)下小于10乇。
13.权利要求6的方法，其中辉光放电电极位于壳体中，而衬底位于单体等离子体的下游。
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CN107058982A (zh) * 2017-01-23 2017-08-18 无锡荣坚五金工具有限公司 一种具有多层结构防液涂层的制备方法
CN107058982B (zh) * 2017-01-23 2018-06-19 江苏菲沃泰纳米科技有限公司 一种具有多层结构防液涂层的制备方法

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US20010019747A1 (en) 2001-09-06
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US6627267B2 (en) 2003-09-30
CN1272142A (zh) 2000-11-01
US6656537B2 (en) 2003-12-02
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