CN110718691A - 采用半结晶粘合剂的高性能电极 - Google Patents
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Abstract
公开了用于具有半结晶粘合剂的电化学设备的高性能电极。形成电极的方法包括形成电极浆料,将电极浆料涂敷到集电器以形成电极,以及固化电极,从而形成半结晶粘合剂。电极浆料包括溶剂、半结晶粘合剂前体溶液、电活性材料、以及导电性填料。半结晶粘合剂包括电活性材料和通过其分散的导电性填料。半结晶粘合剂包括多个聚合物链。多个聚合物链的每个都包括与多个无定形位点一起散布的多个结晶位点。半结晶粘合剂能够形成氢键。
Description
引言
本公开涉及用于锂离子电化学设备的高性能电极,并且更具体地涉及用于优化锂离子电化学设备中的电极性能的半结晶粘合剂。
诸如锂离子蓄电池之类的高能量密度电化学电池可以用于各种消费产品,诸如包括膝上型电脑、平板电脑和蜂窝电话的移动设备和诸如混合动力电动车(“HEV”)和电动车(“EV”)的车辆等。
用于电化学电池的高性能电极具有明显的缺点。例如,具有含硅电活性材料的电极在充电-放电循环期间会经历大量的库仑衰减。充电-放电循环期间的体积变化可能会限制蓄电池的性能和/或寿命。
发明内容
虽然不受理论束缚,但是据信蓄电池的缩减性能和/或寿命通常是由于具有电活性材料的导电填料和集电器的物理接触的破坏,这是由电活性颗粒在充电-放电循环期间经历的体积变化引起的。虽然不受理论束缚,但是据信蓄电池的缩减性能和/或寿命也是由于在充电-放电循环期间体积变化期间电活性颗粒上的固体电解质中间相的破裂和重新形成。
根据本公开的系统和方法通过使用稳定的半结晶粘合剂提供了蓄电池的优化性能和/或寿命。半结晶粘合剂包括结晶相和无定形相。有利地,结晶相提供粘合剂的刚性和抵抗电活性颗粒膨胀的弹性,并且无定形相允许粘合剂在其收缩期间保持与电活性颗粒的物理接触。参考详细的描述将认识到由半结晶粘合剂提供的进一步益处。
根据本公开的方面,形成用于电化学电池的电极的方法包括形成电极浆料,将电极浆料涂敷到集电器,并且固化电极浆料,从而形成具有半结晶粘合剂的电极。电极浆料包括半结晶粘合剂前体溶液、电活性材料和导电性填料。半结晶粘合剂包括电活性材料和通过其分散的导电性填料。半结晶粘合剂包括多个聚合物链。多个聚合物链的每个都包括与多个无定形位点一起散布的多个结晶位点。多个结晶位点的每个通过重复聚合物链的链段之间的相互作用来限定。
根据本公开的进一步方面,半结晶粘合剂前体溶液包括第一单体和第二单体,对该第一单体和该第二单体进行选择以产生聚合物链,该聚合物链具有基于聚合物链中原子的至少25原子%的芳香性和配置成与每个重复单元中的相邻聚合物链形成氢键的至少一个位点。
根据本公开的进一步方面,半结晶粘合剂前体溶液是通过结晶芳族聚酰胺处理所获得的无定形芳族聚酰胺。该处理包括将结晶芳族聚酰胺溶解在含盐有机溶液中从而形成溶液,用水处理该溶液从而形成无定形芳族聚酰胺,并且将无定形芳族聚酰胺溶解在纯有机溶液中以产生无定形芳族聚酰胺溶液。
根据本公开的进一步方面,结晶芳族聚酰胺通过将第一单体与第二单体混合并使该第一单体和该第二单体聚合来形成以形成结晶芳族聚酰胺。对第一单体和第二单体进行选择以产生聚合物链,该聚合物链具有基于聚合物链中原子的至少25原子%的芳香性和配置成与相邻聚合物链形成氢键的至少一个位点。
根据本公开的进一步方面,多个聚合物链的每个都包括基于相应聚合物链内原子的大于约25原子%的芳香性和提供物理交联并与活性材料表面形成良好粘附性的多个氢键。
根据本公开的进一步方面,每个聚合物链包括基于相应聚合物链内原子的大于约15原子%的量的氢。
根据本公开的进一步方面,半结晶前体由为二胺的第一单体和为酰氯的第二单体来形成。
根据本公开的进一步方面,二胺是间苯二胺,其中酰氯是间苯二甲酰二氯。
根据本公开的进一步方面,半结晶粘合剂是芳族聚酰胺。
根据本公开的进一步方面,芳族聚酰胺是聚(间苯二甲酰间苯二胺)。
根据本公开的进一步方面,固化半结晶粘合剂包括干燥电极,将干电极暴露于液体电解质,并且在环境温度下将液体电解质达预定时间。
根据本公开的进一步方面,预定时间是至少一周。
根据本公开的进一步方面,固化包括干燥电极并将干电极暴露于升高的温度达第一预定时间。
根据本公开的进一步方面,升高的温度在半结晶粘合剂的玻璃化转变温度与半结晶粘合剂的分解温度之间。
根据本公开的方面,电极包括电活性材料、导电性填料和半结晶粘合剂,该半结晶粘合剂具有电活性材料和通过其分散的导电性填料。电活性材料在蓄电池单元的充电和放电期间经历了体积变化。导电性填料配置成输送来自电活性材料的电能。半结晶粘合剂包括多个聚合物链。多个聚合物链的每个都包括与多个无定形位点一起散布的多个结晶位点。多个结晶位点的每个通过重复聚合物链的链段之间的相互作用来限定。
根据本公开的进一步方面,电活性材料包括硅、二氧化硅、或硅合金。
根据本公开的进一步方面,半结晶粘合剂是芳族聚酰胺。
根据本公开的进一步方面,半结晶粘合剂是聚(间苯二甲酰间苯二胺)。
根据本公开的进一步方面,多个聚合物链的每个都包括基于相应聚合物链内原子的大于约25原子%的芳香性和提供物理交联并与活性材料表面形成良好粘附性的多个氢键。
根据本公开的进一步方面,多个聚合物链的每个都包括基于相应聚合物链内原子的大于约37原子%的芳香性。
当结合附图考虑时,从用于执行本公开的最佳模式的以下详细描述中,本公开的上述特点和优点以及其它特点和优点将是显而易见的。
附图说明
这些附图是说明性的并非旨在限制由权利要求所限定的主题。示例性方面在以下详细描述中来讨论并在附图中来示出,其中:
图1示出了根据本公开的方面的包括半结晶粘合剂的示例性电化学蓄电池单元的示意图。
图2示出了图1的电极的示意图。
图3示出了图2的电极的半结晶粘合剂的示意图。
图4示出了形成图2的电极的方法。
图5示出了将示例性半结晶粘合剂与其它粘合剂进行比较的容量与循环数的曲线图。
具体实施方式
本公开涉及电化学电池,并且更具体地涉及具有优化电极的高性能锂离子电化学电池(例如,锂离子蓄电池)。
诸如硅的用于形成电极的某些电活性材料可以提供较高的比容量,但在充电-放电循环期间经历了较大的体积变化。例如,据信含硅电活性材料在标准充电-放电循环期间使体积膨胀300%或更多。虽然不受理论束缚,但是据信使用这些电极的蓄电池单元的降低性能(例如,库仑衰减)是由于在充电-放电循环期间较大的体积变化而发生的。而且,这些电极所经历的每个充电-放电循环通常会降低电极的库仑充电容量。虽然不受理论束缚,但是据信电活性材料与电极的其它组分(例如,导电性填料和粘合剂)之间的物理接触在电活性材料的膨胀与收缩期间的破坏有助于库仑衰减。除了库仑衰减和降低的性能之外,高性能电活性材料的较大体积变化可能会通过干燥电解质和使电极组件破裂而导致有限的可操作寿命。
令人惊奇地,在不需要化学交联和/或与电活性材料的化学附着的情况下,使用如本文中所述的半结晶粘合剂优化了电极性能和使用寿命。虽然不受理论束缚,但是据信根据本公开的半结晶粘合剂优化了电极的机械强度、电极的电解质亲和力、电极内的离子转移、半结晶粘合剂和导电性填料与电活性材料和集电器两者表面的接触、和/或固体电极界面的保持。进一步地,虽然不受理论束缚,但是据信根据本公开的半结晶粘合剂抑制了电解质烧干并抑制了固体电极界面的过度形成。
例如,据信根据本公开的半结晶粘合剂抵抗了电极内的粘合剂蠕变。进一步地,据信根据本公开的半结晶粘合剂平衡了粘合剂刚性和粘合剂弹性。例如,据信半结晶粘合剂的刚性减轻了电活性材料的膨胀,而半结晶粘合剂的弹性可以在电活性材料膨胀期间抵抗电极开裂。再进一步地,根据本公开的半结晶粘合剂允许半结晶粘合剂和导电性填料两者在电活性材料的膨胀与收缩期间与电活性材料和集电器两者的继续接触。虽然不受理论束缚,但是据信继续接触至少部分地由于在例如粘合剂与电活性材料之间形成较强的氢键来提供。更进一步地,根据本公开的半结晶粘合剂用电解质亲和性和通过电极的离子传导性平衡了电极的机械特性。此外,根据本公开的半结晶粘合剂通过抑制固体电解质中间相的过度裂化和随后生长而延长了电解质的使用寿命。
现在参照图1,蓄电池单元10根据本公开的方面来示出。蓄电池单元10包括设置在第一电极14与第二电极16之间的隔板12。隔板12允许离子转移并抑制通过其的电子转移。
第一电极14配置成在蓄电池单元10正在充电时嵌入阳离子,并且在蓄电池单元10正在放电时去嵌入离子。如下面将关于图2进行进一步解释,第一电极14包括第一电活性材料202、导电性填料204、和半结晶粘合剂206。
第一电极14设置在第一集电器18上。第一集电器18配置成经由外部电路22在第一电极14与第二电极16之间收集并移动自由电子。外部电路22可以包括外部设备24,外部设备24可以是消耗来自蓄电池单元10的电力的负载和/或将电力提供到蓄电池单元10的电源。
第二电极16配置成当蓄电池单元10正在放电时嵌入从第一电极14接收的阳离子,并且在蓄电池单元10正在充电时去嵌入阳离子以传输到第一电极14。第二电极16包括第二电活性材料(未示出)并设置在第二集电器20上。第二电活性材料由与第一电活性材料202配合的材料形成,以促进第一电极14与第二电极16之间的离子流动和电子流动。第二集电器20配置成经由外部电路22在第一电极14与第二电极16之间收集并移动自由电子。
第一电极14、第二电极16、和隔板12中的每个都可以进一步包括电解质26。电解质26配置成在锂离子电池10的充电和放电期间促进离子在第一电极14与第二电极16之间的移动。电解质可以是液体、凝胶、或固体电解质。
图2是第一电极14的示意图,第一电极14包括第一电活性材料202、导电性填料204、和设置在第一集电器18上的半结晶粘合剂206。半结晶粘合剂206使第一电活性材料202和导电性填料204悬浮。
第一电活性材料202配置成在蓄电池单元10充电期间接收并嵌入阳离子。第一电活性材料202进一步配置成在蓄电池单元10放电期间去嵌入并释放阳离子。在一些方面中,阳离子是锂,并且第一电活性材料202包括锂-石墨插层化合物、锂-硅插层化合物、锂-锡插层化合物、锂合金、其组合等。
如本文中所用,第一电活性材料202是电活性材料,该电活性材料在蓄电池单元10的设计参数内的充电-放电循环期间经历了至少50%的较大体积变化。在一些方面中,第一电活性材料202包括硅、二氧化硅、和/或硅合金。有利地,具体地与石墨相比,含硅电活性材料为锂离子蓄电池提供了最高的理论充电容量。
导电性填料204配置成在第一电活性材料202与第一集电器18之间输送电荷。导电性填料204以等于或高于渗透阈值的浓度分散在第一电极14内。导电性填料204可以是合适的材料,诸如含碳材料。在一些方面中,导电性填料204选自下组,该组是炭黑、碳纤维、石墨、其组合等。
图3是半结晶粘合剂206的示意图。半结晶粘合剂206包括多个聚合物链302。多个聚合物链302的每个都包括多个无定形位点304和多个结晶位点306。多个无定形位点304的每个都与多个结晶位点306的每个一起来散布。多个结晶位点306的每个通过重复聚合物链302的链段之间的相互作用来限定。有利地,多个聚合物链302的每个都包括第一结晶位点306a和第二结晶位点306b,第一结晶位点306a包括第一组聚合物链302,第二结晶部位306b包括第二组聚合物链302。
聚合物链302包括较高的芳香性以提供所需的刚性,并且多个氢键形成在聚合物链302与第一电活性材料202的表面之间以提供改进的界面粘附性。
在一些方面中,每个聚合物链302都具有基于相应聚合物链中原子的高于25原子%的芳香性。在一些方面中,每个聚合物链302都具有基于相应聚合物链302中原子的高于37原子%的芳香性。
在一些方面中,每个聚合物链302都包括每个重复单元至少一个能够形成氢键的位点。在一些方面中,每个聚合物链302都包括每个重复单元至少两个能够形成氢键的位点。
在一些方面中,每个聚合物链302都包括基于相应聚合物链302内原子的大于约15原子%的量的氢。在一些方面中,聚合物链302是芳族聚酰胺。在一些方面中,聚合物链302是聚(间苯二甲酰间苯二胺)。
图4示出了形成诸如第一电极14的电极的方法400。方法400包括形成402电极浆料,将电极浆料涂敷404到诸如第一集电器18的集电器,并且固化406电极浆料,从而形成电极。
电极浆料以合适的比例包括溶剂、半结晶粘合剂前体溶液、第一电活性材料202、以及导电性填料204。在一些方面中,基于电极浆料中固体的重量,第一电活性材料202是在约30重量%与约95重量%之间,导电性填料204是在约3重量%与约50重量%之间,并且半结晶粘合剂前体溶液是在约2重量%至约40重量%之间。
半结晶粘合剂前体溶液在固化时配置成形成半结晶粘合剂206。在一些方面中,半结晶粘合剂前体溶液是通过处理结晶芳族聚酰胺所获得的无定形芳族聚酰胺溶液。例如,结晶芳族聚酰胺的处理可以包括将结晶芳族聚酰胺溶解在含盐有机溶液中,用水处理含盐有机溶液从而形成无定形芳族聚酰胺,并且将无定形芳族聚酰胺溶解在纯有机溶液中以产生无定形芳族聚酰胺溶液。例如,含盐有机溶液可以是合适的有机溶剂内的含氯化物的盐。在一些方面中,含盐有机溶液是氯化钙或氯化锂在N-甲基-2-吡咯烷酮(“NMP”)中的混合物。在一些方面中,纯有机溶剂是NMP。
在一些方面中,结晶芳族聚酰胺通过将第一单体与第二单体混合并使该第一单体和该第二单体聚合来形成以形成结晶芳族聚酰胺。对第一单体和第二单体进行选择以产生聚合物链,该聚合物链具有基于聚合物链中原子的至少50原子%的芳香性和配置成形成氢键的至少一个位点。
在一些方面中,半结晶粘合剂前体溶液是通过使第一单体和第二单体聚合所获得的无定形芳族聚酰胺溶液。对第一单体和第二单体进行选择以产生聚合物链,该聚合物链具有基于聚合物链中原子的至少约50原子%的芳香性和配置成形成氢键的至少一个位点。在一些方面中,第一单体是二胺且第二单体是酰氯。例如,二胺可以是间苯二胺且酰氯可以是间苯二甲酰二氯。
在一些方面中,固化406电极浆料包括在环境温度下将电极浆料暴露于液体电解质达第一预定时间。预定时间段是延长的时间段,诸如至少一周。有利地,除在生产设施处之外,延长的时间段还可以发生在供应链中的点处。例如,如果至少一周将不使用锂离子电池10,则锂离子电池10可以在固化406之前来构造并运输。在一些方面中,固化406包括干燥电极并将干电极暴露于升高的温度达第一预定时间。升高的温度可以在半结晶粘合剂的玻璃化转变温度与半结晶粘合剂的分解温度之间。
如本文中所用,术语“结晶的”应解释为基本上结晶的而不是完全结晶的。虽然本领域普通技术人员容易理解术语“基本上”的边界和界限,但是在一些方面中,术语“基本上结晶的”表明该化合物是至少95%结晶的。
如本文中所用,术语“无定形的”应解释为基本上无定形的而不是完全无定形的。虽然本领域普通技术人员容易理解术语“基本上”的边界和界限,但是在一些方面中,术语“基本上结晶的”表明该化合物是至少95%结晶的。
虽然已经详细描述了用于执行本公开的最佳模式,但是熟悉本公开所涉及领域的技术人员将会在所附权利要求的范围内认识到实践本公开的各种替代设计和实施例。
示例1
电极浆料通过基于电极浆料的重量混合81重量%的NMP、11.4重量%的硅、3.8重量%的导电性碳、以及3.8重量%的芳族聚酰胺来形成。芳族聚酰胺以在NMP中8wt%溶液的形式来添加。将浆料混合直至基本上均匀。然后将电极浆料浇铸在集电器上并在80℃下进行真空干燥过夜以除去NMP溶剂而形成干电极。将干电极加热至275℃并在该温度下保持达2小时以诱导半结晶结构的形成。
图5是比较包括示例半结晶粘合剂至其它粘合剂的纽扣电池的容量与循环数的曲线图。线502示出了具有半结晶粘合剂206的所制备纽扣电池的容量。线504示出了用羧甲基纤维素粘合剂所制备的电池的容量。线506示出了用聚偏二氟乙烯所制备的电池的容量。如可以看到,包括半结晶粘合剂的示例电池随着循环数增大展现出更大的容量保持和减小的容量衰减。例如,所有三个电池都以大约0.0024安培-小时的容量开始。在150个循环后,示例电池提供了0.0015安培-小时的容量,而此相同的容量对于羧甲基纤维素粘合剂而言在大约20个循环后达到,并且对于聚偏二氟乙烯粘合剂而言大约2个循环。
示例2
电极浆料通过基于电极浆料的重量混合81重量%的NMP、11.4重量%的硅、3.8重量%的导电性碳、以及3.8重量%的芳族聚酰胺来形成。芳族聚酰胺以在NMP中8wt%溶液的形式来添加。将浆料混合直至基本上均匀。然后将电极浆料浇铸在集电器上并在80℃下进行真空干燥过夜以除去NMP溶剂而形成干电极。将干电极组装到蓄电池单元中,并且当使这些电池休息两周的时间段以形成具有结合到纽扣电池中的半结晶芳族聚酰胺粘合剂的电极时,这些电池中电解质的存在也可以诱导半结晶结构形成。
Claims (10)
1.一种形成用于电化学电池的电极的方法,所述方法包括:
形成电极浆料,所述电极浆料包括半结晶粘合剂前体溶液、电活性材料、和导电性填料;
将所述电极浆料涂敷到集电器上;并且
固化所述电极浆料,从而形成具有半结晶粘合剂的所述电极,所述半结晶粘合剂具有所述电活性材料和通过其分散的所述导电性填料,所述半结晶粘合剂包括多个聚合物链,所述多个聚合物链的每个都包括与多个无定形位点一起散布的多个结晶位点,所述多个聚合物链的每个配置成形成氢键。
2.根据权利要求1所述的方法,其中所述半结晶粘合剂前体溶液包括第一单体和第二单体,对所述第一单体和所述第二单体进行选择以产生聚合物链,所述聚合物链具有基于所述聚合物链中原子的至少25原子%的芳香性和配置成形成氢键的至少一个位点。
3.根据权利要求1所述的方法,其中所述半结晶粘合剂前体溶液是通过结晶芳族聚酰胺的处理所获得的无定形芳族聚酰胺,所述处理包括:
将所述结晶芳族聚酰胺溶解在含盐有机溶液中,从而形成溶液;
用水处理所述溶液,从而形成无定形芳族聚酰胺;并且
将所述无定形芳族聚酰胺溶解在纯有机溶液中以产生无定形芳族聚酰胺溶液。
4.根据权利要求3所述的方法,其中所述结晶芳族聚酰胺通过以下步骤来形成:
混合所选择的第一单体和第二单体以产生聚合物链,所述聚合物链具有基于所述聚合物链中原子的至少25原子%的芳香性和配置成形成所述氢键的至少一个位点;并且
使所述第一单体和所述第二单体聚合以形成所述结晶芳族聚酰胺。
5.根据权利要求1所述的方法,其中所述多个聚合物链的每个都包括基于所述相应聚合物链内原子的大于约25原子%的芳香性和多个氢键。
6.根据权利要求5所述的方法,其中每个聚合物都包括基于所述相应聚合物链内原子的大于约15原子%的量的氢。
7.根据权利要求1所述的方法,其中所述半结晶前体由为二胺的第一单体和为酰氯的第二单体来形成。
8.根据权利要求1所述的方法,其中所述半结晶粘合剂是芳族聚酰胺。
9.根据权利要求8所述的方法,其中所述芳族聚酰胺是聚(间苯二甲酰间苯二胺)。
10.根据权利要求1所述的方法,其中固化所述半结晶粘合剂包括干燥所述电极,将所述干电极暴露于液体电解质,并且在环境温度下将所述液体电解质保持达预定时间。
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