CN109937496A - 制造高负载电极的方法 - Google Patents
制造高负载电极的方法 Download PDFInfo
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- CN109937496A CN109937496A CN201880004103.1A CN201880004103A CN109937496A CN 109937496 A CN109937496 A CN 109937496A CN 201880004103 A CN201880004103 A CN 201880004103A CN 109937496 A CN109937496 A CN 109937496A
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- electrode
- electrode layer
- mold release
- release film
- battery
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Abstract
提供一种制造高负载电极的方法，其防止粘合剂从电极层漂浮的现象，防止在干燥电极浆料时的问题发生，并且防止切断时角部处电极层的损坏和电极强度降低的问题发生。所述制造高负载电极的方法包括：施涂电极浆料到脱模膜上以制造附着有所述脱模膜的电极层的步骤；将附着有所述脱模膜的所述电极层切断成单元电极的尺寸的步骤；和从所述经切断的电极层分离并除去所述脱模膜，然后在集电器上将所述电极层放置两层以上并压延的步骤。
Description
技术领域
本公开内容涉及一种制造高负载电极的方法，且更特别地讲，涉及一种通过如下方式制造高负载电极的方法：在脱模膜上施涂电极浆料从而制造附着有所述脱模膜的电极层，将附着有所述脱模膜的所述电极层冲压成单元电极的尺寸，和从所述经冲压的电极层分离并除去所述脱模膜，然后将所述电极层在集电器上放置至少两层并进行压延。
背景技术
随着移动装置技术的发展和对移动装置需求的增加，对作为能源的二次电池的需求迅速增加。近年来，二次电池目前作为电源用于电动车辆(EV)和混合动力车辆(HEV)，并且特别是存在对具有高能量密度、高放电电压和输出稳定性的锂二次电池的高度需求。
特别地讲，用作电动车辆(EV)或混合动力车辆(HEV)的电源的锂二次电池需要能够表现出高能量密度和在短时间内高输出的特性。
通常，锂二次电池通过如下方式制造：使用能够插入和脱离锂离子的材料作为负极和正极，在正极和负极之间填充有机电解液或聚合物电解液，并且通过在正极和负极中插入和脱离锂离子时的氧化和还原反应产生电能。
此时，负极和正极在各电极的集电器上包含电极层。例如，通过将粘合剂和溶剂以及(如果需要)导电剂和分散剂混合并搅拌来制备浆料，然后可以将浆料涂覆在金属材料的集电器上，压缩，然后干燥从而制造电极。
通过在各集电器上将电极浆料涂覆一次来制造这种常规电极。通过将其中适当混合了电极活性材料、粘合剂和导电材料的浆料施涂到正极/负极集电器上，然后进行热处理工序来制造常规电极。也就是说，在正极/负极集电器上形成包含粘合剂和导电材料的电极层。
在该结构中，如果增加电极层的厚度以增加电池的容量，则锂离子传输路径变长，从而发生锂嵌入远离集电器的活性材料中/从其中脱嵌，电子经集电器的移动受到限制。而且，由于包含在电极层中的粘合剂相对轻，所以其不均匀地分散在电极层中，并且发生漂浮在表面上的现象。电极层越厚，该分离越大，因此无法避免由于在充电/放电过程中产生的集电器与活性材料的分离引起的电池循环特性的劣化和电池寿命的减少。
此外，当将大量浆料放置在集电器上并干燥时，一部分浆料未被干燥，或者如果被撞击，则会出现诸如角部处的电极层损坏和电极强度由于电极层厚度增加而减小的问题。
因此，需要一种能够解决上述问题以制造具有改善的能量密度的高负载电极的新结构电极的制造方法。
发明内容
技术问题
本公开内容的一个目的是提供一种高负载电极，其防止粘合剂漂浮的现象，不会引起电极浆料的干燥，并且不会引起冲压时电极层的损坏和角部处电极强度的降低。
技术方案
根据本公开内容的一个方面，提供一种制造高负载电极的方法，所述方法包括：在脱模膜上施涂电极浆料从而制造附着有所述脱模膜的电极层；将附着有所述脱模膜的所述电极层冲压成单元电极的尺寸；和从所述经冲压的电极层分离并除去所述脱模膜，然后将所述电极层在集电器上放置至少两层并进行压延。
所述电极可以包含由不同材料制成的两种以上电极层。
所述电极可以包含具有不同厚度的两层以上电极层。
所述电极层的厚度可以在40μm和150μm之间。
根据本公开内容的另一方面，提供一种通过上述方法制造的高负载电极。
根据本公开内容的又一方面，提供一种包含上述电极的二次电池。
所述电池可以是选自锂离子电池、锂聚合物电池和锂离子聚合物电池中的任一种。
根据本公开内容的又一方面，提供一种电池组，包含至少一个上述二次电池。
根据本公开内容的又一方面，提供一种包含上述电池组作为电源的装置。
所述装置可以是选自手机、便携式计算机、智能电话、智能平板、上网本、可穿戴电子装置、LEV(轻型电动车辆)、电动车辆、插电式混合动力车辆和蓄电装置中的任一种。
发明效果
根据本公开内容，通过如下方式制造高负载电极：在脱模膜上施涂电极浆料从而制造附着有所述脱模膜的电极层，将附着有所述脱模膜的所述电极层冲压成单元电极的尺寸，和从所述经冲压的电极层分离并除去所述脱模膜，然后将所述电极层在集电器上放置至少两层并进行压延，由此防止粘合剂漂浮的现象，不会引起电极浆料的干燥，并且不会引起冲压时角部处电极层的损坏和电极强度的降低。
附图说明
图1显示根据常规技术的制造电极的方法。
图2显示根据本公开内容的制造单一成分多层电极的方法。
图3显示根据本公开内容的制造异种成分多层电极的方法。
具体实施方式
在下文中，将详细描述本公开内容的优选实施方式。应当注意，本公开内容不限于本公开内容的范围，而仅仅是示例，并且可以在不背离本公开内容的技术主旨的情况下进行各种修改。
根据本公开内容的制造高负载电极的方法包括通过在脱模膜上施涂电极浆料从而制造附着有所述脱模膜的电极层，将电极层冲压成单元电极的尺寸的部件，并且在从经冲压的电极层分离脱模膜并除去脱模膜之后，将所述电极层在集电器上放置至少两层并进行压延。
能够在施涂并干燥电极浆料12之后分离的任何脱模膜可以用作脱模膜11。例如，可以使用PET膜、PE膜、丙烯酸类膜等，并且可以在表面上使用硅或氟涂层来改善脱模性质。
附着有脱模膜的电极层15通过在脱模膜11上施涂电极浆料来制造。在正极的情况下，电极浆料12通过混合粘合剂和导电剂与电极活性材料来制造，并且如果需要，可以进一步将填料添加到混合物中。在负极的情况下，可以根据需要进一步将填料添加到负极材料中以制造电极浆料12。
根据本公开内容的正极活性材料可以与使用锂嵌入材料作为主要成分的化合物一起使用，所述化合物诸如层状化合物，诸如锂钴氧化物(LiCoO2)和锂镍氧化物(LiNiO2)，以及被一种以上过渡金属置换的化合物；锂锰氧化物(LiMnO2)，诸如Li1+xMn2-xO4(此处，x在0和0.33之间)、LiMnO3、LiMn2O3、LiMnO2等；锂铜氧化物(Li2CuO2)；钒氧化物，诸如LiV3O8、LiFe3O4、V2O5、Cu2V2O7；锂化的镍氧化物，表示为化学式LiNi1-xMxO2(此处，M＝Co、Mn、Al、Cu、Fe、Mg、B或Ga，且x＝0.01至0.3)；锂锰复合氧化物，表示为化学式LiMn2-xMxO2(此处，M＝Co、Ni、Fe、Cr、Zn或Ta，x＝0.01至0.1)或Li2Mn3MO8(此处，M＝Fe、Co、Ni、Cu或Zn)；其中部分锂被碱土金属离子置换的LiMn2O4；二硫化物化合物；Fe2(MoO4)3；或由其组合形成的复合氧化物。
基于包含正极活性材料的混合物的总重量计，通常添加1重量％至50重量％的量的导电剂。此类导电剂不受特别限制，只要其具有导电性而不会引起电池中的化学变化即可，并且其实例包括石墨，诸如天然石墨和人造石墨；炭黑，诸如炭黑、乙炔黑、科琴黑、槽法炭黑、炉黑、灯黑和夏黑；导电纤维，诸如碳纤维和金属纤维；金属粉末，诸如氟化碳、铝和镍粉末；导电晶须，诸如氧化锌和钛酸钾；导电氧化物，诸如钛氧化物；导电材料，诸如聚亚苯基衍生物等。
粘合剂是有助于活性材料与导电材料的粘合以及与集电器1的粘合的组分，并且基于包含正极活性材料的混合物的总重量，通常以1重量％至50重量％的量添加。此类粘合剂的实例包括聚偏二氟乙烯、聚乙烯醇、羧甲基纤维素(CMC)、淀粉、羟丙基纤维素、再生纤维素、聚乙烯基吡咯烷酮、四氟乙烯、聚乙烯、聚丙烯、乙烯-丙烯-二烯三元共聚物(EPDM)、磺化EPDM、苯乙烯丁烯橡胶、氟橡胶、各种共聚物等。
填料任选地作为用于抑制正极膨胀的组分使用，并且不受特别限制，只要其是不会引起电池中的化学变化的纤维材料即可。填料的实例包括烯烃聚合物，诸如聚乙烯和聚丙烯；纤维材料，诸如玻璃纤维和碳纤维。
负极活性材料可以包含非晶碳或结晶碳，具体地为诸如非石墨化碳或石墨碳的碳；LixFe2O3(0≤x≤1)、LixWO2(0≤x≤1)、SnxMe1-xMe'yOz(Me：Mn、Fe、Pb、Ge；Me'：Al、B、P、Si、元素周期表的第1族、第2族、第3族元素、卤素；金属复合氧化物，诸如0<x≤1；1≤y≤3；1≤z≤8)；锂金属；锂合金；硅基合金；锡合金；氧化物，诸如SnO、SnO2、PbO、PbO2、Pb2O3、Pb3O4、Sb2O3、Sb2O4、Sb2O5、GeO、GeO2、Bi2O3、Bi2O4、Bi2O5；导电聚合物，诸如聚乙炔；Li-Co-Ni类材料。
电极浆料12被施涂并涂覆在脱模膜11上，以形成电极层15，并且电极层15的厚度优选在40μm和150μm之间。如果厚度小于40μm，则电极层15可能不易于与脱模膜11分离，并且如果厚度大于150μm，则可能由粘合剂产生间隙，这不适合于高负载电极。
图1显示根据常规技术的制造电极的方法。过去，(a)将电极浆料2在电极集电器1上堆叠得厚，(b)压延(3)，然后(c)冲压(4)以制造单层单元电极。然而，在这种情况下，单个电极层变厚，因此当干燥电极层时，电极层可能仅部分被干燥或者可能未被干燥，并且当冲压电极层时，可能损坏电极的角部。另外，可能由粘合剂产生间隙，这不适合于高负载。
图2显示根据本公开内容的制造单一成分多层电极17的方法。(a)将电极浆料12施涂并涂覆在脱模膜11上，然后(b)被冲压13为单元电极尺寸。(c)将经冲压(13)的电极层15在电极集电器上放置2层以上，(d)然后利用辊压延(16)，以制造单一成分多层电极17。根据本公开内容，电极浆料12被薄薄地施涂在脱模膜11上，因此当电极层被干燥时，不会发生电极层仅部分地被干燥或未被干燥的问题。
涂覆的电极层15被冲压13为单元电极尺寸，并且由于电极层的厚度仅在约40μm和150μm之间，所以在冲压时不会损坏电极的角部。
从经冲压13的电极层15除去脱模膜11，并且将电极层15在电极集电器14上放置2层以上并且压延16以成为单元电极。由于一个电极层是薄的，因此负载低，但如果通过制成2层以上然后压延来制造单元电极，则可以制造高负载电极。可以使一个电极层15具有不同的厚度或不同的成分。因此，可以将两种以上成分的电极层放置为2层以上，然后进行压延，以制造异种成分多层电极18的高负载电极，并且单一成分多层电极17的高负载电极可以通过将两个不同厚度的电极层放置为2层以上并且压延电极层来制造。另外，可以通过放置厚度和成分均不同的电极层来制造高负载电极。
图3显示根据本公开内容的制造异种成分多层电极18的方法。(a)将异种成分的电极浆料12分别施涂在待涂覆的脱模膜11上，且(b)以单元电极尺寸冲压13电极层15。(c)将经冲压13的电极层15在电极集电器14上放置2层以上，并且(d)利用辊压延16，从而(e)制造异种成分多层电极18。
与制造具有单个电极层的高负载电极的常规技术相比，根据本公开内容的制造高负载电极的方法不会产生电极浆料12仅部分地被干燥或未被干燥的问题以及在冲压时电极角部受损的问题，并且可以防止由粘合剂产生间隙的现象。根据本公开内容的制造电极的方法可以应用于正极和负极两者。
电极层15通过施涂电极浆料12而制造，并且单元电极通过冲压13电极层15并将电极层15放置为两层以上而制造，因此可以根据需要设计各种电极。所述电极可以根据电池的所需性能如稳定性和循环寿命设计。另外，增加放置在集电器14上的电极层15的数量以容易地制造高负载电极，并且可以根据电极层15的数量制造从低负载电极到高负载电极的各种负载的电极。另外，与利用单个电极层制造电极时相比，可能更少地发生电极强度降低的问题。
同时，本公开内容的特征还在于提供一种包含通过上述方法制造的高负载电极的二次电池。
根据本公开内容的二次电池包含电极组件，其通过不同极性的电极在由隔膜分隔的状态下进行层压而制造，并且该电极组件含有包含正极活性材料的正极、包含负极活性材料的负极、和隔膜。
具体地讲，正极例如通过在正极集电器1上施涂正极活性材料、导电剂和粘合剂的混合物，然后干燥正极集电器1来制造，并且可以将填料添加到混合物中。
正极集电器1通常制造成具有3μm至500μm的厚度。正极集电器1不受特别限制，只要其具有高导电性，而不会引起电池中的化学变化即可。正极集电器1的实例包括不锈钢；铝；镍；钛；焙烧碳；和用碳、镍、钛、银等表面处理过的不锈钢或铝。集电器1可以在其表面上具有细小的不规则性以增加正极活性材料的粘附性，并且可以具有各种形式，诸如膜、片、箔、网、多孔体、泡沫和无纺布。
负极可以通过在负极集电器1上施涂负极材料并干燥所述负极材料来形成。如果需要，负极还可以包含上述组分。
负极集电器1通常制造成具有3μm至500μm的厚度。负极集电器1不受特别限制，只要其具有导电性，而不会引起电池中的化学变化即可，并且其实例包括铜；不锈钢；铝；镍；钛；焙烧碳；和用碳、镍、钛或银表面处理过的铜或不锈钢；和铝-镉合金。此外，与正极集电器1一样，可以在表面上形成细小的不均匀性以增强负极活性材料的粘合力，并且其可以以各种形式如膜、片、箔、网、多孔体、泡沫和无纺布等使用。
作为用于在正极和负极之间使所述电极绝缘的隔膜，可以使用通常已知的聚烯烃类隔膜、和在所述烯烃类基材上形成有有机复合层和无机复合层的复合隔膜，并且不受特别限制。
根据本公开内容的电解质是含有锂盐的非水性电解质，其由非水性电解质和锂盐组成。作为所述非水性电解质，使用非水性电解液、有机固体电解质、无机固体电解质等。
非水性电解液的实例包括N-甲基-2-吡咯烷酮、碳酸亚丙酯、碳酸亚乙酯、碳酸亚丁酯、碳酸二甲酯、碳酸二乙酯、γ-丁内酯、1,2-二甲氧基乙烷、四氢呋喃、2-甲基四氢呋喃、二甲亚砜、1,3-二氧戊环、甲酰胺、二甲基甲酰胺、二氧戊环、乙腈、硝基甲烷、甲酸甲酯、乙酸甲酯、磷酸三酯、三甲氧基甲烷、二氧戊环衍生物、环丁砜、甲基环丁砜、1,3-二甲基-2-咪唑烷酮、碳酸亚丙酯衍生物、四氢呋喃衍生物、醚、焦磷酸甲酯、丙酸乙酯等。
有机固体电解质的实例包括聚合物，诸如聚乙烯衍生物、聚环氧乙烷衍生物、聚环氧丙烷衍生物、磷酸酯聚合物、聚海藻酸盐赖氨酸(an agitation lysine)、聚酯硫醚、聚乙烯醇、聚偏二氟乙烯和含有离子解离基团的聚合物。
无机固体电解质的实例包括Li的氮化物、卤化物、硫酸盐，诸如Li3N、LiI、Li5NI2、Li3N-LiI-LiOH、LiSiO4、LiSiO4-LiI-LiOH、Li2SiS3、Li4SiO4、Li4SiO4-LiI-LiOH、Li3PO4-Li2S-SiS2等。
锂盐是可溶于非水性电解质中的物质，且其实例包括LiCl、LiBr、LiI、LiClO4、LiBF4、LiB10Cl10、LiPF6、LiCF3SO3、LiCF3CO2、LiAsF6、LiSbF6、LiAlCl4、CH3SO3Li、CF3SO3Li、(CF3SO2)2NLi、氯硼烷锂、低级脂族羧酸锂、4-苯基硼酸锂、亚氨基锂等。
为了改善充/放电特性和阻燃性的目的，可以将吡啶、亚磷酸三乙酯、三乙醇胺、环醚、乙二胺、甘醇二甲醚、六甲基磷酰三胺、硝基苯衍生物、硫、醌亚胺染料、N-取代的唑烷酮、N,N-取代的咪唑烷、乙二醇二烷基醚、铵盐、吡咯、2-甲氧基乙醇、三氯化铝等添加到非水性电解质中。在一些情况下，可以进一步添加诸如四氯化碳或三氟乙烯的含卤素溶剂以赋予不易燃性，或者可以进一步添加二氧化碳气体以改善高温储存特性。
所述电池是选自锂离子电池、锂聚合物电池和锂离子聚合物电池中的任一种。这是根据电解液的特性进行的分类。正极和负极以及电解质如上所述。
本公开内容可以提供一种包含一个或多个二次电池的电池组。
另外，还可以提供包含所述电池组作为电源的装置，因此所述装置可以是选自由手机、便携式计算机、智能电话、智能平板、上网本、可穿戴电子装置、轻型电动车辆(LEV)、电动车辆、混合动力车辆、插电式混合动力车辆和蓄电装置组成的组中的一种。
将通过以下实施例详细描述本公开内容。然而，解释以下实施例和实验例是为了说明本公开内容，并且本公开内容的范围不限于这些实施例和实验例。
<实施例1>
将LiNi0.55Mn0.30Co0.15O2(正极活性材料)、丹卡黑(denka black，导电剂)和聚偏二氟乙烯(PVDF)(粘合剂)以96:2:2的重量比混合，然后添加NMP(N-甲基吡咯烷酮)以制造浆料。将浆料施涂在PET膜上以制造电极层。电极层的厚度设定为120μm。将电极层以单元电极尺寸冲压并除去脱模膜，然后将其在铝箔集电器上放置2层并进行压延以制造正极。
使用所制造的正极制造电极组件，然后将电极组件置于铝袋中并连接到电极引线。此后，将含有1M LiPF6的碳酸酯类复合溶液注入电解质中，然后密封以组装锂二次电池。
<实施例2至8>
除了具有下表1中所示的层的厚度和层数之外，用与实施例1中相同的方法制造正极和锂二次电池。
<实施例9>
将LiNi0.55Mn0.30Co0.15O2(正极活性材料)、丹卡黑(导电剂)和聚偏二氟乙烯(PVDF)(粘合剂)以96:2:2的重量比混合，然后添加NMP(N-甲基吡咯烷酮)以制造浆料。将浆料施涂在PET膜上以制造第一电极层。第一电极层的厚度设定为120μm。
将LiCoO2(正极活性材料)、丹卡黑(导电剂)和聚偏二氟乙烯(PVDF)(粘合剂)以80:5:15的重量比混合，然后添加NMP(N-甲基吡咯烷酮)以制造浆料。将浆料施涂在PET膜上以制造第二电极层。第二电极层的厚度设定为120μm。
将第一电极层和第二电极层以单元电极尺寸冲压并除去脱模膜，并交替地放置在铝箔集电器上以形成总共两层并压延，从而制造电极。
使用所制造的正极制造电极组件，将其置于铝袋中并连接电极引线，然后将含有1M LiPF6的碳酸酯类复合溶液注入电解质中并密封以组装锂二次电池。
<实施例10至13>
除了具有下表1中所示的层的厚度和层数之外，用与实施例9中相同的方法制造正极和锂二次电池。
<比较例1至5>
将LiNi0.55Mn0.30Co0.15O2(正极活性材料)、丹卡黑(导电材料)和聚偏二氟乙烯(PVDF)(粘合剂)以96:2:2的重量比混合，然后添加NMP(N-甲基吡咯烷酮)以制造浆料。将浆料施涂在铝箔集电器上，然后压延和冲压，从而制造正极。在电极中，电极层的厚度示于下表1中。
使用所制造的正极制造电极组件，然后将其置于铝袋中并连接电极引线，然后将含有1M LiPF6的碳酸酯类复合溶液注入电解质中并密封以组装锂二次电池。
在下表1中，在制造电极层的过程中电极表面存在裂缝的情况或者在冲压电极层的过程中电极角部存在损坏的情况表示为“O”，并且不存在裂缝或损坏的情况表示为“X”。
【表1】
如上表1中所示，在根据本公开内容的实施例1至13的电极中未发现裂缝或角部损坏，但在现有技术的比较例1至5的电极中发现裂缝和角部损坏。
另外，对实施例1至13和比较例1至5中制造的锂二次电池执行电池容量、倍率特性和循环特性的实验，且结果示于下表2中。
【表2】
如上表2中所示，与现有技术的比较例1至5相比，根据本公开内容的实施例1至13的电池的电池容量、倍率特性和循环特性得到改善。
在上文中，通过有限的实施方式和附图解释了本公开内容，但是本公开内容不限于此，并且本领域的普通技术人员可以在本公开内容的技术构思和所附权利要求的范围内以各种方式进行修改和改进。
符号说明
1：电极集电器
2：电极浆料
3：辊
4：冲压
5：单层电极
11：脱模膜
12：电极浆料
13：冲压
14：电极集电器
15：电极层
16：辊
17：单一成分多层电极
18：异种成分多层电极
Claims (10)
1.一种制造高负载电极的方法，所述方法包括：
在脱模膜上施涂电极浆料从而制造附着有所述脱模膜的电极层；
将附着有所述脱模膜的所述电极层冲压成单元电极的尺寸；和
从所述经冲压的电极层分离并除去所述脱模膜，然后将所述电极层在集电器上放置至少两层并进行压延。
2.根据权利要求1所述的方法，其中所述电极包含由不同材料制成的两种以上电极层。
3.根据权利要求1所述的方法，其中所述电极包含具有不同厚度的两层以上电极层。
4.根据权利要求1所述的方法，其中所述电极层的厚度在40μm和150μm之间。
5.一种高负载电极，通过根据权利要求1至4中任一项所述的方法制造。
6.一种二次电池，包含根据权利要求5所述的电极。
7.根据权利要求6所述的二次电池，其中所述电池是选自锂离子电池、锂聚合物电池和锂离子聚合物电池中的任一种。
8.一种电池组，包含至少一个根据权利要求7所述的二次电池。
9.一种装置，包含根据权利要求8所述的电池组作为电源。
10.根据权利要求9所述的装置，其中所述装置是选自手机、便携式计算机、智能电话、智能平板、上网本、可穿戴电子装置、LEV(轻型电动车辆)、电动车辆、插电式混合动力车辆和蓄电装置中的任一种。
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| PCT/KR2018/002738 WO2018182195A1 (ko) | 2017-03-30 | 2018-03-08 | 고로딩 전극의 제조 방법 |
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| EP (1) | EP3518323B1 (zh) |
| KR (1) | KR102314029B1 (zh) |
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| CN112750971A (zh) * | 2019-10-31 | 2021-05-04 | 三星Sdi株式会社 | 制造电极板的方法以及通过其制造的电极板 |
| CN114223071A (zh) * | 2019-08-19 | 2022-03-22 | 宝马股份公司 | 用于锂电池或锂离子电池的复合电极以及为此的制造方法 |
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| JPWO2023063389A1 (zh) * | 2021-10-14 | 2023-04-20 |
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Also Published As
| Publication number | Publication date |
|---|---|
| EP3518323B1 (en) | 2024-01-03 |
| KR102314029B1 (ko) | 2021-10-18 |
| US11043663B2 (en) | 2021-06-22 |
| CN109937496B (zh) | 2022-05-17 |
| PL3518323T3 (pl) | 2024-04-02 |
| EP3518323A1 (en) | 2019-07-31 |
| ES2969537T3 (es) | 2024-05-21 |
| WO2018182195A1 (ko) | 2018-10-04 |
| US20200035995A1 (en) | 2020-01-30 |
| KR20180110758A (ko) | 2018-10-11 |
| EP3518323A4 (en) | 2019-10-09 |
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