CN103171208B - 锂电池隔膜 - Google Patents

锂电池隔膜 Download PDF

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CN103171208B
CN103171208B CN 201110461239 CN201110461239A CN103171208B CN 103171208 B CN103171208 B CN 103171208B CN 201110461239 CN201110461239 CN 201110461239 CN 201110461239 A CN201110461239 A CN 201110461239A CN 103171208 B CN103171208 B CN 103171208B
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CN103171208A (zh )
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钟立涵
龚丹诚
冯名正
李治宏
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财团法人工业技术研究院
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Abstract

本发明提供一种锂电池隔膜,包括:一聚酯不织布支撑材;一聚偏氟乙烯或其衍生物层,形成于该聚酯不织布支撑材上;以及一紫外光固化或热固化高分子层,形成于该聚偏氟乙烯或其衍生物层上。

Description

锂电池隔膜

技术领域

[0001] 本发明涉及一种锂电池隔膜,特别是涉及一种高耐热锂电池隔膜。

背景技术

[0002] 二次锂电池因其具有高能量密度等优点,已成为电动车主要能量来源之一。随着电动车动力需求提高,动力电池能量密度提高,电池功率输出需求与尺寸也随之增大,致使在高功率电池运作时会产生更大量的热。由于电解液为非水性且易燃的溶剂,因此,电池内部零件安全性的提升具有绝对必要性,若无法有效率地将热能排除,将造成电池温度上升。

[0003] 如何防止电池因过热而导致溶剂起火发生爆炸,安全保证即成为重要课题之一。因此,各方努力研究追求的目标是设计一种锂电池隔膜,使其具有控制电流,避免电解液直接接触以及高耐热的特性,并且具有良好的机械性质以及热稳定性,不因电极膨胀产生破裂,或是受到压缩而降低电池功率,以及不因耐热性不佳破裂造成电池短路等。

发明内容

[0004] 本发明一实施例提供一种锂电池隔膜,包括:一聚酯不织布支撑材;一形成于该聚酯不织布支撑材上的聚偏氟乙烯(PVDF)或其衍生物层;以及一形成于该聚偏氟乙烯(PVDF)或其衍生物层上的紫外光固化或热固化高分子层。

[0005] 该聚酯不织布支撑材包括聚对苯二甲酸乙二酯(PET)、聚对苯二甲酸丙二酯(PPT)、聚对苯二甲酸环己二甲酯(PCT)或上述的组合。

[0006] 该聚偏氟乙烯(PVDF)或其衍生物层包括聚偏氟乙烯(PVDF)、聚偏氟乙烯-六氟丙烯(PVDF-HFP)共聚物、聚偏氟乙烯-三氟氯乙烯(PVDF-CTFE)共聚物或其衍生物或组合。该聚偏氟乙烯(PVDF)或其衍生物层的熔点介于160〜175°C。该聚偏氟乙烯(PVDF)或其衍生物层的涂布量(coating weight)介于35.6〜89g/m2。

[0007] 该紫外光固化或热固化高分子层包括聚二甲基硅氧烷(PDMS)或环氧化物。该聚二甲基硅氧烷(PDMS)由末端具有二甲基乙烯基、二甲基己烯基或三甲基硅氧烷基的二甲基硅氧烷或其组合所制备。该聚二甲基硅氧烷(PDMS)为交联型聚二甲基硅氧烷。该紫外光固化或热固化高分子层的涂布量介于19.4〜36.4g/m2。

[0008] 本发明所制备的复合隔膜包含三种材料:⑴多孔性聚酯不织布、(2)聚偏氟乙烯(PVDF)或其衍生物以及(3)紫外光固化或热固化高分子,如聚二甲基硅氧烷(PDMS)或环氧化物(epoxy)的,其中诸如聚二甲基硅氧烷(PDMS)或环氧化物的紫外光固化或热固化高分子的功能为调整整体复合隔膜的气体穿透度,而聚偏氟乙烯(PVDF)或其衍生物则主要扮演具有耐热功能的隔离层角色,另外多孔性聚酯不织布则作为高温下具备尺寸稳定性的支撑层。本发明由上述三种材料所制备而成的复合隔膜可有效提升锂电池使用的安全性。

附图说明

[0009] 图1是根据本发明一实施例,经200°C、烘烤20分钟后,本发明复合隔膜的视图。

具体实施方式

[0010] 为了使本发明的上述目的、特征及优点能更明显易懂,下文特举一较佳实施例作详细说明。

[0011] 本发明一实施例提供一种锂电池隔膜。锂电池隔膜包括一聚酯不织布支撑材、一聚偏氟乙烯(PVDF)或其衍生物层以及一紫外光固化或热固化高分子层。聚偏氟乙烯(PVDF)或其衍生物层形成于聚酯不织布支撑材上。紫外光固化或热固化高分子层形成于聚偏氟乙烯(PVDF)或其衍生物层上。

[0012] 上述聚酯不织布支撑材可包括聚对苯二甲酸乙二酯(PET)、聚对苯二甲酸丙二酯(PPT)、聚对苯二甲酸环己二甲酯(PCT)或其组合,例如聚对苯二甲酸乙二酸环己二甲酯(poly(cyclohexylene dimethylene terephthalate)acid, PCTA)或聚对苯二甲酸乙二醇环己二甲酉旨(poly (cyclohexylene dimethylene terephthalate) glycol,PCTG)。

[0013] 上述聚偏氟乙烯(PVDF)或其衍生物层为多孔性,其可包括聚偏氟乙烯(PVDF)、聚偏氟乙烯-六氟丙烯(PVDF-HFP)共聚物、聚偏氟乙烯-三氟氯乙烯(PVDF-CTFE)共聚物或其衍生物或组合,熔点介于160〜175°C,涂布量介于35.6〜89g/m2。

[0014] 上述紫外光固化或热固化高分子层可包括聚二甲基硅氧烷(PDMS)或环氧化物,其涂布量介于19.4〜36.4g/m2。上述聚二甲基硅氧烷(PDMS)可由末端具有二甲基乙烯基、二甲基己烯基或三甲基硅氧烷基的二甲基硅氧烷或其组合所制备。上述聚二甲基硅氧烷(PDMS)可为交联型聚二甲基硅氧烷。

[0015] 本发明一实施例提供一种锂电池隔膜的制备方法。在一实施例中,所制备的隔膜为”三层”复合隔膜(A/B/C)。A层为多孔性聚酯不织布,例如聚对苯二甲酸乙二酯(PET)、聚对苯二甲酸丙二酯(PPT)、聚对苯二甲酸环己二甲酯(PCT)或其组合,膜厚约30〜40 μm。B层为聚偏氟乙烯(PVDF)或其衍生物,例如聚偏氟乙烯(PVDF)、聚偏氟乙烯-六氟丙烯(PVDF-HFP)共聚物、聚偏氟乙烯-三氟氯乙烯(PVDF-CTFE)共聚物或其衍生物或组合。C层为紫外光固化或热固化高分子,例如聚二甲基硅氧烷(PDMS)或环氧化物。A层是以熔融喷丝或是湿式抄纸(wet-laid)制备而成。再将聚偏氟乙烯(PVDF)或其衍生物溶解于例如N-甲基吡咯酮(NMP)的溶剂中形成固含量介于10〜25被%的溶液。再将此溶液以湿式涂布法涂布在A层上,经水凝固、清洗及干燥后,制备得B层。随后,将聚二甲基硅氧烷(PDMS)或环氧化物溶解(稀释)于例如正己烷或丁酮(MEK)的溶剂中配制成固含量介于40〜75wt%的聚二甲基硅氧烷(PDMS)或环氧化物溶液。

[0016] 之后,分别加入相对于聚二甲基硅氧烷(PDMS)固含量的5wt%,例如甲基氢硅氧烧(methyl hydrogen siloxane)的交联剂与相对于聚二甲基娃氧烧(PDMS)或环氧化物固含量的5wt%,例如铂金属错合物的催化剂于上述聚二甲基硅氧烷(PDMS)溶液,或是将环氧化物溶液稀释于丁酮中,待搅拌均匀后,将聚二甲基硅氧烷(PDMS)或环氧化物溶液涂布于聚偏氟乙烯(PVDF)或其衍生物层/聚酯不织布上。经100〜120°C交联反应后,即形成本发明复合隔膜。

[0017] 本发明所制备的复合隔膜包含:⑴多孔性聚酯不织布、(2)聚偏氟乙烯(PVDF)或其衍生物以及(3)紫外光固化或热固化高分子,例如聚二甲基硅氧烷(PDMS)或环氧化物,等等,其中例如聚二甲基硅氧烷(PDMS)或环氧化物的紫外光固化或热固化高分子的功能为调整整体复合隔膜的气体穿透度,而聚偏氟乙烯(PVDF)或其衍生物则主要扮演具有耐热功能的隔离层角色,另多孔性聚酯不织布则作为高温制程下具备尺寸稳定性的支撑层。本发明由上述三种材料所制备而成的复合隔膜可有效提升锂电池使用的安全性。

[0018]【实施例1】本发明隔膜的制备(I)

[0019] 本实施例所制备的隔膜为三层复合隔膜(A/B/C)。A层为多孔性聚对苯二甲酸乙二酯(PET)不织布,膜厚约30〜40 μ m,B层为聚偏氟乙烯(PVDF),C层为聚二甲基硅氧烷(PDMS)。A层是以熔融喷丝压制而成。将聚偏氟乙烯(PVDF)溶解于N-甲基吡咯酮(NMP)中形成固含量14wt%的溶液。再将此溶液涂布在A层上,经水的凝固、清洗及干燥后,制备得B层。随后,将聚二甲基硅氧烷(PDMS)溶解(稀释)于正己烷中配制成固含量40被%的溶液。随即分别加入5wt%甲基氢娃氧烧(methyl hydrogen siloxane)(交联剂)与5wt%铂金属错合物(催化剂),上述含量以聚二甲基硅氧烷(PDMS)固含量为基准。待搅拌均匀后,将聚二甲基硅氧烷(PDMS)溶液涂布于聚偏氟乙烯(PVDF)/聚对苯二甲酸乙二酯(PET)不织布上。经120°C交联反应后,即形成本实施例的复合隔膜。本实施例复合隔膜的气体穿透度(Gurley值)约为6.3sec/10cc,抗张强度为305kgf/cm2。此复合隔膜经过200°C、烘烤20分钟后仍能保有隔膜的完整性,如图1所示,此时,其气体穿透度(Gurley值)约为3.lsec/10cco

[0020]【实施例2】本发明隔膜的制备(2)

[0021] 本实施例所制备的隔膜为三层复合隔膜(A/B/C)。A层为多孔性聚对苯二甲酸乙二酯(PET)不织布,膜厚约30〜40 μ m,B层为聚偏氟乙烯(PVDF),C层为聚二甲基硅氧烷(PDMS)。A层是以熔融喷丝压制而成。将聚偏氟乙烯(PVDF)溶解于N-甲基吡咯酮(NMP)中形成固含量14wt%的溶液。再将此溶液涂布在A层上,经水的凝固、清洗及干燥后,制备得B层。随后,将聚二甲基硅氧烷(PDMS)溶解(稀释)于正己烷中配制成固含量50被%的溶液。随即分别加入5wt%甲基氢硅氧烷(交联剂)与5wt%铂金属错合物(催化剂),上述含量以聚二甲基硅氧烷(PDMS)固含量为基准。待搅拌均匀后,将聚二甲基硅氧烷(PDMS)溶液涂布于聚偏氟乙烯(PVDF)/聚对苯二甲酸乙二酯(PET)不织布上。经120°C交联反应后,即形成本实施例的复合隔膜。本实施例复合隔膜的气体穿透度(Gurley值)约为21.2sec/10cc,抗张强度为325kgf/cm2。此复合隔膜经过200°C、烘烤20分钟后仍能保有隔膜的完整性,此时,其气体穿透度(Gurley值)约为10.6sec/10cc。

[0022]【实施例3】本发明隔膜的制备(3)

[0023] 本实施例所制备的隔膜为三层复合隔膜(A/B/C)。A层为多孔性聚对苯二甲酸乙二酯(PET)不织布,膜厚约30〜40 μ m,B层为聚偏氟乙烯(PVDF),C层为聚二甲基硅氧烷(PDMS)。A层是以熔融喷丝压制而成。将聚偏氟乙烯(PVDF)溶解于N-甲基吡咯酮(NMP)中形成固含量14wt%的溶液。再将此溶液涂布在A层上,经水的凝固、清洗及干燥后,制备得B层。随后,将聚二甲基硅氧烷(PDMS)溶解(稀释)于正己烷中配制成固含量60被%的溶液。随即分别加入5wt%甲基氢硅氧烷(交联剂)与5wt%铂金属错合物(催化剂),上述含量以聚二甲基硅氧烷(PDMS)固含量为基准。待搅拌均匀后,将聚二甲基硅氧烷(PDMS)溶液涂布于聚偏氟乙烯(PVDF)/聚对苯二甲酸乙二酯(PET)不织布上。经120°C交联反应后,即形成本实施例的复合隔膜。本实施例复合隔膜的气体穿透度(Gurley值)约为79.3sec/10cc,抗张强度为350kgf/cm2。此复合隔膜经过200°C、烘烤20分钟后仍能保有隔膜的完整性,此时,其气体穿透度(Gurley值)约为46.5sec/10cco

[0024]【实施例4】本发明隔膜的制备(4)

[0025] 本实施例所制备的隔膜为三层复合隔膜(A/B/C)。A层为多孔性聚对苯二甲酸乙二酯(PET)不织布,膜厚约30〜40 μ m,B层为聚偏氟乙烯(PVDF),C层为聚二甲基硅氧烷(PDMS)。A层是以熔融喷丝压制而成。将聚偏氟乙烯(PVDF)溶解于N-甲基吡咯酮(NMP)中形成固含量14wt%的溶液。再将此溶液涂布在A层上,经水的凝固、清洗及干燥后,制备得B层。随后,将聚二甲基硅氧烷(PDMS)溶解(稀释)于正己烷中配制成固含量75被%的溶液。随即分别加入5wt%甲基氢硅氧烷(交联剂)与5wt%铂金属错合物(催化剂),上述含量以聚二甲基硅氧烷(PDMS)固含量为基准。待搅拌均匀后,将聚二甲基硅氧烷(PDMS)溶液涂布于聚偏氟乙烯(PVDF)/聚对苯二甲酸乙二酯(PET)不织布上。经120°C交联反应后,即形成本实施例的复合隔膜。本实施例复合隔膜的气体穿透度(Gurley值)约为185.2sec/10cc,抗张强度为411kgf/cm2。此复合隔膜经过200°C、烘烤20分钟后仍能保有隔膜的完整性,此时,其气体穿透度(Gurley值)约为32sec/10cc。

[0026]【比较例I】现有隔膜的制备

[0027] 本实施例所制备的隔膜为二层复合隔膜(A/B)。A层为多孔性聚对苯二甲酸乙二酯(PET)不织布,膜厚约30〜40 μ m,B层为聚偏氟乙烯(PVDF)。A层是以熔融喷丝压制而成。将聚偏氟乙烯(PVDF)溶解于N-甲基吡咯酮(NMP)中形成固含量14wt%的溶液。再将此溶液涂布在A层上,经水的凝固、清洗及干燥后,制备得B层,即形成本实施例的复合隔膜。本实施例复合隔膜的气体穿透度(Gurley值)约为1.5sec/10cc,抗张强度为290kgf/cm2。此复合隔膜经过200°C、烘烤20分钟后复合隔膜的气体穿透度(Gurley值)小于lsec/lOcc而无法量测,不适用于电池隔膜。

[0028] 虽然本发明已以较佳实施例揭露如上,然而其并非用以限定本发明,任何本领域技术人员,在不脱离本发明的精神和范围内,可作修改与改变,因此本发明的保护范围一权利要求书所界定为准。

Claims (5)

1.一种锂电池隔膜,包括: 一聚酯不织布支撑材,其中该聚酯不织布支撑材包括聚对苯二甲酸乙二酯、聚对苯二甲酸丙二酯、聚对苯二甲酸环己二甲酯或其组合; 一聚偏氟乙烯或其衍生物层,形成于该聚酯不织布支撑材上,其中该聚偏氟乙烯或其衍生物层包括聚偏氟乙烯、聚偏氟乙烯-六氟丙烯共聚物、聚偏氟乙烯-三氟氯乙烯共聚物或其衍生物或组合;以及 一紫外光固化或热固化高分子层,形成于该聚偏氟乙烯或其衍生物层上,其中该紫外光固化或热固化高分子层的涂布量介于19.4〜36.4g/m2,其中该紫外光固化或热固化高分子层包括聚二甲基硅氧烷或环氧化物。
2.根据权利要求1所述的锂电池隔膜,其中该聚偏氟乙烯或其衍生物层的熔点介于160 〜175℃。
3.根据权利要求1所述的锂电池隔膜,其中该聚二甲基硅氧烷由末端具有二甲基乙烯基、二甲基己烯基或三甲基硅氧烷基的二甲基硅氧烷或其组合所制备。
4.根据权利要求1所述的锂电池隔膜,其中该聚二甲基硅氧烷为交联型聚二甲基硅氧烷。
5.根据权利要求1所述的锂电池隔膜,其中该聚偏氟乙烯或其衍生物层的涂布量介于.35.6 〜89g/m2。
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