JP2010534910A - コアシェル構造の電極活物質 - Google Patents
コアシェル構造の電極活物質 Download PDFInfo
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- JP2010534910A JP2010534910A JP2010518127A JP2010518127A JP2010534910A JP 2010534910 A JP2010534910 A JP 2010534910A JP 2010518127 A JP2010518127 A JP 2010518127A JP 2010518127 A JP2010518127 A JP 2010518127A JP 2010534910 A JP2010534910 A JP 2010534910A
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- 239000007772 electrode material Substances 0.000 title claims abstract description 77
- 239000011258 core-shell material Substances 0.000 title claims abstract description 28
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 31
- 229910052751 metal Inorganic materials 0.000 claims abstract description 28
- 239000002184 metal Substances 0.000 claims abstract description 28
- 239000003792 electrolyte Substances 0.000 claims abstract description 27
- 229920000642 polymer Polymers 0.000 claims abstract description 25
- 230000009477 glass transition Effects 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 47
- 229910002804 graphite Inorganic materials 0.000 claims description 28
- 239000010439 graphite Substances 0.000 claims description 28
- 239000002131 composite material Substances 0.000 claims description 18
- 239000008151 electrolyte solution Substances 0.000 claims description 18
- 239000002202 Polyethylene glycol Substances 0.000 claims description 17
- 229920001223 polyethylene glycol Polymers 0.000 claims description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 15
- 229910052744 lithium Inorganic materials 0.000 claims description 14
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 13
- -1 polyethylene Polymers 0.000 claims description 12
- 229910052752 metalloid Inorganic materials 0.000 claims description 8
- 150000002738 metalloids Chemical class 0.000 claims description 8
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- 229910044991 metal oxide Inorganic materials 0.000 claims description 5
- 150000004706 metal oxides Chemical class 0.000 claims description 5
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 8
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
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- 229910013870 LiPF 6 Inorganic materials 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
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- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 2
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- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 2
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- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
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- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
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- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 1
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- GEWWCWZGHNIUBW-UHFFFAOYSA-N 1-(4-nitrophenyl)propan-2-one Chemical compound CC(=O)CC1=CC=C([N+]([O-])=O)C=C1 GEWWCWZGHNIUBW-UHFFFAOYSA-N 0.000 description 1
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- CASZBAVUIZZLOB-UHFFFAOYSA-N lithium iron(2+) oxygen(2-) Chemical class [O-2].[Fe+2].[Li+] CASZBAVUIZZLOB-UHFFFAOYSA-N 0.000 description 1
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- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical class [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920005735 poly(methyl vinyl ketone) Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- CFJRPNFOLVDFMJ-UHFFFAOYSA-N titanium disulfide Chemical compound S=[Ti]=S CFJRPNFOLVDFMJ-UHFFFAOYSA-N 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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Abstract
本発明では、前記シェル(b)によって電池の初期充電時においてSEI膜の形成が抑制され、初期容量の低下が防止されるため、高容量電池を実現することができる。また、本発明に係るコアシェル構造の電極活物質、特にコアシェル構造の(半)金属系電極活物質は、従来の電極活物質、特に従来の(半)金属系電極活物質に比べて多少高い電気容量を有することができると共に、充放電中におけるガス発生を極力抑制することができる。
Description
1−1.電極活物質の製造
エチルアルコール100重量部にポリエチレングリコールメチルエーテルを0.1重量部溶解した後、この溶液に黒鉛粉末を溶液100重量部当り10重量部で添加した。これを12時間攪拌した後、ろ過し、黒鉛粉末にポリエチレングリコールメチルエーテルが約25nm厚さでコートされたコアシェル構造の電極活物質を製造した。
上記実施例1-1で製造した電極活物質、スチレンブタジエンゴム(SBR)及びカルボキシメチルセルロース(CMC)を、夫々96:2:2の重量比で混合し、水を加えてスラリーを製造した。このスラリーを10μm厚さの銅薄膜に塗布、乾燥して電極を製造した後、ロールプレスを行った。
上記実施例1-2で製造した電極と、そのカウンタ電極としてリチウム金属薄膜を使用し、前記陰極と陽極との間にポリエチレン製のセパレータを介在させた後、電解液を注入して二次電池を製造した。なお、前記電解液は、エチレンカーボネート(EC):ジエチルカーボネート(DEC)=1:2(体積比)の1M LiPF6溶液を使用した。
上記実施例1−2で製造した電極の代わりに、ポリエチレングリコールメチルエーテルがコートされていない通常の黒鉛粉末を電極活物質として含む電極を使用した以外は、上記実施例1−3と同様にして二次電池を製造した。
上記実施例1−1で使用したポリエチレングリコールメチルエーテルを電解液に含浸した後、−100℃から150℃まで5℃/分の速度で昇温しながら、DSCでガラス転移温度を測定した。なお、前記電解液としては、実施例1−3と同様に、エチレンカーボネート(EC):ジエチルカーボネート(DEC)=1:2(体積比)の1M LiPF6溶液を使用した。
上記実施例1及び比較例1で製造した二次電池を、25℃で5mVまで0.1Cの速度で充電し、5mVで0.005Cの電流になるまで充電し、1Vまで0.1Cの速度で放電するようにして2回の充放電を行った。次に、上記と同様にして、0.5C/0.5Cの速度で充放電を行い、サイクルにおける放電容量維持率及び充放電効率を測定し、その結果を表1及び図1、2に示す。
2−1.電極活物質の製造
エチルアルコール100重量部に、ポリエチレングリコールメチルエーテルを0.1重量部溶解した後、この溶液にSi/黒鉛複合粒子(直径20μm)を溶液100重量部当り10重量部で添加した。これを12時間攪拌した後、ろ過し、ポリエチレングリコールメチルエーテルが約25nmの厚さでコートされたコアシェル構造のSi/黒鉛複合電極活物質を製造した。
上記実施例2-1で製造したコアシェル構造のSi/黒鉛複合電極活物質、前記コアシェル構造の黒鉛系電極活物質、スチレンブタジエンゴム(SBR)及びカルボキシメチルセルロース(CMC)を、夫々4.8:91.2:2:2の重量比で混合し、水を加えてスラリーを製造した。このスラリーを10μm厚さの銅薄膜に塗布、乾燥して電極を製造した後、ロールプレスを行った。
上記実施例2−2で製造した電極と、そのカウンタ電極としてリチウム金属薄膜を使用し、前記両電極の間にポリエチレン製のセパレータを介在させた後、電解液を注入して二次電池を製造した。なお、前記電解液は、エチレンカーボネート(EC):ジエチルカーボネート(DEC)=1:2(体積比)の1M LiPF6溶液を使用した。
上記実施例2−1のコアシェル構造のSi/黒鉛複合電極活物質の製造時、ポリエチレングリコールメチルエーテルをエチルアルコール100重量部当り0.5重量部で使用してポリエチレングリコールメチルエーテルが約43nmの厚さでコートされたコアシェル構造のSi/黒鉛複合電極活物質を製造した以外は、上記実施例2と同様にして電極活物質、電極及び二次電池を製造した。
電極の製造時、上記実施例2−1で製造したコアシェル構造のSi/黒鉛複合電極活物質及びコアシェル構造の黒鉛系電極活物質の代わりに、通常のSi/黒鉛複合粒子を電極活物質として使用した以外は、上記実施例2−3と同様にして二次電池を製造した。
上記実施例2、3及び比較例2で製造した二次電池を25℃で5mVまで0.1Cの速度で充電し、5mVで0.005Cの電流になるまで充電し、1Vまで0.1Cの速度で放電するようにして2回の充放電を行った後、上記と同様にして、0.5C/0.5Cの速度で充放電を行った。なお、50サイクルを行った後、電池の厚さ増加率を測定し、その結果を表2に示す。また、サイクルにおける放電容量維持率及び充放電効率を測定し、その結果を表3及び図3、4に示す。
4−1.電極活物質の製造
エチルアルコール100重量部にポリエチレングリコールメチルエーテルを0.1重量部溶解した後、この溶液にSiO/黒鉛複合粒子(直径20μm)を溶液100重量部当り10重量部で添加した。これを12時間攪拌した後、ろ過し、ポリエチレングリコールメチルエーテルが約25nm厚さでコートされたコアシェル構造のSiO/黒鉛複合電極活物質を製造した。
上記実施例4−1で製造したコアシェル構造のSiO/黒鉛複合電極活物質、前記コアシェル構造の黒鉛系電極活物質、スチレンブタジエンゴム及びカルボキシメチルセルロースを、夫々14.6:82.4:1.5:1.5の重量比で混合し、水を加えてスラリーを製造した。このスラリーを10μm厚さの銅薄膜に塗布、乾燥して電極を製造した後、ロールプレスを行った。
実施例2−2で製造した電極の代わりに、実施例4−2で製造した電極を使用した以外は、上記実施例2−3と同様にして二次電池を製造した。
電極の製造時、上記実施例4−1で製造したコアセル構造のSiO/黒鉛複合電極活物質及びコアシェル構造の黒鉛系電極活物質の代わりに、通常のSiO/黒鉛複合粒子を電極活物質として使用した以外は、上記実施例4−3と同様にして二次電池を製造した。
上記実施例4及び比較例3で製造した二次電池を25℃で5mVまで0.1Cの速度で充電し、5mVで0.005Cの電流になるまで充電し、1.5Vまで0.1Cの速度で放電するようにして2回の充放電を行った後、上記と同様にして、0.5C/0.5Cの速度で充放電を行った。なお、50サイクルを行った後、電池の厚さ増加率を測定し、その結果を表4に示す。また、サイクルにおける放電容量維持率及び充放電効率を測定し、その結果を表5及び図5、6に示す。
Claims (10)
- コアシェル構造を有する電極活物質であって、
(a)リチウムイオンを吸蔵及び脱離できるコアと、及び
(b)電解液含浸時のガラス転移温度が25℃以下であるポリマー又はオリゴマーからなるシェルを備えてなり、
前記コアの表面にシェルがコートされたことを特徴とする、電極活物質。 - 前記シェル(b)が、電解液含浸時のガラス転移温度が−20℃以下であるポリマー又はオリゴマーから構成されることを特徴とする、請求項1に記載の電極活物質。
- 前記シェル(b)のポリマー又はオリゴマーが、イーサー(ether, −O−)基を含むことを特徴とする、請求項1に記載の電極活物質。
- 前記シェル(b)が、ポリエチレングリコール、ポリエチレンオキシド、ポリエチレングリコールメチルエーテル、ポリエチレングリコールジメチルエーテル、ポリプロピレンオキシド、ポリエチレン、ポリプロピレン、ポリイソブチレン、及びポリ塩化ビニリデンからなる群から選択されたポリマー又はオリゴマーから構成されることを特徴とする、請求項1に記載の電極活物質。
- 前記シェル(b)の厚さが0.001μm〜1μmであることを特徴とする、請求項1に記載の電極活物質。
- 前記コア(a)が、カーボン、石油コークス、活性炭、黒鉛、炭素繊維及び金属酸化物からなる群から選択されることを特徴とする、請求項1に記載の電極活物質。
- 前記コア(a)が、
(i)Si、Al、Sn、Sb、Bi、As、Ge、Pb及びLiからなる群から選択される金属又は半金属、
(ii)前記(i)の群から選択される金属又は半金属の酸化物、
(iii)前記(i)の群から選択される2種以上の金属又は半金属の合金、
(iv)前記(i)の群から選択される金属又は半金属と炭素材との複合体、或いは、
(v)前記(i)の群から選択される金属又は半金属の酸化物と炭素材との複合体であることを特徴とする、請求項1に記載の電極活物質。 - 請求項1〜7の何れか一項に記載の電極活物質を使用して製造された、電極。
- 請求項8に記載の電極を備えてなる、二次電池。
- 前記電極が、陰極であることを特徴とする、請求項9に記載の二次電池。
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WO2009014399A2 (en) | 2009-01-29 |
EP2183803A4 (en) | 2013-05-29 |
WO2009014399A3 (en) | 2009-03-19 |
EP2183803B1 (en) | 2015-04-29 |
CN101803071A (zh) | 2010-08-11 |
US20140099546A1 (en) | 2014-04-10 |
JP5558351B2 (ja) | 2014-07-23 |
EP2183803A2 (en) | 2010-05-12 |
CN102945963A (zh) | 2013-02-27 |
US8632698B2 (en) | 2014-01-21 |
US20110129729A1 (en) | 2011-06-02 |
CN102945963B (zh) | 2016-08-10 |
CN101803071B (zh) | 2014-09-10 |
US9349497B2 (en) | 2016-05-24 |
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