CN111770907A - 用于操控锂金属的工具的涂层、工具和用于制造这种工具的方法 - Google Patents

用于操控锂金属的工具的涂层、工具和用于制造这种工具的方法 Download PDF

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CN111770907A
CN111770907A CN201980015265.XA CN201980015265A CN111770907A CN 111770907 A CN111770907 A CN 111770907A CN 201980015265 A CN201980015265 A CN 201980015265A CN 111770907 A CN111770907 A CN 111770907A
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lithium
tool
coating
lithium metal
metal
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D.A.韦伯
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Volkswagen AG
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Abstract

本发明涉及一种用于操控锂金属(3)的工具(1、4、5)的涂层(2)，所述涂层包含排斥锂的材料。此外，本发明还涉及一种具有这种涂层(2)的工具(1、4、5)和用于制造这种工具(1、4、5)的方法(6、7)。

Description

用于操控锂金属的工具的涂层、工具和用于制造这种工具的 方法
本发明涉及一种用于操控锂金属的工具的涂层，所述工具优选被应用于可反复充电的锂电池以及基于锂的超级电容器、例如混合动力车或电动车的锂电池以及基于锂的超级电容器的研发和生产。此外，本发明还涉及一种用于操控锂金属的工具以及用于制造这种工具的方法。
鉴于在汽车领域中对高效电池和超级电容器、尤其对高效高压电池不断提升的关注，锂金属的重要性也不断提高。然而，锂金属无论是以颗粒还是以薄膜形式在几乎所有材料表面上都发生粘附，甚至也粘附在传统的涂层上，如其在文献DE 10 2005 017 459 A1、DE 10 2010 011 185 A1和DE 10 2010 040 430 A1中所述。因此，难以进行处理，尤其例如通过轧制、压印、冲制等完成的加工。
为了简化对锂金属的处理，迄今在锂金属中加入添加剂或对锂金属本身进行化学改性、例如氟化，如在文献US 2007/0006680 A1中所述。此外，尤其在轧制时使用润滑剂。此外，如文献EP 0 692 831 B1所述，可以使用由聚缩醛制成的轧制筒，在所述轧制筒上仅小程度地出现锂的粘附。其他解决方案规定了锂在纸质或树脂或聚合物基材上的层压(键合)，以便改进可处理性并且尤其简化冲制。
所有迄今已知的解决方案都包含辅助材料或添加剂的使用，辅助材料或添加剂必须被繁琐地干燥或本身首先提纯到充足的纯净度。此外，有时还形成明显数量的废料(如在层压情况下)，所述废料又必须在将锂引入电池单体结构中之后被弃除。
由于将来在下一代电池和超级电容器型号中使用极薄的锂金属箔，所期待的锂金属箔的制造和处理的方法应减少或完全克服所述技术问题。
本发明所要解决的技术问题在于，提供一种用于操控(Handhabung)锂金属的工具的涂层、一种工具和用于制造所述工具的方法，其至少部分克服上述弊端。
所述技术问题通过根据权利要求1所述的用于操控锂金属的工具的涂层、根据权利要求5所述的工具和根据权利要求10所述的用于制造所述工具的方法解决。
根据第一方面，本发明涉及一种用于操控锂金属的工具的涂层，所述涂层包含排斥锂的材料。
根据第二方面，本发明涉及一种用于操控锂金属的工具，其中，所述工具的工具表面设有根据第一方面的涂层。
根据第三方面，本发明涉及一种用于制造根据第二方面的用于操控锂金属的工具的方法，所述方法包括：
提供排斥锂的材料；
将所提供的排斥锂的材料敷设在工具的工具表面上；并且
对敷设有排斥锂的材料的工具进行热处理。
本发明的其他有利的设计方式由对以下借助本发明的优选实施例的描述给出。
本发明涉及一种用于操控锂金属的工具的涂层，所述工具优选被应用于可反复充电的锂电池和/或基于锂的超级电容器、例如用于混合动力车或电动车的可反复充电的锂电池和/或基于锂的超级电容器的研发和生产，所述锂电池例如是锂金属电池、锂离子电池、锂硫电池、锂氧电池、锂空气电池、锂石墨烯电池、锂碳电池、锂碳纳米管电池、固液电解质混合电池和/或固体电池。所述工具可以例如包括用于运输、加工和/或存储锂金属的工具。锂金属可以在操控时以箔形式、液体形式、作为粉末或以其他形式存在。
锂金属可以由氯化锂获得。锂金属例如可以通过由氯化锂和氯化钾构成的低共熔混合物的熔融电解或通过氯化锂的电解获得。锂金属在获得之后被继续加工，例如被加工成型为箔、液化或粉末化。
根据本发明的用于操控锂金属的工具的涂层包含排斥锂的材料。所述涂层尤其由排斥锂的材料或包含排斥锂的材料的混合物制成。排斥锂的材料优选是所谓的疏锂材料，所述疏锂材料不与锂互混并且阻止与锂的接触。也就是说，排斥锂的材料即使在与锂接触时也试图尽快消除与锂的接触。锂金属和疏锂材料之间的关系与水和疏水材料之间的关系相类似，其中，水通常在疏水材料滚落而不附着在疏水材料上。
根据本发明的涂层由此避免锂金属粘附在相应的工具上，并且由此允许在不使用添加剂或其他助剂的情况下锂金属本身能够在高压下被加工。
在一些实施方式中，排斥锂的材料可以包含导锂陶瓷或者是导锂陶瓷。普遍而言的陶瓷和具体的导锂陶瓷可以被加工，从而使其构成非常光滑的表面，由此可以进一步降低例如锂金属的粘附。
在一些实施方式中，导锂陶瓷可以包含导锂的石榴石类的陶瓷或者是导锂的石榴石类的陶瓷。已知导锂的石榴石在大气中的一定停留时间后在表面上形成碳酸锂，所述碳酸锂引发强疏锂性质、也即排斥锂的性质。其结果是锂金属不再发生粘附。
在一些实施方式中，导锂的石榴石类的陶瓷可以包含锆酸镧锂(Li7La3Zr2O12)或者是锆酸镧锂(Li7La3Zr2O12)。锆酸镧锂具有高达1200℃的耐热性，非常坚硬，并且在大气中在表面上形成碳酸锂。锆酸镧锂由此能够实现锂金属本身在高压和高温下的加工。
其他导锂的石榴石的示例包括但不限于：Li3相锂石榴石(例如Li3CTe2O12，其中，C是镧系元素、诸如Y、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Zr、Ta或上述元素的组合，和/或Li3+xNd3Te2-xO12，其中，x＝0.05至1.5)、Li5相锂石榴石(例如Li5La3M1 2O12，其中，M1＝Nb、Zr、Ta、Sb或上述元素的组合，阳离子置换的Li5La3M1 2O12，诸如Li6ALa3M1 2O12，其中，A＝Mg、Ca、Sr、Ba或上述元素的组合，和/或Li7La3B2O12，其中，B＝Zr、Sn或上述元素的组合)、Li6相锂石榴石(例如Li6DLa2M3 2O12，其中，D＝Mg、Ca、Sr、Ba或上述元素的组合，而且M3＝Nb、Ta或上述元素的组合，阳离子掺杂的Li6La2BaTa2O12和/或阳离子掺杂的Li6BaY2M1 2O12，其中，掺杂阳离子是钡、钇、锌或上述元素的组合)、Li7相锂石榴石(例如立方晶型的Li7La3Zr2O12和/或Li7Y3Zr2O12，)、阳离子掺杂的Li7La3Zr2O12、Li5+2xLa3Ta2-xO12，其中，x＝0.1至1，Li6.8(La2.95Ca0.05)(Zr1.75Nb0.25)O12(LLCZN)、Li6.4Y3Zn0.4Ta0.6O12、Li6.5La2.5Ba0.5TaZrO12、Li6BaY2M1 2O12、Li7Y3Zr2O12、Li6.75BaLa2Nb1.75Zn0.25O12和/或Li6.75BaLa2Ta1.75Zn0.25O12。导锂的石榴石的其他示例包含立方晶型的化合物、例如3mol％的YSZ掺杂Li7.06La3Zr0.94Y0.06O12和8mol％的YSZ掺杂Li7.16La3Zr0.94Y0.06O12。
导锂的石榴石的其他示例包含但不限于：Li5La3Nb2O12、Li5La3Ta2O12、Li7La3Zr2O12、Li6La2SrNb2O12、Li6La2BaNb2O12、Li6La2SrTa2O12、Li6La2BaTa2O12、Li7Y3Zr2O12、Li6.4Y3Zr1.4Ta0.06O12、Li6.5La2.5Ba0.5TaZrO12、Li7Y3Zr2O12、Li6.75BaLa2Nb1.75Zr0.25O12和/或Li6.75BaLa2Ta1.75Zr0.25O12。
作为备选，排斥锂的材料还可以包含碳酸锂的涂层或者是碳酸锂的涂层。如上所述，碳酸锂是强烈疏锂的，并且有效阻止了金属的粘附。然而应在由碳酸锂制备涂层时省去烧结，这是因为碳酸锂在通常的烧结温度下会释出CO2并且会降低碳酸锂的疏锂性质。取代烧结，可以实施在较低温度下的热处理。
作为备选，涂层的排斥锂的材料可以包括未涂层的碳纤维和/或铜或者由其制成。无论是未涂层的碳纤维还是铜都具有疏锂性质。
此外，本发还涉及一种用于操控锂金属的工具，其中，所述工具的工具表面设有涂层，所述涂层包含排斥锂的材料、尤其导锂陶瓷、例如锆酸镧锂或碳酸锂。所述工具尤其具有如上所述的涂层。锂金属的操控可以包括锂金属的抓取、加工、存储和/或对锂金属的其他处理。所述工具优选在敷设有涂层的区域中具有金属材料、例如钢、尤其奥氏体钢或其他合金。作为备选，工具也可以在该区域中具有非金属的材料，该材料是耐热的，这是因为涂层的涂覆优选包括烧结步骤。
根据本发明的工具允许便捷地操控(或者说搬运)锂金属，因为其涂层有效避免锂金属的粘附。根据本发明的工具由此适用于加工锂金属的所有生产段、尤其用于具有锂金属阳极的电池或超级电容器的所有产品的生产段，并且适用于研究和研发设备。
在一些实施方式中，所述工具可以是抓取工具、例如镊子、钳子等。作为备选，所述工具可以是用于加工、例如轧制的工具、冲制工具、压印工具、压机、刀具、刀刃、搅拌工具、漏斗、尖端、挤出机等。工具的涂层可以降低或者甚至避免锂的粘附，并且例如在抓取或加工锂箔、尤其厚度在10μm至35μm范围内的锂箔时减少凹槽和微孔的形成，其中，可以完全摒弃润滑剂、添加剂等的使用。作为备选，工具可以是用于存储的工具、例如容器、放置板、用于堆叠电池单体的真空抽吸机等。作为备选，工具还可以包括输送带的链节或轧光机。所述涂层又可以降低或甚至避免在工具上的粘附。
在一些实施方式中，在操控锂金属时与锂金属发生接触的所有工具表面都设有所述涂层。在镊子和钳子中，优选可以为两臂的尖端在其相互面对的内侧上和必要时在其外侧上设置涂层。在辊子中，可以为轧制筒的至少一个周向面(所述周向面优选可以由奥氏体钢制成)和必要时轧制筒的两个端侧设置涂层。在冲制工具中，可以为冲头涂覆涂层。类似地，在操控锂金属时与锂金属发生接触的其他工具的表面可以被所述涂层涂覆。
在一些实施方式中，涂层可以具有0.5μm至10μm范围内的厚度、尤其1μm至5μm范围内的厚度。具有该厚度的涂层是有耐受力的并且降低锂金属的粘附。
在一些实施方式中，设有涂层的工具表面可以具有小于2μm、尤其小于1μm、优选小于0.5μm的平均粗糙度。通过涂层或者说工具表面的更低的粗糙度能够进一步降低锂金属的粘附。此外，还降低了锂、尤其锂箔受损的风险。具有粗糙度较低的涂层的辊子尤其实现了薄锂箔、尤其厚度在5μm至50μm、优选10μm至35μm范围内的锂箔的制造。
根据本发明的工具实现了锂金属的便捷操控，并且省去了在现有技术中已知的润滑剂、基材或化学改性的使用。
此外，本发明还涉及一种制造用于操控锂金属的工具的方法、尤其用于制造上述工具的方法，所述工具的工具表面设有涂层，所述涂层包含排斥锂的材料。
根据本发明的制造方法包括提供排斥锂的材料、尤其导锂陶瓷、例如锆酸镧锂或碳酸锂。在此，排斥锂的材料例如可以为了稍后的浸涂而分散成悬浊液，或者为了稍后的粉末涂层而被粉末化，并且与粘合剂互混。
此外，所述制造方法还包括将被提供的排斥锂的材料敷设在工具的工具表面上。为此，可以使用浸涂，其中，工具的表面、尤其在操控锂金属时与锂金属发生接触的工具表面浸入带有悬浊分散的排斥锂的材料的溶液中。例如镊子的尖端、辊子的轧制筒或压印工具的冲头可以浸入溶液中。作为备选，可以使用粉末涂层，其中，工具的表面、尤其在操控锂金属时与锂金属发生接触的工具表面被喷涂由排斥锂的材料和粘合剂组成的混合物。例如镊子臂的尖端、辊子的轧制筒或压印工具的冲头可以被所述混合物喷涂。
也可以考虑借助物理沉积方法的涂层。例如排斥锂的材料可以借助气化渗镀、离心涂镀或借助阴极雾化(溅射)被敷设在工具表面上。
脉冲激光沉积被认为对于导锂的石榴石是合适的。在此，优选将材料压制成靶材，并且随后利用激光在真空室中沉积在工具表面上。
此外，所述制造方法还包括对敷设有排斥锂的材料的工具进行热处理。当排斥锂的材料是导锂陶瓷、例如锆酸镧锂时，热处理可以是烧结工艺。当排斥锂的材料是碳酸锂时，在低于400℃的温度下实施谨慎的热处理。
现在示例性地且借助附图描述本发明的实施例。在附图中：
图1示意性示出呈辊子形式的根据本发明的工具的第一实施例；
图2示意性示出呈镊子形式的根据本发明的工具的第二实施例；
图3示意性示出呈冲制工具形式的根据本发明的工具的第三实施例；
图4示出用于制造呈辊子形式的根据本发明的工具的第一方法的流程图；并且
图5示出用于制造呈辊子形式的根据本发明的工具的第二方法的流程图。
图1示出用于由锂金属制造厚度为10μm至35μm的箔(薄锂箔3‘)的轧制设备1的示意图。轧制设备1具有两个由奥氏体钢制成的轧制筒10，所述轧制筒的周向面11涂覆了由锆酸镧锂制成的涂层2。通过与大气的接触在涂层2的表面上形成由碳酸锂制成的薄膜(未示出)，所述薄膜具有排斥锂的作用。由碳酸锂制成的薄膜的表面构成在轧制时直接与锂金属形成接触的辊子面12，并且构成易于无意地与锂金属发生接触的周边区域。
轧制筒10利用其纵轴线13相互平行地定向。轧制筒10的纵轴线13之间的距离A是可调节的，从而使得辊子面12之间的最小距离B适用于由厚度约为200μm的厚锂箔3轧制成厚度在10μm至35μm范围内的薄锂箔3‘。
通过涂层2避免了薄锂箔3‘粘附在辊子表面13上。由此可以直接在轧制之后将薄锂箔顺利地从辊子面上取下。辊子1可以使用传统的轧制筒，所述轧制筒随后仅设有由锆酸镧锂制成的涂层。
图2左侧示出用于冲制锂箔3的冲制工具4在冲制之前的情况，而右侧示出在冲制之后的情况。冲制工具4包括冲头40，其带有两个顶芯状的冲制尖端41和固持件42，所述固持件承载冲头40。冲制尖端41的表面敷设有由锆酸镧锂制成的涂层2。通过与大气的接触在涂层2的表面上构成由碳酸锂制成的薄膜(未示出)，所述薄膜具有排斥锂的作用。由碳酸锂制成的薄膜的表面构成在冲制时直接与锂金属形成接触的冲制面43，并且构成易于无意地与锂金属发生接触的周边区域。
为冲制锂箔3，冲制工具4相对于平面延展的锂箔3垂直地向其运动(箭头C)，并且带有涂层的顶芯状的突起41的尖端44切割锂箔3。随后，冲制工具4沿相反的方向(箭头D)从锂箔3离开并且在锂箔3中留下冲制图样30。
通过顶芯状的凸起41的涂层2可以避免锂箔粘附在顶芯状的凸起41上，并且避免在冲制工具4离开时损伤锂箔。冲头40可以使用传统的冲制冲头，所述冲制冲头随后设有由锆酸镧锂制成的涂层。
图3示出用于抓取锂箔3的镊子5。镊子5包括两个由不锈钢制成的臂50和使两个臂50在臂端部上连接的连接元件51。固持尖端52处于与连接元件5相对置的臂端部上，所述固持尖端的表面被由锆酸镧锂制成的涂层2涂覆。通过与大气的接触，在涂层2的表面上构成由碳酸锂制成的薄膜(未示出)，所述薄膜具有排斥锂的作用。由碳酸锂制成的薄膜的表面构成在抓取时直接与锂金属形成接触的固持面53，并且构成易于无意地与锂金属发生接触的周边区域。
通过涂层2避免在松开时锂金属粘附在镊子的固持面上。镊子5可以使用传统的镊子，所述镊子随后仅设有由锆酸镧锂制成的涂层。
轧制筒的、冲制冲头的和镊子的涂层都可以包括与锆酸镧锂不同的排斥锂的材料或者由其制成。
图4示出用于制造轧制筒的方法6的流程图，如在参照图1所示的轧制设备中所使用的轧制筒。
在步骤60中提供涂层的排斥锂的材料，在此为锆酸镧锂。为此将锆酸镧锂分散成悬浊液。
在步骤61中将由奥氏体钢制成的轧制筒的坯件浸入带有悬浊分散的锆酸镧锂的悬浊液中，从而使锆酸镧锂完全润湿坯件的周向面(浸涂)。
在步骤62中将用悬浊分散的锆酸镧锂润湿的轧制筒烧结，以便使涂层变硬且具有耐受力。
图5示出用于制造轧制筒的另一方法7的流程图，所述轧制筒被应用在参照图1所示的轧制设备中。
在步骤70中提供涂层的排斥锂的材料，在此为锆酸镧锂。为此将锆酸镧锂粉碎成粉末并且与粘合剂互混。
在步骤71中为轧制筒的周向面喷涂由排斥锂的材料与粘合剂组成的混合物(粉末涂层)，从而利用所述混合物均匀覆盖周向面。
在步骤72中将用由锆酸镧锂和粘合剂组成的混合物润湿的轧制筒烧结，以便使粘合剂燃尽以及使涂层变硬且具有耐受力。
所述方法6、7还可以类似地应用于其他工具、例如如图2所示的冲制冲头或如图3所示的镊子的制造。除了锆酸镧锂，也可以使用其他导锂陶瓷作为排斥锂的材料。
此外，还可以优化所述方法6、7，从而使用碳酸锂作为涂层材料。在此，烧结的步骤63、73被替换为在温度400℃下的谨慎的热处理。
附图标记清单
1 用于制造薄锂箔的轧制设备
10 轧制筒
11 轧制筒的周向面
12 辊子面
13 轧制筒的纵轴线
2 由锆酸镧锂制成的涂层
3 厚锂箔
3‘ 薄锂箔
30 冲制图样
4 用于冲制锂箔的冲制工具
40 冲头
41 顶芯状的冲制尖端
42 固持部
43 冲制面
5 镊子
50 臂
51 连接元件
52 固持尖端
53 固持面
6、7 用于制造轧制筒的方法
60、70 提供锆酸镧锂
61、71 敷设被提供的锆酸镧锂
62、72 烧结
A 轧制筒的纵轴线之间的距离
B 辊子面之间的最小距离
C、D 方向箭头，其表示冲制工具的运动方向

Claims (10)

1.一种用于操控锂金属(3)的工具(1、4、5)的涂层(2)，所述涂层包含排斥锂的材料。
2.根据权利要求1所述的涂层(2)，其中，所述排斥锂的材料是导锂陶瓷或碳酸锂。
3.根据权利要求2所述的涂层(2)，其中，所述导锂陶瓷是导锂的石榴石类的陶瓷。
4.根据权利要求3所述的涂层(2)，其中，所述导锂的石榴石类的陶瓷是锆酸镧锂。
5.一种用于操控锂金属(3)的工具(1、4、5)，其中，所述工具(1)的工具表面(11)设有根据权利要求1至4中任一项所述的涂层(2)。
6.根据权利要求5所述的工具(1、4、5)，其中，在操控锂金属(3)时与锂金属发生接触的所有工具表面都设有所述涂层(2)。
7.根据权利要求5或6所述的工具(1、4、5)，其中，所述工具是辊子(1)、镊子(5)、冲制工具(4)、尖端、搅拌工具、漏斗或容器。
8.根据权利要求5至7中任一项所述的工具(1、4、5)，其中，所述涂层(2)具有0.05μm至5μm范围内的厚度。
9.根据权利要求5至8中任一项所述的工具(1、4、5)，其中，所述设有涂层(2)的工具表面(11)具有小于2μm的平均粗糙度。
10.一种用于制造根据权利要求5至9中任一项所述的用于操控锂金属(3)的工具(1、4、5)的方法(6、7)，所述方法包括：
提供(60、70)排斥锂的材料；
将提供的排斥锂的材料敷设(61、71)在工具(1、4、5)的工具表面(11)上；并且
对敷设有排斥锂的材料的工具(1、4、5)进行热处理(62、72)。
CN201980015265.XA 2018-02-26 2019-02-20 用于操控锂金属的工具的涂层、工具和用于制造这种工具的方法 Pending CN111770907A (zh)

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