TW202324814A - 用於全固態鋰離子電池的陽極塗層 - Google Patents
用於全固態鋰離子電池的陽極塗層 Download PDFInfo
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- TW202324814A TW202324814A TW111136375A TW111136375A TW202324814A TW 202324814 A TW202324814 A TW 202324814A TW 111136375 A TW111136375 A TW 111136375A TW 111136375 A TW111136375 A TW 111136375A TW 202324814 A TW202324814 A TW 202324814A
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- Prior art keywords
- coating
- lithium
- anode
- component
- solid
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- 238000000576 coating method Methods 0.000 title claims abstract description 56
- 239000011248 coating agent Substances 0.000 title claims abstract description 54
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 20
- 239000007787 solid Substances 0.000 title abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- -1 poly(vinylidene fluoride) Polymers 0.000 claims description 36
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 28
- 229910052744 lithium Inorganic materials 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 18
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 claims description 17
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 11
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 claims description 10
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 9
- 229910010941 LiFSI Inorganic materials 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 9
- 239000007784 solid electrolyte Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-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
- 229910003002 lithium salt Inorganic materials 0.000 claims description 8
- 159000000002 lithium salts Chemical class 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 150000002148 esters Chemical class 0.000 claims description 7
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- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 6
- 239000011149 active material Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- BGTOWKSIORTVQH-UHFFFAOYSA-N cyclopentanone Chemical compound O=C1CCCC1 BGTOWKSIORTVQH-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
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 6
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 5
- 239000000178 monomer Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- RHLVCLIPMVJYKS-UHFFFAOYSA-N 3-octanone Chemical compound CCCCCC(=O)CC RHLVCLIPMVJYKS-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
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- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-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
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-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
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 3
- 150000001244 carboxylic acid anhydrides Chemical class 0.000 claims description 3
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 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
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
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- 238000002156 mixing Methods 0.000 claims description 3
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- 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
- CDOOAUSHHFGWSA-OWOJBTEDSA-N (e)-1,3,3,3-tetrafluoroprop-1-ene Chemical compound F\C=C\C(F)(F)F CDOOAUSHHFGWSA-OWOJBTEDSA-N 0.000 claims description 2
- DMUPYMORYHFFCT-UPHRSURJSA-N (z)-1,2,3,3,3-pentafluoroprop-1-ene Chemical compound F\C=C(/F)C(F)(F)F DMUPYMORYHFFCT-UPHRSURJSA-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
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- 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
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
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- CVVIFWCYVZRQIY-UHFFFAOYSA-N lithium;2-(trifluoromethyl)imidazol-3-ide-4,5-dicarbonitrile Chemical compound [Li+].FC(F)(F)C1=NC(C#N)=C(C#N)[N-]1 CVVIFWCYVZRQIY-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
本發明總體而言有關於鋰離子型可充電蓄電池中存儲電能的領域。更具體地,本發明有關於用於全固態鋰離子電池的陽極塗層。本發明還有關於用於製備該塗層的方法。本發明還有關於塗有此塗層的陽極、用於製造此陽極的方法以及包含此陽極的鋰離子蓄電池。
Description
發明領域
本發明總體而言有關於鋰離子型可充電蓄電池中存儲電能的領域。更具體地,本發明有關於用於全固態鋰離子電池的陽極塗層。本發明還有關於用於製備該塗層的方法。本發明還有關於塗覆有此塗層的陽極、用於製造此陽極的方法以及包含此陽極的鋰離子蓄電池。
技術背景
鋰蓄電池可作為各種電子設備的電源,範圍從手機、筆記型電腦、家用小型電子設備到汽車及大容量儲能設備等等,對於鋰蓄電池的需求不斷地增長。
現有的鋰蓄電池一般使用含有機物質的液態電解質。這些液態電解質具有高離子傳導率的優點,但由於存在液體逸出、起火或在高溫下爆炸的風險,因此需要額外的安全裝置。
為了嘗試解決與液態電解質相關的安全問題,近來已開發了使用固態電解質的全固態電池。
全固態電池一般包括正極、固態電解質和負極。正極包含正極活性材料及固態電解質,且另外包含電子傳導材料及黏合劑。固態電解質包含來自以下所列的一或多種元素:聚合物、塑化劑、鋰鹽、無機顆粒、離子液體。與正極一樣,負極包含負極活性材料及固態電解質,且另外包含傳導性材料及黏合劑。
然而,目前還沒有一種固態電解質能夠滿足全固態電池批量使用的規範。這是因為,對固態電解質而言,通常很難將離子傳導率、電化學穩定性、機械強度及與陽極或陰極材料的相容性結合在一起。
例如,可以特別提及無機化合物,其表現出非常高的離子傳導率,但在陽極處的電位及陰極處的高電位方面表現出電化學不穩定。( Y. Zhu, ACS Appl. Mater. Interfaces, 2015, 7, 23685-23693)
仍然需要開發能夠使陽極與全固態鋰離子電池中的固態電解質相容的解決方案。尤其是需要解決在充電及放電循環過程期間陽極體積變化的問題。最後,特別是在鋰金屬陽極之情況下,需要提供通過有效的方法防止樹狀晶形成之陽極。
因此,本發明的一個目的是提供一種塗層,其可直接施用於鋰離子電池的負極,使得能夠在固態電解質與電極活性物質之間具有物理性分隔。因此,本發明提供一種負極,其包含由一常用負極所組成之一第一層,及由根據本發明之陽極塗層所組成之一第二層。
本發明還旨在提供一種用於製造該陽極塗層的方法。最後,本發明有關於一種表現出此種塗層的陽極及用於製造此種陽極的方法。
最後,本發明旨在提供一種包含此種陽極的可充電鋰離子蓄電池。
發明概要
本發明提出的技術方案是提供一種陽極塗層,其使得該陰極能與全固態電池中的固態電解質相容。
本發明首先有關於一種陽極塗層,其由下列所組成:
a. 一或多種聚(二氟亞乙烯),
b. 一鋰鹽,及
c. 一傳導性添加劑。
本發明還有關於一種使用通過混合該塗層的所有成分所獲得的油墨來製造陽極塗層的方法。
本發明還有關於一種用於鋰離子電池的陽極,該陽極由一層塗覆有根據本發明之塗層之層之負極活性材料所組成。
本發明還有關於一種用於製造鋰離子電池之負極的方法,該方法包含以下操作:
- 提供一陽極,
- 在該陽極上沉積一塗層之層。
本發明的另一主題是一種鋰離子蓄電池,其包含一負極、一正極及一全固態電解質,其中該陽極如上所述。
本發明使得克服現有技術的缺點成為可能。其提供了一種具有介電常數均勻分佈的離子傳導塗層,同時維持足夠的機械強度以防止樹狀晶的形成。此塗層顯示出良好的還原穩定性及良好的可撓性,從而使其在充電與放電循環過程期間能夠耐受陽極體積的變化。
特別是在鋰陽極之情況下,根據本發明之塗層使得能夠停止可能導致短路之樹狀晶的生長,良好的介電常數均勻度使得能夠防止高濃度鋰離子之區域的形成。此塗層還使得能夠形成穩定的且對鋰金屬具有低電阻率之固態電解質界面(SEI),從而改善全固態電池之性能及夀命。
本發明實施例之說明
現在在下面的說明中以非限制性的方式更詳細地描述本發明。
根據第一個態樣,本發明有關於一種陽極塗層,其由下列組成:
a. 一或多種聚(二氟亞乙烯) (組分A),
b. 至少一種鋰鹽(組分B),及
c. 至少一種傳導性添加劑(組分C)。
根據各種實施方式,如果適當組合,該塗層包含以下特性。除非另有說明,否則所示含量均以重量表示。
組分A
本發明中所使用的半結晶氟聚合物是一種基於二氟亞乙烯的聚合物,通常用縮寫PVDF表示。
根據一個實施例,該PVDF是聚(二氟亞乙烯)均聚物,或二氟亞乙烯均聚物的混合物。
根據一個實施例,該PVDF是聚(二氟亞乙烯)均聚物,或二氟亞乙烯與至少一種與該二氟亞乙烯相容的共聚單體之共聚物。
根據一個實施例,該PVDF是半結晶的。
與二氟亞乙烯相容的共聚單體可為鹵化的(氟化的、氯化的或溴化的)或非鹵化的。
合適的氟化共聚單體之例子是:氟乙烯、四氟乙烯、六氟丙烯、三氟丙烯,特別是3,3,3-三氟丙烯、四氟丙烯,特別是2,3,3,3-四氟丙烯或1,3,3,3-四氟丙烯、六氟異丁烯、全氟丁基乙烯、五氟丙烯,特別是1,1,3,3,3-五氟丙烯或1,2,3,3,3-五氟丙烯、全氟化烷基乙烯醚,特別是通式為Rf-O-CF-CF
2的那些,Rf為烷基,較佳地C
1至C
4烷基(較佳例子為全氟(丙基乙烯醚)及全氟(甲基乙烯醚))。
該氟化共聚單體可包含氯或溴原子。其尤其是可選自溴三氟乙烯、氯氟乙烯、氯三氟乙烯及氯三氟丙烯。氯氟乙烯可意指1-氯-1-氟乙烯或1-氯-2-氟乙烯。1-氯-1-氟乙烯異構物係較佳的。氯三氟丙烯較佳地為1-氯-3,3,3-三氟丙烯或2-氯-3,3,3-三氟丙烯。
該VDF共聚物還可包含非鹵化單體,如乙烯,及/或丙烯酸或甲基丙烯酸共聚單體。
該氟聚合物較佳地含有至少50莫耳%的二氟亞乙烯。
根據一個實施例,該PVDF是二氟亞乙烯(VDF)與六氟丙烯(HFP)的共聚物(P(VDF-HFP)),相對於該共聚物之重量,具有2重量%至23重量%,較佳地4重量%至15%重量的六氟丙烯單體單元。
根據一個實施例,該PVDF是聚(二氟亞乙烯)均聚物與VDF-HFP共聚物的混合物。
根據一個實施例,該PVDF是二氟亞乙烯與四氟乙烯(TFE)的共聚物。
根據一個實施例,該PVDF是二氟亞乙烯與氯三氟乙烯(CTFE)的共聚物。
根據一個實施例,該PVDF是VDF-TFE-HFP三元共聚物。根據一個實施例,該PVDF是VDF-TrFE-TFE三元共聚物(TrFE是三氟乙烯)。在這些三元共聚物中,VDF的含量為至少10重量%,該共聚單體以不同的比例存在。
根據一個實施例,該PVDF是二或多種VDF-HFP共聚物的混合物。HFP類型之共聚單體的存在,使得能夠改善該塗層對鋰金屬之化學穩定性。
根據一個實施例,該PVDF包含帶有至少一種以下官能之單體單元:羧酸、羧酸酐、羧酸酯、環氧基(如,環氧丙基)、醯胺、羥基、羰基、巰基、硫化物、㗁唑啉、酚基、酯、醚、矽氧烷、磺的、硫的、磷的或膦的。該官能是根據此領域技術人員熟知之技術,通過化學反應引入,該化學反應可為氟化單體與帶有至少一個該官能基及能夠與該氟化單體共聚合的乙烯基官能之單體的接枝或共聚合。
根據一個實施例,該官能基帶有羧酸官能,其是選自丙烯酸、甲基丙烯酸、(甲基)丙烯酸羥乙酯、(甲基)丙烯酸羥丙酯和(甲基)丙烯酸羥乙基己酯的(甲基)丙烯酸類型的基團。
根據一個實施例,該帶有羧酸官能之單元額外地包含選自氧、硫、氮和磷的雜原子。
根據一個實施例,該官能性係在合成過程中通過使用的轉移劑之方式引入。該轉移劑是具有莫耳質量小於或等於20 000克/莫耳,帶有選自以下基團之官能基的聚合物:羧酸、羧酸酐、羧酸酯、環氧基(如,環氧丙基)、醯胺、羥基、羰基、巰基、硫化物、㗁唑啉、酚基、酯、醚、矽氧烷、磺的、硫的、磷的或膦的。這種類型的轉移劑之例子為丙烯酸寡聚物。
該PVDF中該官能基的含量為至少0.01莫耳%,較佳地至少0.1莫耳%及最多15莫耳%,較佳地最多10莫耳%。
該PVDF較佳地具有高分子量。本文中使用的術語“高分子量”應理解為意指具有熔體黏度大於100Pa.s,較佳地大於500Pa.s,更佳地大於1000Pa.s,有利地大於2000 Pa.s.的PVDF。該黏度係根據標準ASTM D3825,使用毛細管流變儀或平行板流變儀,在232℃、100 s
-1的剪切梯度下測量。這兩種方法得到相似的結果。
本發明中所使用的PVDF均聚物及VDF共聚物可通過諸如乳化聚合之已知的聚合方法獲得。
根據一個實施例,其等係在無氟化界面活性劑之存在下,通過乳化聚合方法製備。
該PVDF的聚合產生乳膠,其通常具有固體含量從10重量%至60重量%,較佳地從10重量%至50重量%,及具有重量平均顆粒尺寸小於1微米,較佳地小於1000nm,較佳地小於800nm及更佳地小於600nm。該顆粒的重量平均尺寸通常為至少10nm,較佳地至少50nm,且有利地該平均尺寸在從100至400nm之範圍內。該聚合物顆粒可形成稱為二次顆粒的黏聚物,其重量平均尺寸小於5000μm,較佳地小於1000μm,有利地介於1至80微米之間及較佳地從2至50微米。在配製及施用至基材期間,該黏聚物會分解成個別的顆粒。
根據一些實施例,該PVDF均聚物及該VDF共聚物係由生物基VDF組成。術語“生物基”是指“由生物質產生”。這使得能夠改善塗層的生態足跡。生物基VDF之特徵在於可再生碳的含量,亦即根據標準NF EN 16640,由
14C的含量測定,源自生物材料或生物質的天然碳為至少1原子%。術語“可再生碳”表示碳是天然來源且源自生物材料(或生物質),如下所示。根據一些實施例,該VDF之生物碳含量可大於5%,較佳地大於10%,較佳地大於25%,較佳地大於或等於33%,較佳地大於50%,較佳地大於或等於至66%,較佳地大於75%,較佳地大於90%,較佳地大於95%,較佳地大於98%,較佳地大於99%,有利地等於100%。
組份B
作為非限制性例子,該鋰鹽(或鋰鹽等)係選自LiPF
6(六氟磷酸鋰)、LiFSI (雙(氟磺醯基)亞胺化鋰)、TFSI (雙(三氟甲基磺醯基)亞胺化鋰)、LiTDI (2-三氟甲基-4,5-二氰基咪唑酸鋰)、LiPOF
2、LiB(C
2O
4)
2、LiF
2B(C
2O
4)
2、LiBF
4、LiNO
3、LiClO
4及二或多種所述鹽的混合物。
組分C
該傳導性添加劑可為能夠在不溶解該氟聚合物的情況下使其膨脹且具有大於1的介電常數之有機分子或有機分子的混合物。根據一個實施例,該組分C係選自醚類(直鏈或環狀)、酯類、內酯類、腈類、碳酸鹽類及離子液體。
作為非限制性例子,在該醚類中可提到直鏈或環狀醚,例如二甲氧基乙烷(DME)、2至5個氧乙烯單元的寡聚乙二醇的甲基醚、二氧戊環、二㗁烷、二丁醚、四氫呋喃及其等之混合物。
在酯類中,可以提到磷酸酯或亞硫酸酯。例如,可以提到甲酸甲酯、乙酸甲酯、丙酸甲酯、乙酸乙酯、乙酸丁酯、γ-丁內酯或其等之混合物。
在內酯類中,尤其可以提到環己酮。
在腈類中,可以提到例如乙腈、丙酮腈、丙腈、甲氧基丙腈、二甲胺基丙腈、丁腈、異丁腈、戊腈、新戊腈(pivalonitrile)、異戊腈、戊二腈、甲氧基戊二腈、2-甲基戊二腈、3-甲基戊二腈、己二腈、丙二腈及其等之混合物。
在碳酸酯中,可以提及例如環狀碳酸酯,例如碳酸伸乙酯(EC) (CAS:96-49-1)、碳酸丙烯酯(PC) (CAS:108-32-7) 、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)、苯碳酸甲酯(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)、碳酸伸乙烯酯(VC) (CAS:872-36-6)、碳酸氟伸乙酯(FEC) (CAS:114435) -02-8)、碳酸三氟丙烯酯(CAS:167951-80-6)或其等之混合物。
在離子液體中,可以特別提及EMIM:FSI、PYR:FSI、EMIM:TFSI、PYR:TFSI、EMIM:BOB、PYR:BOB、EMIM:TDI、PYR:TDI、EMIM:BF4或PYR:BF4。
根據本發明之陽極塗層的重量組成為:
- 組分A,重量比率介於20%與80%之間;
- 組分B,重量比率介於1%與40%之間;
- 組分C,重量比率介於2%與50%之間;
此等比率之總和為100%。
本發明還有關於通過溶劑途徑,由將該塗層的所有成分混合在溶劑中所獲得的油墨來製造上述陽極塗層的方法。
使製備該塗層成為可能的油墨,可通過本領域技術人員已知的任何類型的混合器產生,如行星式混合器、離心機、軌道式混合器、攪拌軸或Ultra-Turrax。該油墨的不同成分沒有按精確的順序添加。該油墨可在不同溫度下製造,範圍從環境溫度最高到用於製造該油墨的溶劑之沸點。
所用的溶劑較佳地為漢森參數大於2的極性溶劑。作為非限制性例子,可特別提及丙酮、乙醯基檸檬酸三乙酯(TEAC)、γ-丁內酯(GBL)、環己酮(CHO)、環戊酮(CPO)、鄰苯二甲酸二丁酯(DBP)、癸二酸二丁酯(DBS) 、碳酸二乙酯(DEC)、鄰苯二甲酸二乙酯(DEP)、二氫左旋葡萄糖酮(Cyrene)、二甲基乙醯胺(DMAc)、N,N-二甲基甲醯胺(DMF)、二甲基亞碸(DMSO)、1,4-二㗁烷、3-庚酮、六甲基磷醯胺(HMPA)、3-己酮、甲基乙基酮(MEK)、N-甲基-2-吡咯啶酮(NMP)、3-辛酮、3-戊酮、碳酸丙烯酯(PC)、四氫呋喃(THF)、四甲基脲(TMU)、三乙酸甘油酯、檸檬酸三乙酯(TEC)、磷酸三乙酯(TEP)、磷酸三甲酯(TMP)、N,N'-四丁基丁二醯胺(TBSA)或上述溶劑中二或多種之混合物。
根據一個實施例,根據本發明之塗層陽極的孔隙率小於10%,較佳地小於5%。
該塗層電極(CE)的孔隙率係根據以下M. Cai, Nature Communications, 10, 2019, 4597公開刊物中描述的計算獲得:
其中V
CE代表該塗層電極的真實體積,且係經由該塗層電極的表面積乘以該塗層電極的厚度計算而得。V
緻密CE表示無任何孔隙之各成分所佔的體積,且係按以下公式計算:
V
緻密CE是該塗層電極中各成分所佔體積的總和。
此塗層之厚度範圍可從0.1至100µm,較佳地從0.1至50µm及更佳地從0.1至35μm。
本發明還有關於用於全固態鋰離子電池的陽極,該陽極包含下列,較佳地由下列所組成:塗覆有根據本發明之塗層之層之一活性物質。較佳地,該陽極中之該活性物質係沉積在一金屬載體上。
根據一個實施例,該負極中之活性物質係選自石墨、Li
4Ti
5O
12型之鈦酸鋰、氧化鈦TiO
2、矽或鋰/矽合金、氧化錫、鋰介金屬化合物、鋰金屬或其等之混合物。
除了該鋰金屬外,該活性物質還混合與一電子傳導物質及一黏合劑。
該電子傳導物質係選自碳黑、天然或合成石墨、碳纖維、碳奈米管、金屬纖維及粉末以及傳導性金屬氧化物。較佳地,其等係選自碳黑、天然或合成石墨、碳纖維及碳奈米管。
用於製造該陽極的黏合劑係選自下列之聚合物:聚烯烴(例如:聚乙烯或聚丙烯)、可表現出酸官能之氟聚合物(PVDF)、聚丙烯酸(PAA)、聚丙烯腈(PAN)、纖維素類聚合物、聚苯碸、聚醚碸、酚醛樹脂、乙烯基酯樹脂、環氧樹脂、PTFE或液晶聚合物。
因此,該陽極包含下列,較佳地由下列所組成:塗覆有根據本發明之塗層之層之活性物質,該塗層較佳地由:a)至少一種聚(二氟亞乙烯) (組分A)、b)至少一種鋰鹽(組分B)及至少一種傳導性添加劑(組分C)所組成。較佳地,該陽極具有如本申請案中所定義的孔隙率。
本發明還有關於一種用於製造鋰離子電池之負極的方法,該方法包含以下操作:
- 提供一陽極,
- 在該陽極上沉積根據本發明之塗層之層。
因此,本發明提供一種負極,其包含下列,較佳地由下列所組成:一金屬載體,其上沈積塗覆有根據本發明之塗層之層之活性物質,該塗層包含下列,較佳地由下列所組成:a)至少一種聚(二氟亞乙烯) (組分A)、b)至少一種鋰鹽(組分B)及至少一種傳導性添加劑(組分C)。
該塗層可通過本領域技術人員已知的任何沉積方法產生,如通過溶劑途徑、浸漬提拉法、離心塗佈法、噴塗法或通過壓延塗佈的方法塗佈。這些沉積技術可在從5℃最高180℃的不同溫度下進行。
該陽極之金屬載體通常係由銅製成。該金屬載體可為表面經處理的且具有厚度為5μm或更大的導電底漆。該載體也可為由碳纖維製成的織物或非織物。
本發明的另一主題是一種全固態鋰離子蓄電池,其包含一負極、一正極及一全固態電解質,其中該陽極如上所述。
根據一個實施例,該電池之該陰極上也塗覆有根據本發明之塗層之層。
範例
以下範例以非限制性方式說明本發明的範圍。
氟聚合物(FP)溶液之製備
為獲得完全的溶解,使用行星式混合器,於2000rpm下1分鐘、6次將14.992g HFP含量為23重量%的VDF-HFP共聚物溶解在85.753g丙酮中。
用於塗層:FP/LiFSI/S1 60/20/20之油墨I的製備
使用磁力攪拌器在21℃下10分鐘,將0.441g LiFSI溶解在0.449g四乙二醇二甲醚(CAS 143-24-8)中。然後,加入8.826g之15% FP丙酮溶液。
用於塗層:FP/LiFSI/MPCN 60/20/20之油墨II的製備
使用磁力攪拌器在21℃下10 分鐘,將0.3986 g LiFSI溶解在0.3986g甲氧基丙腈(CAS 110-67-8)中。然後,加入7.972g之15% FP丙酮溶液。
用於塗層:FP/LiFSI/S1 40/30/30之油墨III的製備
使用磁力攪拌器在21℃下10分鐘,將0.528 g LiFSI溶解在0.528g四乙二醇二甲醚(CAS 143-24-8)中。然後,加入4.675g之15% FP丙酮溶液。
使用該油墨III塗佈鋰金屬
使用油墨III,以塗佈刮刀輔助,塗佈厚度200 µm之鋰金屬薄片。所沈積的濕膜之厚度為50 µm。在環境溫度下乾燥2小時後,該沈積膜的厚度經測量為38 µm。之後對該電極進行壓延,在該鋰金屬上獲得2 µm的沈積物。利用阻抗頻譜術測量離子傳導性。所獲得的值為0.553 mS/cm。
樹狀晶測試:
進行樹狀晶測試,比較鋰金屬上使用油墨III獲得的塗層與標準液態電解質。
方法:該方法包含將對稱鋰金屬/鋰金屬電池充電及放電;然後測量該電池之電位。此電位與電極之表面積成正比,因此樹狀晶的出現會導致電位增加。
所使用的系統:
陰極:塗層或非塗層鋰金屬
陽極:鋰金屬
使用0.25 mA的正電流將電池充電至能量密度為0.25 mAh。之後使用0.25 mA的負電流將該電池放電至能量密度為0.25 mAh。
在液態電解質之情況下,將多孔性PE隔板浸泡在含有配製於EC/EMC 3/7 (以體積計)中之1 M LiFSI的電解質溶液中。
使電池之起始電位翻倍所需的時間示於表1中。
[表1]
技術 | 時間 |
油墨III塗層 | >384H |
液態電解質 | 24H |
(無)
Claims (15)
- 一種陽極塗層,其由下列組成: a. 至少一種聚(二氟亞乙烯) (PVDF) (組分A), b. 至少一種鋰鹽(組分B),及 c. 至少一種傳導性添加劑(組分C)。
- 如請求項1之塗層,其中該組分A係選自聚(二氟亞乙烯)均聚物及二氟亞乙烯與至少一個選自於下列之共聚單體之共聚物:氟乙烯、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、六氟異丁烯、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(丙基乙烯醚)、全氟(甲基乙烯醚)、溴三氟乙烯、氯氟乙烯、氯三氟乙烯、氯三氟丙烯、乙烯及其等之混合物。
- 如請求項1或2之塗層,其中該PVDF包含帶有至少一種以下官能之單體單元:羧酸、羧酸酐、羧酸酯、環氧基(如,環氧丙基)、醯胺、羥基、羰基、巰基、硫化物、㗁唑啉、酚基、酯、醚、矽氧烷、磺的、硫的、磷的或膦的。
- 如請求項1至3中任一項之塗層,其中該組分B係選自LiPF 6(六氟磷酸鋰)、LiFSI (雙(氟磺醯基)亞胺化鋰)、TFSI (雙(三氟甲基磺醯基)亞胺化鋰)、LiTDI (2-三氟甲基-4,5-二氰基咪唑酸鋰)、LiPOF 2、LiB(C 2O 4) 2、LiF 2B(C 2O 4) 2、LiBF 4、LiNO 3、LiClO 4及二或多種所述鹽的混合物。
- 如請求項1至4中任一項之塗層,其中該組分C係選自醚類,其為直鏈或環狀、酯類、內酯類、腈類、碳酸鹽類及離子液體。
- 如請求項1至5中任一項之塗層,其具有範圍從0.1至100µm,較佳地從0.1至50µm,及更佳地從0.1至35μm之厚度。
- 如請求項1至6中任一項之塗層,其具有下列重量組成: - 組分A,比率介於20%與80%之間; - 組分B,比率介於1%與40%之間; - 組分C,比率介於2%與50%之間; 此等比率之總和為100%。
- 一種用於製造如請求項1至7中任一項之陽極塗層之方法,其係由通過將該塗層的所有成分混合在溶劑中所獲得的油墨來製造。
- 如請求項8之方法,其中該溶劑係選自下列:丙酮、乙醯基檸檬酸三乙酯、γ-丁內酯、環己酮、環戊酮、鄰苯二甲酸二丁酯、癸二酸二丁酯 、碳酸二乙酯、鄰苯二甲酸二乙酯、二氫左旋葡萄糖酮(dihydrolevoglucosenone)、二甲基乙醯胺、N,N-二甲基甲醯胺、二甲基亞碸、1,4-二㗁烷、3-庚酮、六甲基磷醯胺、3-己酮、甲基乙基酮、N-甲基-2-吡咯啶酮、3-辛酮、3-戊酮、碳酸丙烯酯、四氫呋喃、四甲基脲、三乙酸甘油酯、檸檬酸三乙酯、磷酸三乙酯、磷酸三甲酯、N,N'-四丁基丁二醯胺(N,N’-tetrabutylsuccinamide)及其等之混合物。
- 一種用於全固態鋰離子電池的陽極,該陽極由下列所組成:塗覆有如請求項1至7中任一項之一塗層之層之一活性物質。
- 如請求項9之陽極,其中該活性物質係選自石墨、Li 4Ti 5O 12型之鈦酸鋰、氧化鈦TiO 2、矽或鋰/矽合金、氧化錫、鋰介金屬化合物,或其等之混合物。
- 如請求項10或11之陽極,其具有小於10%,較佳地小於5%之孔隙率。
- 一種用於製造鋰離子電池之負極的方法,該方法包含以下操作: - 提供一陽極, - 在該陽極上沉積如請求項1至7中任一項之一塗層之層。
- 一種全固態鋰離子蓄電池,其包含一陰極、如請求項10至12中任一項之陽極及一全固態電解質。
- 如請求項15之電池,其中該陰極上塗覆有如請求項1至7中任一項之一塗層之層。
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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 |
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TW202324814A true TW202324814A (zh) | 2023-06-16 |
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EP (1) | EP4409652A1 (zh) |
KR (1) | KR20240067957A (zh) |
CN (1) | CN118020162A (zh) |
FR (1) | FR3127634A1 (zh) |
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WO2016205653A1 (en) * | 2015-06-19 | 2016-12-22 | SolidEnergy Systems | Multi-layer polymer coated li anode for high density li metal battery |
EP3526845A4 (en) * | 2016-10-11 | 2020-05-06 | GRST International Limited | Anode slurry for lithium-ion batteries |
US10727531B2 (en) * | 2018-06-21 | 2020-07-28 | Global Graphene Group, Inc. | Lithium metal secondary battery featuring an anode-protecting layer |
JP7272120B2 (ja) * | 2018-12-11 | 2023-05-12 | Tdk株式会社 | リチウム二次電池 |
JP7314739B2 (ja) * | 2019-09-21 | 2023-07-26 | Tdk株式会社 | リチウム二次電池 |
CN110993945B (zh) * | 2019-11-13 | 2021-08-27 | 宁德新能源科技有限公司 | 用于锂金属电池的负极保护材料和负极极片及其制备方法 |
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2021
- 2021-09-27 FR FR2110145A patent/FR3127634A1/fr active Pending
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- 2022-09-23 WO PCT/FR2022/051795 patent/WO2023047065A1/fr active Application Filing
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KR20240067957A (ko) | 2024-05-17 |
FR3127634A1 (fr) | 2023-03-31 |
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