JP6748645B2 - 有機リチウム電池 - Google Patents
有機リチウム電池 Download PDFInfo
- Publication number
- JP6748645B2 JP6748645B2 JP2017530293A JP2017530293A JP6748645B2 JP 6748645 B2 JP6748645 B2 JP 6748645B2 JP 2017530293 A JP2017530293 A JP 2017530293A JP 2017530293 A JP2017530293 A JP 2017530293A JP 6748645 B2 JP6748645 B2 JP 6748645B2
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- JP
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- Prior art keywords
- lithium
- electrolyte
- battery according
- battery
- positive electrode
- 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.)
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- 229910052744 lithium Inorganic materials 0.000 title claims description 37
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 26
- -1 polypropylene Polymers 0.000 claims description 45
- 239000003792 electrolyte Substances 0.000 claims description 37
- 239000005518 polymer electrolyte Substances 0.000 claims description 33
- 229910003002 lithium salt Inorganic materials 0.000 claims description 32
- 159000000002 lithium salts Chemical class 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 31
- 229920000570 polyether Polymers 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 27
- 125000004122 cyclic group Chemical group 0.000 claims description 26
- 239000011244 liquid electrolyte Substances 0.000 claims description 26
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 22
- 229920001577 copolymer Polymers 0.000 claims description 21
- 230000001747 exhibiting effect Effects 0.000 claims description 18
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 claims description 17
- 125000001979 organolithium group Chemical group 0.000 claims description 17
- 229920005596 polymer binder Polymers 0.000 claims description 17
- 239000002491 polymer binding agent Substances 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 17
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
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- 229920001519 homopolymer Polymers 0.000 claims description 14
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 125000000524 functional group Chemical group 0.000 claims description 10
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- 229910052717 sulfur Inorganic materials 0.000 claims description 10
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- 239000011593 sulfur Substances 0.000 claims description 9
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 8
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 8
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 7
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- 238000007254 oxidation reaction Methods 0.000 claims description 7
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 6
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 6
- 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 6
- 238000000034 method Methods 0.000 claims description 6
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- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 claims description 4
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 4
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- 229910013063 LiBF 4 Inorganic materials 0.000 claims description 4
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- HZRMTWQRDMYLNW-UHFFFAOYSA-N lithium metaborate Chemical compound [Li+].[O-]B=O HZRMTWQRDMYLNW-UHFFFAOYSA-N 0.000 claims description 3
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 3
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- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 18
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- 239000011230 binding agent Substances 0.000 description 14
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- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 4
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- FQVOWPCGHLYSLB-UHFFFAOYSA-N pyrene-4,5,9,10-tetrone Chemical compound C12=C(C(C3=O)=O)C=CC=C2C(=O)C(=O)C2=C1C3=CC=C2 FQVOWPCGHLYSLB-UHFFFAOYSA-N 0.000 description 1
- 150000004059 quinone derivatives Chemical class 0.000 description 1
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- UUBIWGRMBVAUIK-UHFFFAOYSA-N tetracyclo[5.5.2.04,13.010,14]tetradeca-1(13),4,6,10(14),11-pentaene Chemical compound C1CC2=CC=C3CCC4=CC=C1C2=C43 UUBIWGRMBVAUIK-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
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Description
・充放電サイクル中の活物質の体積の変化に起因するストレスに耐えるための適切な機械的強度;
・腐食性の高い溶液(すなわち、電解液)中に浸漬するため、長期間持ちこたえることを保証する十分な化学耐性;並びに、
・電解質のアニオン及びカチオンの拡散を可能にし、且つ、一方の電極から他方の電極への活物質の輸送を防止する適切な多孔質構造。
− リチウム金属又はリチウム金属の合金を含む負極;
− 任意に集電体に支持された正極(前記正極は、1つ以上の酸化還元有機構造体と、少なくとも1つのポリマーバインダーP1と、電子伝導性を発現する少なくとも1つの物質とを含み、前記酸化還元有機構造体は、元素硫黄S8及び少なくとも1つのS−S結合を含む硫黄含有有機化合物から選択される硫黄含有物とは異なる);並びに、
− 電解質で含浸された多孔質セパレータ;
前記有機リチウム電池は、該多孔質セパレータが少なくともポリプロピレンを含む二軸延伸セパレータであり、該電解質が少なくとも1つの低分子量の液体直鎖又は環状ポリエーテルと少なくとも1つのリチウム塩L1とを含むことを特徴とする。
* 式H−[O−CH2−CH2]m−OH(式中、mは1〜13である)のポリエチレングリコール;
* 式R−[O−CH2−CH2]p−O−R’(式中、pは1〜13であり、R及びR’は、同一又は異なって、1〜20個の炭素原子含むことができる直鎖、分岐状又は環状アルキル基である)のグリコールエステル;
* 式R1−[CH2−O]q−R1’(式中、qは1〜13であり、R1及びR1’は、同一又は異なって、1〜20個の炭素原子及び任意にヘテロ原子を含むことができる直鎖、分岐状又は環状アルキル基である)のエーテル;
* 2〜20個の炭素原子を含むことができる環状エーテル;3〜40個の炭素原子を含むことができる環状ポリエーテル;並びに、
* それらの混合物の1つ。
a)電極ペーストを得るために、少なくとも1つの酸化還元有機構造体を、少なくとも1つの電子伝導性を発現する物質、少なくとも1つのポリマーバインダーP1、任意に少なくとも1つのリチウム塩L2、任意に少なくとも1つの低分子量の液体直鎖又は環状ポリエーテル及び任意に前記ポリマーバインダーP1の少なくとも1つの溶媒と混合すること;
b)前記電極ペーストを少なくとも1つの支持体に塗布すること;
c)支持されたフィルムの形状の正極を得るために、前記電極ペーストを乾燥させること、によって調製することができる。
A)特に、少なくとも1つの低分子量の液体直鎖又は環状ポリエーテルを少なくとも1つのリチウム塩L1と混合することによる、本発明で定義される液体電解質又はゲル化ポリマー電解質の調製工程;
B)本発明で定義される正極、負極及び多孔質セパレータを組み立てる工程;
前記方法は、さらに以下の工程の一方又は他方を含む:
C−1)工程A)で調製した液体電解質を用いて、B)工程で得られた組み立て品を含浸する工程;又は
C−2)工程B)の組み立ての前に、工程A)で調製したゲル化ポリマー電解質を用いて、多孔質セパレータを含浸する工程。
− Ketjenblack 600JD(商標)カーボンブラック,AkzoNobel;
− アントラキノン(純度97%),Sigma Aldrich;
− ポリエチレンイミン(PEI)の50重量%水溶液,Fluka,Sigma Aldrich;
− LiTFSI,3M;
− シリコーン処理PETフィルム,Mitsubishi;
− 純度99%のテトラエチレングリコールジメチルエーテル(TEGDME),Sigma Aldrich;
− 分子量約105g.mol−1のPEOのコポリマー(co−PEO),ZSN 8100,Zeospan;
− ポリプロピレンS−1製の二軸延伸単層セパレータ,BPF220,Bollore;
− ポリプロピレンS−2製の単層セパレータ,Celgard 2500。
本発明の有機リチウム電池の製造
1.1 正極の調製
周囲温度で、2.25gのKetjenblack カーボンブラックと31.5gのアントラキノンを手動によって混合した。
テトラエチレングリコールジメチルエーテル(TEGDME)中のLiTFSIからなり、30.1重量%のLiTFSIを含む液体電解質を調製した。このようにして、1.51mol/lのリチウム塩のTEGDME溶液が得られた。
固体ポリマー電解質は、リチウム塩(LiTFSI)、PEO Zeospan(商標)のコポリマー及びPVDF−co−HFPの混合物を押出し、次いで、シリコーン処理されたPETの2つのプラスチックフィルムの間で、125℃で得られた電解質ペーストを積層することによって調製した。
3つの電池B−1、B−2及びB−3を、無水環境下(露点が−40℃未満の空気下)、大気温度で、手動積層によって下記を組み立てることにより作製した。
− 上記実施例1.1で得られた正極E−1;
− 約100μmの厚さのリチウム金属フィルムの形状のリチウム金属を含む負極;及び、
− 上記実施例1.2で得られた電解液を含浸させたセパレータS−1若しくは上記実施例1.2で得られた電解液を含浸したセパレータS−2又は上記実施例1.3で得られた固体ポリマー電解質SP−1。
Claims (22)
- − リチウム金属又はリチウム金属の合金を含む負極、
− 任意に集電体に支持された正極であって、少なくとも1つの酸化還元有機構造体と、少なくとも1つのポリマーバインダーP1と、少なくとも1つの電子伝導性を発現する物質とを含み、前記酸化還元有機構造体が、元素硫黄S8及び少なくとも1つのS−S結合を含む硫黄含有有機化合物から選択される硫黄含有物とは異なる正極、及び、
− 電解質で含浸された多孔質セパレータ
を含む有機リチウム電池であって、
該多孔質セパレータが少なくともポリプロピレンを含む二軸延伸セパレータであり、該電解質が少なくとも1つの低分子量の液体直鎖又は環状ポリエーテルと少なくとも1つのリチウム塩L1とを含むことを特徴とする有機リチウム電池。 - 低分子量の液体直鎖又は環状ポリエーテルが、10000g・mol−1以下のモル質量を有する液体直鎖又は環状ポリエーテルであることを特徴とする請求項1に記載の電池。
- 多孔質セパレータが、5μm〜50μmの範囲の厚さを示すことを特徴とする請求項1又は2に記載の電池。
- 多孔質セパレータが、50体積%以上の空孔率を示すことを特徴とする請求項1〜3のいずれか一項に記載の電池。
- 多孔質セパレータが、50nm〜3μmの平均サイズを有する細孔を示すことを特徴とする請求項1〜4のいずれか一項に記載の電池。
- 多孔質セパレータが、少なくとも5mmの破断時伸びを示すことを特徴とする請求項1〜5のいずれか一項に記載の電池。
- 多孔質セパレータが、50〜500s/100cm3の範囲のガーレー型の多孔性を示すことを特徴とする請求項1〜6のいずれか一項に記載の電池。
- 多孔質セパレータが、どのような厚みでも、厳密に15%未満の縦方向の熱収縮及び/又は横方向の熱収縮を示すことを特徴とする請求項1〜7のいずれか一項に記載の電池。
- リチウム塩L1が、フッ素酸リチウム(LiFO3)、リチウムビス(トリフルオロメタンスルホニル)イミド(LiTFSI)、ヘキサフルオロリン酸リチウム(LiPF6)、フルオロホウ酸リチウム(LiBF4)、メタホウ酸リチウム(LiBO2)、過塩素酸リチウム(LiClO4)、硝酸リチウム(LiNO3)、リチウムビス(フルオロスルホニル)イミド(LiFSI)、リチウムビス(オキサラト)ボレート(LiBOB又はLiB(C2O4)2)及びそれらの混合物から選択されることを特徴とする請求項1〜8のいずれか一項に記載の電池。
- 電解質がゲル化ポリマー電解質であり、さらに少なくとも1つのポリマーバインダーP2を含むことを特徴とする請求項1〜9のいずれか一項に記載の電池。
- ポリマーバインダーP2が、エチレンのホモポリマー及びコポリマー;プロピレンのホモポリマー及びコポリマー;エチレンオキシド、メチレンオキシド、プロピレンオキシド、エピクロロヒドリン又はアリルグリシジルエーテルのホモポリマー及びコポリマー並びにそれらの混合物;ハロゲン化ポリマー;アニオン型の非電子伝導性ポリマー;ポリアクリレート;カチオン型のポリマー;並びにそれらの混合物の1つから選択できることを特徴とする請求項10に記載の電池。
- ゲル化ポリマー電解質が、該ゲル化ポリマー電解質の全重量に対して、20〜70重量%のポリマーバインダーP2を含むことを特徴とする請求項10又は11に記載の電池。
- ゲル化ポリマー電解質が、該ゲル化ポリマー電解質の全重量に対して、15〜45重量%のリチウム塩L1を含むことを特徴とする請求項10〜12のいずれか一項に記載の電池。
- ゲル化ポリマー電解質が、該ゲル化ポリマー電解質の全重量に対して、5〜40重量%の低分子量の液体直鎖又は環状ポリエーテルを含むことを特徴とする請求項10〜13のいずれか一項に記載の電池。
- 電解質が液体電解質であり、該液体電解質中のリチウム塩L1の濃度が0.5〜8モル/lであることを特徴とする請求項1〜9のいずれか一項に記載の電池。
- 正極が、該正極の全重量に対して少なくとも45重量%の酸化還元有機構造体を含むことを特徴とする請求項1〜15のいずれか一項に記載の電池。
- 酸化還元有機構造体が、少なくとも2つのカルボニルC=O官能基、2つのチオンC=S官能基又は2つのイミンC=N官能基を含むことを特徴とする請求項1〜16のいずれか一項に記載の電池。
- 正極が、該正極の全重量に対して、1〜30重量%の電子伝導性を発現する物質を含むことを特徴とする請求項1〜17のいずれか一項に記載の電池。
- 電子伝導性を発現する物質が、カーボンブラック、spカーボン、アセチレンブラック、炭素繊維及びナノ繊維、カーボンナノチューブ、グラフェン、グラファイト、金属粒子及び繊維、並びに、それらの混合物の1つから選択されることを特徴とする請求項1〜18のいずれか一項に記載の電池。
- 正極が、該正極の全重量に対して、2〜30重量%のポリマーバインダーP1を含むことを特徴とする請求項1〜19のいずれか一項に記載の電池。
- ポリマーバインダーP1が、エチレンのホモポリマー及びコポリマー;プロピレンのホモポリマー及びコポリマー;エチレンオキシド、メチレンオキシド、プロピレンオキシド、エピクロロヒドリン若しくはアリルグリシジルエーテルのホモポリマー及びコポリマー並びにそれらの混合物;ハロゲン化ポリマー;ポリアクリレート;ポリアルコール;電子伝導性ポリマー;カチオン型のポリマー;アニオン型のポリマー;並びにそれらの混合物の1つから選択されることを特徴とする請求項1〜20のいずれか一項に記載の電池。
- 請求項1〜21のいずれか一項に記載の有機リチウム電池の製造方法であって、以下の工程を含むことを特徴とする方法:
A)請求項1〜21のいずれか一項に定義される液体電解質又はゲル化ポリマー電解質の調製工程;及び、
B)請求項1〜21のいずれか一項に定義される正極、負極及び多孔質セパレータを組み立てる工程、
該方法は、さらに以下の工程の一方又は他方を含む:
C−1)工程A)で調製した液体電解質を用いて、B)工程で得られた組み立て品を含浸する工程;又は
C−2)工程B)の組み立ての前に、工程A)で調製したゲル化ポリマー電解質を用いて、多孔質セパレータを含浸する工程。
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