CN101903560B - 用于电解质膜的溅射靶的方法 - Google Patents

用于电解质膜的溅射靶的方法 Download PDF

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CN101903560B
CN101903560B CN200880122197.9A CN200880122197A CN101903560B CN 101903560 B CN101903560 B CN 101903560B CN 200880122197 A CN200880122197 A CN 200880122197A CN 101903560 B CN101903560 B CN 101903560B
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B·纽德克尔
J·维特克瑞
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Phonex Corp
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Abstract

本发明提出了一种用于薄膜电解质的替代性溅射靶组合物或结构，从而使得溅射靶材料体系具有足够的电导率，可以使用(脉冲)DC靶能量进行溅射沉积。在由电导性溅射靶材料系统进行反应性溅射沉积之后，所述电解质膜材料获得了它们所需的电绝缘和可传导锂离子的性质。

Description

用于电解质膜的溅射靶的方法
相关申请
本发明涉及并根据35 U.S.C.§119要求2007年12月21日提交的题为″用于电解质膜的溅射靶的方法(METHOD FOR SPUTTER TARGETSFOR ELECTROLYTE FILMS)″的美国专利申请系列第61/016,038号的优先权，该申请全文通过参考结合入本文中。
技术领域
本发明涉及用于薄膜电化学能量存储和转化装置的锂离子薄膜电解质的制备。
发明背景
目前，人们使用射频(RF)激发(1MHz-1GHz)将锂离子电介质层与RF调谐器和RF匹配网络一起从陶瓷绝缘溅射靶沉积到溅射靶上。该方法的主要原因在于，可以将陶瓷靶的组成或化学计量比制成与待沉积的锂离子电解质层相同或至少非常类似。但是，由于使用陶瓷绝缘溅射靶和RF溅射法成本高，沉积面积和速率受到限制，其硬件复杂且存在困难，因此人们不希望使用陶瓷绝缘溅射靶和RF溅射法。
所述电绝缘类靶在溅射的时候通常需要使用RF激发。然而，当不使用RF激发的时候，例如使用直流电(DC)，脉冲DC(例如250kHz)或较低频率的交流电(AC；例如100kHz)激发的时候，靶的表面会显著充电，以电弧的形式将累积的电荷释放到基材、室壁和/或暗区屏蔽罩(dark space shield)。电弧放电可能过于剧烈，使得与溅射靶相连的电源无法防止该情况发生，这会对基材上的膜的生长造成不利影响，或者电源的保护性电子元件过于频繁地中断溅射过程，因而可能无法进行溅射沉积。不幸的是，溅射靶周围的全部RF电子元件都相当昂贵，而且需要真空沉积室以便适应RF。用于半导体制造的大部分大型溅射沉积装置仅仅适于直流电(DC)或脉冲DC。如果要设计和建造新的大型真空沉积室，会花费大量的时间和金钱，因为这样的室不是大量地建造和出售的。
RF溅射的另一个问题在于，对于氧化物电介质膜的沉积，陶瓷靶通常由多个较小的板条(tile)组成，这是因为在陶瓷靶的厚度(例如1/4英寸)适用于溅射工艺的前提下，制造大面积陶瓷溅射靶受到限制。另外，RF溅射所需的反应器相当复杂。具体来说，在RF系统中，对溅射阴极施加低电容高效RF功率分布的工程设计是相当困难的。低电容布设路径将电能输送到反应室的真空容器和从该真空容器返回的时候，经常以某种方式使得电能路径暴露，由此在匹配网络阻抗调谐的某些条件下，会发生等离子体扩散放电。
通常难以制造大面积、绝缘的陶瓷溅射靶，这是因为其组成板条尺寸(使用单个板条或多个板条)受到目前可行的陶瓷加工方法的限制(冷压加上随后的烧结，或者对合适的原料粉末进行热压)，这是因为在高速溅射沉积的热应力之下进行溅射的时候，对陶瓷溅射靶板条的性能有一定的要求。但是，由于陶瓷板条本身的脆性以及当其用于磁控管溅射靶时有限的实际厚度(对于实际应用，通常厚度约为1/2至1/4英寸)，其中磁控管的磁场必须能够良好地通过溅射靶板条的厚度，因此板条制造者们面临的困难任务是在靶板条的厚度受到限制的情况下，制造尽可能大的靶板条。因此，对于每种靶板条材料，靶制造者们在面积/厚度比上遇到了一个模糊限定的极限，若超出该极限，靶板条的制造产率将过低，无法用于商业。对于实际应用的性能良好的Li3PO4溅射靶板条，目前对厚1/4英寸的靶的板条尺寸极限为：直径约10英寸，或者对于非圆盘形的板条约为7英寸×7英寸。
经证实在高速溅射沉积中具有足够机械弹性的大面积绝缘陶瓷溅射靶，除了难以制造、甚至不可能制造以外，诸如局部带电/电弧放电，与其他区域串扰，电源和沉积环境之间严重、可变的阻抗失配这样的问题综合起来，使成熟的陶瓷溅射材料(例如Al2O3)的标称实际溅射靶面积极限约小于1000厘米2，而不太成熟的陶瓷材料(例如Li3PO4)的标称实际溅射靶面积极限约为500厘米2。
鉴于陶瓷板条制造以及与RF靶激发相关的问题，如果可能的话，人们希望从陶瓷靶板条转到金属靶板条，这是因为对于金属板条，需要进行必要的反应性溅射沉积，而厚度大约1/4英寸的大面积金属板更易于制造。使用金属靶代替陶瓷靶的另一个内在优点在于，延性高得多的金属靶可以在高得多的沉积功率和沉积速率下进行溅射，在溅射靶板条内产生强烈的温度梯度，由此金属靶板条处理起来比脆性的陶瓷板条容易得多。
大规模制造锂离子薄膜电化学储存和转化器件的经济性很大程度上依赖于特定生产输出量的基建投资，而生产输出量又受到沉积速率、沉积面积、沉积产率和设备开机时间的影响。关于这一点，所述必须使用较小的脆性陶瓷溅射靶或靶板条以及RF溅射靶激发的问题，会给将锂离子薄膜电化学存储和转化器件的生产工艺规模放大到工业水平带来显著的经济上的障碍。
为了避免RF溅射涉及的成本和装置问题，人们可以尝试使用DC或脉冲DC靶激发能量，由导电溅射靶溅射沉积所述电解质或电介质层。在此情况下，充电和电弧放电问题较少，通常是可以处理的。这两种DC溅射法都比RF更廉价，而且在真空沉积系统中更容易进行。但是，为了由导电性溅射靶获得电绝缘但是能够传导离子(此处为锂离子)的电解质或电介质层，人们不得不在活性气氛中溅射沉积靶材料，以得到具有正确化学计量比的电绝缘膜组成。在一些情况下，人们可以选择由合适的第二溅射靶，通过共溅射获得正确的膜化学计量比，而如果第二溅射靶是电绝缘的，则需要RF能量激发，如果第二溅射靶是导电的，则也可通过DC或脉冲DC激发来进行溅射。
在制造溅射沉积靶的领域中，并没有实质的记录提到在沉积制造具有电解性质的含锂的绝缘/介电膜的时候，可以采用DC或脉冲DC沉积。也没有大量的公开的工作专门提到可以使用替代的溅射靶组成或构形，对溅射的材料进行DC沉积，因在沉积的时候变成电绝缘的但可传导离子，该溅射材料变为电解质。不仅在锂离子方面，而且在所有的电解质方面，公开的信息或专利都是极少的。在此领域的公开的工作大都把注意力集中在如何增大靶的面积，或者如何改进硬件上。然而，本发明的动机是制造一种导电性靶组合物，该组合物可以使用DC或脉冲DC靶溅射能量来更廉价、更快捷地获得锂离子电解质薄膜。
美国专利申请第2006/0054496号揭示了一种通过DC溅射法由金属靶材料形成和沉积的氧化物和氧氮化物膜。但是，该专利将注意力集中在溅射器硬件上，而没有解决例如对靶的组成/结构进行改良，以促进溅射材料的DC沉积的问题，所述材料的物理气相沉积膜变为薄膜电解质。
美国专利第5,753,385号(″385专利″)使用锆和钇的金属溅射靶形成氧化物，所述氧化物可以在固体氧化物燃料电池中用作高温氧离子传导薄膜。尽管这些薄膜具有电解质性质，但是它们仅具有高温电解质性质，而且仅仅与阳离子有关。与之相对的是，本发明将注意力集中于例如常温锂离子电解质。形成氧离子电解质和锂离子电解质的相关化学参数和物理参数是有很大不同的。例如，高温氧离子电解质需要是晶态的，而本发明的锂离子电解质仅仅需要是玻璃态的或者无定形的。实际上，如果本发明的锂离子电解质在制造过程中或者之后其寿命中的任意时间是晶态的或者变成晶态的，则相关的锂薄膜电化学存储和转化器件便会被严厉地限制为仅能使用非金属锂离子阳极，这是因为金属锂阳极可能会由于晶体电解质内部的颗粒边界扩散，形成从阳极到阴极的电化学短路路径，使得锂薄膜电化学存储和转化器件短路。如果不存在(玻璃态或无定形的锂离子电解质)或基本不存在(纳米晶体锂离子电解质)颗粒边界，则不会导致不利的不希望出现的电化学短路路径的形成。″385专利之所以可以使用(高温氧离子)晶体电解质，主要是由于该燃料电池装置不会发生蠕变、不容易扩散、不会形成短路以及金属锂阳极。由于本发明与″385专利的目的和优点存在极大的区别，本领域普通技术人员无法例如想出一种方法，通过″385专利所用的非RF溅射沉积技术制造锂离子薄膜电解质。
美国专利第7,179,350 B2号揭示了一种混合方法，该方法经过最优化，用于反应溅射，使得磁控管头同时被DC和RF控制器驱动。但是，其注意力集中在溅射硬件的改良上，而不是对靶组成进行改良，以制造锂电解质膜。
尽管人们通过射频(RF)溅射沉积电池和燃料电池薄膜电解质已经有超过10年时间，但是在此发展过程中所用的设备相对较小：目前仅有用于研发或工业试生产的系统。当该种技术按比例放大到所需的(能够获得收益的)完全工业规模的时候，人们需要更为经济的设备以及较为节约成本的消耗品。因此，如果能够通过使用较大的金属靶和较为廉价的DC类溅射靶激发，更快更廉价地溅射沉积面积非常大的电解质和电介质层，将会是非常吸引人的，合适的方案将会在大规模生产中显著地节约时间和金钱。
发明内容
以下将会更详细地通过实施例描述本发明的各个方面和各种实施方式，这些方面和实施方式解决了背景技术中的某些缺陷，满足了相关领域的新需求。因此，本发明涉及例如溅射靶和用来形成溅射靶的方法，所述溅射靶和方法基本上解决了相关领域的局限性和缺陷造成的一个或多个缺点或问题。
在本发明中，当用术语″导电的″和“电绝缘的”描述材料的时候，它们可以分别与术语“传导电子的”和“电子绝缘的”互换使用。当使用这些术语描述一种材料的时候，既未排除也未包括所述材料还传导离子或不传导离子的情况。
薄膜电化学存储和转化装置包括电绝缘但是可传导离子(ionicallyconducting)的层，即所谓的电解质或电介质层。当溅射沉积这些层的时候，可以使用电绝缘的溅射靶或导电性溅射靶。本发明的薄膜电化学存储和转化装置使用锂离子电解质层(一种离子传导层)，其主要传导锂离子。
本发明实施方式的一个方面包括使用较为廉价的DC或脉冲DC法溅射沉积电绝缘但是可传导锂离子的膜(传导性陶瓷膜)，相比于更复杂、更昂贵的RF法，所述DC和脉冲DC法都可以在任意真空沉积装置/室内更简单、更可靠地进行。该DC或脉冲DC法使用导电性溅射靶，通过反应溅射沉积，将它们的组成转化为正确的膜化学计量比。
本发明实施方式的另一个方面涉及克服溅射靶尺寸(表面积和厚度)和/或多板条组成的溅射靶中溅射板条尺寸受到的实际限制，所述靶可以用来沉积所需的电绝缘的锂离子传导性电解质或电介质层。
本发明实施方式的另一个方面涉及金属靶一般高于相应陶瓷靶的热导性。这样就可以使用更厚的金属溅射靶，因为对于给定的溅射靶厚度，使用金属靶的时候，从受到冷却的靶背板通过溅射靶的整个主体对靶进行冷却要更为高效，同时金属板中的热梯度通常要小得多。使用较厚的金属靶带来的一个优点在于，较厚的溅射靶在需要更换之前可以操作更长的时间，因此维护的频率可以更小，缩短了生产设备的停机时间，从而降低了薄膜电化学存储和转化装置的生产成本。可能需要在靶厚度与溅射靶表面的磁控管作用之间寻找平衡点，以使得溅射设备的生产性能最优化。
附图简要说明
参照某些优选实施方式的附图描述了本发明的一些特征和优点，这些实施方式仅仅是用来举例说明，本发明并不受限于此。
附图用来帮助进一步理解本发明，它们结合在说明书中，构成说明书的一部分，显示了本发明的示例性实施方式，与说明书一起用来解释本发明的原理。附图中：
图1是根据本发明一个实施方式，可以用来制造用于薄膜电化学能量存储和转化装置的锂离子薄膜电解质的加工步骤流程图。
图2显示了在O2/N2反应性等离子体溅射羽流(plume)中，由Li3P溅射靶溅射沉积电解质膜的一个实施方式，其中基材浸没在所述反应性等离子体溅射羽流中，从而在所述基材上沉积电解质膜。
图3显示了由LixP相和Li2O相组成的复合溅射靶溅射沉积电解质膜的一个实施方式。
图4显示了图3的溅射沉积的实施方式，其中用Li3N代替Li2O。
图5显示了在基材上溅射沉积电解质膜的一个实施方式，所述基材浸没在由两个不同的溅射靶形成的两种等离子体中。
图6显示了在基材上沉积电解质膜的一个实施方式，其中所述电解质膜是通过同时将溅射沉积过程中的等离子体溅射羽流和电阻蒸发过程中的蒸气流引导到基材上而形成的。
图7显示了用于溅射沉积电解质膜的厚金属溅射靶的方法的实施方式。
优选实施方式详述
下面将结合附图所示的示例性实施方式更详细描述本发明的这些方面和其它方面。
应当理解，本发明不限于本文所述的这些特定的方法、化合物、材料、制造技术、应用以及用途，因为它们可以变化。还应当理解，本文所使用的术语仅仅是为了描述特定的实施方式，而不是为了限制本发明的范围。应注意到，本文和所附权利要求书所用的单数形式“一个”、“一种”和“这种”包括复数含义，除非另有明确说明。因此，例如，当描述″一个元件″的时候，表示一个或多个元件，包括本领域技术人员已知的等价形式。类似地，再例如，当描述″一个步骤″或″一种方式″的时候，可以包括一个或多个步骤以及一种或多种方式，可以包括子步骤和从属的方式。所有的连词应理解为包括最大范围的可能的含义。因此，词语″或″应理解为逻辑定义上的″或″，而不应理解为逻辑上″排它性的或″，除非上下文明确地有相反的描述。本文所述的结构应当理解为表示该结构的各种功能等价形式。除非另外有明确的说明，否则，对于可以理解为表达近似含义的语句，应当作如是理解。
除非另有说明，本文所用的所有科技术语具有本发明所属领域普通技术人员所理解的通常含义。本文中描述了优选的方法、技术、装置和材料，但是也可以使用与本文所述类似或等价的任何方法、技术、装置或材料来实施或测试本发明。本文所述的结构应当理解为还表示该结构的功能等价形式。除非说明书和权利要求书中有不同的说明，例如，术语″靶″和″靶板条″可以互换使用。
所有提到的专利和其它公开出版物都通过参考结合入本文中，用于描述和揭示地目的，例如，这种公开出版物中描述的方法可以用于本发明。本文提供这些出版物仅仅是由于其公开日早于本申请的申请日。应当注意，关于这一点，不应理解为本发明人承认自己不能借助在先发明或者其它理由而拥有早于这些公开内容的相关日期。
图1是用来制造用于本发明一些实施方式的薄膜电化学能量存储和转化装置的锂离子薄膜电解质的示例性方法100的一个实施方式。方法100包括制造步骤101，例如制造机械牢固的、基本具有传导性的溅射靶；步骤103，提供真空沉积室；步骤105，溅射所述机械牢固的、基本具有传导性的溅射靶；以及步骤107，在反应性溅射气氛中沉积所述锂离子薄膜电解质。
在步骤101中，根据本发明的实施方式，所述溅射靶是使用导电性的或至少半导电性的靶材料制造的，所述靶材料在室温下的电导率约大于10-4S/cm。对于本发明，室温下的电导率优选至少为10-8S/cm，最优选在室温下为1S/cm。通过为溅射靶选用合适的材料，并在反应性气体环境中进行操作，可以沉积电绝缘但是可传导锂离子的膜。该效果依赖于使用反应性溅射气体环境，从而使得喷射的靶材料互相反应以及与溅射等离子体中的中性组分和/或离子化组分的一些亚组反应，在基材上形成新的化合物。在步骤107中，在反应性溅射气氛中进行沉积可以将从锂离子传导性溅射靶溅射出来的材料转化为电绝缘并且可传导锂离子的电解质膜。在步骤107中，可能的气体组分包括以气态形式引入溅射反应器的氧、氮、氟、氯、溴、碘、硫、硒、碲、磷、砷、锑、铋、铅、碳、氢、硅、锂、钠、镁以及锆，它们可以为化学元素的形式或者化合物的形式。可能的靶组分包括锂、磷、氧、氮、氟、氯、溴、碘、硫、硒、碲、砷、锑、铋、铅、碳、氢、硅、镁和锆，以及以下材料：磷酸锂(Li3PO4)，氮化磷酸锂，磷化锂和亚磷化锂(LixP，其中1≤x≤100)，氮化锂和亚氮化锂(LixN，其中3≤x≤100)，氧化磷和亚氧化磷(POx，其中x≤2.5)，氮化磷和亚氮化磷(PNx，其中x≤1.7)，以及氧化锂和亚氧化锂(LixO，其中1≤x≤100)。还对材料体系进行选择，使得任何可能通过与溅射气体反应在靶表面上形成的绝缘膜不会显著阻碍随后的沉积。导致溅射的组分和气体组分转化为电解质膜的反应发生在正在沉积的膜的表面上。
通过使靶具有导电性，靶激发的种类不再限于RF能量。因此，在步骤103中，所提供的真空沉积室不再必须能够适应RF，否则将难以用于大型制造装置。类似地，相较于RF，步骤105中的溅射过程可以使用更廉价的DC或脉冲DC能量电子器件，以更高的速度进行。另外，相较于之前的RF法，步骤107中的沉积法可以更快、更廉价地完成。
根据本发明的一些实施方式，可以使用RF(1MHz至1GHz)、AC、脉冲DC和DC能量(单独使用，或者以各种组合结合使用)的任意组合来实施步骤103、105和107，以制备所需的膜。还有可能在步骤107中，使用非溅射技术，例如热蒸发、化学气相沉积或阴极电弧沉积，依次沉积一种以上的膜组分。所述非溅射的组分可以由电绝缘的来源或导电性来源沉积。后一种来源材料最优选包括在反应性气氛中(相对于来源材料的化学活性)进行沉积。
根据本发明的实施方式，步骤101中的溅射靶可以由单独的化合物制成，由多组分复合材料制成，或者由在靶的限制范围之内的具有显著不同组成的一系列靶板条制成。在所有的情况下，独立的板条部分优选大于300cm2。如果需要一个以上不同种类的靶来形成所需的膜，人们可以将基材的平移与任选的靶切换结合使用，以及/或者与来自多个溅射阴极的沉积结合使用，所述多个溅射阴极溅射出的物质同时朝向基材上生长的膜。本发明一个附加的优点在于，导电性的靶的热导性必然高于常规的电绝缘性的靶。所述热导率的增大使得可以使用较厚的靶(最高达5cm)(相较于之前较薄的靶(0.6cm))，从而减小了更换靶的频率(降低总体制造成本)。
提供以下实施例以帮助更进一步地理解本发明，这些实施例结合在说明书中，构成说明书的一部分，显示了本发明的示例性实施方式。
实施例1(图2)提供了方法100的示例性实施方式，它是对组成为Li3P的半导体靶201进行DC、脉冲DC、AC或RF反应性溅射，在基材207上沉积组成为Li2.9PO3.3N0.46的LIPON电解质膜205，所述沉积是在半导体靶浸没在溅射等离子体羽流203中的条件下进行的，所述等离子体羽流203包含溅射的材料以及氧气和氮气的反应性气体混合物，其中加入氩气之类的惰性气体，或者不加入惰性气体。O2/N2之比宜小于1/100，因为沉积的Li和P物质与氧的亲合性远高于与氮的亲合性。对于真空沉积反应器内的特定的氧/氮比(例如1/1000)，动力学和热力学因素都会决定生长的LixPOyN2膜的最终化学计量关系参数x、y和z。动力学参数包括靶溅射功率(例如对于直径为10英寸的Li3P，为2000W)、脉冲占空周期(例如通电2μs，然后断电2μs)、靶与基材的距离(例如，7.5cm)、沉积速率(例如，3μm/h)、基材温度(例如，150℃)、基材偏压(例如，-70V)、氮气流速(例如300sccm)，以及氧气流速(例如0.3seem，可以通过包含0.1体积％的O2的N2供气源间接建立)。与动力学参数相呼应，热力学因素，例如基材温度(温度是随溅射靶功率等因素变化的)以及生长膜表面处的氧气/氮气比，对生长的LIPON膜中的化学计量比具有重要影响。
实施例2(图3)提供了方法100的一个示例性实施方式，其中可以通过DC、脉冲DC、AC或RF反应性溅射，由复合靶301沉积组成为Li2.9PO3.3N0.46的LIPON电解质膜205，所述复合靶301由富含锂的LixP(x＞＞3)305和Li2O 307组成，具体来说是通过将LixP板条和Li2O板条以微米尺度或者以厘米尺度互相紧靠地复合而形成，使得当在溅射等离子体羽流303中对该靶进行溅射的时候，所得Li/P浓度比约为2.9，O/P比约为3.3，而N/P比约为0.46，所述溅射等离子体羽流303是至少包含氮气的反应性溅射等离子体羽流，其中添加氩气之类的惰性气体，或者不添加惰性气体。LixP(x＞＞3)305和Li2O 307的微观组成可优选为厘米尺度上的复合体，因为它提供了可以在DC或脉冲溅射条件下操作靶的溅射靶301的半导体性表面。
实施例3(图4)提供了方法100的一个示例性实施方式，其中溅射靶401用Li3N 407代替实施例2中的Li2O 307，由此制造的溅射靶401可以在至少包含氮气和氧气的等离子体羽流403中进行DC、脉冲DC、AC或RF溅射。
实施例4提供了方法100的一个示例性实施方式，其中溅射靶包含P2O5来代替实施例3(图4)中提供的LixP(x＞＞3)，由此制造的溅射靶可以在至少包含氮气的气氛中进行DC、脉冲DC、AC或RF溅射。
实施例5提供了方法100的一个示例性实施方式，其中溅射靶包含PN来代替实施例4中提供的P2O5，由此制造的溅射靶可以在至少包含氮气和氧气的气氛中进行DC、脉冲DC、AC或RF溅射。
实施例6提供了方法100的一个示例性实施方式，其中溅射靶由金属锂和PN的微观复合体制成，由此制造的溅射靶可以在至少包含氮气和氧气的气氛中进行DC、脉冲DC、AC或RF溅射。
实施例7(图5)提供了方法100的一个示例性实施方式，其中可以由至少两个独立的溅射靶201和501通过DC、脉冲DC、AC或RF反应性溅射沉积组成为Li2.9PO3.3N0.46的LIPON电解质膜205，所述两个溅射靶的溅射等离子体羽流503和503A都朝向基材207，在基材上生长Li2.9PO3.3N0.46电解质膜205。第一溅射靶201可以按照实施例1(图2)所述制造，而第二溅射靶501可以通过实施例5所述制造。为了在组成上改进膜的均一性，在厚度之类的其它所需的均一性特征以外，人们可以在组成略微不同的溅射等离子体羽流503和503A中，使基材207绕着其垂直轴505旋转。可以为真空沉积反应器添加第三个溅射靶，其组成与第一个靶相同或者与第二个靶相同，或者可以具有不同的组成，例如实施例6中提供的靶。
实施例8(图6)提供了方法100的一个示例性实施方式，其中通过实施例3(图4)提供的LIPON膜205的沉积可以通过非溅射沉积法600来进行，例如由合适的坩锅601(例如Ta)进行金属锂的电阻蒸发。朝向生长的LIPON膜205的锂蒸气603不仅调节了膜205中的锂浓度，而且改变了通过在包含氮气和氧气的气氛403和605中沉积锂而共同沉积入膜中的氧和氮的浓度。为了在组成方面改进膜的均一性，在厚度之类的其它所需的均一性特征以外，人们可以使基材207绕着其垂直轴505旋转。
实施例9提供了方法100的一种示例性的实施方式，其中通过实施例8提供的沉积可以包括开闭机构，由此可以暂时地中断溅射沉积或非溅射沉积数秒至几分钟，以便形成不同电活性层的层状叠置物，可以在沉积过程中或沉积之后，对LIPON膜进行热处理，使得这些层扩散入彼此之内，也可以不进行该扩散。
实施例10(图7)提供了方法100的一个示例性实施方式，其中溅射靶701由Li50Al50合金制造，在由溅射的材料和F2-Ar反应性气体混合物组成的溅射等离子体羽流703中进行DC、脉冲DC、AC或RF溅射沉积，形成玻璃态锂离子电解质LiAlF4705。所述Li50Al50是金属导体，可以在氩气之类的惰性气氛中通过标准冶金法制成最高达5厘米的厚度。溅射如此厚的靶701仍然是可能的，这是因为其具有高的热导性，使得可以通过靶背板709冷却711靶的后侧707。这种较厚的靶所需的更换频率小于较薄的靶，因此(i)缩短了真空沉积反应器的维护间隔期和(ii)降低了操作成本。
以上所述的实施方式和实施例仅仅是示例性的。本领域技术人员通过此处具体描述的实施方式能够想到各种变化，这些变化包括在本发明范围之内。因此，本发明的范围仅仅由所附权利要求书限制。因此，本发明意图覆盖对本发明的修改和变动，只要这些修改和变动在所附权利要求及其等同方案的范围之内即可。

Claims (25)

1.一种制造锂离子薄膜电解质的方法，该方法包括：
提供在室温下的电导率至少为10-8S/cm的导电性溅射靶；
提供真空沉积室；
对所述导电性溅射靶进行溅射；
在反应性溅射气氛中沉积锂离子薄膜电解质。
2.如权利要求1所述的方法，其特征在于，所述薄膜电解质包含氧氮化磷锂。
3.如权利要求1所述的方法，其特征在于，所述锂离子薄膜电解质包含选自以下的至少一种元素：氧，氮，氟，氯，溴，碘，硫，硒，碲，磷，砷，锑，铋，铅，碳，氢，硅，钠，镁和锆。
4.如权利要求1所述的方法，其特征在于，所述真空沉积室是不与RF相容的。
5.如权利要求1所述的方法，其特征在于，所述反应性溅射气氛包含选自以下的至少一种元素：氧，氮，氟，氯，溴，碘，硫，硒，碲，磷，砷，锑，铋，铅，碳，氢，硅，锂，钠，镁和锆。
6.如权利要求5所述的方法，其特征在于，所述方法还包括在溅射沉积工艺条件下，以气态化学元素的形式为所述反应性溅射气氛提供所述至少一种元素。
7.如权利要求5所述的方法，其特征在于，所述方法还包括在溅射沉积工艺条件下，以气态化化合物的形式为所述反应性溅射气氛提供所述至少一种元素。
8.如权利要求1所述的方法，其特征在于，所述导电性溅射靶包含选自以下的至少一种元素：氧，氮，氟，氯，溴，碘，硫，硒，碲，磷，砷，锑，铋，铅，碳，氢，硅，锂，钠，镁和锆。
9.如权利要求1所述的方法，其特征在于，所述导电性溅射靶包含选自以下的至少一种材料：磷化锂和亚磷化锂(LixP，其中1≤x≤100)，氮化锂和亚氮化锂(LixN，其中3≤x≤100)，氧化磷和亚氧化磷(POx，其中x≤2.5)，氮化磷和亚氮化磷(PNx，其中x≤1.7)，以及氧化锂和亚氧化锂(LixO，其中1≤x≤100)，以及元素态磷。
10.如权利要求1所述的方法，其特征在于，所述方法还包括用频率为1MHz至1GHz的射频(RF)能量为所述导电性溅射靶提供能量。
11.如权利要求1所述的方法，其特征在于，所述方法还包括用频率为1Hz至1MHz的交流电(AC)能量为所述导电性溅射靶提供能量。
12.如权利要求1所述的方法，其特征在于，所述方法还包括用直流电(DC)能量为所述导电性溅射靶提供能量。
13.如权利要求1所述的方法，其特征在于，所述方法还包括用脉冲直流电(脉冲DC)能量为所述导电性溅射靶提供能量。
14.如权利要求1所述的方法，其特征在于，所述方法还包括用RF、AC、脉冲DC和DC的组合组成的混合能量为所述导电性溅射靶提供能量。
15.如权利要求1所述的方法，其特征在于，所述导电性溅射靶在室温下的电子电导率大于10-4S/cm。
16.如权利要求1所述的方法，其特征在于，所述导电性溅射靶在室温下的电子电导率大于1S/cm。
17.如权利要求1所述的方法，其特征在于，所述方法还包括在基材表面处将所述导电性溅射靶材料转化为薄膜电解质材料。
18.如权利要求1所述的方法，其特征在于，所述方法还包括使用一个以上的导电性溅射靶沉积所述薄膜电解质。
19.如权利要求1所述的方法，其特征在于，所述方法还包括在生长膜区域上提供一个或多个非溅射沉积层。
20.如权利要求1所述的方法，其特征在于，所述方法还包括以周期性交替的方式在生长膜区域上提供一个或多个非溅射沉积层。
21.如权利要求19所述的方法，其特征在于，所述方法还包括由材料来源提供所述非溅射沉积，所述材料来源是电导性的或者电绝缘性的。
22.如权利要求1所述的方法，其特征在于，所述导电性溅射靶的厚度为0.6-5cm。
23.如权利要求1所述的方法，其特征在于，所述导电性溅射靶包含靶板条部分。
24.如权利要求23所述的方法，其特征在于，所述靶板条部分包含选自以下的至少一种元素：单相材料、多相材料、材料复合体。
25.如权利要求23所述的方法，其特征在于，所述靶板条部分中至少有一个部分大于300cm2。
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