JP5279047B2 - リチウム二次電池用負極材料組成物及びリチウム二次電池 - Google Patents
リチウム二次電池用負極材料組成物及びリチウム二次電池 Download PDFInfo
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- JP5279047B2 JP5279047B2 JP2010548597A JP2010548597A JP5279047B2 JP 5279047 B2 JP5279047 B2 JP 5279047B2 JP 2010548597 A JP2010548597 A JP 2010548597A JP 2010548597 A JP2010548597 A JP 2010548597A JP 5279047 B2 JP5279047 B2 JP 5279047B2
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- negative electrode
- lithium secondary
- secondary battery
- electrode material
- acrylic acid
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- 229910052744 lithium Inorganic materials 0.000 title claims description 71
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 64
- 239000007773 negative electrode material Substances 0.000 title claims description 64
- 239000000203 mixture Substances 0.000 title claims description 53
- 239000011230 binding agent Substances 0.000 claims description 52
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 34
- 229920002126 Acrylic acid copolymer Polymers 0.000 claims description 29
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 22
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 22
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- 239000004020 conductor Substances 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 239000011149 active material Substances 0.000 claims description 14
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- 238000012360 testing method Methods 0.000 description 6
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- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 5
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
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- 230000007423 decrease Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 4
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- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 229910003002 lithium salt Inorganic materials 0.000 description 4
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- 239000011871 silicon-based negative electrode active material Substances 0.000 description 3
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- 238000002791 soaking Methods 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
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- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
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- 229910004283 SiO 4 Inorganic materials 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
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- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 description 2
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- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 2
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 2
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- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
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- VROAXDSNYPAOBJ-UHFFFAOYSA-N lithium;oxido(oxo)nickel Chemical compound [Li+].[O-][Ni]=O VROAXDSNYPAOBJ-UHFFFAOYSA-N 0.000 description 1
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- LRMHVVPPGGOAJQ-UHFFFAOYSA-N methyl nitrate Chemical compound CO[N+]([O-])=O LRMHVVPPGGOAJQ-UHFFFAOYSA-N 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 125000002560 nitrile group Chemical group 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 229910021470 non-graphitizable carbon Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920005596 polymer binder Polymers 0.000 description 1
- 239000002491 polymer binding agent Substances 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 229920005608 sulfonated EPDM Polymers 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000011366 tin-based material Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Description
前記溶液に炭素および黒鉛材料と、リチウムと合金が可能な金属およびこのような金属を含む化合物と、金属およびその化合物と炭素および黒鉛材料の複化合物と、リチウム含有窒化物とからなる群より選択される一つの負極活物質および導電材を混合してリチウム二次電池用負極材料組成物を作製するステップと、
前記組成物を集電体に塗布するステップと、
前記組成物および集電体を200℃以下で乾燥するステップとを含むリチウム二次電池用負極の製造方法を提供する。
以下、本発明を実施例に基づいて詳細に説明するが、本発明はこれらの実施例に限定されるものではない。
分子量が1,120,000であり、アクリロニトリル/アクリル酸のモル比が9.4/0.6のポリアクリロニトリル-アクリル酸共重合体2.5gにNMPを47.5gを加え撹はんしながら10分に亘って80℃まで昇温した。この温度で2時間維持しながら完全に溶解させた後、室温まで冷却して5重量%のバインダー溶液を得た。これを銅箔上に1mm厚さでコーティングした後、130℃で2時間乾燥してバインダーフィルムを得た。
分子量が1,030,000であり、アクリロニトリル/アクリル酸のモル比が8.3/1.7のポリアクリロニトリル-アクリル酸共重合体2.5gを使用したことを除いては実施例1と同様の方法でバインダーフィルムを製造した。
分子量が1,050,000であり、アクリロニトリル/アクリル酸のモル比が7.3/2.7のポリアクリロニトリル-アクリル酸共重合体2.5gを使用したことを除いては実施例1と同様の方法でバインダーフィルムを製造した。
分子量が2,100,000であり、アクリロニトリル/アクリル酸のモル比が10/0のポリアクリロニトリル-アクリル酸共重合体、即ち、ポリアクリロニトリル高分子2.5gを使用したことを除いては実施例1と同様の方法でバインダーフィルムを製造した。
分子量が500,000以上であり、アクリロニトリル/アクリル酸のモル比が2.8/7.2のポリアクリロニトリル-アクリル酸共重合体2.5gを使用したことを除いては実施例1と同様の方法でバインダーフィルムを製造した。
分子量が500,000以上であり、アクリロニトリル/アクリル酸のモル比が1.3/8.7のポリアクリロニトリル-アクリル酸共重合体2.5gを使用したことを除いては実施例1と同様の方法でバインダーフィルムを製造した。
実施例1に記載された方法で製造されたポリアクリロニトリル-アクリル酸共重合体溶液10g、シリコン系活物質9.4g、そしてカーボンブラック導電材0.1gを混合して電極材料組成物を製造した。ここで全体固形分の含有量が30重量%となるようにNMPを後添加した。前記組成物をドクターブレードを用いて銅ホイルに150μm厚さでコーティングした後、130℃のドライオーブンに入れて30分間乾燥した後、適当な厚さに圧延して負極を製造した。
実施例2に記載された方法で製造されたポリアクリロニトリル-アクリル酸共重合体溶液10gを使用したことを除いては実施例4と同様の方法で電極を製造した。
実施例3に記載された方法で製造されたポリアクリロニトリル-アクリル酸共重合体溶液10gを使用したことを除いては実施例4と同様の方法で電極を製造した。
比較例1に記載された方法で製造されたポリアクリロニトリル-アクリル酸共重合体溶液10gを使用したことを除いては実施例4と同様の方法で電極を製造した。
比較例2に記載された方法で製造されたポリアクリロニトリル-アクリル酸共重合体溶液10gを使用したことを除いては実施例4と同様の方法で電極を製造した。
比較例3に記載された方法で製造されたポリアクリロニトリル-アクリル酸共重合体溶液10gを使用したことを除いては実施例4と同様の方法で電極を製造した。
前記実施例4で製造された負極極板を表面積1.49cm2の円状に開けてこれを作用極とし、表面積1.77cm2の円状に開けたリチウムコバルト酸化物を対極としてコイン(coin)型フルセル(full-cell)を作製した。作用極と対極間にポリオレフィン微細多孔膜で作られた分離膜を介し、その後、EC(ethylene carbonate):DEC(diethyl carbonate):EMC(ethyl methyl carbonate)=4:3:3(体積比)の混合溶媒を使用し、LiPF6の電解質を1Mの濃度で溶解させた電解液を投入してリチウム二次電池を完成した。
実施例5で完成された負極を使用したことを除いては、実施例7と同様の方法でリチウム二次電池を完成した。
実施例6で完成された負極を使用したことを除いては、実施例7と同様の方法でリチウム二次電池を完成した。
比較例4で完成された負極を使用したことを除いては、実施例7と同様の方法でリチウム二次電池を完成した。
比較例5で完成された負極を使用したことを除いては、実施例7と同様の方法でリチウム二次電池を完成した。
比較例6で完成された負極を使用したことを除いては、実施例7と同様の方法でリチウム二次電池を完成した。
{耐電解液性テスト}
電解液に対する高分子フィルムの膨潤程度を測定するために、1モル濃度のLiPF6を含むEC(ethylene carbonate)、DEC(diethyl carbonate)、EMC(ethyl methyl carbonate)をそれぞれ4、3、3の割合で混合し、実施例1〜3、そして比較例1〜3で製造された高分子フィルムを直径1.8cmの円形状に切った後、前記混合溶液10mlに浸けて密封し、25℃の恒温槽に保管した。7日後にフィルムを電解液から引き出してフィルムの表面に残っている電解液を乾燥紙で拭い、初期重さと比較して重さの変化を測定した。電解液に対する膨潤率は下記式で計算した。評価は4個以上のフィルムに対し膨潤程度を測定した後平均値に定め、実験結果は下記表1に記載されている。通常、膨潤率が低いほど耐電解液性は高い。
膨潤率(%)=(電解液に浸けた後の質量−電解液に浸ける前の質量)/(電解液に浸ける前の質量)×100
{接着力テスト}
本発明の高分子をバインダーとして用いた際の負極材料組成物と集電体間の接着力を測定するために、製造された負極極板を一定の大きさに切ってスライドグラスに固定させた後、集電体を剥離して180°剥離強度を測定した結果、前記実施例4〜6の電極の接着力は、本出願人が先出願した特許に記載された高分子量のポリアクリロニトリルをバインダーとして用いた電極と類似の程度の高い接着力を示した(実験例1参照)。又、アクリロニトリルに比べて相対的にアクリル酸の含有量が多い共重合体をバインダーとして用いた電極(比較例5、比較例6)の接着力は、実施例4〜6の電極に比べ若干低下することを確認した。
{電池テスト}
前記実施例および比較例で製造されたコイン型タイプの電池の充放電実験を行った。先ず、充放電電流密度を0.1Cにし、充電終止電圧を4.2V(Li/Li+)、放電終止電圧を2.5V(Li/Li+)にした充放電試験を2回施した。続いて、充放電電流密度を0.5Cにし、充電終止電圧4.2V(Li/Li+)、放電終止電圧を2.5V(Li/Li+)にした充放電試験を38回施した。全ての充電は定電流/定電圧で行い、定電圧充電の終止電流は0.005Cにした。総40サイクルの試験を完了した後、第1サイクルの充放電効率(放電容量/充電容量、初期効率)を求めた。そして、40サイクルの充電容量を第1サイクルの充電容量で割った容量比(40th/1st)を求めて容量維持率と見なした。これらの結果を下記表2に示す。
Claims (6)
- 負極活物質、バインダーおよび導電材を含むリチウム二次電池用負極材料組成物において、前記バインダーは、アクリロニトリルに対しアクリル酸のモル比が0.204〜2のポリアクリロニトリル−アクリル酸共重合体であって、分子量が1,030,000〜5,000,000の範囲内のポリアクリロニトリル−アクリル酸共重合体であり、
前記ポリアクリロニトリル−アクリル酸共重合体は、アクリロニトリル(C 3 H 3 N)単量体とアクリル酸(C 3 H 4 O 2 )単量体の共重合体であり、
これを含む前記バインダーは、全負極材料組成物に対し1〜30重量%が含まれていることを特徴とするリチウム二次電池用負極材料組成物。 - 前記活物質は、炭素および黒鉛材料と、リチウムと合金が可能な金属およびこのような金属を含む化合物と、金属およびその化合物と炭素および黒鉛材料の複化合物と、リチウム含有窒化物とからなる群より選択される一つであることを特徴とする請求項1に記載のリチウム二次電池用負極材料組成物。
- 前記導電材は、黒鉛、カーボンブラック、導電性繊維、金属粉末、導電性ウイスキー、導電性金属酸化物、又は伝導性高分子であることを特徴とする請求項1または2に記載のリチウム二次電池用負極材料組成物。
- 前記導電材は、全負極材料に対し1〜50重量%含まれることを特徴とする請求項3に記載のリチウム二次電池用負極材料組成物。
- 前記リチウム二次電池用負極材料組成物は、充填剤をさらに含んでいることを特徴とする請求項1から4の何れか1項に記載のリチウム二次電池用負極材料組成物。
- 請求項1〜5のいずれか1項に記載のリチウム二次電池用負極材料組成物が含まれたリチウム二次電池。
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