CN112771690A - 负极和包含其的二次电池 - Google Patents
负极和包含其的二次电池 Download PDFInfo
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- CN112771690A CN112771690A CN201980064027.8A CN201980064027A CN112771690A CN 112771690 A CN112771690 A CN 112771690A CN 201980064027 A CN201980064027 A CN 201980064027A CN 112771690 A CN112771690 A CN 112771690A
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- active material
- anode
- additive
- weight
- negative electrode
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
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- Chemical & Material Sciences (AREA)
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- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
本发明涉及一种负极和包含其的二次电池,所述负极包含负极活性材料层,所述负极活性材料层包含负极活性材料粒子和添加剂,其中基于100重量份的所述负极活性材料粒子,所述添加剂的含量为1.8重量份至3.2重量份,并且所述添加剂包含选自如下中的至少一种:LATP、LAGP、LLTO和LLZO。
Description
技术领域
相关申请的交叉引用
本申请要求于2018年10月12日在韩国知识产权局提交的韩国专利申请10-2018-0121540号的权益,其公开内容通过引用被整体并入本文中。
技术领域
本发明涉及一种负极,所述负极包含负极活性材料层,所述负极活性材料层包含负极活性材料粒子和添加剂,其中基于100重量份的所述负极活性材料粒子,所述添加剂的含量为1.8重量份至3.2重量份,并且所述添加剂包含选自如下中的至少一种:LATP、LAGP、LLTO和LLZO。
背景技术
随着近年来移动装置的技术发展和需求的增加,对作为能源的二次电池的需求已经迅速增加。因此,已经对可以满足各种需求的电池进行了各种研究。特别地,已经对作为这种装置的电源的具有高能量密度和优异的寿命和循环性能的锂二次电池积极地进行了研究。
锂二次电池是指如下电池,该电池在电极组件中包含:正极,所述正极包含能够嵌入/脱嵌锂离子的正极活性材料;负极,所述负极包含能够嵌入/脱嵌锂离子的负极活性材料;和非水电解液,所述非水电解液含有锂离子,所述电极组件具有插置在所述正极与所述负极之间的微孔隔膜。作为负极活性材料,使用锂金属、锂合金、晶态或无定形碳、碳复合材料、石墨类活性材料、硅类活性材料等。
另一方面,在锂二次电池的情况下,存在低温下的输出劣化的问题。为了解决上述问题,已经为了使得锂二次电池在低温下具有优异的输出性能而进行了各种尝试。
例如,存在通过在非水电解液中包含碳酸亚丙酯来改善电池的低温性能的方法。然而,当使用碳酸亚丙酯时,存在的问题是,石墨类活性材料的中间层分层,从而导致电池性能劣化。又例如,存在制造并使用纳米尺寸的负极活性材料的方法。然而,由于纳米结构的多晶本性,所以电荷迁移阻力增加,使得电池性能可能劣化。
因此,本发明介绍了一种能够提高锂二次电池的低温输出性能的新方法。
发明内容
技术问题
本发明的目的是通过允许负极包含适当量的特定添加剂以在使锂二次电池的容量劣化和电阻升高最小化的同时改善锂二次电池的低温输出性能。
技术方案
根据本发明的一个方面,提供一种负极,所述负极包含负极活性材料层,所述负极活性材料层包含负极活性材料粒子和添加剂,其中基于100重量份的所述负极活性材料粒子,所述添加剂的含量为1.8重量份至3.2重量份,并且所述添加剂包含选自如下中的至少一种:LATP、LAGP、LLTO和LLZO。
根据本发明的另一个方面,提供一种二次电池,所述二次电池包含所述负极、正极、插置在所述正极与所述负极之间的隔膜以及电解液。
有益效果
根据本发明,负极活性材料层以适当的量包含选自如下中的至少一种:LATP、LAGP、LLTO和LLZO。因此,可以在使锂二次电池的容量下降和电阻升高最小化的同时提高锂离子的扩散速率和传导性。因此,可以改善锂二次电池在低温下、特别是在-10℃以下的温度下的输出性能。
附图说明
图1是示出了使用根据实施例1、比较例1和比较例2的每一种负极的电池的低温输出性能的图;
图2是示出了使用根据比较例1、比较例3和比较例4的每一种负极的电池的低温输出性能的图;
图3是示出了使用根据实施例1、比较例1和比较例2的每一种负极的电池的容量性能的图;
图4是示出了使用根据比较例1、比较例3和比较例4的每一种负极的电池的容量性能的图;
图5是示出了使用根据实施例1、比较例1和比较例2的每一种负极的电池的电阻性能的图;
图6是示出了使用根据比较例1、比较例3和比较例4的每一种负极的电池的电阻性能的图。
具体实施方式
下文中,将更详细地描述本发明,以有助于理解本发明。在此情况下,将理解,说明书和权利要求书中所使用的词语或术语不应被解释为具有常用字典中定义的含义。将进一步理解,基于发明人可以适当定义词语或术语的含义以对本发明进行最佳解释的原则,所述词语或术语应被解释为具有与其在本发明的相关领域背景和技术理念中的含义一致的含义。
在本说明书中,可以将平均粒径(D50)定义为与粒子的粒径分布曲线中的50%累积量对应的粒径。平均粒径(D50)可以通过例如激光衍射法来测量。激光衍射法通常能够测量从亚微米区域到几毫米的粒径,从而可以获得高再现性和高分辨率的结果。
<负极>
根据本发明的实施方案的负极包含负极活性材料层,所述负极活性材料层包含负极活性材料粒子和添加剂,其中基于100重量份的所述负极活性材料粒子,所述添加剂的含量为1.8重量份至3.2重量份,并且所述添加剂包含选自如下中的至少一种:LATP、LAGP、LLTO和LLZO。
负极可以包含集电器。集电器不受特别限制,只要其具有导电性且不引起电池中的化学变化即可。例如,作为集电器,可以使用:铜;不锈钢;铝;镍;钛;烧制碳;或经碳、镍、钛、银等中的一种表面处理过的铝或不锈钢。具体地,可以使用良好地吸附碳的过渡金属(如铜和镍)作为集电器。集电器的厚度可以为6μm至20μm,但是集电器的厚度不限于此。
可以将负极活性材料层设置在集电器上。负极活性材料层可以覆盖集电器的一个表面或两个表面。负极活性材料层可以包含负极活性材料粒子和添加剂。
(1)负极活性材料粒子
负极活性材料粒子可以包含硅类活性材料粒子和石墨类活性材料粒子中的至少一种。作为硅类活性材料粒子,可以使用选自如下中的一种或多种:Si、SiOx(0<x≤2)、Si-C复合材料和Si-Y合金(其中Y是选自如下中的元素:碱金属、碱土金属、过渡金属、13族元素、14族元素、稀土元素及其组合)。石墨类活性材料粒子可以包含选自如下中的一种或多种:人造石墨、天然石墨、石墨化碳纤维和石墨化中间相碳微珠。更具体地,负极活性材料粒子可以包含人造石墨和SiOx(0<x≤2)。
基于负极活性材料层,负极活性材料粒子的含量可以为80重量%至97重量%、具体是85重量%至96重量%。当满足上述范围时,可以确保所制造的电池的容量。
(2)添加剂
当锂二次电池处于低温时,添加剂可以用于改善锂离子在负极表面上的固体电解质界面(SEI)层中的传导性并且改善锂在负极中的扩散。
添加剂可以是选自如下中的至少一种:Li1+m1Alm1Ti2-m1(PO4)3(0<m1≤1,LATP)、Li1+m2Alm2Ge2-m2(PO4)3(0<m2≤1,LAGP)、Li3m3La2/3-m3TiO3(0.2≤m3≤0.05,LLTO)和Li3m4La2/3-m4ZrO3(0.2≤m4≤0.05,LLZO)。添加剂可以帮助锂离子在负极内部和在负极表面上的SEI层中的移动,从而可以改善低温下的电池输出性能。
特别地,添加剂可以是LATP。所述LATP由于其高的离子传导性而可以进一步改善低温下的电池输出性能。
在负极活性材料层中,基于100重量份的负极活性材料粒子,添加剂的含量可以为1.8重量份至3.2重量份。当小于1.8重量份时,所述量太小,使得添加剂难以均匀地存在于负极表面上。因此,难以改善电池的低温输出性能。相反,当大于3.2重量份时,负极活性材料粒子的表面被添加剂过度覆盖,从而存在电池容量明显降低的问题。具体地,基于100重量份的负极活性材料粒子,添加剂的含量可以为2重量份至3重量份,更具体是2重量份至2.5重量份。
添加剂的平均粒径(D50)可以为0.1μm至5μm,具体是0.2μm至2μm。当满足上述范围时,可以进一步改善电池的低温输出性能。更具体地,添加剂的平均粒径(D50)可以为0.8μm至2μm。当满足上述范围时,抑制了负极浆料粘度的过度增加,从而在制造负极时容易涂覆负极浆料,并且可以抑制在添加剂的表面杂质与电解液之间发生的副反应。
(3)其它成分
负极活性材料层还可以包含粘合剂。粘合剂可以是:聚偏二氟乙烯-六氟丙烯共聚物(PVDF-共-HFP)、聚偏二氟乙烯、聚丙烯腈、聚甲基丙烯酸甲酯、聚乙烯醇、羧甲基纤维素(CMC)、淀粉、羟丙基纤维素、再生纤维素、聚乙烯吡咯烷酮、聚四氟乙烯、聚乙烯、聚丙烯、三元乙丙橡胶(EPDM)、磺化EPDM、苯乙烯丁二烯橡胶(SBR)、氟橡胶和聚丙烯酸;或其氢由Li、Na或Ca取代的聚合物等;或诸如以上材料的各种共聚物的各种粘合剂聚合物。
负极活性材料层还可以包含导电材料。导电材料不受特别限制,只要其具有导电性且不引起电池中的化学变化即可。例如,可以使用:碳类材料,如炭黑、乙炔黑、科琴黑、槽黑、炉黑、灯黑和热裂法炭黑;导电纤维,如碳纤维和金属纤维;导电管,如碳纳米管;氟化碳粉末;金属粉末,如铝粉末和镍粉末;导电晶须,如氧化锌和钛酸钾;导电金属氧化物,如氧化钛;导电材料,如聚亚苯基衍生物等。导电材料可以优选为炭黑,更具体地,可以是具有几十纳米的平均粒径的炭黑。
<二次电池>
本发明提供一种二次电池,所述二次电池包含正极、负极、电解质以及插置在正极与负极之间的隔膜。所述负极与上述实施方案的负极相同,并且所述二次电池可以是锂二次电池。
二次电池可以通过本领域中已知的典型方法来制造。例如,可以通过将隔膜设置在正极与负极之间并注入溶解有锂盐的电解液来制造二次电池。
正极可以包含正极活性材料。作为正极活性材料,可以优选使用锂过渡金属氧化物。例如,可以使用选自如下中的一种或两种以上的混合物:Lix1CoO2(0.5<x1<1.3)、Lix2NiO2(0.5<x2<1.3)、Lix3MnO2(0.5<x3<1.3)、Lix4Mn2O4(0.5<x4<1.3)、Lix5(Nia1Cob1Mnc1)O2(0.5<x5<1.3,0<a1<1,0<b1<1,0<c1<1,a1+b1+c1=1)、Lix6Ni1-y1Coy1O2(0.5<x6<1.3,0<y1<1)、Lix7Co1-y2Mny2O2(0.5<x7<1.3,0≤y2<1)、Lix8Ni1-y3Mny3O2(0.5<x8<1.3,0≤y3<1)、Lix9(Nia2Cob2Mnc2)O4(0.5<x9<1.3,0<a2<2,0<b2<2,0<c2<2,a2+b2+c2=2)、Lix10Mn2-z1Niz1O4(0.5<x10<1.3,0<z1<2)、Lix11Mn2-z2Coz2O4(0.5<x11<1.3,0<z2<2)、Lix12CoPO4(0.5<x12<1.3)和Lix13FePO4(0.5<x13<1.3)。
作为根据本发明的锂二次电池中所包含的隔膜,可以单独或以其层压形式使用典型的多孔聚合物膜,例如由聚烯烃类聚合物(如乙烯均聚物、丙烯均聚物、乙烯-丁烯共聚物、乙烯-己烯共聚物和乙烯-甲基丙烯酸酯共聚物)制备的多孔聚合物膜。可替代地,可以使用典型的多孔无纺布,例如由具有高熔点的玻璃纤维或聚对苯二甲酸乙二醇酯纤维形成的无纺布,但是本发明不限于此。
根据本发明的锂二次电池中所包含的电解液可以是选自如下中的一种或多种的混合有机溶剂:碳酸亚丙酯(PC)、碳酸亚乙酯(EC)、碳酸二乙酯(DEC)、碳酸二甲酯(DMC)、碳酸二丙酯(DPC)、二甲基亚砜、乙腈、二甲氧基乙烷、二乙氧基乙烷、四氢呋喃、N-甲基-2-吡咯烷酮(NMP)、碳酸乙甲酯(EMC)、γ-丁内酯(GBL)、氟代碳酸亚乙酯(FEC)、甲酸甲酯、甲酸乙酯、甲酸丙酯、乙酸甲酯、乙酸乙酯、乙酸丙酯、乙酸戊酯、丙酸甲酯、丙酸乙酯和丙酸丁酯。
另外,根据本发明的电解液还可以包含锂盐,并且锂盐的负极离子可以是选自如下中的一种或多种:F-、Cl-、Br-、I-、NO3 -、N(CN)2 -、BF4 -、ClO4 -、PF6 -、(CF3)2PF4 -、(CF3)3PF3 -、(CF3)4PF2 -、(CF3)5PF-、(CF3)6P-、F3SO3 -、CF3CF2SO3 -、(CF3SO2)2N-、(FSO2)2N-、CF3CF2(CF3)2CO-、(CF3SO2)2CH-、(SF5)3C-、(CF3SO2)3C-、CF3(CF2)7SO3 -、CF3CO2 -、CH3CO2 -、SCN-和(CF3CF2SO2)2N-。
根据本发明的锂二次电池可以是圆筒型、长方体型或袋型二次电池,但是不限于此,只要其是充电/放电装置即可。
另外,本发明提供一种包含所述锂二次电池作为单元电池的电池模块和包含所述电池模块的电池组。
电池组可以用作一种或多种中型到大型装置的电源,所述中型到大型装置为:例如电动工具;电动汽车,包括电动车辆(EV)、混合动力电动车辆(HEV)和插电式混合动力电动车辆(PHEV);或电力存储系统。
下文中,将对本发明的实施例进行详细描述,使得本领域技术人员可以容易地实施本发明。然而,本发明可以以许多不同的形式来实施,并且不限于本文中所阐述的实施例。
实施例1:负极的制造
使用将人造石墨和SiO以95:5的重量比混合的混合物作为负极活性材料粒子。将负极活性材料粒子;作为粘合剂的苯乙烯丁二烯橡胶(SBR)和羧甲基纤维素(CMC);作为导电材料的Super C65;和平均粒径(D50)为1μm的LATP添加并混合在蒸馏水中,以制备在混合物中具有47%固体的负极浆料。此时,负极活性材料粒子、苯乙烯丁二烯橡胶(SBR)、羧甲基纤维素(CMC)和导电材料的重量比为95:1.5:2.3:1.2,并且基于100重量份的负极活性材料粒子,LATP为2重量份。
将负极浆料涂布在厚度为20μm的铜集电器上,以制备初步电极。此时,循环空气的温度为80℃。此后,在Gap20的压力下对初步电极进行辊压,将其在真空烘箱中在130℃下干燥10小时,然后将其冲压成17.34cm2的单电池尺寸,以制造负极。
比较例1:负极的制造
除了不使用LATP之外,以与实施例1中相同的方式制造比较例1的负极。
比较例2:负极的制造
除了使用1重量份的LATP之外,以与实施例1中相同的方式制造比较例2的负极。
比较例3:负极的制造
除了使用5重量份的LATP之外,以与实施例1中相同的方式制造比较例3的负极。
比较例4:负极的制造
除了使用5重量份的0.4μm的LATP来代替1μm的LATP之外,以与实施例1中相同的方式制造比较例4的负极。
[表1]
实验例
使用实施例和比较例中的每一种负极以如下方式制造电池。
将作为正极活性材料的Li[Ni0.8Co0.1Mn0.1]O2、作为导电材料的炭黑、作为粘合剂的聚偏二氟乙烯和作为分散剂的H-NBR以97.5:1:1.35:0.15的重量比混合在作为溶剂的N-甲基-2-吡咯烷酮中,以制备正极浆料。以使得电极装载量(mg/cm2)为每单位面积645mg的方式将所制备的正极浆料涂布到厚度为12μm的铝(Al)集电器上,将其在真空烘箱中在120℃下干燥10小时,然后对其进行辊压,以制造最终厚度(集电器+活性材料层)为158.0μm的正极。使用堆叠法对实施例和比较例的每一种负极、正极和多孔聚乙烯隔膜进行组装,并且向所组装的电池中注入电解液(碳酸亚乙酯(EC)/碳酸乙甲酯(EMC)=3/7(体积比),六氟磷酸锂(1摩尔的LiPF6)),以制造锂二次电池。
此后,通过如下方法对其低温输出性能、容量性能和电阻性能进行评价。
(1)实验例1:低温输出性能及评价
当将充电成SOC 35%的每一种电池在-10℃下连续放电至SOC20%并以5.5C的电流速率连续放电至2.5V的最低极限电压时,确认终止电流(end I)值,并且将所述值除以初始容量,以确认终止电流下的C倍率。通过上述内容,对低温输出性能进行了比较(参见表2以及图1和图2-实施例1:(a);比较例1:(b);比较例2:(c);比较例3:(d);比较例4:(e))。
(2)实验例2:容量性能评价
将每一种电池在恒定电流/恒定电压(CC/CV)条件下以0.33C的恒定电流(CC)充电,然后以恒定电流(CC)充电直至充电电流变为0.05C(在充满电时为4.2V)为止。其后,将每一种电池以0.33C的恒定电流(CC)放电至2.5V。将充电和放电曲线示于图3和图4中(实施例1:(a);比较例1:(b);比较例2:(c);比较例3:(d);比较例4:(e)),并且将放电容量示于表2中。
(3)实验例3:电阻评价
将每一种电池充电至0.33C,以确认其容量,并将电池设定成容量的50%(SOC50%)。此后,在将每一种电池放电至2.5C的同时,将测量出的电压值除以电流值2.5C,以得出电阻值。将结果示于图5和图6中(实施例1:(a);比较例1:(b);比较例2:(c);比较例3:(d);比较例4:(e))。
[表2]
终止电流(mA) | C倍率(C) | 容量(mAh) | |
实施例1 | 80.2 | 0.55 | 143.0 |
比较例1 | 72.7 | 0.49 | 148.2 |
比较例2 | 72.6 | 0.49 | 147.3 |
比较例3 | 82.9 | 0.67 | 123.3 |
比较例4 | 77.2 | 0.63 | 122.4 |
根据图1至图6和表1,在以满足适当范围的含量(2重量份)使用添加剂的实施例1的情况下,终止电流高于比较例1、2和4的每一种电池的终止电流,并且因为实施例1的C倍率在低温下较高,所以能够看出,其低温性能良好。另外,当与不使用添加剂的比较例1进行比较时,实施例1的容量下降不大,并且其电阻与比较例1的电阻类似。因此能够看出,当使用根据本发明的负极时,可以在使容量劣化和电阻升高最小化的同时改善低温输出性能。
在比较例2的情况下,添加剂的含量小至1重量份,使得对低温输出性能几乎没有改善。在比较例3和4的情况下,添加剂的含量过高至5重量份,使得电池容量过度下降。
Claims (10)
1.一种负极,所述负极包含负极活性材料层,所述负极活性材料层包含负极活性材料粒子和添加剂,
其中基于100重量份的所述负极活性材料粒子,所述添加剂的含量为1.8重量份至3.2重量份,并且所述添加剂包含选自如下中的至少一种:LATP、LAGP、LLTO和LLZO。
2.根据权利要求1所述的负极,其中基于100重量份的所述负极活性材料粒子,所述添加剂的含量为2重量份至2.5重量份。
3.根据权利要求1所述的负极,其中所述添加剂是LATP。
4.根据权利要求1所述的负极,其中所述添加剂的平均粒径(D50)为0.1μm至5μm。
5.根据权利要求1所述的负极,其中所述添加剂的平均粒径(D50)为0.8μm至2μm。
6.根据权利要求1所述的负极,其中所述负极活性材料粒子包含如下中的至少一种:硅类活性材料粒子和石墨类活性材料粒子。
7.根据权利要求1所述的负极,其中所述负极活性材料粒子包含人造石墨和SiOx(0<x≤2)。
8.根据权利要求1所述的负极,其中基于所述负极活性材料层,所述负极活性材料粒子的含量为80重量%至97重量%。
9.根据权利要求1所述的负极,其中所述负极活性材料层还包含导电材料。
10.一种二次电池,所述二次电池包含:
根据权利要求1所述的负极;
正极;
隔膜,所述隔膜插置在所述正极与所述负极之间;和
电解液。
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