CN118020162A - 用于全固体Li离子电池的阳极涂层 - Google Patents
用于全固体Li离子电池的阳极涂层 Download PDFInfo
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- CN118020162A CN118020162A CN202280064866.1A CN202280064866A CN118020162A CN 118020162 A CN118020162 A CN 118020162A CN 202280064866 A CN202280064866 A CN 202280064866A CN 118020162 A CN118020162 A CN 118020162A
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- anode
- lithium
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- coating
- coating according
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- 238000000576 coating method Methods 0.000 title claims abstract description 61
- 239000011248 coating agent Substances 0.000 title claims abstract description 57
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 21
- 239000007787 solid Substances 0.000 title claims description 14
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 30
- -1 bromotrifluoroethylene, chlorofluoroethylene, chlorotrifluoroethylene, chlorotrifluoropropylene, ethylene Chemical group 0.000 claims description 24
- 229910052744 lithium Inorganic materials 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 19
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 claims description 17
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 15
- 239000007784 solid electrolyte Substances 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000013543 active substance Substances 0.000 claims description 7
- 150000002148 esters Chemical class 0.000 claims description 7
- 125000000524 functional group Chemical group 0.000 claims description 7
- 229920001519 homopolymer Polymers 0.000 claims description 7
- 229910003002 lithium salt Inorganic materials 0.000 claims description 7
- 159000000002 lithium salts Chemical class 0.000 claims description 7
- 239000000178 monomer Substances 0.000 claims description 7
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 7
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000002482 conductive additive Substances 0.000 claims description 6
- BGTOWKSIORTVQH-UHFFFAOYSA-N cyclopentanone Chemical compound O=C1CCCC1 BGTOWKSIORTVQH-UHFFFAOYSA-N 0.000 claims description 6
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 6
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 claims description 6
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 claims description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 5
- FFTOUVYEKNGDCM-OWOJBTEDSA-N (e)-1,3,3-trifluoroprop-1-ene Chemical compound F\C=C\C(F)F FFTOUVYEKNGDCM-OWOJBTEDSA-N 0.000 claims description 4
- RHLVCLIPMVJYKS-UHFFFAOYSA-N 3-octanone Chemical compound CCCCCC(=O)CC RHLVCLIPMVJYKS-UHFFFAOYSA-N 0.000 claims description 4
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 4
- 150000002170 ethers Chemical class 0.000 claims description 4
- NGAZZOYFWWSOGK-UHFFFAOYSA-N heptan-3-one Chemical compound CCCCC(=O)CC NGAZZOYFWWSOGK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002608 ionic liquid Substances 0.000 claims description 4
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 4
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 claims description 4
- 235000011007 phosphoric acid Nutrition 0.000 claims description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 claims description 4
- AVQQQNCBBIEMEU-UHFFFAOYSA-N 1,1,3,3-tetramethylurea Chemical compound CN(C)C(=O)N(C)C AVQQQNCBBIEMEU-UHFFFAOYSA-N 0.000 claims description 3
- IMSODMZESSGVBE-UHFFFAOYSA-N 2-Oxazoline Chemical compound C1CN=CO1 IMSODMZESSGVBE-UHFFFAOYSA-N 0.000 claims description 3
- PYGXAGIECVVIOZ-UHFFFAOYSA-N Dibutyl decanedioate Chemical compound CCCCOC(=O)CCCCCCCCC(=O)OCCCC PYGXAGIECVVIOZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 3
- DOOTYTYQINUNNV-UHFFFAOYSA-N Triethyl citrate Chemical compound CCOC(=O)CC(O)(C(=O)OCC)CC(=O)OCC DOOTYTYQINUNNV-UHFFFAOYSA-N 0.000 claims description 3
- 239000011149 active material Substances 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 3
- 150000001244 carboxylic acid anhydrides Chemical class 0.000 claims description 3
- 150000001733 carboxylic acid esters Chemical class 0.000 claims description 3
- 150000001735 carboxylic acids Chemical class 0.000 claims description 3
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 claims description 3
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 claims description 3
- 150000002596 lactones Chemical class 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 150000002825 nitriles Chemical class 0.000 claims description 3
- 150000002989 phenols Chemical class 0.000 claims description 3
- 150000003009 phosphonic acids Chemical class 0.000 claims description 3
- 150000003016 phosphoric acids Chemical class 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 150000003460 sulfonic acids Chemical class 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical class S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 239000001069 triethyl citrate Substances 0.000 claims description 3
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 claims description 3
- 235000013769 triethyl citrate Nutrition 0.000 claims description 3
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 3
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 3
- KBMBVTRWEAAZEY-UHFFFAOYSA-N trisulfane Chemical compound SSS KBMBVTRWEAAZEY-UHFFFAOYSA-N 0.000 claims description 3
- ULPMRIXXHGUZFA-UHFFFAOYSA-N (R)-4-Methyl-3-hexanone Natural products CCC(C)C(=O)CC ULPMRIXXHGUZFA-UHFFFAOYSA-N 0.000 claims description 2
- KHXKESCWFMPTFT-UHFFFAOYSA-N 1,1,1,2,2,3,3-heptafluoro-3-(1,2,2-trifluoroethenoxy)propane Chemical compound FC(F)=C(F)OC(F)(F)C(F)(F)C(F)(F)F KHXKESCWFMPTFT-UHFFFAOYSA-N 0.000 claims description 2
- BLTXWCKMNMYXEA-UHFFFAOYSA-N 1,1,2-trifluoro-2-(trifluoromethoxy)ethene Chemical compound FC(F)=C(F)OC(F)(F)F BLTXWCKMNMYXEA-UHFFFAOYSA-N 0.000 claims description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 2
- PFCHFHIRKBAQGU-UHFFFAOYSA-N 3-hexanone Chemical compound CCCC(=O)CC PFCHFHIRKBAQGU-UHFFFAOYSA-N 0.000 claims description 2
- 229910000733 Li alloy Inorganic materials 0.000 claims description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 2
- 229910000676 Si alloy Inorganic materials 0.000 claims description 2
- 229910009866 Ti5O12 Inorganic materials 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 150000004292 cyclic ethers Chemical class 0.000 claims description 2
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 claims description 2
- 239000001087 glyceryl triacetate Substances 0.000 claims description 2
- 235000013773 glyceryl triacetate Nutrition 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910000765 intermetallic Inorganic materials 0.000 claims description 2
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 2
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 2
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 claims description 2
- XKLXIRVJABJBLQ-UHFFFAOYSA-N lithium;2-(trifluoromethyl)-1h-imidazole-4,5-dicarbonitrile Chemical compound [Li].FC(F)(F)C1=NC(C#N)=C(C#N)N1 XKLXIRVJABJBLQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 2
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 229960002622 triacetin Drugs 0.000 claims description 2
- WEAPVABOECTMGR-UHFFFAOYSA-N triethyl 2-acetyloxypropane-1,2,3-tricarboxylate Chemical compound CCOC(=O)CC(C(=O)OCC)(OC(C)=O)CC(=O)OCC WEAPVABOECTMGR-UHFFFAOYSA-N 0.000 claims description 2
- QMIWYOZFFSLIAK-UHFFFAOYSA-N 3,3,3-trifluoro-2-(trifluoromethyl)prop-1-ene Chemical group FC(F)(F)C(=C)C(F)(F)F QMIWYOZFFSLIAK-UHFFFAOYSA-N 0.000 claims 1
- GVEUEBXMTMZVSD-UHFFFAOYSA-N 3,3,4,4,5,5,6,6,6-nonafluorohex-1-ene Chemical group FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C=C GVEUEBXMTMZVSD-UHFFFAOYSA-N 0.000 claims 1
- 238000004146 energy storage Methods 0.000 abstract description 2
- 239000002033 PVDF binder Substances 0.000 description 19
- 229920002313 fluoropolymer Polymers 0.000 description 13
- 239000004811 fluoropolymer Substances 0.000 description 13
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- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 description 6
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Abstract
本发明一般地涉及在可充电的二次Li离子电池中电能存储的领域。更具体地,本发明涉及用于全固态Li离子电池的阳极涂层。本发明还涉及用于制备所述涂层的方法。本发明还涉及涂覆有该涂层的阳极、用于生产这样的阳极的工艺以及包含这样的阳极的二次Li离子电池。
Description
技术领域
本发明一般地涉及在Li离子型的可充电蓄电池中存储电能的领域。更具体地,本发明涉及用于全固体Li离子电池的阳极涂层(涂料)。本发明还涉及用于制备所述涂层的工艺。本发明还涉及覆盖有该涂层的阳极、用于制造这样的阳极的工艺以及还涉及包含这样的阳极的Li离子蓄电池。
背景技术
锂蓄电池可作为电源用于各种电子设备,其范围从手机、笔记本电脑和小型家用电子设备到车辆和到大容量能量存储设备等,并且对锂蓄电池的需求正在不断增长。
现有的锂蓄电池一般使用含有有机物质的液体电解质。这些液体电解质有利地具有高的离子传导率,但需要额外的安全设备,原因是液体的逸出、高温下起火或爆炸的风险。
为了试图解决与液体电解质相关联的安全问题,最近开发出了使用固体电解质的完全固体电池。
全固体电池一般包含正极、固体电解质和负极。正极包含正极活性材料和固体电解质,以及此外包含电子传导材料和粘合剂。固体电解质包含来自以下列表的一种或多种要素:聚合物、增塑剂、锂盐、无机颗粒、离子液体。像正极那样,负极包含负极活性材料和固体电解质,以及此外包含传导性的材料和粘合剂。
然而,目前没有满足对于全固体电池的批量使用的规范的固体电解质。这是因为,对于固体电解质而言,一般难以将离子传导率、电化学稳定性、机械强度以及与阳极或阴极材料的相容性结合起来。
举例来说,可特别提及表现出非常高的离子传导率但是对于阳极处的电位和阴极处的高电位显示出电化学不稳定性的无机化合物。(Y.Zhu,ACS Appl.Mater.Interfaces,2015,7,23685-23693)
仍存在开发一种方案的需要,其使得可使阳极在全固体Li离子电池中与固体电解质相容。最重要的是,存在解决在充电和放电循环期间阳极的体积的变化的问题的需要。最后,在锂金属阳极的特定情况下,存在提供一种阳极的需要,所述阳极通过有效方法受到保护以抵抗枝晶的形成。
因此,本发明的目的是提供可直接施加至Li离子电池负极的涂层,其随后使得可在固体电解质与电极活性物质之间具有物理隔离。因此,本发明提供负极,其包含由通常的负极组成的第一层和由根据本发明的阳极涂层组成的第二层。
本发明还旨在提供用于制造所述阳极涂层的工艺。最后,本发明涉及表现出这样的涂层的阳极以及用于制造这样的阳极的工艺。
最后,本发明旨在提供包含这样的阳极的可充电Li离子蓄电池。
发明内容
本发明提出的技术方案是提供阳极涂层,其使阴极在全固体电池中与固体电解质相容。
本发明首先涉及阳极涂层,其由以下组成:
a.一种或多种聚(偏氟乙烯),
b.锂盐,以及
c.传导性添加剂。
本发明还涉及从通过混合涂层的所有成分获得的墨来制造阳极涂层的工艺。
本发明还涉及用于锂离子电池的阳极,所述阳极由覆盖有根据本发明的涂层的负极活性材料层组成。
本发明还涉及用于制造Li离子电池负极的工艺,所述工艺包含以下操作:
-提供阳极,
-在所述阳极上沉积涂层。
本发明的另一主题是包含负极、正极和全固体电解质的Li离子蓄电池,其中阳极如上所述。
本发明使得可克服现有技术的缺点。其提供这样的离子传导涂层,所述离子传导涂层的介电常数的均匀分布,同时维持足够的机械强度以避免枝晶的形成。该涂层表现出良好的还原稳定性和良好的柔性,从而允许其承受在充电和放电循环期间阳极体积的变化。
在锂阳极的特定情况下,根据本发明的涂层使得可抑制可导致短路的枝晶的生长,良好的介电常数均匀性,这使得可避免形成具有高浓度的锂离子的区域。该涂层还使得可在锂金属上形成稳定且具有低电阻率的固体电解质界面(SEI),从而改进全固体电池的性能和使用寿命。
具体实施方式
现在在以下描述中更详细地并且以非限制性方式描述本发明。
根据第一方面,本发明涉及阳极涂层,其由以下组成:
a.一种或多种聚(偏氟乙烯)(组分A),
b.至少一种锂盐(组分B),以及
c.至少一种传导性添加剂(组分C)。
根据不同的实施方案,所述涂层包含以下特性,如果适当地结合的话。除非另有说明,否则所示含量均以重量表示。
组分A
本发明中使用的半结晶含氟聚合物是基于偏二氟乙烯的聚合物并且一般地通过缩写PVDF表示。
根据一个实施方案,PVDF是聚(偏氟乙烯)均聚物或偏氟乙烯(vinylidenefluoride,偏二氟乙烯)均聚物的混合物。
根据一个实施方案,PVDF是聚(偏氟乙烯)均聚物或偏二氟乙烯与至少一种与偏二氟乙烯相容的共聚单体的共聚物。
根据一个实施方案,PVDF是半结晶的。
与偏二氟乙烯相容的共聚单体可以是卤化的(氟化、氯化或溴化)或非卤化的。
适当的氟化共聚单体的实例是:乙烯基氟(vinyl fluoride)、四氟乙烯、六氟丙烯、三氟丙烯并且特别是3,3,3-三氟丙烯、四氟丙烯并且特别是2,3,3,3-四氟丙烯或1,3,3,3-四氟丙烯、六氟异丁烯、全氟丁基乙烯、五氟丙烯并且特别是1,1,3,3,3-五氟丙烯或1,2,3,3,3-五氟丙烯、全氟化的烷基乙烯基醚并且特别是通式Rf-O-CF-CF2的那些,Rf是烷基基团,优选地是C1至C4烷基基团(优选的实例是全氟(丙基乙烯基醚)和全氟(甲基乙烯基醚))。
氟化共聚单体可包含氯原子或溴原子。其特别地可选自溴三氟乙烯、氯氟乙烯、氯三氟乙烯和氯三氟丙烯。氯氟乙烯可表示1-氯-1-氟乙烯或1-氯-2-氟乙烯。优选1-氯-1-氟乙烯异构体。氯三氟丙烯优选为1-氯-3,3,3-三氟丙烯或2-氯-3,3,3-三氟丙烯。
VDF共聚物还可以包含非卤化单体,诸如乙烯和/或丙烯酸类或甲基丙烯酸类共聚单体。
含氟聚合物优选地含有至少50mol%的偏二氟乙烯。
根据一个实施方案,PVDF是偏氟乙烯(VDF)和六氟丙烯(HFP)的共聚物(P(VDF-HFP)),相对于所述共聚物的重量,其具有2重量%至23重量%、优选地4重量%至15重量%的六氟丙烯单体单元的重量百分比。
根据一个实施方案,PVDF是聚(偏氟乙烯)均聚物和VDF-HFP共聚物的混合物。HFP类共聚单体的存在使得可改进涂层相对于锂金属的化学稳定性。
根据一个实施方案,PVDF是偏氟乙烯和四氟乙烯(TFE)的共聚物。
根据一个实施方案,PVDF是偏氟乙烯和氯三氟乙烯(CTFE)的共聚物。
根据一个实施方案,PVDF是VDF-TFE-HFP三元共聚物。根据一个实施方案,PVDF是VDF-TrFE-TFE三元共聚物(TrFE是三氟乙烯)。在这些三元共聚物中,VDF的重量含量为至少10%,共聚单体以可变的比例存在。
根据一个实施方案,PVDF是两种或更多种VDF-HFP共聚物的混合物。
根据一个实施方案,PVDF包含带有以下官能团中的至少一个的单体单元:羧酸、羧酸酸酐、羧酸酯、环氧(诸如缩水甘油基)、酰胺、羟基、羰基、巯基、硫化物、噁唑啉、酚类、酯、醚、硅氧烷、磺酸类、硫酸类、磷酸类或膦酸类。所述官能团是通过化学反应引入的,根据本领域技术人员熟知的技术,化学反应可以是氟化单体与带有所述官能基团中的至少一个和能够与氟化单体共聚的乙烯基官能团的单体的共聚反应或接枝。
根据一个实施方案,所述官能基团带有羧酸官能团,所述羧酸官能团是选自丙烯酸、甲基丙烯酸、(甲基)丙烯酸羟乙酯、(甲基)丙烯酸羟丙酯和(甲基)丙烯酸羟乙基己酯的(甲基)丙烯酸类型的基团。
根据一个实施方案,带有羧酸官能团的单元另外地包含选自氧、硫、氮和磷的杂原子。
根据一个实施方案,官能度是借助于在合成工艺期间使用的转移试剂引入的。转移试剂是具有小于或等于20 000g/mol的摩尔质量的带有选自以下基团的官能基团的聚合物:羧酸、羧酸酸酐、羧酸酯、环氧(诸如缩水甘油基)、酰胺、羟基、羰基、巯基、硫化物、噁唑啉、酚类、酯、醚、硅氧烷、磺酸类、硫酸类、磷酸类或膦酸类。该类型的转移试剂的实例是丙烯酸(类)低聚物。
PVDF中官能基团的含量为至少0.01mol%、优选地至少0.1mol%、并且至多15mol%、优选地至多10mol%。
PVDF优选地具有高分子量。术语“高分子量”,如本文所使用的,理解为意指具有大于100Pa.s、优选地大于500Pa.s、更优选地大于1000Pa.s、有利地大于2000Pa.s的熔体粘度的PVDF。粘度是根据标准ASTM D3825,使用毛细管流变仪或平行板流变仪,以100s-1的剪切梯度,在232℃下测量的。两种方法提供相似的结果。
本发明中使用的PVDF均聚物和VDF共聚物可通过已知的聚合方法(如乳液聚合)获得。
根据一个实施方案,其是在没有氟化表面活性剂的情况下通过乳液聚合工艺制备的。
PVDF的聚合产生胶乳,其一般地具有10重量%-60重量%、优选地10%-50%的固体含量,并且具有小于1微米、优选地小于1000nm、优选地小于800nm且更优选地小于600nm的重量平均颗粒尺寸。颗粒的重量平均尺寸一般地为至少10nm、优选地至少50nm,并且平均尺寸有利地在100到400nm范围之内。聚合物颗粒可以形成团聚体,称为二次颗粒,其重量平均尺寸小于5000μm、优选地小于1000μm、有利地在1和80微米之间并且优选地在2到50微米之间。在配制和施加到基底期间,团聚体会碎裂成离散的颗粒。
根据某些实施方式,PVDF均聚物和VDF共聚物由生物基VDF组(构)成。术语“生物基”意指“得自生物质的”。这使得可改进涂层的生态足迹。生物基VDF的特征可以在于至少1原子%的可再生碳的含量,也就是说源自生物材料或生物质的天然来源的碳的含量,如根据标准NF EN 16640通过14C的含量来确定的。如下所述,术语“可再生碳”表示碳是天然来源的并且源自生物材料(或生物质)。根据某些实施方案,VDF的生物碳含量可以大于5%、优选大于10%、优选大于25%、优选大于或等于33%、优选大于50%、优选大于或等于66%、优选大于75%、优选大于90%、优选大于95%、优选大于98%、优选大于99%、有利地等于100%。
组分B
作为非限制性实例,锂盐(或多种锂盐)选自LiPF6(六氟磷酸锂)、LiFSI(双氟磺酰亚胺锂)、TFSI(双三氟甲基磺酰亚胺锂)、LiTDI(2-三氟甲基-4,5-二氰基咪唑锂)、LiPOF2、LiB(C2O4)2、LiF2B(C2O4)2、LiBF4、LiNO3、LiClO4以及提及的盐的两种或更多种的混合物。
组分C
传导性添加剂可以是有机分子或有机分子混合物,其能够在不溶解含氟聚合物的情况下溶胀含氟聚合物且具有大于1的介电常数。根据一个实施方案,组分C选自醚(线性或环状的)、酯、内酯、腈、碳酸酯/盐和离子液体。
作为非限制性实例,在醚中可以提及线性或环状的醚,诸如,例如二甲氧基乙烷(DME)、2至5个氧乙烯单元的低聚乙二醇的甲醚、二氧戊环、二氧六环、二丁基醚、四氢呋喃及其混合物。
在酯中,可提及磷酸的酯或亚硫酸酯。例如,可提及甲酸甲酯、乙酸甲酯、丙酸甲酯、乙酸乙酯、乙酸丁酯、γ-丁内酯或其混合物。
在内酯中,可提及环己酮。
在腈中,可提及例如乙腈、丙酮腈、丙腈、甲氧基丙腈、二甲基氨基丙腈、丁腈、异丁腈、戊腈、新戊腈、异戊腈、戊二腈、甲氧基戊二腈、2-甲基戊二腈、3-甲基戊二腈、己二腈、丙二腈以及其混合物。
在碳酸酯中,例如可提及环状碳酸酯,诸如例如碳酸亚乙酯(碳酸乙烯酯)(EC)(CAS:96-49-1),碳酸亚丙酯(碳酸丙烯酯)(PC)(CAS:108-32-7),碳酸亚丁酯(碳酸丁烯酯)(BC)(CAS:4437-85-8),碳酸二甲酯(DMC)(CAS:616-38-6),碳酸二乙酯(DEC)(CAS:105-58-8),碳酸甲乙酯(EMC)(CAS:623-53-0),碳酸二苯酯(CAS:102-09-0),甲基苯基碳酸酯(CAS:13509-27-8),碳酸二丙酯(DPC)(CAS:623-96-1),碳酸甲丙酯(MPC)(CAS:1333-41-1),碳酸乙丙酯(EPC),碳酸亚乙烯酯(VC)(CAS:872-36-6),碳酸氟亚乙酯(FEC)(CAS:114435-02-8),碳酸三氟亚丙酯(CAS:167951-80-6)或其混合物。
在离子液体中,可特别提及EMIM:FSI、PYR:FSI、EMIM:TFSI、PYR:TFSI、EMIM:BOB、PYR:BOB、EMIM:TDI、PYR:TDI、EMIM:BF4或PYR:BF4。
按重量计,根据本发明的阳极涂层的组成(组合物,成分)为:
-具有在20%和80%之间的重量比例的组分A,
-具有在1%和40%之间的重量比例的组分B,
-具有在2%和50%之间的重量比例的组分C,
这些比例的总和为100%。
本发明还涉及从通过在溶剂中混合涂层的所有成分获得的墨通过溶剂途径来制造上述阳极涂层的工艺。
使得可制备涂层的墨可以通过本领域技术人员所知的任何类型的混合器来生产,诸如行星混合器、离心机、轨道混合器、混合器轴或Ultra-Turrax。墨的不同成分不以精确的顺序添加。墨可以在不同的温度下制造,所述温度的范围从环境温度到最高达制造墨所用溶剂的沸点。所用溶剂优选地是具有大于2的Hansen参数的极性溶剂。作为非限制性实例,可特别提及丙酮、乙酰柠檬酸三乙酯(TEAC)、γ-丁内酯(GBL)、环己酮(CHO)、环戊酮(CPO)、邻苯二甲酸二丁酯(DBP)、癸二酸二丁酯(DBS)、碳酸二乙酯(DEC)、邻苯二甲酸二乙酯(DEP)、二氢左旋葡萄糖酮(Cyrene)、二甲基乙酰胺(DMAc)、N,N-二甲基甲酰胺(DMF)、二甲基亚砜(DMSO)、1,4-二氧六环(1,4-dioxane)、3-庚酮、六甲基磷酰胺(HMPA)、3-己酮、甲乙酮(MEK)、N-甲基-2-吡咯烷酮(NMP)、3-辛酮、3-戊酮、碳酸亚丙酯(PC)、四氢呋喃(THF)、四甲基脲(TMU)、三醋酸甘油酯、柠檬酸三乙酯(TEC)、磷酸三乙酯(TEP)、磷酸三甲酯(TMP)、N,N,N’,N’-四丁基琥珀酰二胺(TBSA)或提及的溶剂的两种或更多种的混合物。
根据一个实施方案,根据本发明的涂覆的阳极的孔隙率小于10%、优选地小于5%。
涂覆的电极(CE)的孔隙率是根据由M.Cai在出版物Nature Communications,2019,10,4597中描述的以下计算获得的:
其中,VCE代表涂覆的电极的真实体积,并且是通过将涂覆的电极的表面积乘以涂覆的电极的厚度来计算的。VdenseCE表示每种成分在没有任何孔隙的情况下所占据的体积,并且是根据以下公式计算的:
VdenseCE是涂覆的电极的各个成分所占据的体积的总和。
该涂层的厚度范围可为从0.1到100μm、优先地从0.1到50μm并且更优先地从0.1到35μm。
本发明还涉及用于全固体锂离子电池的阳极,所述阳极包含覆盖有根据本发明的涂层的活性物质,优选地,所述阳极由覆盖有根据本发明的涂层的活性物质组成。优选地,阳极的所述活性物质沉积在金属支撑物上。
根据一个实施方案,负极中的活性物质选自石墨、Li4Ti5O12型的钛酸锂、氧化钛TiO2、硅或锂/硅合金、氧化锡、锂金属间化合物、金属锂或其混合物。
除了锂金属外,活性物质还与电子传导物质和粘合剂混合。
电子传导物质选自碳黑,天然或合成的石墨,碳纤维,碳纳米管,金属纤维和粉末以及传导性的金属氧化物。优先地,其选自碳黑,天然或合成的石墨,碳纤维,碳纳米管。
用于制造阳极的粘合剂是选自以下的聚合物:聚烯烃(例如:聚乙烯或聚丙烯)、可表现出酸官能团的含氟聚合物(PVDF)、聚丙烯酸(PAA)、聚丙烯腈(PAN)、纤维素型的聚合物、聚苯砜、聚醚砜、酚醛树脂、乙烯基酯树脂、环氧树脂、PTFE或液晶聚合物。
因此,所述阳极包含覆盖有根据本发明的涂层的活性物质,优选地,所述阳极由覆盖有根据本发明的涂层的活性物质组成,所述根据本发明的涂层包含:a)至少一种聚(偏氟乙烯)(组分A)、b)至少一种锂盐(组分B)和至少一种传导性添加剂(组分C),优选地,所述根据本发明的涂层由a)至少一种聚(偏氟乙烯)(组分A)、b)至少一种锂盐(组分B)和至少一种传导性添加剂(组分C)组成。优选地,所述阳极具有如本申请中所定义的孔隙率。
本发明还涉及用于制造锂离子电池负极的工艺,所述工艺包含以下操作:
-提供阳极,
-在所述阳极上沉积根据本发明的涂层。
因此,本发明提供负极,所述负极包含金属支撑物,优选地,所述负极由金属支撑物组成,在所述金属支撑物上沉积覆盖有根据本发明的涂层的活性物质,所述根据本发明的涂层包含:a)至少一种聚(偏氟乙烯)(组分A)、b)至少一种锂盐(组分B)和至少一种传导性添加剂(组分C),优选地,所述根据本发明的涂层由a)至少一种聚(偏氟乙烯)(组分A)、b)至少一种锂盐(组分B)和至少一种传导性添加剂(组分C)组成。
这种涂层可以通过本领域技术人员已知的任何沉积方法生产,诸如通过溶剂途径涂覆、浸渍-取出法、离心涂覆法、喷涂法或通过压延涂覆的方法。这些沉积技术可在不同温度下进行,所述温度范围可从5℃到最高达180℃。
阳极的金属支撑物一般由铜制成。金属支撑物可进行表面处理,并具有厚度为5μm或更大的传导性的底漆。所述支撑物也可以是由碳纤维制成的织造或非织造的织物。
本发明的另一主题是包含负极、正极和全固体电解质的全固体Li离子蓄电池,其中阳极如上所述。
根据一个实施方案,所述电池的阴极也覆盖有根据本发明的涂层。
实施例
以下实施例以非限制性的方式示出了本发明的范围。
制备含氟聚合物(FP)溶液:
将具有23%的HFP的重量含量的14.992g的VDF-HFP共聚物溶解在85.753g的丙酮中,使用行星混合器在2000rpm下持续六次1min以完全溶解。
制备用于涂层:FP/LiFSI/S1 60/20/20的墨I
使用磁力搅拌器在21℃下持续10分钟将0.441g的LiFSI溶解在0.449g的三缩四乙二醇二甲基醚(CAS 143-24-8)中。随后,添加8.826g的FP在丙酮中的15%溶液。
制备用于涂层:FP/LiFSI/MPCN 60/20/20的墨II
使用磁力搅拌器在21℃下持续10分钟将0.3986g的LiFSI溶解在0.3986g的甲氧基丙睛(CAS 110-67-8)中。随后,添加7.972g的FP在丙酮中的15%溶液。
制备用于涂层:FP/LiFSI/S1 40/30/30的墨III
使用磁力搅拌器在21℃下持续10分钟将0.528g的LiFSI溶解在0.528g的三缩四乙二醇二甲基醚(CAS 143-24-8)中。随后,添加4.675g的FP在丙酮中的15%溶液。
用墨III涂覆锂金属:
借助于涂覆刀片,用墨III涂覆具有200μm的厚度的锂金属箔。沉积的湿膜的厚度为50μm。在环境温度下干燥2小时后,沉积的膜的厚度测量得出38μm。随后,将电极压延到在锂金属上获得2μm的沉积物。通过阻抗谱法测量离子电导率。获得的值为0.553mS/cm。
枝晶测试:
进行枝晶测试,以比较用墨III在锂金属上所获得的涂层和标准液体电解质。
方法:该方法由以下组成:对对称Li金属/Li金属电池进行充电和放电;随后测量电池的电位。该电位与电极的表面积成正比,因此枝晶的出现导致电位增加。
所使用的体系:
阴极:涂覆的或未涂覆的锂金属
阳极:锂金属
使用0.25mA的正电流将电池充电至0.25mAh的能量密度。随后使用0.25mA的负电流将电池放电至0.25mAh的能量密度。
在液体电解质的情况下,将多孔的PE隔板浸泡在含有1M LiFSI(按体积计,EC/EMC3/7)的电解质溶液中。
表1显示电池的初始电位翻倍所需的时间。
[表1]
技术 | 时间 |
墨III涂层 | >384H |
液体电解质 | 24H |
Claims (15)
1.阳极涂层,其由以下组成:
a.至少一种聚(偏氟乙烯)(PVDF)(组分A),
b.至少一种锂盐(组分B),以及
c.至少一种传导性添加剂(组分C)。
2.根据权利要求1所述的涂层,其中所述组分A选自聚(偏氟乙烯)均聚物和偏二氟乙烯与至少一种共聚单体的共聚物,所述共聚单体选自以下列表:乙烯基氟、四氟乙烯、六氟丙烯、3,3,3-三氟丙烯、2,3,3,3-四氟丙烯、1,3,3,3-四氟丙烯、六氟异丁烯、全氟丁基乙烯、1,1,3,3,3-五氟丙烯、1,2,3,3,3-五氟丙烯、全氟(丙基乙烯基醚)、全氟(甲基乙烯基醚)、溴三氟乙烯、氯氟乙烯、氯三氟乙烯、氯三氟丙烯、乙烯及其混合物。
3.根据权利要求1和2中任一项所述的涂层,其中PVDF包含带有以下官能团中的至少一种的单体单元:羧酸、羧酸酸酐、羧酸酯、环氧(诸如缩水甘油基)、酰胺、羟基、羰基、巯基、硫化物、噁唑啉、酚类、酯、醚、硅氧烷、磺酸类、硫酸类、磷酸类或膦酸类。
4.根据权利要求1至3中任一项所述的涂层,其中所述组分B选自LiPF6(六氟磷酸锂)、LiFSI(双氟磺酰亚胺锂)、TFSI(双三氟甲基磺酰亚胺锂)、LiTDI(2-三氟甲基-4,5-二氰基咪唑锂)、LiPOF2、LiB(C2O4)2、LiF2B(C2O4)2、LiBF4、LiNO3、LiClO4以及提及的盐的两种或更多种的混合物。
5.根据权利要求1至4中一项所述的涂层,其中组分C选自线性或环状的醚,酯,内酯,腈,碳酸酯/盐和离子液体。
6.根据权利要求1至5中一项所述的涂层,所述涂层具有从0.1到100μm、优先地从0.1到50μm并且更优先地从0.1到35μm范围的厚度。
7.根据权利要求1至6中任一项所述的涂层,其按重量计具有以下组成:
-具有在20%和80%之间的比例的组分A;
-具有在1%和40%之间的比例的组分B;
-具有在2%和50%之间的比例的组分C;
这些比例的总和为100%。
8.用于从墨制造根据权利要求1至7中一项所述的阳极涂层的工艺,所述墨是通过将涂层的所有成分在溶剂中混合而获得的。
9.根据权利要求8所述的工艺,其中所述溶剂选自以下列表:丙酮、乙酰柠檬酸三乙酯、γ-丁内酯、环己酮、环戊酮、邻苯二甲酸二丁酯、癸二酸二丁酯、碳酸二乙酯、邻苯二甲酸二乙酯、二氢左旋葡萄糖酮、二甲基乙酰胺、N,N-二甲基甲酰胺、二甲基亚砜、1,4-二氧六环、3-庚酮、六甲基磷酰胺、3-己酮、甲乙酮、N-甲基-2-吡咯烷酮、3-辛酮、3-戊酮、碳酸亚丙酯、四氢呋喃、四甲基脲、三醋酸甘油酯、柠檬酸三乙酯、磷酸三乙酯、磷酸三甲酯、N,N’-四丁基琥珀酰二胺及其混合物。
10.用于全固体锂离子电池的阳极,所述阳极由覆盖有根据权利要求1至7中一项所述的涂层的活性物质组成。
11.根据权利要求9所述的阳极,其中所述活性物质选自石墨、Li4Ti5O12型的钛酸锂、氧化钛TiO2、硅或锂/硅合金、氧化锡、锂金属间化合物、或其混合物。
12.根据权利要求10和11中任一项所述的阳极,其具有小于10%、优选地小于5%的孔隙率。
13.用于制造Li离子电池负极的工艺,所述工艺包含以下操作:
-提供阳极,
-在所述阳极上沉积根据权利要求1至7中一项所述的涂层。
14.全固体Li离子蓄电池,其包含阴极、根据权利要求10至12中一项的阳极和全固体电解质。
15.根据权利要求15所述的电池,其中阴极覆盖有根据权利要求1至7中一项所述的涂层。
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FR2110145A FR3127634A1 (fr) | 2021-09-27 | 2021-09-27 | Revetement d’anode pour batterie li-ion tout solide |
FRFR2110145 | 2021-09-27 | ||
PCT/FR2022/051795 WO2023047065A1 (fr) | 2021-09-27 | 2022-09-23 | Revetement d'anode pour batterie li-ion tout solide |
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