JP4984384B2 - 電極の製造方法 - Google Patents
電極の製造方法 Download PDFInfo
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- JP4984384B2 JP4984384B2 JP2004294067A JP2004294067A JP4984384B2 JP 4984384 B2 JP4984384 B2 JP 4984384B2 JP 2004294067 A JP2004294067 A JP 2004294067A JP 2004294067 A JP2004294067 A JP 2004294067A JP 4984384 B2 JP4984384 B2 JP 4984384B2
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- Prior art keywords
- active material
- electrode
- material layer
- battery
- iron
- Prior art date
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- 229910052742 iron Inorganic materials 0.000 claims description 34
- 239000002002 slurry Substances 0.000 claims description 30
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- 229910052783 alkali metal Inorganic materials 0.000 claims description 10
- 150000001340 alkali metals Chemical class 0.000 claims description 10
- 239000011255 nonaqueous electrolyte Substances 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 5
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- 239000000178 monomer Substances 0.000 description 15
- 239000002245 particle Substances 0.000 description 14
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- 238000000034 method Methods 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Description
該電極は前記活物質層のスティフネス値が60mN以下であることが好ましい。また、上記鉄含有活物質は、炭素材料と複合化されたものであることが好ましい。
ここで炭素材料とは、炭素の同素体を表し、具体的には、アセチレンブラック、ケッチェンブラック、グラファイトなどの導電性を有するものが好ましい。炭素材料の形状は、格別な限定はないが、通常は粒子状のものが用いられる。炭素材料の平均粒子径は、特に限定されるものではないが、鉄含有活物質の粒子に複合化するという観点から、通常1〜1000nm、好ましくは5〜100nmの範囲のものが用いられる。炭素材料の平均粒子径が過度に小さい場合は、鉄含有活物質との複合化が困難になる場合があり、また、過度に大きい場合は導電性向上の効果が小さい場合がある。
スラリーの塗布方法としては、常法に従えばよく、例えば、ドクターブレード法、ディップ法、リバースロール法、ダイレクトロール法、グラビア法、エクストルージョン法、ハケ塗り等の方法を挙げることができる。スラリーの塗布量としては、使用目的に応じて適宜選択されるが、乾燥後の活物質層の厚さが通常0.001〜10mm、好ましくは0.005〜5mm、好ましくは0.01〜1mmとなるように調整される。
電池としては、例えば、本発明の電極を正極として用い、従来公知の負極、電解液、セパレーター等の部品と組み合せることで得ることができる。具体的な製造方法としては、例えば、負極と正極とをセパレーターを介して重ね合わせ、これを電池形状に応じて巻く、折るなどして電池容器に入れ、電池容器に電解液を注入して封口する。また必要に応じてエキスパンドメタルや、ヒューズ、PTC素子などの過電流防止素子、リード板などを入れ、電池内部の圧力上昇、過充放電の防止をする事もできる。電池の形状は、コイン型、ボタン型、シート型、円筒型、角形、扁平型など何れであってもよい。
直径5cmのアルミ皿にスラリー約1gを精秤し、120℃のオーブンで1時間乾燥する。乾燥前後の重量から次式によりスラリーの固形分濃度を求める。
(乾燥後のスラリー皿の重量−空のアルミ皿)÷(乾燥前のスラリー皿の重量−空のアルミ皿)×100=電極スラリーの固形分濃度(%)
(2)平滑性
ロールプレス前の電極について、JIS B0601に準じて、活物質層の表面の20μm四方の算術平均粗さ(Ra)を原子間力顕微鏡で観察して測定した。
(3)ピール強度
電極を幅2.5cm×長さ10cmの矩形に切って試験片とし、活物質層面を上にして固定する。試験片の活物質層表面にセロハンテープを貼り付けた後、試験片の一端からセロハンテープを50mm/分の速度で180°方向に引き剥がしたときの応力を測定した。測定を10回行い、その平均値を求めてこれを活物質層と集電体層とのピール強度とした。ピール強度が大きいほど活物質層と集電体層との密着性が大きいことを示す。
電極を幅1cm×長さ8cmの矩形に切って試験片とする。試験片の集電体側の面を外側にしてループ状にし、平行に配置した金属板で挟む。次いで、ループ ステフネステスタ(東洋精機製作所社製)を用い、0.35mm/秒の速度で電極ループを圧縮し、ループを10mmまで圧縮した時の応力としてつぶれ抵抗値を求める。集電体のみで作成したループについて同様の測定を行いつぶれ抵抗値を求め、電極ループのつぶれ抵抗値から集電体のつぶれ抵抗値を差し引いた値をスティフネス値とした。スティフネス値が小さいほど、電極は柔軟性に優れる。
(5)電池容量および充放電サイクル特性
実施例および比較例で得られたコイン型電池を用いて、2.5Vから4.0Vまで、23℃で0.1Cの定電流法によって充放電を繰り返した。10サイクル目および100サイクル目の放電容量を測定し、10サイクル目の放電容量を電池容量とした。単位はmAh/g(活物質当たり)である。また、100サイクル目の放電容量に対する10サイクル目の放電容量の割合を百分率で算出して充放電サイクル特性とした。この値が大きいほど繰り返し充放電による容量減が少ないことを示す。
攪拌機およびコンデンサーを装着した反応器に、窒素雰囲気下、674.9部の脱イオン水と28%ラウリル硫酸ソーダ水溶液を7.1部、トリポリリン酸ナトリウム0.8部を供給した。次に、反応器の内容物を攪拌しながら75℃に加温した。次に開始剤水溶液として2.44%過硫酸アンモニウム水溶液82部を反応器に添加し、続いてアクリル酸2−エチルヘキシル296部、アクリル酸ブチル80部、アクリロニトリル20部およびエチレングリコールジメタクリレート4部からなる単量体組成物を2時間かけて一定の速度で反応器に添加した。添加終了後、反応温度を80℃として3時間反応を継続して共重合体ラテックスを得た。重合転化率は99%であり、重合体の組成比は、単量体組成物の組成比と一致した。このラテックスにアンモニア水を加えてpHを7にした後に減圧濃縮して残留単量体を除去し、固形分濃度を40%とした。
次に、正極活物質として、特開2003−36889号公報記載の方法に基づき、1.6%の炭素を含有し、50%体積累積径が2.9μmであるオリビン構造のLiFePO4を製造した。
混合機として用いるビーズミル中に、製造例1で得た正極活物質100部、導電材としてアセチレンブラック10部、バインダーとして上記で得たラテックス7.5部(固形分量:3部)、および増粘剤としてカルボキシメチルセルロース(セロゲンWSC、第一工業製薬社製)の2%水溶液75部(固形分量:1.5部)を供給した。ここに水を加えて固形分濃度を70%とし、ビーズミルを用いて室温で、回転数750サイクル/分で1.5時間混合してスラリーを得た。得られたスラリーを厚さ20μmのアルミニウム箔にドクターブレード法によって均一に塗布し、120℃、15分間乾燥機で乾燥して活物質層の厚みが120μmの電極を得た。得られた電極の表面粗さ(Ra)を測定した結果を表1に示す。この電極を2軸のロールプレスで圧縮し、さらに真空乾燥機にて0.6kPa、250℃で10時間減圧乾燥して活物質層の厚みを100μmとした。得られたプレス後の電極のピール強度及びスティフネス値を測定した結果を表1に示す。
混合機および混合条件を表1に示す条件とした他は、実施例1と同様にして電極および電池を得た。ただし、混合機としてプラネタリーミキサーを用いる場合は、回転数は自転100rpm、公転50rpmとした。得られた電極および電池の各特性を測定した結果を表1に示す。
混合機として用いるプラネタリーミキサー中に、製造例1で得た正極活物質100部、導電材としてアセチレンブラック10部、バインダーとしてスチレンプタジエンラテックス(固形分量:2部)、および増粘剤としてポリアクリル酸アンモニウム塩(固形分量:1部)を供給し、回転数は自転100rpm、公転50rpmで3時間混練した。次いで、得られた混練物をN−メチル−2−ピロリドンに分散させてスラリーにした。
得られたスラリーを用いた他は実施例1と同様にして電極および電池を得た。得られた電極および電池の各特性をを測定すると、活物質層の表面粗さは2.10μm、ピール強度は0.10N/cm、電極のステフィネスは62mN、電池の初期容量は65mAh/g、充放電サイクル特性は45%であった。
Claims (3)
- 一般式:AyFeXO4(一般式中、Aはアルカリ金属を表し、Xは第4族〜第7族、または第14〜第17族の元素から選ばれる少なくとも一種の元素を表す)で表されるアルカリ金属含有鉄複合酸化物からなる鉄含有活物質、バインダー及び溶媒を、予め固形分濃度40〜90重量%に調製し、次いで、メディアミル型分散機を用いて、混合してスラリーを作る工程、該スラリーを集電体上に塗布する工程、及び溶媒を除去することにより活物質層を集電体層上に形成する工程を含んでなる、活物質層のJIS B0601に準じて測定される表面粗さが1.60μm以下であり、かつ活物質層と集電体層とのピール強度が0.1N/cm以上である非水電解質二次電池用電極の製造方法。
- 前記活物質層のスティフネス値が60mN以下である請求項1記載の製造方法。
- 鉄含有活物質が、炭素材料と複合化されたものである請求項1記載の製造方法。
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JP2004294067A JP4984384B2 (ja) | 2004-10-06 | 2004-10-06 | 電極の製造方法 |
US11/664,880 US8802289B2 (en) | 2004-10-06 | 2005-10-05 | Composition for electrode comprising an iron compound with carbon and a (meth)acrylate-nitrile copolymer |
CN200580041895.2A CN101073170B (zh) | 2004-10-06 | 2005-10-05 | 电极组合物、电极和电池 |
KR1020077010198A KR101245064B1 (ko) | 2004-10-06 | 2005-10-05 | 전극 조성물, 전극 및 전지 |
CN2010105519187A CN102034966B (zh) | 2004-10-06 | 2005-10-05 | 电极组合物、电极和电池 |
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