CN111916624B - 隔离膜和电化学装置 - Google Patents
隔离膜和电化学装置 Download PDFInfo
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- CN111916624B CN111916624B CN201910380301.4A CN201910380301A CN111916624B CN 111916624 B CN111916624 B CN 111916624B CN 201910380301 A CN201910380301 A CN 201910380301A CN 111916624 B CN111916624 B CN 111916624B
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Abstract
本申请提供了隔离膜和电化学装置。隔离膜包括:多孔基材;第一涂层,位于多孔基材的至少一个表面上;其中,第一涂层包括第一聚合物粘结剂和第一无机颗粒,第一聚合物粘结剂为核壳结构的颗粒。本申请通过在第一涂层中采用第一无机颗粒,在确保第一聚合物粘结剂发挥粘结作用的同时,促进了电解液传输,提高了电化学装置的倍率性能。
Description
技术领域
本申请涉及电化学装置领域,更具体地,涉及隔离膜和电化学装置。
背景技术
隔离膜中的聚合物粘结剂在经过电解液溶胀以及化成工序热压后会被压扁粘连成膜,影响电化学装置(例如,锂离子电池)的倍率性能以及循环性能,甚至导致循环过程中的负极析锂。隔离膜的聚合物粘结剂多为弱极性聚合物粘结剂,与电解液亲和性差,导致电解液传输困难,在高压密材料体系中容易发生电解液浸润不良。
为了克服上述问题,目前通常采用以下两种手段:第一,通过增加聚合物粘结剂的交联度,用以降低聚合物粘结剂的溶胀度;第二,调整化成工序条件,例如,降低化成工序温度,减小化成工序压力,缩短化成工序流程时间。然而,增加聚合物粘结剂的交联度会增加聚合物粘结剂的颗粒的刚性,导致聚合物粘结剂的粘结力下降。另外,通常难以精确地通过交联度的改变来调整溶胀度。而通过调整化成工序条件,会使得隔离膜与极片之间的界面粘结力下降,电化学装置容易发生变形。此外,在电化学装置界面平整度下降时,容易产生界面析锂,进而影响电化学装置的循环性能。
发明内容
本申请通过在隔离膜的多孔基材上形成包括无机颗粒的粘结剂涂层,防止粘结剂在电解液溶胀以及化成工序热压后被压扁粘连成膜,同时提高了隔离膜的电解液亲和性,促进了电解液的传输。
本申请提供了一种隔离膜,包括:多孔基材;第一涂层,位于所述多孔基材的至少一个表面上;其中,所述第一涂层包括第一聚合物粘结剂和第一无机颗粒,所述第一聚合物粘结剂为核壳结构的颗粒。
在上述隔离膜中,还包括设置在所述多孔基材和所述第一涂层之间的第二涂层,所述第二涂层包括第二聚合物粘结剂和第二无机颗粒。
在上述隔离膜中,所述第一涂层还包括辅助粘结剂,所述第一聚合物粘结剂、所述第一无机颗粒和所述辅助粘结剂的质量比为10-80:85-5:5-15。
在上述隔离膜中,所述第一涂层为颗粒单层结构。
在上述隔离膜中,所述第一聚合物粘结剂满足下式(1)-(3):
300nm≤Dv50≤5000nm 式(1);
Dv90≤1.5*Dv50 式(2);
Dn10≤200nm 式(3);
其中,Dv50表示在体积基准的粒度分布中,从小粒径侧起、达到体积累积50%的粒径,Dv90表示在体积基准的粒度分布中,从小粒径侧起、达到体积累积90%的粒径,Dn10表示在数量基准的粒度分布中,从小粒径侧起、达到数量累积10%的粒径。
在上述隔离膜中,所述隔离膜满足下式(4):
0.3*第一聚合物粘结剂Dv50≤第一无机颗粒Dv50≤0.7*第一聚合物粘结剂Dv50式(4)。
在上述隔离膜中,所述第一聚合物粘结剂的核选自以下单体中的至少一种聚合形成的聚合物:丙烯酸乙酯、丙烯酸丁酯、甲基丙烯酸乙酯、苯乙烯、氯苯乙烯、氟苯乙烯、甲基苯乙烯、丙烯酸、甲基丙烯酸、马来酸。
在上述隔离膜中,所述第一聚合物粘结剂的壳选自以下单体中的至少一种聚合形成的聚合物:丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、乙烯、氯苯乙烯、氟苯乙烯、甲基苯乙烯、丙烯腈、甲基丙烯腈。
在上述隔离膜中,所述第一无机颗粒选自三氧化二铝、二氧化硅、氧化镁、氧化钛、二氧化铪、氧化锡、二氧化铈、氧化镍、氧化锌、氧化钙、氧化锆、氧化钇、碳化硅、勃姆石、氢氧化铝、氢氧化镁、氢氧化钙、硫酸钡中的一种或多种。
本申请还提供了一种电化学装置,包括:正极极片;负极极片;以及上述隔离膜,所述隔离膜设置在所述正极极片和所述负极极片之间。
本申请通过在第一涂层中采用第一无机颗粒,在确保第一聚合物粘结剂发挥粘结作用的同时,促进了电解液传输,提高了电化学装置的倍率性能。
附图说明
图1示出了根据本申请的一些实施例的隔离膜的示意图。
图2示出了根据本申请的实施例2的10000倍放大下的隔离膜的扫描电子显微镜(SEM)图。
具体实施方式
下面详细充分地说明示例性实施例,不过,这些示例性实施例可以用不同的方式来实施,并且,不应被解释为局限于本申请所阐述的这些实施例。相反,提供这些实施例的目的在于使本申请公开彻底和完整,以及将本申请的范围充分地传达给本领域所属技术人员。
图1示出了根据本申请的一些实施例的隔离膜的示意图。参见图1,本申请的隔离膜包括多孔基材1以及设置在多孔基材1上的第一涂层2。虽然图1中将第一涂层2示出为位于多孔基材1的一个表面上,但是应该理解,可以将第一涂层2设置在多孔基材1的两个表面上。
多孔基材1为由选自以下任一种聚合物或两种以上的混合物形成的聚合物膜、多层聚合物膜、或无纺布:聚乙烯、聚丙烯、聚对苯二甲酸乙二醇酯、聚苯二甲酰苯二胺、聚对苯二甲酸丁二醇酯、聚酯、聚缩醛、聚酰胺、聚碳酸酯、聚酰亚胺、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、聚苯硫醚和聚乙烯萘。聚乙烯选自高密度聚乙烯、低密度聚乙烯、超高分子量聚乙烯中的至少一种组分。多孔基材1的平均孔径为0.001μm~10μm。多孔基材1的孔隙率为5%~95%。另外,多孔基材1具有0.5μm至50μm之间的厚度。
第一涂层2包括第一聚合物粘结剂3和第一无机颗粒4。第一聚合物粘结剂3为核壳结构的颗粒。第一聚合物粘结剂3的核选自以下单体中的至少一种聚合形成的聚合物:丙烯酸乙酯、丙烯酸丁酯、甲基丙烯酸乙酯、苯乙烯、氯苯乙烯、氟苯乙烯、甲基苯乙烯、丙烯酸、甲基丙烯酸、马来酸。第一聚合物粘结剂3的壳选自以下单体中的至少一种聚合形成的聚合物:丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、乙烯、氯苯乙烯、氟苯乙烯、甲基苯乙烯、丙烯腈、甲基丙烯腈。在本申请中,通过采用核壳颗粒结构的第一聚合物粘结剂,一方面有助于提高聚合物粘结剂的颗粒的均匀性,另一方面,在后期加热工艺中,第一聚合物粘结剂的壳可以首先软化,之后,第一聚合物粘结剂的核可以起到粘结作用。第一聚合物粘结剂的核壳结构的颗粒可以通过本领域常用的乳液聚合法得到。
在一些实施例中,第一无机颗粒4选自三氧化二铝、二氧化硅、氧化镁、氧化钛、二氧化铪、氧化锡、二氧化铈、氧化镍、氧化锌、氧化钙、氧化锆、氧化钇、碳化硅、勃姆石、氢氧化铝、氢氧化镁、氢氧化钙、硫酸钡中的一种或多种。第一无机颗粒4为高硬度的无机材料,在电解液溶胀以及化成工序热压后无明显变化,可以起到支撑骨架作用,同时第一无机颗粒4有良好的电解液亲和性,有利于电解液传输。
在一些实施例中,隔离膜还包括设置在多孔基材1和第一涂层2之间的第二涂层,第二涂层包括第二聚合物粘结剂和第二无机颗粒。第二涂层中的第二聚合物粘结剂选自偏二氟乙烯-六氟丙烯的共聚物、偏二氟乙烯-三氯乙烯的共聚物、聚苯乙烯、聚丙烯酸酯、聚丙烯酸、聚丙烯酸盐、聚丙烯腈、聚乙烯基吡咯烷酮、聚乙酸乙烯酯、乙烯-乙酸乙烯酯的共聚物、聚酰亚胺、聚氧化乙烯、乙酸纤维素、乙酸丁酸纤维素、乙酸丙酸纤维素、氰基乙基支链淀粉、氰基乙基聚乙烯醇、氰基乙基纤维素、氰基乙基蔗糖、支链淀粉、羧甲基纤维素、羧甲基纤维钠、羧甲基纤维素锂、丙烯腈-苯乙烯-丁二烯的共聚物、聚苯二甲酰苯二胺、聚乙烯醇、苯乙烯-丁二烯的共聚物和聚偏二氟乙烯中的一种或多种。聚丙烯酸酯包括聚甲基丙烯酸甲酯、聚丙烯酸乙酯、聚丙烯酸丙酯和聚丙烯酸丁酯中一种或多种。
在一些实施例中,第二无机颗粒也可以选自三氧化二铝、二氧化硅、氧化镁、氧化钛、二氧化铪、氧化锡、二氧化铈、氧化镍、氧化锌、氧化钙、氧化锆、氧化钇、碳化硅、勃姆石、氢氧化铝、氢氧化镁、氢氧化钙、硫酸钡中的一种或多种。对第二无机颗粒的含量没有特别限定。但是,以第二涂层的总重量为100%计,第二无机颗粒的重量百分比为40%~99%。如果第二无机颗粒的重量百分比小于40%,则第二聚合物粘结剂大量存在,从而降低了第二无机颗粒间形成的间隙体积,并降低了孔径和孔隙率,导致锂离子的传导变慢,电化学装置的性能下降。如果第二无机颗粒的重量百分比大于99%,则第二聚合物粘结剂的含量太低以致不能使第二无机颗粒间充分的附着,导致最终形成的隔离膜的机械性能降低。
在一些实施例中,第一涂层2还包括辅助粘结剂,第一聚合物粘结剂、第一无机颗粒和辅助粘结剂的质量比为10-80:85-5:5-15。在一些实施例中,辅助粘结剂选自偏二氟乙烯-六氟丙烯的共聚物、偏二氟乙烯-三氯乙烯的共聚物、聚苯乙烯、聚丙烯酸酯、聚丙烯酸、聚丙烯酸盐、聚丙烯腈、聚乙烯基吡咯烷酮、聚乙酸乙烯酯、乙烯-乙酸乙烯酯的共聚物、聚酰亚胺、聚氧化乙烯、乙酸纤维素、乙酸丁酸纤维素、乙酸丙酸纤维素、氰基乙基支链淀粉、氰基乙基聚乙烯醇、氰基乙基纤维素、氰基乙基蔗糖、支链淀粉、羧甲基纤维素、羧甲基纤维钠、羧甲基纤维素锂、丙烯腈-苯乙烯-丁二烯的共聚物、聚苯二甲酰苯二胺、聚乙烯醇、苯乙烯-丁二烯的共聚物和聚偏二氟乙烯中的一种或多种。聚丙烯酸酯包括聚甲基丙烯酸甲酯、聚丙烯酸乙酯、聚丙烯酸丙酯和聚丙烯酸丁酯中一种或多种。第一聚合物粘结剂的含量太少,粘结性能会下降,第一聚合物粘结剂的含量过多,电化学装置的倍率性能下降。辅助粘结剂有助于增加第一涂层的粘结性,辅助粘结剂的含量太少,粘结性能的提升不明显,辅助粘结剂的含量过多,电化学装置的倍率性能变差。第一无机颗粒的添加量太小起不到支撑效果,添加量太大,影响第一聚合物粘结剂的粘结作用的发挥。
如图1所示,在一些实施例中,第一涂层2为颗粒单层结构。颗粒单层结构有助于电化学装置的能量密度提升,同时可以改善电化学装置的倍率性能以及循环性能。
在一些实施例中,第一聚合物粘结剂为球形或类球形颗粒,第一聚合物粘结剂满足下式(1)-(3):
300nm≤Dv50≤5000nm 式(1);
Dv90≤1.5*Dv50 式(2);
Dn10≤200nm 式(3);
其中,Dv50表示在体积基准的粒度分布中,从小粒径侧起、达到体积累积50%的粒径,Dv90表示在体积基准的粒度分布中,从小粒径侧起、达到体积累积90%的粒径,Dn10表示在数量基准的粒度分布中,从小粒径侧起、达到数量累积10%的粒径。满足上式的第一聚合物粘结剂的颗粒的一致性较高,颗粒一致性高有助于第一聚合物粘结剂发挥粘结作用,并且能提升电化学装置的厚度一致性。第一聚合物粘结剂的粒径太小,电化学装置的倍率性能会下降,第一聚合物粘结剂的粒径过大,粘结性能会受影响。
在一些实施例中,隔离膜满足下式(4):
0.3*第一聚合物粘结剂Dv50≤第一无机颗粒Dv50≤0.7*第一聚合物粘结剂Dv50式(4)。
第一无机颗粒的主要作用是防止第一聚合物粘结剂在化成工序中被压扁,第一无机颗粒的粒径太小,无法起到支撑作用。而如果第一无机颗粒的粒径太大,例如接近或大于第一聚合物粘结剂粒径,热压时第一聚合物粘结剂将无法发挥粘结作用,导致粘结失效。另外,第一无机颗粒支撑起的厚度空间有助于电解液传输。
本申请还提供了包括上述隔离膜的锂离子电池。在本申请中,锂离子电池仅作为电化学装置的示例性实例,电化学装置还可以包括其他合适的装置。锂离子电池还包括正极极片、负极极片以及电解质,其中,本申请的隔离膜插入在正极极片和负极极片之间。正极极片包括正极集流体,负极极片包括负极集流体,正极集流体可以为铝箔或镍箔,负极集流体可为铜箔或镍箔。
正极极片
正极极片包括正极材料,正极材料包括能够吸收和释放锂(Li)的正极材料(下文中,有时称为“能够吸收/释放锂Li的正极材料”)。能够吸收/释放锂(Li)的正极材料的例子可以包括钴酸锂、镍钴锰酸锂、镍钴铝酸锂、锰酸锂、磷酸锰铁锂、磷酸钒锂、磷酸钒氧锂、磷酸铁锂、钛酸锂和富锂锰基材料。
具体的,钴酸锂的化学式可以如化学式1:
LixCoaM1bO2-c 化学式1
其中M1表示选自镍(Ni)、锰(Mn)、镁(Mg)、铝(Al)、硼(B)、钛(Ti)、钒(V)、铬(Cr)、铁(Fe)、铜(Cu)、锌(Zn)、钼(Mo)、锡(Sn)、钙(Ca)、锶(Sr)、钨(W)、钇(Y)、镧(La)、锆(Zr)和硅(Si)中的至少一种,x、a、b和c值分别在以下范围内:0.8≤x≤1.2、0.8≤a≤1、0≤b≤0.2、-0.1≤c≤0.2;
镍钴锰酸锂或镍钴铝酸锂的化学式可以如化学式2:
LiyNidM2eO2-f 化学式2
其中M2表示选自钴(Co)、锰(Mn)、镁(Mg)、铝(Al)、硼(B)、钛(Ti)、钒(V)、铬(Cr)、铁(Fe)、铜(Cu)、锌(Zn)、钼(Mo)、锡(Sn)、钙(Ca)、锶(Sr)、钨(W)、锆(Zr)和硅(Si)中的至少一种,y、d、e和f值分别在以下范围内:0.8≤y≤1.2、0.3≤d≤0.98、0.02≤e≤0.7、-0.1≤f≤0.2;
锰酸锂的化学式可以如化学式3:
LizMn2-gM3gO4-h 化学式3
其中M3表示选自钴(Co)、镍(Ni)、镁(Mg)、铝(Al)、硼(B)、钛(Ti)、钒(V)、铬(Cr)、铁(Fe)、铜(Cu)、锌(Zn)、钼(Mo)、锡(Sn)、钙(Ca)、锶(Sr)和钨(W)中的至少一种,z、g和h值分别在以下范围内:0.8≤z≤1.2、0≤g<1.0和-0.2≤h≤0.2。
负极极片
负极极片包括负极材料,负极材料包括能够吸收和释放锂(Li)的负极材料(下文中,有时称为“能够吸收/释放锂Li的负极材料”)。能够吸收/释放锂(Li)的负极材料的例子可以包括碳材料、金属化合物、氧化物、硫化物、锂的氮化物例如LiN3、锂金属、与锂一起形成合金的金属和聚合物材料。
碳材料的例子可以包括低石墨化的碳、易石墨化的碳、人造石墨、天然石墨、中间相碳微球、软碳、硬碳、热解碳、焦炭、玻璃碳、有机聚合物化合物烧结体、碳纤维和活性碳。其中,焦炭可以包括沥青焦炭、针状焦炭和石油焦炭。有机聚合物化合物烧结体指的是通过在适当的温度下煅烧聚合物材料例如苯酚塑料或者呋喃树脂以使之碳化获得的材料,将这些材料中的一些分成低石墨化碳或者易石墨化的碳。聚合物材料的例子可以包括聚乙炔和聚吡咯。
在能够吸收/释放锂(Li)的这些负极材料中,更进一步地,选择充电和放电电压接近于锂金属的充电和放电电压的材料。这是因为负极材料的充电和放电电压越低,电化学装置(例如锂离子电池)越容易具有更高的能量密度。其中,负极材料可以选择碳材料,因为在充电和放电时它们的晶体结构只有小的变化,因此,可以获得良好的循环特性以及大的充电和放电容量。尤其可以选择石墨,因为它可以给出大的电化学当量和高的能量密度。
此外,能够吸收/释放锂(Li)的负极材料可以包括单质锂金属、能够和锂(Li)一起形成合金的金属元素和半金属元素,包括这样的元素的合金和化合物等等。特别地,将它们和碳材料一起使用,因为在这种情况中,可以获得良好的循环特性以及高能量密度。除了包括两种或者多种金属元素的合金之外,这里使用的合金还包括包含一种或者多种金属元素和一种或者多种半金属元素的合金。该合金可以处于以下状态固溶体、共晶晶体(共晶混合物)、金属间化合物及其混合物。
金属元素和半金属元素的例子可以包括锡(Sn)、铅(Pb)、铝(Al)、铟(In)、硅(Si)、锌(Zn)、锑(Sb)、铋(Bi)、镉(Cd)、镁(Mg)、硼(B)、镓(Ga)、锗(Ge)、砷(As)、银(Ag)、锆(Zr)、钇(Y)和铪(Hf)。上述合金和化合物的例子可以包括具有化学式:MasMbtLiu的材料和具有化学式:MapMcqMdr的材料。在这些化学式中,Ma表示能够与锂一起形成合金的金属元素和半金属元素中的至少一种元素;Mb表示除锂和Ma之外的金属元素和半金属元素中的至少一种元素;Mc表示非金属元素中的至少一种元素;Md表示除Ma之外的金属元素和半金属元素中的至少一种元素;并且s、t、u、p、q和r满足s>0、t≥0、u≥0、p>0、q>0和r≥0。
此外,可以在负极中使用不包括锂(Li)的无机化合物,例如MnO2、V2O5、V6O13、NiS和MoS。
电解质
上述锂离子电池还包括电解质,电解质可以是凝胶电解质、固态电解质和电解液中的一种或多种,电解液包括锂盐和非水溶剂。
锂盐选自LiPF6、LiBF4、LiAsF6、LiClO4、LiB(C6H5)4、LiCH3SO3、LiCF3SO3、LiN(SO2CF3)2、LiC(SO2CF3)3、LiSiF6、LiBOB和二氟硼酸锂中的一种或多种。例如,锂盐选用LiPF6,因为它可以给出高的离子导电率并改善循环特性。
非水溶剂可为碳酸酯化合物、羧酸酯化合物、醚化合物、其它有机溶剂或它们的组合。
碳酸酯化合物可为链状碳酸酯化合物、环状碳酸酯化合物、氟代碳酸酯化合物或其组合。
链状碳酸酯化合物的实例为碳酸二乙酯(DEC)、碳酸二甲酯(DMC)、碳酸二丙酯(DPC)、碳酸甲丙酯(MPC)、碳酸乙丙酯(EPC)、碳酸甲乙酯(MEC)及其组合。所述环状碳酸酯化合物的实例为碳酸亚乙酯(EC)、碳酸亚丙酯(PC)、碳酸亚丁酯(BC)、碳酸乙烯基亚乙酯(VEC)及其组合。所述氟代碳酸酯化合物的实例为碳酸氟代亚乙酯(FEC)、碳酸1,2-二氟亚乙酯、碳酸1,1-二氟亚乙酯、碳酸1,1,2-三氟亚乙酯、碳酸1,1,2,2-四氟亚乙酯、碳酸1-氟-2-甲基亚乙酯、碳酸1-氟-1-甲基亚乙酯、碳酸1,2-二氟-1-甲基亚乙酯、碳酸1,1,2-三氟-2-甲基亚乙酯、碳酸三氟甲基亚乙酯及其组合。
羧酸酯化合物的实例为乙酸甲酯、乙酸乙酯、乙酸正丙酯、乙酸叔丁酯、丙酸甲酯、丙酸乙酯、丙酸丙酯、γ-丁内酯、癸内酯、戊内酯、甲瓦龙酸内酯、己内酯、甲酸甲酯及其组合。
醚化合物的实例为二丁醚、四甘醇二甲醚、二甘醇二甲醚、1,2-二甲氧基乙烷、1,2-二乙氧基乙烷、乙氧基甲氧基乙烷、2-甲基四氢呋喃、四氢呋喃及其组合。
其它有机溶剂的实例为二甲亚砜、1,2-二氧戊环、环丁砜、甲基环丁砜、1,3-二甲基-2-咪唑烷酮、N-甲基-2-吡咯烷酮、甲酰胺、二甲基甲酰胺、乙腈、磷酸三甲酯、磷酸三乙酯、磷酸三辛酯、和磷酸酯及其组合。
虽然上面以锂离子电池进行了举例说明,但是本领域技术人员在阅读本申请之后,能够想到本申请的隔离膜可以用于其他合适的电化学装置。这样的电化学装置包括发生电化学反应的任何装置,它的具体实例包括所有种类的一次电池、二次电池、燃料电池、太阳能电池或电容。
该电化学装置可以用本领域技术人员知道的传统方法制造。在制造电化学装置的方法的一个实施方案中,该电化学装置用插入在正极极片和负极极片之间的隔离膜形成电化学装置,然后将液态电解质注入到该电化学装置中,由此提供电化学装置。根据最终产品的制造方法和所需要的性能,在电化学装置的制造过程期间,可以在合适的步骤注入液态电解质。换句话说,可以在组装电化学装置之前或在组装电化学装置期间的最后步骤注入液态电解质。
具体地,本申请的电化学装置可以为锂离子电池,锂离子电池的电化学装置可以为卷绕型、层压(堆叠)型和折叠型。
下面以锂离子电池为例并且结合具体的实施例说明锂离子电池的制备,本领域的技术人员将理解,本申请中描述的制备方法仅是实例,其他任何合适的制备方法均在本申请的范围内。
本申请的实施例与对比例的锂离子电池的制备过程如下所示:
对比例1
(1)隔离膜的制备
将勃姆石与聚丙烯酸酯依照质量比90:10混合并将其溶入到去离子水中以形成第二涂层浆料。随后采用微凹涂布法将所述第二涂层浆料均匀涂布到多孔基材(聚乙烯,厚度7μm,平均孔径为0.073μm,孔隙率为26%)的其中一面上,经过干燥处理以获得所述第二涂层与所述多孔基材的双层结构。
将聚偏二氟乙烯与聚丙烯酸酯依照质量比96:4混合并将其溶入到去离子水中以形成第一涂层浆料,聚偏二氟乙烯的Dv50为600nm。随后采用微凹涂布法将所述第一涂层浆料均匀涂布到上述第二涂层与多孔基材双层结构的两个表面上,经过干燥处理以获得所需隔离膜。
(2)正极极片的制备
将正极活性物质钴酸锂、导电剂乙炔黑、粘结剂聚偏二氟乙烯(PVDF)按质量比94:3:3在N-甲基吡咯烷酮溶剂体系中充分搅拌混合均匀后,涂覆于正极集流体Al箔上,经烘干、冷压、分条,得到正极极片。
(3)负极极片的制备
将负极活性物质人造石墨、导电剂乙炔黑、粘结剂丁苯橡胶(SBR)、增稠剂羧甲基纤维素钠(CMC)按质量比96:1:1.5:1.5在去离子水溶剂体系中充分搅拌混合均匀后,涂覆于负极集流体Cu箔上,经烘干、冷压、分条,得到负极极片。
(4)电解液的制备
将锂盐LiPF6与非水有机溶剂(碳酸乙烯酯(EC):碳酸亚丙酯(PC)=50:50,质量比)按质量比8:92配制而成的溶液作为锂离子电池的电解液。
(5)锂离子电池的制备
将正极极片、隔离膜、负极极片按顺序叠好,使隔离膜处于正极极片和负极极片中间起到安全隔离的作用,并卷绕得到电化学装置。将电化学装置置于包装壳中,注入电解液并封装,获得锂离子电池。
对比例2
与对比例1的制备方法一致,不同的是对比例2中聚偏二氟乙烯与聚丙烯酸酯的质量比为84:16。
对比例3
与对比例1的制备方法一致,不同的是对比例3的隔离膜的制备方法为:
将勃姆石与聚丙烯酸酯依照质量比90:10混合并将其溶入到去离子水中以形成第二涂层浆料。随后采用微凹涂布法将所述第二涂层浆料均匀涂布到多孔基材(聚乙烯,厚度7μm,平均孔径为0.073μm,孔隙率为26%)的其中一面上,经过干燥处理以获得所述第二涂层与所述多孔基材的双层结构。
将第一聚合物粘结剂(核为聚甲基丙烯酸乙酯,壳为甲基丙烯酸甲酯-甲基苯乙烯的共聚物)加入搅拌器中,第一聚合物粘结剂的Dv50为600nm,Dv90为823nm,Dn10为121nm。然后加入辅助粘结剂聚丙烯酸酯,继续搅拌均匀,最后加入去离子水,调整浆料粘度。第一聚合物粘结剂与辅助粘结剂的质量比为90:10。将浆料涂覆在上述第二涂层与多孔基材的双层结构的两个表面上,在两表面形成第一涂层,干燥,即得所需隔离膜。
实施例1
与对比例1的制备方法一致,不同的是实施例1的隔离膜的制备方法为:
将勃姆石与聚丙烯酸酯依照质量比90:10混合并将其溶入到去离子水中以形成第二涂层浆料。随后采用微凹涂布法将所述第二涂层浆料均匀涂布到多孔基材(聚乙烯,厚度7μm,平均孔径为0.073μm,孔隙率为26%)的其中一面上,经过干燥处理以获得所述第二涂层与所述多孔基材的双层结构。
将第一聚合物粘结剂(核为聚甲基丙烯酸乙酯,壳为甲基丙烯酸甲酯-甲基苯乙烯的共聚物)加入搅拌器中,第一聚合物粘结剂的Dv50为300nm,Dv90为276nm,Dn10为109nm。然后加入三氧化二铝颗粒(第一无机颗粒),分两次加入,每次50%,搅拌均匀。三氧化二铝颗粒的Dv50为150nm。然后加入辅助粘结剂聚丙烯酸酯,继续搅拌均匀,最后加入去离子水,调整浆料粘度。第一聚合物粘结剂、三氧化二铝与辅助粘结剂的质量比为40:50:10。将浆料涂覆在上述第二涂层与多孔基材的双层结构的两个表面上,在两表面形成第一涂层,颗粒为单层结构,干燥,即得所需隔离膜。
实施例2
与实施例1的制备方法一致,不同的是实施例2中的第一聚合物粘结剂的Dv50为600nm,Dv90为823nm,Dn10为121nm。三氧化二铝颗粒的Dv50为300nm。
实施例3
与实施例1的制备方法一致,不同的是实施例3中的第一聚合物粘结剂的Dv50为1200nm,Dv90为1670nm,Dn10为133nm。三氧化二铝颗粒的Dv50为600nm。
实施例4
与实施例1的制备方法一致,不同的是实施例4中的第一聚合物粘结剂的Dv50为1600nm,Dv90为2253nm,Dn10为136nm。三氧化二铝颗粒的Dv50为800nm。
实施例5
与实施例1的制备方法一致,不同的是实施例5中的第一聚合物粘结剂的Dv50为2800nm,Dv90为3891nm,Dn10为152nm。三氧化二铝颗粒的Dv50为1400nm。
实施例6
与实施例1的制备方法一致,不同的是实施例6中的第一聚合物粘结剂的Dv50为4000nm,Dv90为5391nm,Dn10为172nm。三氧化二铝颗粒的Dv50为2000nm。
实施例7
与实施例1的制备方法一致,不同的是实施例7中的第一聚合物粘结剂的Dv50为5000nm,Dv90为6931nm,Dn10为196nm。三氧化二铝颗粒的Dv50为2500nm。
实施例8
与实施例2的制备方法一致,不同的是实施例8中的第一聚合物粘结剂、三氧化二铝与辅助粘结剂的质量比为10:80:10。
实施例9
与实施例2的制备方法一致,不同的是实施例9中的第一聚合物粘结剂、三氧化二铝与辅助粘结剂的质量比为30:60:10。
实施例10
与实施例2的制备方法一致,不同的是实施例10中的第一聚合物粘结剂、三氧化二铝与辅助粘结剂的质量比为50:40:10。
实施例11
与实施例2的制备方法一致,不同的是实施例11中的第一聚合物粘结剂、三氧化二铝与辅助粘结剂的质量比为60:30:10。
实施例12
与实施例2的制备方法一致,不同的是实施例12中的第一聚合物粘结剂、三氧化二铝与辅助粘结剂的质量比为80:10:10。
实施例13
与实施例2的制备方法一致,不同的是实施例13中的三氧化二铝颗粒的Dv50为180nm。
实施例14
与实施例2的制备方法一致,不同的是实施例14中的三氧化二铝颗粒的Dv50为240nm。
实施例15
与实施例2的制备方法一致,不同的是实施例15中的三氧化二铝颗粒的Dv50为360nm。
实施例16
与实施例2的制备方法一致,不同的是实施例16中的三氧化二铝颗粒的Dv50为420nm。
实施例17
与实施例2的制备方法一致,不同的是实施例17中的第一聚合物粘结剂的Dv90为1132nm,Dn10为182nm。
实施例18
与实施例2的制备方法一致,不同的是实施例18中的第一聚合物粘结剂的Dv90为886nm,Dn10为279nm。
实施例19
与实施例2的制备方法一致,不同的是实施例19中的第一聚合物粘结剂的Dv90为1097nm,Dn10为273nm。
之后,对实施例及对比例的锂离子电池进行粘结力和倍率性能测试,具体测试方法如下:
(1)粘结力测试
采用180°剥离测试标准测试隔离膜与正负极极片干压粘结力,将隔离膜和正负极极片裁切成54.2mm*72.5mm样品,将隔离膜与正极极片/负极极片复合,使用热压机热压,条件85℃、1Mpa、85S,将复合好的样品裁切成15mm*54.2mm小条,按照180°剥离测试标准测试粘结力。
(2)倍率性能测试
将恒温箱温度设定为25℃。0.5C恒流充电至4.4V,恒压充电至0.05C,静置5min,0.1C恒流放电至3V,静置5min。以0.1C放电容量为基准100%。之后以0.5C恒流充电至4.4V,恒压充电至0.05C,静置5min,2C恒流放电至3V,并记录2C放电容量,进行倍率性能测试。2C放电倍率性能=2C放电容量/0.1C放电容量*100%。
实施例1-19以及对比例1-2的实验参数和测量结果如下表1所示。为了方便比较,表1的结果以分组的方式示出。
表1
通过比较实施例1-19和对比例1-2可知,通过在第一涂层中采用第一无机颗粒,隔离膜与正/负极极片的干压粘结力增大,或者锂离子电池的倍率性能显著提高。
通过比较实施例1-7可知,随着第一聚合物粘结剂的颗粒粒径的增大,隔离膜与正/负极极片的干压粘结力呈现减小的趋势,而锂离子电池的倍率性能逐渐提高。
通过比较实施例2和8-12可知,随着第一无机颗粒相对于第一聚合物粘结剂的含量的增大,隔离膜与正/负极极片的干压粘结力呈现减小的趋势,而锂离子电池的倍率性能呈现增强的趋势。
通过比较实施例2和13-16可知,第一无机颗粒Dv50与第一聚合物粘结剂Dv50应满足0.3*第一聚合物粘结剂Dv50≤第一无机颗粒Dv50≤0.7*第一聚合物粘结剂Dv50,这是由于如果第一无机颗粒的粒径太小,无法起到支撑作用;而如果第一无机颗粒的粒径太大,例如接近或大于第一聚合物粘结剂粒径,热压时第一聚合物粘结剂将无法发挥粘结作用,导致粘结失效,并且随着第一无机颗粒Dv50相对于第一聚合物粘结剂Dv50的增大,隔离膜与正/负极极片的干压粘结力呈现减小的趋势,而锂离子电池的倍率性能呈现增强的趋势。
通过比较实施例2和17-19可知,当第一聚合物粘结剂的粒径过大,不满足Dv90≤1.5*Dv50,或者Dn10≤200nm的关系时,第一聚合物粘结剂颗粒的一致性较差,隔离膜与正/负极极片的干压粘结力减小,小颗粒的Dn10会影响锂离子电池的倍率性能。
通过比较实施例2、8-12和对比例3可知,通过在第一涂层中采用第一无机颗粒,锂离子电池的倍率性能显著提高。
此外,对本申请的实施例2制得的隔离膜在放大10000倍数下观察其扫描电子显微镜(SEM)图,其中,5为第一聚合物粘结剂,6为第一无机颗粒,可以看出,第一聚合物粘结剂的颗粒分布均匀。
本领域技术人员应理解,以上实施例仅是示例性实施例,在不背离本申请的精神和范围的情况下,可以进行多种变化、替换以及改变。
Claims (9)
1.一种隔离膜,包括:
多孔基材;
第一涂层,位于所述多孔基材的至少一个表面上;
其中,所述第一涂层包括第一聚合物粘结剂和第一无机颗粒,所述第一聚合物粘结剂为核壳结构的颗粒;
其中,所述隔离膜满足下式(4):
0.3*第一聚合物粘结剂Dv50≤第一无机颗粒Dv50≤0.7*第一聚合物粘结剂Dv50 式(4)。
2.根据权利要求1所述的隔离膜,还包括设置在所述多孔基材和所述第一涂层之间的第二涂层,所述第二涂层包括第二聚合物粘结剂和第二无机颗粒。
3.根据权利要求1所述的隔离膜,其中,所述第一涂层还包括辅助粘结剂,所述第一聚合物粘结剂、所述第一无机颗粒和所述辅助粘结剂的质量比为10-80:85-5:5-15。
4.根据权利要求1所述的隔离膜,其中,所述第一涂层为颗粒单层结构。
5.根据权利要求1所述的隔离膜,其中,所述第一聚合物粘结剂满足下式(1)-(3):
300nm≤Dv50≤5000nm 式(1);
Dv90≤1.5*Dv50 式(2);
Dn10≤200nm 式(3);
其中,Dv50表示在体积基准的粒度分布中,从小粒径侧起、达到体积累积50%的粒径,Dv90表示在体积基准的粒度分布中,从小粒径侧起、达到体积累积90%的粒径,Dn10表示在数量基准的粒度分布中,从小粒径侧起、达到数量累积10%的粒径。
6.根据权利要求1所述的隔离膜,其中,所述第一聚合物粘结剂的核选自以下单体中的至少一种聚合形成的聚合物:丙烯酸乙酯、丙烯酸丁酯、甲基丙烯酸乙酯、苯乙烯、氯苯乙烯、氟苯乙烯、甲基苯乙烯、丙烯酸、甲基丙烯酸、马来酸。
7.根据权利要求1所述的隔离膜,其中,所述第一聚合物粘结剂的壳选自以下单体中的至少一种聚合形成的聚合物:丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、乙烯、氯苯乙烯、氟苯乙烯、甲基苯乙烯、丙烯腈、甲基丙烯腈。
8.根据权利要求1所述的隔离膜,其中,所述第一无机颗粒选自三氧化二铝、二氧化硅、氧化镁、氧化钛、二氧化铪、氧化锡、二氧化铈、氧化镍、氧化锌、氧化钙、氧化锆、氧化钇、碳化硅、勃姆石、氢氧化铝、氢氧化镁、氢氧化钙、硫酸钡中的一种或多种。
9.一种电化学装置,包括:
正极极片;
负极极片;
以及根据权利要求1至8中任一项所述的隔离膜,所述隔离膜设置在所述正极极片和所述负极极片之间。
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