CN112088447A - 用于锂二次电池的隔板、其制造方法以及包括该隔板的锂二次电池 - Google Patents
用于锂二次电池的隔板、其制造方法以及包括该隔板的锂二次电池 Download PDFInfo
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- CN112088447A CN112088447A CN201980030533.5A CN201980030533A CN112088447A CN 112088447 A CN112088447 A CN 112088447A CN 201980030533 A CN201980030533 A CN 201980030533A CN 112088447 A CN112088447 A CN 112088447A
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- heat
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- secondary battery
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- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
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- 229910052714 tellurium Inorganic materials 0.000 description 1
- WMOVHXAZOJBABW-UHFFFAOYSA-N tert-butyl acetate Chemical compound CC(=O)OC(C)(C)C WMOVHXAZOJBABW-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
本发明公开了一种用于锂二次电池的隔板、制造用于锂二次电池的隔板的方法以及包括该隔板的锂二次电池,隔板包括:多孔基板;耐热层,其定位在多孔基板的至少一个表面上,且包括无机颗粒;以及第一粘合层,其定位在耐热层上,且包括第一有机聚合物,其中耐热层包括基于总重量的90wt%至99wt%的无机颗粒,耐热层的厚度为3.5μm至7μm,并且第一粘合层的厚度为0.5μm至3.0μm。
Description
技术领域
本发明公开了一种用于锂二次电池的隔板、其制造方法以及包括该隔板的锂二次电池。
背景技术
用于电化学电池的隔板是将电池中的正电极和负电极分离并连续保持离子传导性以使电池能够充放电的中间膜。顺便提及,当电池由于异常行为而暴露于高温环境时,隔板由于在低温下的熔融特性而机械收缩或损坏。在此情况下,正电极和负电极可彼此接触并且引起电池着火。为了克服该问题,需要一种抑制隔板的收缩并确保电池的稳定性的技术。
在这方面,已知有用具有高耐热性的无机颗粒和粘合性有机粘结剂的混合物涂布隔板以提高耐热性的方法。然而,常规方法可能不能充分确保所需的粘合力,并且难以全面地应用于具有各种尺寸和形状的隔板。因此,需要开发具有高耐热性和优异的粘合力的隔板。
发明内容
【技术问题】
本发明提供一种能够提高粘合力和耐热性的用于锂二次电池的隔板、制造该隔板的方法以及包括该隔板的锂二次电池。
【技术方案】
根据一个实施方式的用于锂二次电池的隔板包括:多孔基板;耐热层,其设置在多孔基板的至少一个表面上,且包括无机颗粒;以及第一粘合层,其设置在耐热层上,且包括第一有机聚合物,其中耐热层包括相对于总重量的90wt%至99wt%的无机颗粒,耐热层的厚度为3.5μm至7μm,并且第一粘合层的厚度为0.5μm至3.0μm。
根据另一实施方式的制造用于锂二次电池的隔板的方法包括:制备耐热层涂布液,该耐热层涂布液包含90wt%至99wt%的无机颗粒和1wt%至10wt%的水溶性聚合物粘结剂;制备包括第一有机聚合物粘结剂的第一粘合层涂布液;以及通过凹版涂布法将耐热层涂布液涂布在多孔基板的至少一个表面上,其中通过模涂法、线棒涂布法及喷涂法中的一种将第一粘合层涂布液施加在耐热层涂布液上,并同时干燥耐热层涂布液和第一粘合层涂布液以形成耐热层和第一粘合层,
其中,耐热层可被形成为3.5μm至7μm的厚度,并且第一粘合层可被形成为0.5μm至3.0μm的厚度。
根据另一实施方式的锂二次电池包括前述的用于锂二次电池的隔板。
【有益效果】
根据实施方式的用于锂二次电池的隔板可以有效地控制活性物质的膨胀并维持锂离子的路径以改善电池容量,并且由于减少的副反应而具有优异的电解质溶液稳定性。
根据另一实施方式的锂二次电池具有优异的初始效率、充电/放电特性和循环寿命特性。
附图说明
图1是示出根据一个实施方式的用于锂二次电池的隔板的示意性截面图。
图2是示出根据图1的示例性变型的用于锂二次电池的隔板的示意性截面图。
图3是根据另一实施方式的锂二次电池的示意图。
<符号说明>
100、113:隔板
110:多孔基板
120:耐热层
120':第一耐热层
130:第一粘合层
140:第二粘合层
150:第二耐热层
200:负电极
300:正电极
400:电池容器
500:密封件
1000:锂二次电池
具体实施方式
在下文中,参考附图详细描述本发明的实施方式。然而,在描述本说明书时,为了使本说明书的要旨清楚,省略了已知的功能或配置的描述。
为了清楚地描述本说明书,已经省略了与说明书无关的部分,并且在整个说明书中,相同或相似的组成元件标注为相同的附图标记。另外,为了便于描述,任意示出了附图中示出的每个构造的尺寸和厚度,因此本描述不一定限于所示出的内容。
在附图中,为了清楚起见,放大了层、膜、面板、区域等的厚度。并且在附图中,为了便于描述,放大了一些层和区域的厚度。将理解,当诸如层、膜、区域或基板的元件被称为在另一元件“上”时,其可以直接在另一元件上,或者也可以存在中间元件。
图1是根据一个实施方式的用于锂二次电池的隔板的示意性截面图。在下文中,参考图1描述根据本发明实施方式的用于锂二次电池的隔板。
参考图1,根据实施方式的用于锂二次电池的隔板包括多孔基板110、耐热层120和第一粘合层130。
多孔基板110具有多个孔,并且可以是在电化学装置中通常使用的基板。多孔基板110可以是由选自以下的一种聚合物形成的聚合物膜:聚烯烃(比如聚乙烯和聚丙烯)、聚酯(比如聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯)、聚缩醛、聚酰胺、聚酰亚胺、聚碳酸酯、聚醚醚酮、聚芳醚酮、聚醚酰亚胺、聚酰胺酰亚胺、聚苯并咪唑、聚醚砜、聚苯醚、环烯烃共聚物、聚苯硫醚、聚萘二甲酸乙二醇酯、玻璃纤维、特氟龙和聚四氟乙烯,或它们的两种或多种的共聚物或混合物,但不限于此。
多孔基板110可以是例如包括聚烯烃的聚烯烃类基板,并且聚烯烃类基板具有改善的关闭功能,从而有助于提高电池安全性。聚烯烃类基板可选自例如聚乙烯单层膜、聚丙烯单层膜、聚乙烯/聚丙烯双层膜、聚丙烯/聚乙烯/聚丙烯三层膜和聚乙烯/聚丙烯/聚乙烯三层膜。另外,除了可以包括烯烃树脂以外,聚烯烃类树脂还可以包括非烯烃树脂,或者可以包括烯烃与非烯烃单体的共聚物。
多孔基板110的厚度可以为约1μm至40μm,例如1μm至30μm、1μm至20μm、5μm至20μm、5μm至15μm或10μm至15μm。
耐热层120可以设置在多孔基板110的至少一个表面上,并且包括无机颗粒(未示出),并且可以通过例如凹版涂布法的涂布方法在多孔基板110的一个表面上形成。
基于耐热层120的总重量,可以包含90wt%至99wt%的无机颗粒。例如,基于耐热层120的总重量,无机颗粒可以为92wt%至98wt%,例如93wt%至98wt%,94wt%至98wt%或95wt%至98wt%。当耐热层120如上所述包含无机颗粒时,根据实施方式的用于锂二次电池的隔板可表现出改善的耐热性、持久性、抗氧化性和稳定性。
耐热层120可以具有3.5μm至7μm的厚度。例如,其可以是3.5μm至6μm,或3.5μm至5μm。
无机颗粒可以是例如Al2O3、SiO2、TiO2、SnO2、CeO2、MgO、NiO、CaO、GaO、ZnO、ZrO2、Y2O3、SrTiO3、BaTiO3、Mg(OH)2、勃姆石或其组合,但是不限于此。另外,除了无机颗粒以外,还可以进一步包括含有丙烯酸化合物、酰亚胺化合物、酰胺化合物或其组合的有机颗粒,但是本发明不限于此。
无机颗粒可以是球状、板状、立方体或无定形的。无机颗粒可以具有在约1nm至2500nm的平均粒径,在上述范围内,100nm至2000nm或200nm至1000nm,例如约300nm至800nm。无机颗粒的平均粒径可以是对应于累积尺寸分布曲线中50%的体积比的粒径(D50)。
耐热层120可以进一步包括水溶性聚合物粘结剂(未示出)。水溶性粘结剂聚合物以点接触或表面接触的方式连接耐热层120中包括的无机颗粒,以防止无机颗粒解吸。
根据实施方式的水溶性聚合物粘结剂可包括丙烯酸类粘结剂、纤维素类粘结剂、偏二氟乙烯类粘结剂或它们的组合。
作为示例,丙烯酸类粘结剂可以包括丙烯酸类共聚物,该丙烯酸类共聚物包括衍生自单体的重复单元,该单体包括衍生自(甲基)丙烯酸烷基酯单体的重复单元。(甲基)丙烯酸烷基酯单体的实例可包括选自以下的一种或多种:(甲基)丙烯酸正丁酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸戊酯、(甲基)丙烯酸己酯、(甲基)丙烯酸庚酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸辛酯、(甲基)丙烯酸壬酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸十一烷基酯、(甲基)丙烯酸十二烷基酯、(甲基)丙烯酸甲酯、(甲基)丙烯酸异冰片酯和(甲基)丙烯酸环己酯,但不限于此。例如,可以使用直链或支链的C1至C20(甲基)丙烯酸烷基酯,或直链或支链的C1至C20(甲基)丙烯酸烷基酯。
纤维素类粘结剂可包括例如羧甲基纤维素、羟丙基纤维素、二乙酰纤维素、乙酸纤维素、乙酸丁酸纤维素、乙酸丙酸纤维素、氰基乙基纤维素、氰基乙基蔗糖、支链淀粉、羧甲基纤维素或其盐。
偏二氟乙烯类粘结剂可以包括例如均聚物,其包含单独地衍生自偏二氟乙烯单体的结构单元,或者包含衍生自偏二氟乙烯的结构单元与衍生自另一单体的结构单元的共聚物。共聚物可以是例如衍生自偏二氟乙烯的结构单元和衍生自氯三氟乙烯、三氟乙烯、六氟丙烯、四氟乙烯和乙烯单体中的一种或多种结构单元,但不限于此。例如,该共聚物可以是聚偏二氟乙烯-六氟丙烯(PVdF-HFP)共聚物,其包括衍生自偏二氟乙烯单体的结构单元和衍生自六氟丙烯单体的结构单元。
例如,偏二氟乙烯类粘结剂可以包括聚偏二氟乙烯(PVdF)均聚物、聚偏二氟乙烯-六氟丙烯(PVdF-HFP)共聚物或它们的组合。在这种情况下,提高了多孔基板110和耐热层120之间的粘合力,且提高了隔板100的稳定性和电解质的浸渍性能,因此可以提高电池的高速充电/放电特性。
在这种情况下,耐热层120可以进一步包括聚乙烯醇类辅助粘结剂(未示出)。聚乙烯醇类辅助粘结剂可以包括聚乙烯醇、改性聚乙烯醇或其组合。在此,改性聚乙烯醇可以是用诸如羧基、磺酸基、氨基、硅烷醇基和硫醇基的官能团改性的聚乙烯醇。
当耐热层120进一步包括聚乙烯醇类辅助粘结剂时,它可以与水溶性聚合物粘结剂交联,从而进一步提高耐热层120的耐热性,并且由于通过交联的脱水反应而降低了水含量。
基于耐热层120的总重量,可以以0.05wt%至2wt%的量包含聚乙烯醇类辅助粘结剂。当在上述范围内包含聚乙烯醇类辅助粘结剂时,根据实施方式的用于锂二次电池的隔板的耐热性可以进一步得到提高,并且可以降低耐热层120中的水含量。
第一粘合层130可以设置在耐热层120上,并且可以包括第一有机聚合物(未示出)。第一有机聚合物可以是颗粒聚合物或非颗粒聚合物。
颗粒型聚合物可以具有100nm至600nm的直径。例如,它可以是100nm至500nm,例如100nm至400nm,150nm至300nm,150nm至250nm,例如150nm至200nm。直径可以是颗粒型聚合物的平均粒径,例如,可以是对应于累积尺寸分布曲线中的50%的体积比的粒径(D50)。当颗粒型聚合物具有上述直径时,当通过涂布法在用于锂二次电池的隔板100上形成第一粘合层130时,可以容易地控制第一粘合层130的厚度。
颗粒型聚合物可以具有100,000g/mol至1,000,000g/mol的重均分子量,例如200,000g/mol至800,000g/mol,例如400,000g/mol至600,000g/mol。当颗粒型聚合物的重均分子量满足上述范围时,颗粒型聚合物和包括该颗粒型聚合物的用于锂二次电池的隔板100可表现出优异的粘合力、耐热性、透气性和抗氧化性。重均分子量可以是通过凝胶渗透色谱法测量的按聚苯乙烯换算的平均分子量。
非颗粒型聚合物以液体形式提供,并且可以通过涂布法直接施加到耐热层120溶液上以形成第一粘合层130。例如,涂布法可以是模涂、线棒涂或喷涂。
另外,第一粘合层130可具有0.5μm至3.0μm的厚度,例如0.5μm至2.0μm,0.5μm至1.5μm或0.5μm至1.0μm。由于第一粘合层130通过如上所述的涂布法形成,因此其可以形成为具有不超过3.0μm的薄的厚度。因此,在有助于剥离锂二次电池的隔板100的同时,可以维持透气性,并且可以确保对电极的高粘合力而不使锂二次电池的性能变差。
同时,由于通过如上所述的模涂法将第一粘合层130涂布在耐热层120上,第一粘合层130可以被更均匀地涂布并且因此可以具有低的表面粗糙度值。例如,第一粘合层130的表面粗糙度可以为0.1μm至1.0μm。例如,第一粘合层130的表面粗糙度可以为0.2μm至0.8μm、0.3μm至0.7μm或0.3μm至0.6μm。
表面粗糙度是通过测量图1中暴露于外部的第一粘合层130的表面的表面粗糙度而获得的值。用表面轮廓仪测量表面粗糙度,并通过十点平均粗糙度(RZ)法计算。
另外,由于耐热层120包括无机材料作为主要组分,因此无机材料的粒径可影响表面粗糙度,因此,耐热层120的表面粗糙度可以是1.0μm至4.0μm,这是有些不平整的。另一方面,当第一粘合层130被涂布在耐热层120上时,第一粘合层130不包括无机材料,因此可以具有相对平整的表面。
同时,为了形成根据示例性实施方式的耐热层120,包括无机颗粒的涂布液可以具有2cp至3000cp的粘度。例如,用于形成耐热层120的涂布液可具有2cp至2000cp的粘度,例如10cp至1000cp或100cp至1000cp。当涂布液的粘度在上述范围内时,可以更清楚地形成稍后将描述的在耐热层120和第一粘合层130之间的界面。因此,包括在耐热层120中的无机颗粒可以不扩散到第一粘合层130中,并且可以仅存在于耐热层120中,从而第一粘合层130不包括用于确保粘合力的无机颗粒。
参考图1,根据实施方式的用于锂二次电池的隔板可以进一步包括第二粘合层140。第二粘合层140可以设置在多孔基板110的与多孔基板110的所述一个表面相对的另一表面上,并且可以包括第二有机聚合物。在这种情况下,第二有机聚合物可以与上述第一有机聚合物相同或不同。
进一步包括第二粘合层140的用于锂二次电池的隔板可以确保对与多孔基板110的另一表面相对应的表面的粘合力,从而当稍后组装到锂二次电池中时,可以进一步提高电极粘合力。
图2是示出根据图1的示例性变型的用于锂二次电池的隔板的示意性截面图。参考图2,根据示例性变型的用于锂二次电池的隔板可包括:第一耐热层120',其在多孔基板110的一个表面上并且在多孔基板110和第一粘合层之间;以及第二耐热层150,其在多孔基板110的另一表面上并且在多孔基板110和第二粘合层140之间。
第一耐热层120'和第二耐热层150可以分别包括无机颗粒,其具体地与包括在耐热层120中的无机颗粒的类型相同。包括在第一耐热层120'和第二耐热层150中的无机颗粒可以相同或不同。如图2所示,进一步包括第二耐热层150的用于锂二次电池的隔板可确保高得多的耐热性。
根据实施方式的用于锂二次电池的隔板100具有优异的耐热性。例如,隔板100在高温下可具有小于或等于2%或小于或等于1%的收缩率。例如,在将隔板100在190℃至210℃下静置20分钟至40分钟之后,垂直方向和水平方向上的收缩率分别小于或等于2%。例如,在将隔板100在200℃下静置30分钟后,垂直方向和水平方向的收缩率分别小于或等于2%。耐热层120相对于多孔基板110的厚度比可以为0.05至0.5,例如0.05至0.4,或0.1至0.4。在本文中,包括多孔基板110和耐热层120的隔板100可表现出优异的透气性、耐热性、粘合力等。
另外,根据实施方式的用于锂二次电池的隔板100可以既不破裂也不变形,而是在大于或等于200℃(例如200℃至250℃)的高温下保持稳定的形状。
当将根据实施方式的用于锂二次电池的隔板100组装到锂二次电池中时,可以获得对正电极300或负电极200的优异的粘合力。隔板100可具有大于或等于0.1gf/mm,例如0.1gf/mm至2.0gf/mm,例如0.2gf/mm至1.0gf/mm的剥离强度。
例如,在使隔板100在250kgf的压力下以150mm/sec在80℃的腔室中通过具有0μm的间隔的辊后,其剥离强度为大于或等于0.1gf/mm,例如0.1gf/mm至2.0gf/mm,或例如0.2gf/mm至1.0gf/mm。
根据实施方式的用于锂二次电池的隔板100可表现出优异的透气性,例如小于1000秒/100cc,例如小于300秒/100cc,例如小于或等于200秒/100cc,或者小于或等于150秒/100cc。换句话说,透气性可以小于40秒/100cc·1μm,例如,小于或等于30秒/100cc·1μm,或者小于或等于25秒/100cc·1μm每单位厚度。在此,透气性是指直到100cc的空气通过单位厚度的隔板所花费的时间(秒)。单位厚度的透过率可通过测量相对于整个厚度的隔板的空气渗透率、然后将其除以厚度来获得。
以上,已经描述了用于锂二次电池的隔板。在下文中描述包括用于锂二次电池的隔板的锂二次电池。
根据隔板的存在和其中使用的电解质的类型,锂二次电池可分为锂离子电池、锂离子聚合物电池和锂聚合物电池。锂二次电池可以具有各种形状和尺寸,因此,可以包括圆柱形、棱柱形、硬币型或袋型电池以及按尺寸分的薄膜型或大体积型。涉及本公开的锂离子电池的结构和制造方法在本领域中是众所周知的。
在此,作为锂二次电池的示例,示例性地描述了圆柱形锂二次电池。图3是根据本发明另一实施方式的锂二次电池的分解透视图。参考图3,锂二次电池1000包括负电极200;正电极300;设置在负电极200与正电极300之间的隔板100;电池容器400,包括浸渍在电池容器400中的电解液(未示出);和密封件500,用于密封电池容器400。
由于隔板100的描述与上述相同,因此将省略多余的描述。
负电极200包括负电极集流体和形成在负电极集流体上的负电极活性物质层。
负电极集流体可以使用铜、金、镍、铜合金等,但不限于此。
负电极活性物质层可包括负电极活性物质、粘结剂和任选的导电材料。负电极活性物质可以是可逆地嵌入/脱嵌锂离子的材料、锂金属、锂金属合金、能够掺杂和去掺杂锂的材料、过渡金属氧化物或它们的组合。
可逆地嵌入/脱嵌锂离子的材料可以是碳材料,其是任何通常使用的碳类负电极活性物质,并且其实例可以是结晶碳、无定形碳或它们的组合。结晶碳的实例可以是石墨,比如无定形、薄板状、片状、球形或纤维状天然石墨或人造石墨。无定形碳的实例可以是软碳或硬碳、中间相沥青碳化产物、焦碳等。锂金属合金可以是锂和选自Na、K、Rb、Cs、Fr、Be、Mg、Ca、Sr、Si、Sb、Pb、In、Zn、Ba、Ra、Ge、Al和Sn的金属的合金。能够掺杂和去掺杂锂的材料可以是Si、SiOx(0<x<2)、Si-C复合材料、Si-Y合金、Sn、SnO2、Sn-C复合材料、Sn-Y合金等,并且这些中的至少一种可以与SiO2混合。元素Y的具体实例可以选自Mg、Ca、Sr、Ba、Ra、Sc、Y、Ti、Zr、Hf、Rf、V、Nb、Ta、Db、Cr、Mo、W、Sg、Tc、Re、Bh、Fe、Pb、Ru、Os、Hs、Rh、Ir、Pd、Pt、Cu、Ag、Au、Zn、Cd、B、Al、Ga、Sn、In、Tl、Ge、P、As、Sb、Bi、S、Se、Te、Po及其组合。过渡金属氧化物可以是氧化钒、锂钒氧化物等。
负电极200中使用的粘结剂和导电材料可以与正电极300的粘结剂和导电材料相同。
正电极300包括正电极集流体和形成在正电极集流体上的正电极活性物质层。正电极活性物质层包括正电极活性物质、粘结剂和任选的导电材料。
正电极集流体可以使用铝、镍等,但不限于此。
正电极活性物质可以使用能够嵌入和脱嵌锂的化合物。例如,可以使用选自钴、锰、镍、铝、铁或其组合的金属的复合氧化物或复合磷酸盐中的至少一种和锂。例如,正电极活性物质可以是锂钴氧化物、锂镍氧化物、锂锰氧化物、锂镍钴锰氧化物、锂镍钴铝氧化物、磷酸锂铁或其组合。
粘结剂提高了正电极活性物质颗粒彼此之间以及与集流体之间的粘合性能,具体实例可以是聚乙烯醇、羧甲基纤维素、羟丙基纤维素、二乙酰纤维素、聚氯乙烯、羧化聚氯乙烯、聚氟乙烯、含环氧乙烷的聚合物、聚乙烯吡咯烷酮、聚脲、聚四氟乙烯、聚偏二氟乙烯、聚乙烯、聚丙烯、苯乙烯-丁二烯橡胶、丙烯酸化的苯乙烯-丁二烯橡胶、环氧树脂、尼龙等,但不限于此。这些可以单独使用或作为两种或多种的混合物使用。
导电材料提高了电极的导电性。其实例可以是天然石墨、人造石墨、炭黑、碳纤维、金属粉末、金属纤维等,但不限于此。这些可以单独使用或作为两种或多种的混合物使用。金属粉末和金属纤维可以使用铜、镍、铝、银等金属。
正电极200和负电极300可通过如下来制造:在溶剂中混合包括每种活性物质和粘结剂以及任选的导电材料的每种活性物质组合物,并将该活性物质组合物涂布在每个集流体上。在此,溶剂可以是N-甲基吡咯烷酮,但不限于此。电极制造方法是众所周知的,因此在本说明书中不再详细描述。
电解质溶液包括有机溶剂锂盐。
有机溶剂用作用于传输参与电池的电化学反应的离子的介质。其实例可以选自碳酸酯类溶剂、酯类溶剂、醚类溶剂、酮类溶剂、醇类溶剂和非质子溶剂。碳酸酯类溶剂可以是碳酸二甲酯、碳酸二乙酯、碳酸二丙酯、碳酸甲丙酯、碳酸乙丙酯、碳酸甲乙酯、碳酸亚乙酯、碳酸亚丙酯、碳酸亚丁酯等,并且酯类溶剂可以是乙酸甲酯、乙酸乙酯、乙酸正丙酯、乙酸1,1-二甲基乙酯、丙酸甲酯、丙酸乙酯、γ-丁内酯、癸内酯、戊内酯、甲羟戊酸内酯、己内酯等。醚类溶剂可以是二丁醚、四甘醇二甲醚、二甘醇二甲醚、二甲氧基乙烷、2-甲基四氢呋喃、四氢呋喃等,并且酮类溶剂可以是环己酮等。醇类溶剂可以是乙醇、异丙醇等,并且非质子溶剂可以是诸如R-CN(R是C2至C20的直链、支链或环状烃基,双键,芳香环或醚键)等的腈类;诸如二甲基甲酰胺的酰胺类;诸如1,3-二氧戊环、环丁砜等的二氧戊环类。
有机溶剂可以单独使用或以两种或多种的混合物使用,并且当有机溶剂以两种或多种的混合物使用时,可以根据所需的电池性能控制混合比例。
锂盐溶解在有机溶剂中,在电池中供应锂离子,基本地操作锂二次电池,并改善其中的负电极200和正电极300之间的锂离子传输。锂盐的实例可以包括LiPF6、LiBF4、LiSbF6、LiAsF6、LiN(SO3C2F5)2、LiN(CF3SO2)2、LiC4F9SO3、LiClO4、LiAlO2、LiAlCl4、LiN(CxF2x+1SO2)(CyF2y+1SO2)(x和y是自然数)、LiCl、LiI、LiB(C2O4)2或它们的组合,但不限于此。
锂盐可以以0.1M至2.0M范围内的浓度使用。当在上述浓度范围内包含锂盐时,由于最佳的电解质电导率和粘度,电解质可以具有优异的性能和锂离子迁移率。
具体实施方式描述
在下文中,参考实施例更详细地示出本公开的以上方面。然而,这些实施例是示例性的,并且本公开不限于此。
实施例
实施例1
将48.61g的氧化铝(Sumitomo Corp.)、0.97g的羧甲基纤维素钠盐(Sigma-Aldrich Co.,Ltd)、0.42g的聚乙烯醇(Daejung Chemicals and Metals Co.,Ltd.)和50g的去离子水混合以制备具有600cp的粘度的耐热层120的涂布液。
将9.68g的聚偏二氟乙烯(Solyvay)、0.32g的聚乙烯醇(Daejung Chemicals&Metals Co.,Ltd.)和90g的去离子水混合以制备用于粘合层130的涂布液。
在厚12μm的聚乙烯基板(SKI)上,通过凹版涂布法将耐热层涂布液涂布为4μm厚,接着,通过模涂法将粘合层涂布液以0.6μm的厚度涂布在耐热层涂布液上。随后,同时干燥耐热层涂布液和粘合层涂布液以制造用于锂二次电池的隔板。
干燥后,耐热层的厚度为4μm,且粘合层的厚度为0.6μm。
实施例2
以凹版涂布法将第一耐热层涂布液以2μm的厚度涂布在12μm厚的聚乙烯基板(SKI)的一个表面上,并以凹版涂布法将第二耐热层涂布液以2μm的厚度涂布在聚乙烯基板(SKI)的另一个表面上,然后,以模涂法将第一粘合层涂布液以0.6μm的厚度涂布在第一耐热层涂布液上,并以模涂法将第二粘合层涂布液以0.6μm的厚度涂布在第二耐热层涂布液上。
在此,按照与实施例1相同的用于涂布耐热层涂布液的方法涂布第一耐热层涂布液和第二耐热层涂布液,按照与实施例1相同的用于涂布粘合层涂布液的方法涂布第一粘合层涂布液和第二粘合层涂布液。
随后,将第一耐热层涂布液和第一粘合层涂布液、以及还有第二耐热层涂布液和第二粘合层涂布液同时干燥,以制造用于锂二次电池的隔板。
干燥后,第一耐热层和第二耐热层的厚度分别为2μm,第一粘合层和第二粘合层的厚度分别为0.6μm。
比较例1
以凹版涂布法将根据实施例1的耐热层涂布液以2μm的厚度涂布在12μm厚的聚乙烯基板(SKI)上,随后,以模涂法将根据实施例1的粘合层涂布液以0.6μm的厚度涂布在耐热层涂布液上。接着,同时干燥耐热层涂布液和粘合层涂布液以制造用于锂二次电池的隔板。
干燥后,耐热层的厚度为2μm,粘合层的厚度为0.6μm。
比较例2
以凹版涂布法将根据实施例1的耐热层涂布液以4μm的厚度涂布在12μm厚的聚乙烯基板(SKI)上,随后,以模涂法将根据实施例1的粘合层涂布液以0.4μm的厚度涂布在耐热层涂布液上。接着,同时干燥耐热层涂布液和粘合层涂布液以制造用于锂二次电池的隔板。
干燥后,耐热层为4μm厚,粘合层为0.4μm厚。
比较例3
将48.61g的氧化铝(Sumitomo Corp.)、0.97g的羧甲基纤维素钠盐(Sigma-Aldrich Co.,Ltd.)和0.42g的聚乙烯醇(Daejung Chemicals and Metals Co.,Ltd.)的混合物以及9.68g的聚偏二氟乙烯(Solvay)、0.32g的聚乙烯醇(Daejung Chemicals andMetals Co.,Ltd.)和40g的去离子水的混合物混合以制备涂布液。
以凹版涂布法将涂布液以4.6μm的厚度涂布在12μm厚的聚乙烯基板上,并干燥以制造用于锂二次电池的隔板。
干燥后,涂层为4.6μm厚。
比较例4
将48.61g的氧化铝(Sumitomo Corp.)、0.97g的羧甲基纤维素钠盐(Sigma-Aldrich Co.,Ltd.)、0.42g的聚乙烯醇(Daejung Chemicals and Metals Co.,Ltd.)和50g的去离子水混合以制备粘度为600cp的耐热层涂布液。
将20g的氧化铝、9.68g的聚偏二氟乙烯(Solvay)、0.32g的聚乙烯醇(DaejungChemicals and Metals Co.,Ltd.)和70g的去离子水混合以制备粘合层涂布液。
在12μm厚的聚乙烯基板上,以凹版涂布法将耐热层涂布液涂布为4μm厚,随后,以模涂法将粘合层涂布液以0.6μm的厚度涂布在耐热层涂布液上,接着,同时干燥耐热层涂布液和粘合层涂布液以制造用于锂二次电池的隔板。
干燥后,耐热层为4μm厚,粘合层为0.6μm厚。
另外,耐热层包含97wt%的无机颗粒,而粘合层包含67wt%的无机颗粒。
比较例5
将48.61g的氧化铝(Sumitomo Corp.)、0.97g的羧甲基纤维素钠盐(Sigma-Aldrich Co.,Ltd.)、0.42g的聚乙烯醇(Daejung Chemicals and Metals Co.,Ltd.)和450g去离子水混合以制备粘度为60Cp的耐热层涂布液。
将9.68g的聚偏二氟乙烯(Solvay)、0.32g的聚乙烯醇(Daejung Chemicals andMetals Co.,Ltd)和120g的去离子水混合以制备粘合层涂布液。
在12μm厚的聚乙烯基板上,以模涂法将耐热层涂布液涂布为4μm厚,随后,以模涂法将粘合层涂布液以0.6μm的厚度涂布在耐热层涂布液上,并同时干燥耐热层涂布液和粘合层涂布液,以制造用于锂二次电池的隔板。
干燥后,涂层为4.6μm厚。
表1示出了根据实施例1和2、比较例1至5的用于锂二次电池单元的隔板中的各层的厚度和含量、界面的存在或不存在以及耐热层涂布液的粘度。
(表1)
实施例评价
耐热性
将根据实施例1和2以及比较例1至5的用于锂二次电池的隔板分别切成10cm×10cm的尺寸,然后在纵向(MD)的中间及从中心向左和向右2.5厘米处的每个点用点标记,并以相同的方式,在横向(TD)上用点标记以制备样品。将强制循环的常规烘箱设置在200℃并等待直到温度保持稳定之后,将样品放入其中并放置10分钟。然后,取出样品以测量热处理后的长度(L1),将该长度(L1)和热处理之前的长度(LO)一起用于根据计算式1计算热收缩率。此外,将每个样品在250℃放置15分钟后测量其热收缩率,并将结果示于表2中。
[计算式1]
收缩率(%)=[(LO-L1)/LO]×100
电极粘合力
将重量比为96:2:2的LiCoO2、聚偏二氟乙烯和炭黑添加到N-甲基吡咯烷酮溶剂中以制备浆料。将浆料涂布在铝薄膜上,然后干燥并压缩以制造正电极。
将重量比为98:1:1的石墨、聚偏二氟乙烯和炭黑添加到N-甲基吡咯烷酮溶剂中以制备浆料。将浆料涂布在铜箔上,然后干燥并压缩以制造负电极。
将根据实施例1和2以及比较例1至5的用于锂二次电池的隔板制备成尺寸为10cm×10cm,并分别放置在尺寸为9cm×9cm的正电极和负电极之间,然后在250kgf的压力下以150mm/sec使它们在80℃的腔室中通过辊,以将隔板粘附到电极板上。将粘附在电极上的隔板切成25mm的宽度和50mm的长度以制备样品。在样品中,将隔板从负电极板分离10mm至20mm远,固定在上夹具中,同时将负电极板固定在下夹具中,两个夹具之间的间隔为20mm,然后拉长,并沿180°方向剥离。在此,剥离速度为20mm/min,将剥离40mm所需的力进行3次测定,然后求平均。其结果示于表2中。
界面的存在或不存在
通过以下来评估耐热层/粘合层之间的界面的存在或不存在:使用粘合性粘结剂中的氟元素(F)与耐热层中包含的金属元素(Al)之间的含量差大于或等于70%,作为通过XPS深度剖面确定界面存在的标准。
(表2)
参考表2,根据实施例1和2的用于锂二次电池的隔板表现出改善的耐热性和电极粘合力。
在上文中,已经描述和示出了本发明的某些示例性实施例,然而,对于本领域技术人员而言显而易见的是,本发明不限于所描述的示例性实施例,并且在不脱离本发明的精神和范围的情况下,可以进行各种修改和变型。因此,这样的修改或变型的示例性实施方式不可与本发明的技术思想和方面分开理解,并且这些修改的示例性实施方式在本发明的权利要求的范围内。
Claims (15)
1.一种用于锂二次电池的隔板,包括:
多孔基板;
耐热层,所述耐热层设置在所述多孔基板的至少一个表面上,且包括无机颗粒;以及
第一粘合层,所述第一粘合层设置在所述耐热层上,且包括第一有机聚合物,
其中所述耐热层包括相对于总重量的90wt%至99wt%的所述无机颗粒,
所述耐热层的厚度为3.5μm至7μm,并且
所述第一粘合层的厚度为0.5μm至3.0μm。
2.根据权利要求1所述的隔板,其中,所述第一粘合层的表面粗糙度为0.1μm至1.0μm。
3.根据权利要求1所述的隔板,其中,
形成于所述耐热层和所述第一粘合层之间的界面的表面粗糙度为1.0μm至4.0μm,并且
所述第一粘合层的暴露于外部的一个表面的表面粗糙度为0.1μm至1.0μm。
4.根据权利要求1所述的隔板,其中,所述耐热层进一步包含水溶性聚合物粘结剂。
5.根据权利要求4所述的隔板,其中,所述水溶性聚合物粘结剂包括丙烯酸类粘结剂、纤维素类粘结剂、偏二氟乙烯类粘结剂或它们的组合。
6.根据权利要求4所述的隔板,其中,所述耐热层进一步包括聚乙烯醇类辅助粘结剂。
7.根据权利要求1所述的隔板,其中,所述第一有机聚合物是颗粒型聚合物或非颗粒型聚合物。
8.根据权利要求7所述的隔板,其中,所述颗粒型聚合物的平均粒径为100nm至600nm。
9.根据权利要求7所述的隔板,其中,所述第一有机聚合物包括丙烯酸类聚合物、偏二氟乙烯类聚合物或它们的组合。
10.根据权利要求1所述的隔板,其中,所述隔板进一步包括第二粘合层,所述第二粘合层设置在所述多孔基板的与所述多孔基板的所述一个表面相对的另一表面上,并且包括第二有机聚合物。
11.根据权利要求10所述的隔板,其中,所述第二有机聚合物与所述第一有机聚合物相同或不同。
12.根据权利要求10所述的隔板,其中,
所述耐热层包括:
第一耐热层,所述第一耐热层在所述多孔基板的一个表面上并且在所述多孔基板与所述第一粘合层之间;和
第二耐热层,所述第二耐热层在所述多孔基板的另一表面上并且在所述多孔基板与所述第二粘合层之间,
其中所述第二耐热层包含无机颗粒。
13.一种制造用于锂二次电池的隔板的方法,包括:
制备耐热层涂布液,所述耐热层涂布液包含90wt%至99wt%的无机颗粒和1wt%至10wt%的水溶性聚合物粘结剂;
制备包含第一有机聚合物粘结剂的第一粘合层涂布液;以及
通过凹版涂布法将所述耐热层涂布液涂布在所述多孔基板的至少一个表面上,其中通过模涂法、线棒涂布法及喷涂法中的一种将所述第一粘合层涂布液施加在所述耐热层涂布液上,并同时干燥所述耐热层涂布液和所述第一粘合层涂布液以形成耐热层和第一粘合层,
其中,所述耐热层形成为3.5μm至7μm的厚度,并且所述第一粘合层形成为0.5μm至3.0μm的厚度。
14.根据权利要求13所述的方法,其中,所述耐热层涂布液具有100cp至1000cp的粘度。
15.一种锂二次电池,包括根据权利要求1至权利要求12中任一项所述的用于锂二次电池的隔板或根据权利要求13或权利要求14制造的用于锂二次电池的隔板。
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