CN102412420A - 图案化聚合物层的方法及封装微电池的方法 - Google Patents
图案化聚合物层的方法及封装微电池的方法 Download PDFInfo
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- CN102412420A CN102412420A CN2011102792020A CN201110279202A CN102412420A CN 102412420 A CN102412420 A CN 102412420A CN 2011102792020 A CN2011102792020 A CN 2011102792020A CN 201110279202 A CN201110279202 A CN 201110279202A CN 102412420 A CN102412420 A CN 102412420A
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- polymerization inhibitor
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- lithium
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Abstract
本发明提供图案化聚合物层的方法及封装微电池的方法。一种图案化布置在支撑件(4)上的聚合物层(22)的方法,该方法包括:在支撑件的第一区域(18a、18b)上沉积由基于锂的聚合抑制剂材料制成的层(16);在聚合抑制剂层以及支撑件的第二区域(18c)上沉积阳离子可聚合材料(20);进行聚合处理,从而在第一区域中形成未固化的牺牲层(20)且在第二区域中形成聚合物层(22);以及去除牺牲层(20)。
Description
技术领域
本发明涉及一种图案化支撑件上的聚合物层的方法,更具体地涉及一种利用聚合物层和屏障层封装微电池的方法。
背景技术
锂微电池通常由被电解质分离的两个电极(正极和负极)形成。锂微电池还包括由铂或者钨制成的金属的集流器(current collector)。正极由具有良好离子传导性的材料例如氧硫化钛(TiOS)制成。电解质是诸如锂磷氧氮(LiPON)的具有高离子传导性的电绝缘体。负极由金属锂或者锂化材料制成。
因为含锂的材料对空气极为敏感,尤其是对氧和湿气极为敏感,所以它们必须被惰性且密封的保护屏障覆盖。制作(mastering)封装是制约微电池随时间的效率的主要因素。
一种封装方案为在微电池上沉积较薄的层。这样,封装器件便包括布置在微电池上的由聚合物材料形成的第一层以及覆盖该第一层的由陶瓷或者金属材料形成的第二层。采用聚合物层的目的一方面是为了限制与基板粗糙度有关的缺陷,另一方面是为了在微电池使用期间适应微电池的变形。陶瓷或者金属材料层形成阻挡氧和湿气的保护屏障。
聚合物层通常旋涂在整个基板上,而屏障层利用物理气相沉积(PVD)或者等离子体增强化学气相沉积(PECVD)形成。
图案化封装器件主要采用两种技术。第一种技术采用掩模来定义图案。然而,会发生阴影及未对准效应,且该阴影及未对准效应引起了要被制造的图案的位置或尺寸的不精确性。这种阴影及未对准效应对小尺寸的微电池而言是至关重要的。于是,趋势是不再采用掩模,而是采用第二种技术,这第二种技术就是光刻。
图1示意性地示出了光刻操作,以形成布置在支撑件4上的微电池2的封装器件。封装器件包括预先沉积在整个微电池2及支撑件4上的聚合物层6和屏障层8。由光致抗蚀剂制成的蚀刻掩模10形成在封装器件上,然后,层6和8通过掩模10被蚀刻。该光刻操作还使得能够建立微电池的电连接,使位于微电池2端部的集流器12部分地暴露。
这种图案化技术不能保证对微电池的侧向保护。屏障层8实际上不覆盖微电池侧面(蚀刻侧面)的聚合物层6,如图1所示。由于聚合物层较低程度的保护,氧和水分易于扩散通过层6而损坏微电池2。
尽管对大尺寸的部件而言微电池的损坏主要发生于顶表面,但是对小尺寸的部件而言微电池的侧向保护变得很重要。因此,为了微型化,有必要用屏障层覆盖整个微电池以延长微电池的寿命。
光刻采用蚀刻溶液来蚀刻封装层6、8并采用清洗溶液来除去蚀刻掩模10。这些溶液也易于渗入微电池2而使微电池2损坏。还存在层6和8的过蚀刻,这进一步降低了对部件的侧向保护。最后,光刻包括大量的显著增加微电池制造方法的持续时间的步骤。
聚合物材料层通常通过旋涂容易地沉积在整个基板上,这就需要简单的方法来图案化这些层,尤其是图案化封装微电池的层。
发明内容
因此,需要提供一种用于图案化支撑件上的聚合物材料层的简单且快速的方法。
该需要旨在以这样的方式来得到满足:在支撑件的第一区域上沉积由基于锂的聚合抑制剂材料制成的层;在聚合抑制剂层以及支撑件的第二区域上沉积阳离子可聚合材料;使阳离子可聚合材料经受聚合处理,从而在第一区域中形成未固化的牺牲层且在第二区域中形成聚合物层;以及去除牺牲层。
本发明也提供了一种快速且易于实施的方法来封装布置在支撑件上的锂微电池,而且该方法也保证了微电池的侧向保护。
该封装方法包括:在支撑件上于微电池的周边沉积由基于锂的聚合抑制剂材料制成的层;在整个微电池以及聚合抑制剂层上沉积阳离子可聚合材料;使阳离子可聚合材料经受聚合处理,从而形成覆盖微电池的聚合物层并在微电池的周边形成牺牲层;沉积在聚合物层上形成保护屏障且覆盖整个微电池的层;以及去除牺牲层和聚合抑制剂层。
附图说明
根据下面对具体实施例的描述,其他优点和特征将变得更加显而易见,下面的具体实施例是出于非限制示例的目的被给出且由附图示出,附图中:
图1示出了根据现有技术利用光刻来图案化微电池的封装层;
图2到4示出了根据本发明实施例的图案化聚合物层的方法的步骤;
图5到10示出了利用图2到图4的方法封装微电池的方法的步骤。
具体实施方式
链式聚合(chain polymerization)是指以共价方式结合到一起的反应分子(通常为线性单体或预聚物)之间的化学反应。这种链式反应由引发剂启动。由于加热或紫外线辐照的作用,引发剂释放结合单体的活性中心。存在两种主要的聚合机理,自由基聚合(radical polymerization)或者阳离子聚合(cationic polymerization),这取决于这些活性中心的特性。
在自由基聚合中,活性中心为自由基,即具有一个或更多个未配对电子的化学物质(chemical species)。联苯甲酰以及偶氮二异丁腈(AIBN)是常用的引发剂。这种类型的聚合所涉及的单体例如是丙烯酸酯或甲基丙烯酸酯。
已知自由基聚合受空气中的氧抑制。空气固定在自由的自由基上而形成非活性的过氧化物基团。然而,可以通过采用敏化剂或者通过增加辐照强度来在存在氧的情况下进行自由基聚合。
阳离子聚合涉及自由离子或者可能涉及离子对作为活性中心。引发剂通常是质子酸(protonic acid),诸如硫酸或三氟甲磺酸(triflic acid)。与自由基聚合不同,阳离子聚合对氧不敏感。
另一方面,本发明的发明人发现:阳离子聚合在存在锂的情况下被抑制。含锂的材料事实上具有捕获作为聚合反应媒介(vector)的离子(活性中心)的能力。自此,这样的材料被称为聚合抑制剂。
建议利用这种现象来使阳离子聚合局部化,即通过在沉积可聚合材料之前沉积聚合抑制剂材料层来使阳离子聚合局部化。
图2到图4示意性地示出了利用基于锂的(lithium-based)材料的聚合物层图案化方法的实施例的步骤。
图2示出了在任何类型的支撑件4上沉积由基于锂的抑制剂材料制成的层16。例如,抑制剂材料制成的层16沉积于支撑件的两个分离区域18a和18b。抑制剂材料优选是金属形式的锂、锂磷氧氮(LiPON)、锂钛氧硫(LiTiOS)、二硫化锂钛(LiTiS2)或者五氧化二矾锂(LiV2O5)。金属锂例如通过真空蒸发而被沉积,而LiPON可以通过PVD而被沉积。层16的厚度优选在50nm到3μm之间变化。
然后,可聚合材料层20沉积在层16上,并且也沉积于支撑件4的在区域18a与18b之间的区域18c中。这种沉积优选通过旋涂而在整个片上进行,即在支撑件4的整个顶表面上进行。这样,层20的厚度依赖于旋转速度而在1μm到5μm之间变化。可以采用其他沉积方法,诸如丝网印刷、微分散或者喷洒(aspersion)。层20的厚度通常在1μm到5μm之间。
可聚合材料是指包括单体(或者预聚物)以及至少一种阳离子类型的引发剂的溶液。可以采用具有乙烯醚基的单体或者杂环单体(环氧化物、内酯、环醚、环氧硅氧烷...)。因为环氧化物单体以及乙烯醚反应性尤其显著,所以它们被优先使用,以便实现快速聚合。
市场上可买到的一些产品(一般称作可光聚合树脂或者热固树脂)包括这些单体,尤其是Epoxy Technology出售的“OG”产品(OG146-178、UVO-114、OG115、OG114-4、OG146...)以及“Epo-Tek”产品(Epo-Tek-301、Epo-Tek-354、Epo-Tek-305、Epo-Tek-H705...)均包括这些单体。
引发剂优选选自质子酸(H2SO4、CF3SO3H...)、无机卤化物(BF3、SnCl2...)、有机金属化合物(Al(CH3)3、Salen络合物...)以及有机盐(R3O+)。引发剂通常包含在上述树脂中。
在图3中,材料20经受聚合处理,以便使材料的引发剂产生离子来引发链式反应。材料20优选经受热处理(在热引发剂的情况下)或者暴露到辐照(在光引发剂的情况下)。例如,层20暴露到波长在300到600nm之间的紫外线辐照,持续时间小于10分钟,功率密度为约100mW/cm2。
在区域18a和18b中,层20的用于触发交联链(cross-linking chain)的离子大部分与基于锂的材料16的原子反应而不能引发聚合反应。因此,区域18a和18b中的层20保持原样或者被轻微聚合。另一方面,在不存在材料16的区域18c中,聚合反应正常地发生。于是,反应完成时便获得聚合物材料的图案22。
换言之,在此步骤中获得了具有性质不同的各部分的层:层16上方的未聚合或者轻微聚合部分以及其他区域的聚合部分。与材料16接触的未聚合部分可溶解于显影剂溶液中,而聚合部分则不溶于显影剂溶液。
未聚合部分在高度方向上可延伸达到约5μm(即,对于层20的5μm或者更小的厚度而言)且在横向达到约1μm(在层16的每侧通常在0.2到1μm之间)。
图4的步骤旨在去除区域18a和18b中保持原样的可聚合材料。该去除步骤优选利用水、溶剂或者诸如丙酮或乙醇的几种溶剂来进行。抑制剂材料层16可以同时被去除,以便在支撑件4上仅保留期望的图案22。
因此,这种方法能够以简单的方式形成聚合物材料层。与现有技术中的技术不同,这种方法精确、快速且容易被实施。这种方法尤其适合于微电子工业,更适合于采用聚合物层封装微电池。
图5到10示出了锂微电池封装方法的实施例的步骤。此优选实施例包括形成微电池。为了形成构成微电池的不同的层,可以采用掩模。以上描述的图案化方法使得能够形成布置在微电池上的封装器件。
图5示出了初始基板4,其包括由例如钛、钨或者金制成的阴极(cathodic)集流器12a和阳极(anodic)集流器12b。这些金属集流器以薄层(约200nm)的形式例如通过PVD被沉积。
然后,阴极24例如通过真空蒸发或者阴极溅射沉积在阴极集流器12a上。阴极由锂***材料(诸如氧硫化钛(TiOS),五氧化二矾(V2O5)或者二硫化钛(TiS2))的层形成。阴极具有约1.5μm的厚度。
在图6中,电解质层26,优选LiPON基电解质,沉积在阴极24上、部分阳极集流器12b上以及使集流器12a和12b分离的基板区域上。层26优选完全覆盖阴极24。沉积例如利用阴极溅射进行,以便获得厚度为约1.5μm的无缺陷的LiPON层。
聚合抑制剂材料的图案16形成在微电池周边。抑制剂材料16优选在基板4上沉积在电解质层26周围,以便形成与层26分离的封闭的周边图案。图案16优选覆盖集流器12a和12b的一部分,正如图6的截面图中所示出的。在此实施例中,与电解质26类似,图案16由LiPON制成,而且图案16的沉积与层26的沉积利用单个掩模同时进行。
图7的步骤对应于在层26上形成阳极28。阳极28优选由金属锂制成且利用真空蒸发来沉积。阳极28的厚度在1μm到3μm之间变化。然后,例如由钛、金、铝或者铜制成的金属层30沉积在阳极28的顶表面以及部分集流器12b上。由此,层30使得阳极28与阳极集流器12b之间能够建立电连接。此金属层能够降低锂层28的表面粗糙度。而且,与锂层28延伸到集流器12b相比,阳极电流传导被改善。
图8到10示出了微电池封装器件的制造步骤。封装器件包括布置在微电池上的聚合物类型的层6以及布置在聚合物层上的保护层8或者屏障层。
正如之前所描述的,聚合物层限制了与基板粗糙度相关的缺陷,以提高屏障层的保护效果。而且,聚合物层使充电和放电期间产生的微电池变形也能够被吸收。为此,优选采用具有高的机械柔性的绝缘聚合物。而且,还期望聚合物易于被施加且能够使微电池平坦化。而且,优选该聚合物具有热稳定性。事实上,微电池(以及其封装器件)在该微电池集成到外部装置期间可以经受温度为约260℃的热处理。
环氧化物基材料满足微电池技术的这些需求,尤其是以上所描述的由Epoxy Technology出售的产品。
图8示出了由可聚合材料层20在微电池上形成聚合物层6的步骤,如同参考图3所描述的。
层20优选通过旋涂沉积在整个片上。这样,材料20覆盖基板4、集流器12a和12b、图案16以及微电池。
通过使材料20经受聚合处理,材料固化以形成聚合物材料,除了位于微电池周边的由抑制剂材料形成的图案16的区域之外。这样,便获得了覆盖微电池大部分的所需的聚合物层6,且该聚合物层6由未聚合材料20围绕。
在图8的示例中,微电池的侧向区域32不被层6覆盖,因为材料20在此区域中直接接触电解质层26。LiPON层26实际上以与图案16相同的方式阻止材料20的聚合。然而,未被聚合物6覆盖的该区域32对微电池的保护无影响。微电池对化学物质(chemical species)的密封性由随后形成的屏障层8来确保,该屏障层8覆盖整个微电池。
图9示出了在聚合物层6以及微电池的未被聚合物覆盖的区域上沉积屏障层8。
层8的材料优选选自氧化硅、氮化硅、氮氧化硅以及氧化铝。屏障层8优选通过PVD、CVD或者ALD(原子层沉积)保形地沉积。屏障层8的厚度在50nm到300nm之间。
在此步骤中,材料8沿着由固相材料的各层限定的轮廓(也称为框架)而沉积。在图9的示例中,此框架由聚合物层6以及区域32中的电解质层26形成。未聚合材料20不属于该框架的任何一部分。
换言之,材料层8沉积在层6的顶表面上且在微电池的侧面处***固体层6与液体材料20之间或者固体层26与液体材料20之间。
这样,通过之前利用抑制剂材料形成聚合物层6,屏障层8沉积在微电池的侧面及顶表面。由此完成微电池的封装。
在图10中,未聚合的材料以及抑制剂材料利用显影剂被去除。LiPON层16和剩余材料20的去除例如可以通过利用磷酸溶液(H3PO4)来进行,然后用水进行清洗。
由于屏障层8覆盖整个微电池,所以显影和清洗溶液不会渗入微电池而使它损坏。而且,进一步地,使微电池的在基板前表面上的电连接便利化。由于抑制剂材料部分沉积在金属集流器12a和12b上,所以当进行显影时集流器实际上被释放。
参考图5到图10所描述的微电池的封装方法有利地包括在微电池形成期间沉积基于锂的抑制剂材料16。材料16和电解质26实际上都由LiPON制成且同时被沉积。然而,也可以在沉积由金属锂制成的阳极或者沉积由LiTiOS、LiTiS2以及LiV2O5制成的阴极的同时进行抑制剂材料的沉积。
在备选实施例中,在微电池已经形成在基板上之后进行抑制剂材料的沉积。于是,与之前描述的优选实施例相比,该沉积构成附加步骤。例如,当电解质由除LiPON之外的材料制成时、当阳极由除了金属锂之外的材料制成时或者当阴极由除了LiTiOS、LiTiS2以及LiV2O5之外的材料制成时,采用该备选实施例。
该封装方法快速且容易被实施。而且,与常规光刻操作相比,该封装方法包括的步骤被减少,且这些步骤与微电子技术相兼容。
Claims (10)
1.一种图案化布置在支撑件(4)上的聚合物层(6,22)的方法,该方法包括以下步骤:
在所述支撑件的第一区域(18a,18b)上沉积由基于锂的聚合抑制剂材料制成的层(16);
在所述聚合抑制剂层(16)上以及所述支撑件的第二区域(18c)上沉积阳离子可聚合材料(20);
使所述阳离子可聚合材料经受聚合处理,从而在所述第一区域中形成未固化的牺牲层(20)且在所述第二区域中形成所述聚合物层(6,22);以及
去除牺牲层(20)。
2.根据权利要求1所述的方法,其特征在于:所述聚合抑制剂材料(16)选自金属锂、LiPON、LiTiOS、LiTiS2以及LiV2O5。
3.根据权利要求1所述的方法,其特征在于:该方法包括在去除所述牺牲层(20)的同时去除所述聚合抑制剂材料(16)。
4.根据权利要求1所述的方法,其特征在于:所述阳离子可聚合材料(20)通过紫外线辐照或者通过热处理而被聚合。
5.根据权利要求1所述的方法,其特征在于:所述阳离子可聚合材料(20)包括环氧化物或者乙烯醚单体以及基于质子酸的引发剂。
6.一种封装布置在支撑件(4)上的锂微电池(2)的方法,包括以下步骤:
在所述支撑件上于所述微电池的周边沉积由基于锂的聚合抑制剂材料制成的层(16);
在整个所述微电池(2)以及所述聚合抑制剂层(16)上沉积阳离子可聚合材料(20);
使所述阳离子可聚合材料经受聚合处理,从而形成覆盖所述微电池(2)的聚合物层(6)并在所述微电池的周边形成未固化的牺牲层(20);
沉积在所述聚合物层(6)上形成保护屏障且覆盖整个所述微电池(2)的层(8);以及
去除所述牺牲层(20)以及所述聚合抑制剂层(16)。
7.根据权利要求6所述的方法,其特征在于:所述聚合抑制剂材料(16)选自金属锂、LiPON、LiTiOS、LiTiS2以及LiV2O5。
8.根据权利要求6所述的方法,其特征在于:该方法包括在所述支撑件(4)上形成所述微电池(2)。
9.根据权利要求8所述的方法,其特征在于:所述微电池(2)包括由金属锂、LiTiOS、LiTiS2、LiV2O5制成的电极(24,28),其中所述聚合抑制剂层(16)的沉积和所述电极的沉积同时进行。
10.根据权利要求8所述的方法,其特征在于:所述微电池(2)包括由LiPON制成的电解质(26),其中所述聚合抑制剂层(16)的沉积和所述电解质的沉积同时进行。
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FR1003726A FR2965110B1 (fr) | 2010-09-20 | 2010-09-20 | Procede de structuration d'une couche polymere et procede d'encapsulation d'une microbatterie |
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JP (1) | JP2012074373A (zh) |
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Cited By (4)
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CN105714277A (zh) * | 2014-12-03 | 2016-06-29 | 珠海方正科技多层电路板有限公司 | 干膜、电器元件的镀金属方法和电路板的线路制作方法 |
WO2017195058A1 (en) * | 2016-05-09 | 2017-11-16 | International Business Machines Corporation | Simplified hermetic packaging of a micro-battery |
CN111999979A (zh) * | 2020-07-31 | 2020-11-27 | 苏州太阳井新能源有限公司 | 一种非光刻图形化掩模的制造方法 |
CN112448022A (zh) * | 2020-11-25 | 2021-03-05 | 上海空间电源研究所 | 一种非对称电解质电池及其制备方法 |
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FR3009437B1 (fr) * | 2013-07-30 | 2015-09-18 | Commissariat Energie Atomique | Microbatterie au lithium protegee par un capot |
US10069138B2 (en) | 2014-04-24 | 2018-09-04 | Toyota Motor Engineering & Manufacturing North America, Inc. | Vanadium oxysulfide based cathode materials for rechargeable battery |
US9711793B2 (en) | 2014-04-24 | 2017-07-18 | Toyota Motor Engineering & Manufacturing North America, Inc. | Vanadium oxysulfide based cathode materials for rechargeable battery |
FR3023418B1 (fr) * | 2014-07-01 | 2016-07-15 | I Ten | Batterie entierement solide comprenant un electrolyte en materiau polymere solide reticule |
FR3027737B1 (fr) | 2014-10-22 | 2016-12-09 | Commissariat Energie Atomique | Dispositif electrochimique, tel qu'une microbatterie ou un systeme electrochrome, et son procede de realisation. |
JP2017182945A (ja) * | 2016-03-29 | 2017-10-05 | Tdk株式会社 | 全固体リチウムイオン二次電池 |
FR3080957B1 (fr) | 2018-05-07 | 2020-07-10 | I-Ten | Electrodes mesoporeuses pour dispositifs electrochimiques en couches minces |
CN114300742B (zh) * | 2021-12-28 | 2023-07-25 | 华中科技大学 | 一种固态电解质及其制备方法、锂离子电池及制备方法 |
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CN105714277A (zh) * | 2014-12-03 | 2016-06-29 | 珠海方正科技多层电路板有限公司 | 干膜、电器元件的镀金属方法和电路板的线路制作方法 |
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US8962080B2 (en) | 2015-02-24 |
EP2432065A1 (fr) | 2012-03-21 |
JP2012074373A (ja) | 2012-04-12 |
US20120070588A1 (en) | 2012-03-22 |
EP2432065B1 (fr) | 2014-01-01 |
KR20120030323A (ko) | 2012-03-28 |
FR2965110A1 (fr) | 2012-03-23 |
FR2965110B1 (fr) | 2012-09-28 |
ES2451370T3 (es) | 2014-03-26 |
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