CN113498561A - 非水电解质二次电池 - Google Patents
非水电解质二次电池 Download PDFInfo
- Publication number
- CN113498561A CN113498561A CN202080016963.4A CN202080016963A CN113498561A CN 113498561 A CN113498561 A CN 113498561A CN 202080016963 A CN202080016963 A CN 202080016963A CN 113498561 A CN113498561 A CN 113498561A
- Authority
- CN
- China
- Prior art keywords
- phosphate particles
- filler layer
- particles
- nonaqueous electrolyte
- secondary battery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000011255 nonaqueous electrolyte Substances 0.000 title claims abstract description 41
- 239000002245 particle Substances 0.000 claims abstract description 134
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 87
- 239000010452 phosphate Substances 0.000 claims abstract description 76
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 76
- 239000000945 filler Substances 0.000 claims abstract description 66
- 239000000463 material Substances 0.000 claims abstract description 50
- 239000010954 inorganic particle Substances 0.000 claims abstract description 34
- 239000011148 porous material Substances 0.000 claims abstract description 31
- 239000002033 PVDF binder Substances 0.000 claims description 33
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 33
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- 230000035515 penetration Effects 0.000 claims description 8
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- 239000010410 layer Substances 0.000 description 79
- 235000021317 phosphate Nutrition 0.000 description 64
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- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical class [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 6
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Abstract
非水电解质二次电池中使用的分隔件具有多孔的基材和配置在前述基材上的填料层,前述填料层包含磷酸盐颗粒和耐热性比前述磷酸盐颗粒高的无机颗粒,前述磷酸盐颗粒的体积基准的10%粒径(D10)为0.02μm以上且0.5μm以下,并且比前述基材的平均孔径小,前述磷酸盐颗粒的BET比表面积为5m2/g以上且100m2/g以下,并且比前述无机颗粒的BET比表面积大,前述无机颗粒的体积基准的50%粒径(D50)比前述磷酸盐颗粒的体积基准的50%粒径(D50)大。
Description
技术领域
本公开涉及非水电解质二次电池。
背景技术
非水电解质二次电池在过充电、内部短路、外部短路、大电流导致的过度的电阻加热等异常时,有时会发热。以往,作为抑制非水电解质二次电池在异常时的温度上升的技术之一,已知有分隔件的隔断功能。隔断功能是分隔件通过热进行熔融从而封堵自身的孔隙的功能。在电池异常时,通过隔断功能,例如正负极间的离子传导(锂离子的移动)被中断,因此电池温度的上升被抑制。
现有技术文献
专利文献
专利文献1:国际公开第2012/137376号
专利文献2:中国专利申请公开第107737702号说明书
发明内容
然而,近年来,随着电池的高容量化的要求,对分隔件的薄膜化进行研究,但若分隔件的厚度变薄,则在电池异常时,会发生分隔件的变形、收缩,变得难以发挥隔断功能,从而难以抑制电池温度的上升。
于是,本公开的目的为:提供在电池异常时可以抑制电池温度的上升的非水电解质二次电池。
作为本公开的一个方式的非水电解质二次电池具备:具有正极、负极和分隔件的电极体;和非水电解质,前述分隔件具有多孔的基材和配置在前述基材上的填料层,前述填料层包含磷酸盐颗粒和耐热性比前述磷酸盐颗粒高的无机颗粒,前述磷酸盐颗粒的体积基准的10%粒径(D10)为0.02μm以上且0.5μm以下,并且比前述基材的平均孔径小,前述磷酸盐颗粒的BET比表面积为5m2/g以上且100m2/g以下,并且比前述无机颗粒的BET比表面积大,前述无机颗粒的体积基准的50%粒径(D50)比前述磷酸盐颗粒的体积基准的50%粒径(D50)大。
通过本公开的一个方式,可以提供在电池异常时能够抑制电池温度的上升的非水电解质二次电池。
附图说明
图1为实施方式的一个例子的非水电解质二次电池的立体图。
图2为示出图1的非水电解质二次电池中使用的电极体的一个例子的部分扩大截面图。
图3为用于说明网格状的聚偏氟乙烯的状态的填料层的部分扩大俯视图。
具体实施方式
作为本公开的一个方式的非水电解质二次电池具备:具有正极、负极和分隔件的电极体;和非水电解质,前述分隔件具有多孔的基材和配置在前述基材上的填料层,前述填料层包含磷酸盐颗粒和耐热性比前述磷酸盐颗粒高的无机颗粒,前述磷酸盐颗粒的体积基准的10%粒径(D10)为0.02μm以上且0.5μm以下,并且比前述基材的平均孔径小,前述磷酸盐颗粒的BET比表面积为5m2/g以上且100m2/g以下,并且比前述无机颗粒的BET比表面积大,前述无机颗粒的体积基准的50%粒径(D50)比前述磷酸盐颗粒的体积基准的50%粒径(D50)大。
通常,多孔的基材具有以下功能:通过电池异常时的热,多孔的基材进行熔融从而封堵自身的孔隙的隔断功能,进而,本公开中,由于电池异常时的热,填料层中包含的磷酸盐颗粒以热为加速因子进行熔融、聚合,填埋多孔的基材的孔隙,因此分隔件的隔断功能提高。特别是通过将磷酸盐颗粒的粒径及BET比表面积设为上述范围,由于电池异常时的热,磷酸盐颗粒易于熔融,可以快速填埋多孔的基材的孔隙。另外,多孔的基材通过电池异常时的热而变形、收缩时,有时无法充分地发挥分隔件的隔断功能。本公开中,填料层中包含耐热性比磷酸盐颗粒高的无机颗粒,因此该填料层具有高耐热性。特别是包含具有上述规定的粒径及BET比表面积的无机颗粒的填料层具有充分的高耐热性。因此,多孔的基材呈被耐热性高的填料层支承的状态,因此在电池异常时,多孔的基材的变形、收缩被抑制,分隔件的隔断功能得到维持。因此,在电池异常时,例如正负极间的锂离子的移动被分隔件迅速地中断,发热反应被充分地抑制,因此电池温度的上升被抑制。
以下,对本公开的非水电解质二次电池的实施方式的一个例子进行详细说明。
图1为实施方式的一个例子的非水电解质二次电池的立体图。非水电解质二次电池10具备电极体11、非水电解质和收纳它们的方形的电池壳体14。电极体11具有正极、负极和分隔件。电极体11为多个正极及多个负极借助分隔件1张张交替层叠而成的层叠型的电极体。需要说明的是,也可应用正极及负极借助分隔件卷绕而成的卷绕型的电极体等其他方式的电极体代替层叠型的电极体。
电池壳体14具有大致箱形的壳体主体15、封堵壳体主体15的开口部的封口体16、与正极电连接的正极端子12、与负极电连接的负极端子13。壳体主体15及封口体16例如由以铝为主要成分的金属材料构成。正极端子12及负极端子13借助绝缘构件17被固定在封口体16上。通常,封口体16上设置有气体排出机构(未图示)。需要说明的是,电池壳体并不限定于方形,例如也可以为圆筒形、硬币形、按钮形等金属制壳体、由树脂薄膜构成的树脂制壳体(层压体)等。
图2为示出图1的非水电解质二次电池中使用的电极体的一个例子的部分扩大截面图。以下,使用图2对正极、负极、分隔件进行说明。
[正极]
正极18具备正极集电体和在该集电体上形成的正极复合材料层。正极集电体可以使用铝等在正极18的电位范围稳定的金属的箔、将该金属配置在表层上的薄膜等。正极复合材料层例如优选包含正极活性物质、导电材料及粘结材料,并形成在正极集电体的两面上。正极18可以通过在正极集电体上涂布包含正极活性物质、导电材料、粘结材料等的正极复合材料浆料,使涂膜干燥后进行轧制,将正极复合材料层形成在正极集电体的两面上来制作。从电池的高容量化的观点来看,正极复合材料层的密度为3.6g/cc以上,优选为3.6g/cc以上且4.0g/cc以下。
作为正极活性物质,可以例示出含有Co、Mn、Ni、Al等金属元素的锂金属复合氧化物。作为锂金属复合氧化物,可以例示出LixCoO2、LixNiO2、LixMnO2、LixCoyNi1-yO2、LixCoyM1- yOz、LixNi1-yMyOz、LixMn2O4、LixMn2-yMyO4、LiMPO4、Li2MPO4F(M:Na、Mg、Sc、Y、Mn、Fe、Co、Ni、Cu、Zn、Al、Cr、Pb、Sb、B之中的至少1种,0.95≤x≤1.2、0.8<y≤0.95、2.0≤z≤2.3)等。
作为正极复合材料层中包含的导电材料,可以例示出炭黑、乙炔黑、科琴黑、石墨、碳纳米管、碳纳米纤维、石墨烯等碳材料。作为正极复合材料层中包含的粘结材料,可举出聚四氟乙烯(PTFE)、聚偏氟乙烯(PVdF)等含氟树脂、聚丙烯腈(PAN)、聚酰亚胺、丙烯酸类树脂、聚烯烃、羧甲基纤维素(CMC)或其盐、丁苯橡胶(SBR)、聚丙烯酸(PAA)或其盐、聚乙烯醇(PVA)、聚氧化乙烯(PEO)等。
[负极]
负极20具备负极集电体和在该集电体上形成的负极复合材料层。负极集电体可以使用铜等在负极20的电位范围稳定的金属的箔、将该金属配置在表层上的薄膜等。负极复合材料层例如优选包含负极活性物质及粘结材料,并形成在负极集电体的两面上。负极20可以通过在负极集电体上涂布包含负极活性物质及粘结材料等的负极复合材料浆料,使涂膜干燥后进行轧制,将负极复合材料层形成在负极集电体的两面上来制作。
作为负极活性物质,只要能够可逆地吸储、释放锂离子就没有特别限定,可举出例如天然石墨、人造石墨等碳材料、硅(Si)、锡(Sn)等与Li合金化的金属、包含Si、Sn等金属元素的氧化物、锂钛复合氧化物等。需要说明的是,使用锂钛复合氧化物时,负极复合材料层优选包含炭黑等导电材料。负极复合材料层中包含的粘结材料可以使用与正极18的情况相同的材料。
[分隔件]
如图2所例示,分隔件22具有多孔的基材24和配置在基材24上的填料层26。填料层26具有磷酸盐颗粒和耐热性比磷酸盐颗粒高的无机颗粒。另外,填料层26优选包含粘结材料。
图2示出的分隔件22中,填料层26配置在基材24的两面上,但也可配置在基材24的两面之中的任意一面上。但是,填料层26中包含的磷酸盐颗粒的熔融、缩聚不仅会由电池异常时的热引起,有时也会由在电池异常时的正极18的电位引起。因此,从使分隔件22的隔断功能迅速地起作用等方面来看,填料层26优选至少配置在与正极18相对的基材24的面上。
基材24由具有离子透过性及绝缘性的多孔片、例如微多孔薄膜、织布、无纺布等构成。作为构成基材24的树脂,可以例示出聚乙烯、聚丙烯、聚乙烯与α烯烃的共聚物等聚烯烃、丙烯酸类树脂、聚苯乙烯、聚酯、纤维素等。基材24例如以聚烯烃为主要成分构成,也可实质上仅由聚烯烃构成。基材24可以为单层结构,也可具有层叠结构。基材24的厚度没有特别限定,例如优选为3μm以上且20μm以下。
从确保锂离子透过性等方面来看,基材24的孔隙率例如优选为30%以上且70%以下。基材24的孔隙率用下述的方法测定。
(1)对基材的10处进行直径2cm的圆形冲孔,分别测定进行了冲孔的基材的小片的中心部的厚度h、质量w。
(2)根据厚度h、质量w,求出10张小片的体积V、质量W,根据以下式算出孔隙率ε。
孔隙率ε(%)=((ρV-W)/(ρV))×100
ρ:构成基材的材料的密度
基材24的平均孔径例如为0.02μm以上且0.5μm以下,优选为0.03μm以上且0.3μm以下。基材24的平均孔径使用能够基于泡点法(JIS K3832、ASTM F316-86)测定孔径的Perm-Porometer(西华产业株式会社制)进行测定。基材24的最大孔径例如为0.05μm以上且1μm以下,优选为0.05μm以上且0.5μm以下。
作为填料层26中包含的磷酸盐颗粒,可以例示出Li3PO4、LiPON、Li2HPO4、LiH2PO4、Na3PO4、Na2HPO4、NaH2PO4、Zr3(PO4)4、Zr(HPO4)2、HZr2(PO4)3、K3PO4、K2HPO4、KH2PO4、Ca3(PO4)2、CaHPO4、Mg3(PO4)2、MgHPO4等。其中,从抑制副反应等观点来看,优选选自磷酸锂(Li3PO4)、磷酸氢二锂(Li2HPO4)、磷酸二氢锂(LiH2PO4)中的至少1种。
填料层26中包含的无机颗粒只要是耐热性比填料层26中包含的磷酸盐颗粒高的无机颗粒(即,熔点比磷酸盐颗粒高的无机颗粒),就没有特别限制,例如,从抑制正负极间的短路发生的方面来看,优选电绝缘性高的无机颗粒。作为无机颗粒,可举出例如金属氧化物、金属氧化物水合物、金属氢氧化物、金属氮化物、金属碳化物、金属硫化物等。
作为金属氧化物、金属氧化物水合物的例子,可举出例如氧化铝(alumina)、勃姆石(Al2O3H2O或AlOOH)、氧化镁、氧化钛、氧化锆、氧化硅或氧化钇、氧化锌等。作为金属氮化物的例子,可举出氮化硅、氮化铝、氮化硼或氮化钛等。作为金属碳化物的例子,可举出碳化硅或碳化硼等。作为金属硫化物的例子,可举出硫酸钡等。作为金属氢氧化物的例子,可举出氢氧化铝等。需要说明的是,对于勃姆石这样的对氧化铝进行改性后熔融的物质的熔点而言,改性后的物质的熔点比磷酸盐颗粒的熔点高是理想的。
另外,无机颗粒也可使用沸石(M2/nO·Al2O3·xSiO2·yH2O、M为金属元素、x≥2、y≥0)等多孔铝硅酸盐、滑石(Mg3Si4O10(OH)2)等层状硅酸盐、钛酸钡(BaTiO3)、钛酸锶(SrTiO3)等矿物。这些之中,从绝缘性、耐热性等观点来看,选自氧化铝、勃姆石、滑石、氧化钛、氧化镁中的至少1种是理想的。
磷酸盐颗粒的BET比表面积为5m2/g以上且100m2/g以下、并且比无机颗粒的BET比表面积大即可,优选为20m2/g以上且80m2/g以下。BET比表面积按照JIS R1626的BET法(氮吸附法)测定。通常,若考虑电池制造时的温度、通常使用时的电池内温度及异常时的电池内温度,则磷酸盐颗粒优选以140℃~190℃左右的温度进行熔融。并且,具有上述范围的BET比表面积的磷酸盐颗粒易于在140℃~190℃左右的温度下熔融,因此通过使用该颗粒,通过电池异常时的热而进行了熔融、缩聚的磷酸盐可以迅速地封堵基材24的孔隙。
无机颗粒的BET比表面积比磷酸盐颗粒的BET比表面积小即可,例如优选为3m2/g以上且12m2/g以下。将无机颗粒的BET比表面积设为比磷酸盐颗粒的BET比表面积小,优选设为3m2/g以上且7m2/g以下,由此可以对填料层26赋予充分的耐热性。
磷酸盐颗粒的体积基准的10%粒径(D10)为0.02μm以上且0.5μm以下,并且比基材24的平均孔径小即可,优选为0.03μm以上且0.3μm以下、并且比基材24的平均孔径小。通过满足上述范围,分隔件22的制造时的磷酸盐颗粒的一部分易于进入基材24的孔隙内,或在电池异常时磷酸盐可以迅速地封堵基材24的孔隙,因此可以有效地抑制在电池异常时的电池温度的上升。从提高填料层26的耐热性等方面来看,无机颗粒的体积基准的10%粒径(D10)例如优选比磷酸盐颗粒的体积基准的10%粒径(D10)大,例如优选为0.3μm以上。上限值并无特别限定,例如为1μm以下。
此处,体积基准的10%粒径(D10)是指磷酸盐颗粒、无机颗粒的粒径分布的体积累积值成为10%的粒径。需要说明的是,后述50%粒径(D50)、90%粒径(D90)分别指粒径分布中体积累积值成为50%、90%的粒径。50%粒径(D50)也称作中值粒径。磷酸盐颗粒、无机颗粒的粒径分布通过激光衍射法(激光衍射散射式粒度分布测定装置)测定。以下,若无特别说明,则10%粒径、50%粒径及90%粒径的含义为体积基准的粒径。
磷酸盐颗粒的50%粒径(D50)例如优选为0.05μm以上且1μm以下,更优选为0.1μm以上且1μm以下。磷酸盐颗粒的50%粒径(D50)在该范围外时,与在该范围内时相比,有时在电池异常时抑制电池温度的上升的效果会减少。需要说明的是,磷酸盐颗粒的50%粒径(D50)也可比基材24的平均孔径小。无机颗粒的50%粒径(D50)比磷酸盐颗粒的50%粒径(D50)大即可,例如优选为0.1μm以上且1μm以下,更优选为0.2μm以上且0.8μm以下。如此,通过将无机颗粒的50%粒径(D50)设为比磷酸盐颗粒的50%粒径(D50)大,可以对填料层26赋予充分的耐热性,从而可以有效地抑制基材24基于热的变形/收缩。
磷酸盐颗粒的90%粒径(D90)比基材24的平均孔径大是理想的。90%粒径(D90)例如优选为0.2μm以上且2μm以下,更优选为0.5μm以上且1.5μm以下。若D90在该范围内,则分隔件22的制造时可以将进入基材24的孔隙内的磷酸盐颗粒的量调节为适度的范围,可以更有效地抑制在电池异常时的电池温度的上升。从提高填料层26的耐热性等方面来看,无机颗粒的90%粒径(D90)例如优选比磷酸盐颗粒的体积基准的90%粒径(D90)大,例如优选为0.4μm以上。上限值并无特别限定,例如为1μm以下。
从设为充分封堵基材24的孔隙的量的方面来看,填料层26中的磷酸盐颗粒的含量优选为40质量%以上且80质量%以下,更优选为50质量%以上且70质量%以下。从使填料层26的耐热性提高等方面来看,填料层26中的无机颗粒的含量优选为10质量%以上且40质量%以下,更优选为20质量%以上且40质量%以下。
分隔件22中,填料层26的磷酸盐颗粒的一部分进入基材24的孔隙内,该颗粒的进入深度的平均值优选为0.02μm以上且2μm以下,更优选为0.1μm以上且1.5μm以下。
此处,磷酸盐颗粒的进入深度是指沿基材24的厚度方向,从基材24的表面到基材24的内部进入的颗粒的端部为止的长度。进入深度可以通过使用扫描型电子显微镜(SEM)或透射式电子显微镜(TEM)的基材24的截面观察来测量。
磷酸盐颗粒优选进入基材24的表面的大致全部区域的孔隙内。即,进入孔隙内的磷酸盐颗粒大致均匀地存在于基材24的表面上。另外,磷酸盐颗粒的上述进入深度优选在基材24的表面的大致全部区域上大致均匀。
相对于基材24的厚度,磷酸盐颗粒的上述进入深度的平均值例如为1%以上且50%以下,优选为5%以上且30%以下。根据基材24的平均孔径调节磷酸盐颗粒的10%粒径(D10)等,能够控制进入基材24的内部的磷酸盐颗粒的深度。
在基材24的两面上设置填料层26时,填料层26的总计厚度(除磷酸盐颗粒的进入深度外的厚度)例如优选为6μm以下,更优选为1μm以上且6μm以下,特别是更优选为1μm以上且4μm以下。1层填料层26的厚度例如优选为4μm以下,更优选为0.5μm以上且2μm以下。
从确保电池的充放电时的良好的离子透过性的方面、确保物理强度等方面来看,填料层26的孔隙率优选为30%以上且70%以下。填料层26的孔隙率用下述式算出。
填料层的孔隙率(%)=100-[[W÷(d×ρ)]×100]
W:填料层的单位面积重量(g/cm2)
d:填料层的厚度(cm)
ρ:填料层的平均密度(g/cm3)
从提高层的机械强度、粘接性等方面来看,填料层26优选包含粘结材料。作为粘结材料,可举出例如聚乙烯、聚丙烯、聚乙烯与α烯烃的共聚物等聚烯烃、PVdF、PTFE、聚氟乙烯(PVF)等含氟树脂、偏二氟乙烯-六氟丙烯-四氟乙烯共聚物、乙烯-四氟乙烯共聚物等含氟橡胶、苯乙烯-丁二烯共聚物及其氢化物、丙烯腈-丁二烯共聚物及其氢化物、丙烯腈-丁二烯-苯乙烯共聚物及其氢化物、甲基丙烯酸酯-丙烯酸酯共聚物、苯乙烯-丙烯酸酯共聚物、丙烯腈-丙烯酸酯共聚物、聚乙酸乙烯酯、聚苯醚、聚砜、聚醚砜、聚苯硫醚、聚醚酰亚胺、聚酰胺酰亚胺、聚酰胺、聚-N-乙烯基乙酰胺、聚酯、聚丙烯腈、纤维素、乙烯-乙酸乙酯共聚物、聚氯乙烯、异戊二烯橡胶、丁二烯橡胶、聚丙烯酸甲酯、聚丙烯酸乙酯、聚乙烯醇、CMC、丙烯酰胺、PVA、甲基纤维素、瓜尔胶、藻酸钠、卡拉胶、黄原胶及这些的盐等。这些之中,从粘接性等方面来看,优选聚-N-乙烯基乙酰胺、聚偏氟乙烯系树脂,从与电极的粘接性、离子透过性等方面来看,更优选网格状的聚偏氟乙烯系树脂。
图3是用于说明网格状的聚偏氟乙烯的状态的填料层的部分扩大俯视图。如图3所示,填料层26中包含的网格状的聚偏氟乙烯系树脂28呈纤维状并彼此三维地连接,形成网格状的网络。需要说明的是,纤维状表示长度(纤维长)相对于直径(纤维径)的比(长径比)为3以上的状态。并且,填料层26内的颗粒30(磷酸盐颗粒、无机颗粒)被聚偏氟乙烯系树脂28的网格状的网络固定。这样的填料层26具有大量的细孔32,呈这些细孔32连接而成的结构。因此,填料层26呈锂离子易于从一面到达另一面的结构。另外,填料层26通过表面的网格状的聚偏氟乙烯系树脂28的锚固效应,相对于电极(正极18、负极20)具有粘接性。粘接电极与填料层26时,例如,在常温或温感下,在电极体11的层叠方向进行压制是理想的。图3示出的填料层26中,颗粒30(磷酸盐颗粒、无机颗粒)的表面的一部分被聚偏氟乙烯系树脂28覆盖,从与电极的粘接性等方面来看,优选磷酸盐颗粒的表面整体被聚偏氟乙烯系树脂28覆盖,更优选磷酸盐颗粒的表面整体及无机颗粒的表面整体被聚偏氟乙烯系树脂28覆盖。
聚偏氟乙烯系树脂可以适宜使用偏二氟乙烯的均聚物(即聚偏氟乙烯)、偏二氟乙烯与其他能够共聚的单体的共聚物、或这些的混合物。能够与偏二氟乙烯共聚的单体可以使用四氟乙烯、六氟丙烯、三氟乙烯、氟乙烯等中的一种或二种以上。从与电极的粘接性等方面来看,聚偏氟乙烯系树脂优选含有70质量%以上作为构成单元的偏二氟乙烯,更优选含有80质量%以上。另外,从与电极的粘接性等方面来看,聚偏氟乙烯系树脂优选含有3质量%以上且15质量%以下的六氟丙烯作为构成单元。
填料层26中的粘结材料例如为2质量%以上且8质量%以下。
使用网格状的聚偏氟乙烯系树脂作为粘结材料时,考虑到与电极的粘接性等,填料层26中的聚偏氟乙烯系树脂的含量优选为15质量%以上且40质量%以下,更优选为15质量%以上且25质量%以下。填料层26中的聚偏氟乙烯系树脂的含量小于15质量%时,与电极的粘接性降低,有正极与负极的对置发生偏差的担忧。另外,填料层26中的聚偏氟乙烯系树脂的含量大于40质量%时,例如,由于填料层26的填料的减少,有时分隔件的耐热性、强度降低。
填料层26还可以包含杂多酸。认为通过添加杂多酸,促进熔融的磷酸盐的缩聚。作为杂多酸,可以例示出磷钼酸、磷钨酸、磷钼钨酸、磷钼钒酸、磷钼钨钒酸、磷钨钒酸、硅钨酸、硅钼酸、硅钼钨酸、硅钼钨钒酸等。
填料层26例如通过在基材24的表面上涂布包含磷酸盐颗粒、无机颗粒、任意粘结材料等的浆料,并进行干燥而形成。另外,例如也可以在基材24的表面上涂布包含磷酸盐颗粒、无机颗粒、聚偏氟乙烯系树脂及分散介质的浆料,使其通过非溶剂中、或非溶剂及分散介质的混合溶剂中从而将分散介质提取(相分离),之后,通过使其干燥的相分离法等形成。通过这样的相分离法,形成包含磷酸盐颗粒、无机颗粒及网格状的聚偏氟乙烯系树脂的填料层26。浆料的涂布方法例如可以为凹版印刷法等以往公知的方法。
相分离法所使用的非溶剂为几乎不溶解聚偏氟乙烯系树脂的溶剂,可举出例如水、醇类、醚类等。分散介质为溶解聚偏氟乙烯系树脂的溶剂,可举出例如N-甲基-2-吡咯烷酮、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺等。使用水作为非溶剂时,从分散介质的提取速度的快慢来看,优选使用N,N-二甲基乙酰胺。
需要说明的是,基材24的孔隙内的磷酸盐颗粒的进入深度可以通过磷酸盐颗粒的粒径、浆料的涂膜的干燥条件、浆料的涂布方法等控制。例如,使磷酸盐颗粒的10%粒径(D10)减小、使涂膜的干燥条件变缓时,磷酸盐颗粒易于进入基材24的内部。另外,使浆料的涂布中使用的凹印辊的转速变慢时,磷酸盐颗粒易于进入基材24的内部。
[非水电解质]
非水电解质包含非水溶剂和溶解在非水溶剂中的电解质盐。非水电解质并不限定于液体电解质(非水电解液),也可以为使用凝胶状聚合物等的固体电解质。非水溶剂可以使用例如酯类、醚类、乙腈等腈类、二甲基甲酰胺等酰胺类及这些的2种以上的混合溶剂等。非水溶剂也可含有这些溶剂的氢的至少一部分被氟等卤素原子取代而成的卤素取代物。
作为上述酯类的例子,可举出碳酸亚乙酯(EC)、碳酸亚丙酯(PC)、碳酸亚丁酯等环状碳酸酯、碳酸二甲酯(DMC)、碳酸甲乙酯(EMC)、碳酸二乙酯(DEC)、碳酸甲丙酯、碳酸乙丙酯、碳酸甲异丙酯等链状碳酸酯、γ-丁内酯(GBL)、γ-戊内酯(GVL)等环状羧酸酯、乙酸甲酯、乙酸乙酯、乙酸丙酯、丙酸甲酯(MP)、丙酸乙酯、γ-丁内酯等链状羧酸酯等。
作为上述醚类的例子,可举出1,3-二氧戊环、4-甲基-1,3-二氧戊环、四氢呋喃、2-甲基四氢呋喃、环氧丙烷、1,2-环氧丁烷、1,3-二氧杂环己烷、1,4-二氧杂环己烷、1,3,5-三氧杂环己烷、呋喃、2-甲基呋喃、1,8-桉树脑、冠醚等环状醚、1,2-二甲氧基乙烷、二乙醚、二丙醚、二异丙醚、二丁醚、二己醚、乙基乙烯醚、丁基乙烯醚、甲基苯醚、乙基苯醚、丁基苯醚、戊基苯醚、甲氧基甲苯、苄基乙醚、二苯醚、二苄醚、邻二甲氧基苯、1,2-二乙氧基乙烷、1,2-二丁氧基乙烷、二乙二醇二甲醚、二乙二醇二乙醚、二乙二醇二丁醚、1,1-二甲氧基甲烷、1,1-二乙氧基乙烷、三乙二醇二甲醚、四乙二醇二甲醚等链状醚类等。
作为上述卤素取代物,优选使用氟代碳酸亚乙酯(FEC)等氟化环状碳酸酯、氟化链状碳酸酯、氟代丙酸甲酯(FMP)等氟化链状羧酸酯等。
电解质盐优选锂盐。作为锂盐的例子,可举出LiBF4、LiClO4、LiPF6、LiAsF6、LiSbF6、LiAlCl4、LiSCN、LiCF3SO3、LiCF3CO2、Li(P(C2O4)F4)、LiPF6-x(CnF2n+1)x(1<x<6,n为1或2)、LiB10Cl10、LiCl、LiBr、LiI、氯硼烷锂、低级脂肪族羧酸锂、Li2B4O7、Li(B(C2O4)F2)等硼酸盐类、LiN(SO2CF3)2、LiN(C1F2l+1SO2)(CmF2m+1SO2){l,m为0以上的整数}等酰亚胺盐类等。锂盐可以单独使用一种,也可混合使用多种。这些之中,从离子传导性、电化学稳定性等观点来看,优选使用LiPF6。锂盐的浓度优选设为每1L非水溶剂0.8~1.8mol。
实施例
以下,通过实施例对本公开进行进一步说明,但本公开并不限定于这些实施例。
<实施例1>
[分隔件的制作]
以下述的步骤,制作具有由填料层/聚乙烯制的多孔基材/填料层形成的3层结构的分隔件。
(1)浆料的制备
以46:46:8的质量比混合BET比表面积为61.3m2/g、D10为0.091μm、D50为0.17μm的磷酸锂颗粒(Li3PO4)、BET比表面积为4.3m2/g、D10为0.35μm、D50为0.46μm的氧化铝(Al2O3)、和聚偏氟乙烯系树脂(包含5质量%的六氟丙烯),添加N-甲基-2-吡咯烷酮(NMP),由此制备浆料。
(2)填料层的形成
在厚度为12μm的单层的聚乙烯制多孔基材的一面上涂布上述浆料后,使其在60℃下干燥6分钟,由此在基材的一面上形成填料层。另外,进行上述同样的操作,在基材的另一面上也形成填料层。聚乙烯制多孔基材的平均孔径为0.5μm。
[正极的制作]
作为正极活性物质,使用Li1.05Ni0.82Co0.15Al0.03O2所示的锂复合氧化物颗粒。在NMP中以100:1:1的质量比混合正极活性物质、炭黑和PVdF,制备正极复合材料浆料。接着,将该正极复合材料浆料涂布在由铝箔形成的正极集电体的两面上,使涂膜干燥后,通过轧辊进行轧制,进而安装铝制的集电片,制作在正极集电体的两面上形成有正极复合材料层的正极。需要说明的是,正极复合材料的填充密度为3.70g/cm3。
[负极的制作]
在水中以98:1:1的固体成分质量比混合人造石墨、羧甲基纤维素钠(CMC-Na)和丁苯橡胶(SBR)的分散剂,制备负极复合材料浆料。接着,将该负极复合材料浆料涂布在由铜箔形成的负极集电体的两面上,使涂膜干燥后,通过轧辊进行轧制,进而安装镍制的集电片,制作在负极集电体的两面上形成有负极复合材料层的负极。需要说明的是,负极复合材料的填充密度为1.70g/cm3。
[非水电解质的制备]
对于以3:3:4的体积比混合有碳酸亚乙酯(EC)、碳酸甲乙酯(EMC)和碳酸二甲酯(DMC)的混合溶剂,以成为1摩尔/升的浓度的方式溶解六氟化磷酸锂(LiPF6)。进而,相对于上述混合溶剂以1质量%的浓度使碳酸亚乙烯酯(VC)溶解,制备非水电解质。
[非水电解质二次电池的制作]
借助上述分隔件将上述负极及上述正极交替地层叠,由此制作层叠型的电极体。在层叠方向上对该电极体进行压制后,与上述非水电解质一起收纳在方形的电池壳体中,制作750mAh的方形试验电池单元。
<实施例2>
浆料的制备中,除使用BET比表面积为10.3m2/g、D10为0.15μm、D50为0.2μm的氧化铝(Al2O3)以外,与实施例1同样地制作非水电解质二次电池。
<实施例3>
浆料的制备中,除使用BET比表面积为6.5m2/g、D10为0.42μm、D50为0.7μm的磷酸锂颗粒(Li3PO4)以外,与实施例1同样地制作非水电解质二次电池。
<比较例1>
浆料的制备中,除使用BET比表面积为3.3m2/g、D10为0.68μm、D50为1.15μm的磷酸锂颗粒(Li3PO4)以外,与实施例1同样地制作非水电解质二次电池。
<比较例2>
填料层的形成中,除使用BET比表面积为8m2/g、D10为0.52μm、D50为0.72μm的磷酸锂颗粒(Li3PO4)以外,与实施例1同样地制作非水电解质二次电池。
<比较例3>
填料层的形成中,除使用BET比表面积为5.2m2/g、D10为0.36μm、D50为0.65μm的磷酸锂颗粒(Li3PO4)以外,与实施例1同样地制作非水电解质二次电池。
[钉刺试验]
在25℃的环境下,以225mA的恒定电流对各实施例及各比较例的电池进行充电至电池电压成为4.2V,之后,以4.2V的恒定电压进行充电至电流值成为37.5mA。在25℃的环境下,在上述充电状态的电池的侧面中央部上,以0.1mm/秒的速度,将的大小的圆钉向电极体的层叠方向穿刺,在完全贯通电池时,使圆钉的穿刺停止。测定距离圆钉穿刺过的电池侧面部5mm的位置的电池温度,求出最高到达温度。将其结果示于表1。
[表1]
实施例1~3与比较例1~3相比,结果钉刺试验中的最高到达温度均较低,即,呈在电池异常时的电池温度的上升被抑制的结果。需要说明的是,此处为测试用电池的试验,因此虽然是层叠型的电池,但未赋予分隔件与电极的粘接性而实施。以产品形式量产时,需要粘接。此时,如前所述,另外设置粘接功能层或利用包含网格状的聚偏氟乙烯系树脂的填料层是理想的。
附图标记说明
10 非水电解质二次电池
11 电极体
12 正极端子
13 负极端子
14 电池壳体
15 壳体主体
16 封口体
17 绝缘构件
18 正极
20 负极
22 分隔件
24 基材
26 填料层
28 聚偏氟乙烯系树脂
30 颗粒
32 细孔。
Claims (6)
1.一种非水电解质二次电池,其具备:
具有正极、负极和分隔件的电极体;和
非水电解质,
所述分隔件具有多孔的基材和配置在所述基材上的填料层,
所述填料层包含磷酸盐颗粒和耐热性比所述磷酸盐颗粒高的无机颗粒,
所述磷酸盐颗粒的体积基准的10%粒径(D10)为0.02μm以上且0.5μm以下,并且比所述基材的平均孔径小,
所述磷酸盐颗粒的BET比表面积为5m2/g以上且100m2/g以下,并且比所述无机颗粒的BET比表面积大,
所述无机颗粒的体积基准的50%粒径(D50)比所述磷酸盐颗粒的体积基准的50%粒径(D50)大。
2.根据权利要求1所述的非水电解质二次电池,其中,所述磷酸盐颗粒的一部分进入所述基材的孔隙内,该颗粒的进入深度的平均值为0.02μm以上且2μm以下。
3.根据权利要求1或2所述的非水电解质二次电池,其中,所述填料层的厚度为4μm以下。
4.根据权利要求1~3中任一项所述的非水电解质二次电池,其中,所述填料层具有网格状的聚偏氟乙烯系树脂,
所述填料层中的所述聚偏氟乙烯系树脂的含量为15质量%以上且40质量%以下。
5.根据权利要求4所述的非水电解质二次电池,其中,所述磷酸盐颗粒的表面整体被所述聚偏氟乙烯系树脂覆盖。
6.根据权利要求4或5所述的非水电解质二次电池,其中,所述聚偏氟乙烯系树脂包含3质量%以上且15质量%以下的六氟丙烯。
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