JPWO2013099520A1 - 正極合剤、正極、およびそれを用いた非水電解質二次電池 - Google Patents
正極合剤、正極、およびそれを用いた非水電解質二次電池 Download PDFInfo
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- JPWO2013099520A1 JPWO2013099520A1 JP2013551551A JP2013551551A JPWO2013099520A1 JP WO2013099520 A1 JPWO2013099520 A1 JP WO2013099520A1 JP 2013551551 A JP2013551551 A JP 2013551551A JP 2013551551 A JP2013551551 A JP 2013551551A JP WO2013099520 A1 JPWO2013099520 A1 JP WO2013099520A1
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- surfactant
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Abstract
正極活物質と、水分散性高分子バインダー樹脂と、導電助剤と、界面活性剤と、を含有する正極合剤である。
Description
<正極合剤>
本発明の正極合剤は、正極活物質と、水分散性高分子バインダー樹脂と、導電助剤と、界面活性剤と、を含有する。正極合剤に界面活性剤を添加することで、正極活物質および水分散性高分子バインダー樹脂を水系の溶媒に短時間で均一に分散させることができる。また、正極活物質および水分散性高分子バインダー樹脂は凝集、沈降を起こしにくくなるため、集電体に対する塗工性も向上する。さらに、本発明の正極合剤を用いた正極は、集電体および正極活物質との密着性および可撓性に優れている。さらにまた、得られた正極を用いた非水電解質二次電池は、充電および放電の繰り返しや、発熱による高温環境下にあっても充電放電サイクルにおける放電容量の低下を抑制でき、長寿命の二次電池を得ることができる。以下、本発明の正極合剤の各成分、およびその製造方法について詳細に説明する。
本発明の正極合剤においては、正極活物質として、例えば、遷移金属酸化物、遷移金属硫化物、およびリチウム含有複合金属酸化物等を用いることができる。遷移金属としては、例えば、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Mo等を挙げることができ、遷移金属酸化物としては、例えば、MnO、MnO2、V2O5、V6O13、TiO2、Cu2V2O3、非晶質V2O−P2O5、MoO3、V2O5、V6O13等を好適に用いることができる。特に、サイクル安定性と容量の観点からMnO、V2O5、V6O13、TiO2が好適である。遷移金属硫化物としては、TiS2、TiS3、非晶質MoS2、FeS等を好適に用いることができる。また、リチウム含有複合金属酸化物の構造については、特に制限はないが、層状構造、スピネル構造、またはオリビン型構造等のものを好適に用いることができる。
本発明の正極合剤においては、水分散性高分子バインダー樹脂とは、後述する水系溶媒に分散することができる高分子バインダー樹脂である。水分散性高分子バインダー樹脂としては、ビニル系重合体、アクリル系重合体、ニトリル系重合体、ポリウレタン系重合体、ジエン系重合体等の非フッ素系重合体や、PVDFやPTFE等のフッ素系重合体を挙げることができる。特に、集電体や正極合剤との接着性の観点から非フッ素系重合体が好ましく、より好ましくは、アクリル樹脂、または、少なくともポリオールとポリイソシアネートとからなる重量平均分子量が8,000〜1,500,000、好適には、重量平均分子量が10,000〜1,000,000のポリウレタン樹脂である。
本発明の正極合剤においては、導電助剤としては、アセチレンブラック、ケッチェンブラック、カーボンブラック、グラファイト、気相成長カーボン繊維、およびカーボンナノチューブ、グラフェン、フラーレン等の導電性カーボンを用いることができる。導電助剤を用いることにより、正極活物質同士の電気的接触を向上させることができ、非水電解質二次電池に用いる場合に、放電レート特性を改善することができる。導電助剤の配合量は、正極活物質100質量部に対して、好ましくは0.1〜20質量部、より好ましくは0.1〜10質量部である。
本発明の正極合剤においては、界面活性剤としては、電解質への分散性が高く、リチウムイオン等との反応性が低く、かつ、電解質中のイオン伝導を妨げない限り、特に制限されるものではない。例えば、界面活性剤としては、カチオン性界面活性剤、アニオン性界面活性剤、両性界面活性剤、非イオン性界面活性剤を挙げることができるが、特に非イオン性界面活性剤を用いることが好ましい。非イオン性界面活性剤は、周囲のイオン(リチウムイオン等)との反応性が低く、電解質中および活物質表面のイオン伝導を妨げないためである。本発明の正極合剤においては、界面活性剤は1種単独で用いてもよく、2種以上を混合して用いてもよい。
HLB値=20×親水部の式量の総和/分子量
にて定義される。
本発明の正極合剤に用いる溶媒としては、水分散性高分子バインダー樹脂および正極活物質を均一に分散および沈降凝集を阻害する界面活性剤と親和するものであれば特に制限はなく、水であっても有機溶媒であってもよい。また、本発明の正極合剤においては、溶媒としては、特に水を好適に用いることができるが、上記効果を阻害しない範囲で、有機溶媒を含んでいてもよい。かかる有機溶媒としては、例えば、シクロペンタン、シクロヘキサン等の環状脂肪族炭化水素類;トルエン、キシレン、エチルベンゼン等の芳香族炭化水素類;アセトン、エチルメチルケトン、ジソプロピルケトン、シクロヘキサノン、メチルシクロヘキサン、エチルシクロヘキサン等のケトン類;メチレンクロライド、クロロホルム、四塩化炭素等の塩素系脂肪族炭化水素;酢酸エチル、酢酸ブチル、γ−ブチロラクトン、ε−カプロラクトン等のエステル類;アセトニトリル、プロピオニトリル等のアシロニトリル類;テトラヒドロフラン、エチレングリコールジエチルエーテル等のエーテル類:メタノール、エタノール、イソプロパノール、エチレングリコール、エチレングリコールモノメチルエーテル等のアルコール類;N−メチルピロリドン、N,N−ジメチルホルムアミド等のアミド類を挙げることができる。
本発明の正極合剤は、正極活物質と、水分散性高分子バインダー樹脂と、導電助剤と、界面活性剤と、を含有することのみが重要であり、それ以外に特に制限はなく、上記成分以外にも電池反応に影響を及ぼさない範囲で添加剤を含んでいてもよい。例えば、本発明の正極合剤には、上記成分の他に、補強材、増粘剤、消泡・レベリング剤、電解液分解抑制剤等の成分が含まれていてもよい。
本発明の正極合剤は、上記の正極活物質と、水分散性高分子バインダー樹脂と、導電助剤と、界面活性剤および溶媒、その他必要に応じてその他の添加剤を混合して得ることができる。本発明の正極合剤を製造するにあたって、混合方法については特に制限はなく、例えば、撹拌式、振とう式、および回転式等の混合装置を使用した方法を採用することができる。また、ホモジナイザー、ボールミル、サンドミル、ロールミル、および遊星式混練機等の分散混練装置を使用した方法を採用してもよい。
次に、本発明の非水電解質二次電池用正極について説明する。
本発明の正極は、上記本発明の正極合剤が集電体に塗布されてなるものである。本発明の正極は、上記本発明の正極合剤を集電体上に塗布する塗布工程と、得られた集電体を乾燥して正極合剤層を形成する乾燥工程と、を経て製造することができる。本発明の正極においては、正極合剤層を集電体の片面に形成してもよいが、両面に形成することが好ましい。以下、本発明の正極の構成および製造方法について詳細に説明する。
本発明の正極に用いる集電体は、電気導電性を有し、かつ電気化学的に耐久性のある材料であれば特に制限されないが、耐熱性を有する金属材料が好ましい。例えば、鉄、銅、アルミニウム、ニッケル、ステンレス鋼、チタン、タンタル、金、白金等を挙げることができる。特に、充電時の酸化劣化が少ないことからアルミニウムまたはアルミニウム合金が好ましい。集電体の形状は特に制限されないが、厚さ5〜100μm程度のシート状のものを好適に用いることができる。
上記本発明の正極合剤を集電体上に塗布する方法についても特に限定はなく、既知の方法を用いることができる。塗布方法としては、例えば、ダイコーティング法、ドクターコーティング法、ディップコーティング法、ロールコーティング法、スプレーコティング法、グラビアコーティング法、スクリーン印刷法、または静電塗装法等を挙げることができる。
上記塗布方法により得られた集電体を乾燥させる方法としては特に制限はないが、例えば、温風、熱風、低湿風による乾燥、真空乾燥、(遠)赤外線や電子線等の照射による乾燥法を挙げることができる。乾燥時間は通常5〜30分間であり、乾燥温度は通常40〜180℃である。
本発明の製造方法においては、塗布工程、乾燥工程を経た後、金型プレスやロールプレス等を用いて、加圧処理により正極合剤層の空隙率を下げる圧延工程を経ることが好ましい。空隙率の好適な範囲は5%〜15%であり、より好適には7%〜13%である。空隙率が15%を超えると充電効率や放電効率が悪化するため、好ましくない。一方、空隙率が5%未満の場合は、高い体積容量が得難かったり、正極合剤層が集電体から剥がれやすく不良を発生しやすいといった問題が生じるおそれがある。なお、バインダー樹脂として硬化性樹脂を用いる場合は、この硬化性樹脂を硬化させる工程を有していることが好ましい。
次に、本発明の非水電解質二次電池について説明する。
本発明の非水電解質二次電池は、上記本発明の正極を用いたものであり、正極、負極、セパレーターおよび電解液を有している。以下、本発明の非水電解質二次電池の構成およびその製造方法について詳細に説明する。
本発明に係る非水電解質二次電池用負極は、負極活物質、導電助剤、水分散性高分子バインダー樹脂、溶媒およびその他必要に応じて添加剤等を混合して負極合剤スラリーを調整し、集電体に塗布、乾燥、必要に応じて圧延を経ることによって製造することができる。
本発明に用いられる電解液については特に制限はないが、例えば、非水系の溶媒に支持電解質としてリチウム塩を溶解したものが使用できる。リチウム塩としては、例えば、LiPF6、LiAsF6、LiBF4、LiSbF6、LiAlCl4、LiClO4、CF3SO3Li、C4F9SO3Li、CF3COOLi、(CF3CO)2NLi、(CF3SO2)2NLi、(C2F5SO2)NLi等を挙げることができる。特に、溶媒に溶けやすく高い解離度を示すLiPF6、LiClO4、CF3SO3Liを好適に用いることができる。これらは1種単独で用いてもよく、2種以上を混合して用いてもよい。支持電解質の添加量は、電解液に対して、通常1質量%以上、好ましくは5質量%以上、また通常は30質量%以下、好ましくは20質量%以下である。支持電解質の量が少なすぎても多すぎてもイオン導電性は低下してしまい、電池の充電特性、放電特性が低下してしまう。
セパレーターは気孔部を有する多孔性基材であって、(a)気孔部を有する多孔性セパレーター、(b)片面または両面上に高分子コート層が形成された多孔性セパレーター、または(c)無機セラミック粉末を含む多孔質の樹脂コート層が形成された多孔性セパレーターを用いることができる、例えば、ポリプロピレン系、ポリエチレン系、ポリオレフィン系、アラミド系多孔性セパレーター、ポリビニリデンフルオリド、ポリエチレンオキシド、ポリアクリロニトリル、ポリビニリデンフルオリドヘキサフルオロプロピレン共重合体等の固体高分子電解質用、ゲル状高分子電解質用の高分子フィルム、ゲル化高分子コート層がコーティングされたセパレーター、または無機フィラー、無機フィラー用分散剤からなる多孔膜層がコーティングされたセパレーター等を挙げることができる。
本発明の非水電解質二次電池の製造方法については、特に制限はない。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、折る等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。本発明の非水電解質二次電池においては、必要に応じてエキスパンドメタルや、ヒューズ、PTC素子等の過電流防止素子、リード板等を入れ、電池内部の圧力上昇、過充放電の防止をすることもできる。電池の形状は、ラミネートセル型、コイン型、ボタン型、シート型、円筒型、角形、扁平型等いずれの形状であってもよい。
<実施例1>
正極活物質として、三元系活物質である日本化学工業社製セルシードNMC−111(LiNi1/3Co1/3Mn1/3O2)を固形分比率95質量%、導電助剤として昭和電工社製VGCF−H(気相成長炭素繊維)を固形分比率2質量%、水分散性高分子バインダー樹脂としてADEKA社製アデカボンタイターHUX−822(ポリウレタンエマルション樹脂:固形分40質量%)を固形分比率1.5質量%、界面活性剤として花王社製エマノーン3299RV(ポリエチレングリコールジステアレート)を固形分比率1.5質量%、および溶媒としての水を合剤固形分が60質量%となるように配合し、1700rpmで10分間プロペラ攪拌を行い、正極合剤を作製した。
水分散性高分子バインダー樹脂、界面活性剤、増粘剤、導電助剤、正極活物質を表1〜4に示すように配合組成を変えた以外は、実施例1と同様にして攪拌・混合を行い、正極合剤を作製し、分散性、沈降凝集の安定性を評価した。作製した正極合剤を用いて、実施例1と同様に塗布・乾燥・圧延を行い、正極板を作製した。評価結果を表1〜4に併記する。
作製した正極合剤をアルミニウム箔の正極集電体に塗工するに際して、分散不良で解れていない粗い活物質粒子の塊やゲル状の樹脂の塊で塗工面にスジ状の跡が付くものを「不良」、若干跡が付くものを「可」、スジ状の跡が付かないものを「良」として、目視評価を行った。
作製した正極合剤を静置し、正極合剤の底面に沈降凝集物が発生した場合や液面に水が分離してしまったものを「不良」、変化していないものを「良」として、評価を行った。
正極合剤を正極集電体に塗布・乾燥した後、塗膜表面に泡、はじき等の塗膜欠陥が発生したものを「不良」、異常のないものを「良」として、塗膜の目視評価を行った。
正極合剤を正極集電体に塗布・乾燥した後、塗膜表面をJIS K−5600に準じ、カット間隔2mmで格子パターン25マスのクロスカットを行い、交点の粉落ちが激しいものを「不良」、粉落ちが少ないものを「可」、粉落ちが全くないものを「良」として、評価を行った。
作製した電極板表面に突起や割れ等が発生しているものを「不良」、異常がなく平滑であるものを「良」として、電極表面の目視評価を行った。
作製した電極板を用い、JIS K−5600に準じ、カット間隔2mmで格子パターン25マスのクロスカット法試験により、集電体と活物質間の密着性を評価した。評価は0〜5の6段階により行い、数字が少ないものほど密着性が良好であることを示す。
作製した電極板表面にテスタ(日置社製 ミリオームハイテスタ3540)を用いて表面の抵抗値を測定した。
2)HSV−900(ポリフッ化ビニリデン樹脂) アルケマ(株)社製
3)モビニールLDM7523(アクリル/シリコーン樹脂) 日本合成化学(株)社製
4)エマノーン3299RV(ポリエチレングリコールジステアレート系非イオン界面活性剤 HLB:19.2 分子量:約11200) 花王(株)社製
5)エマノーン3199V(ポリエチレングリコールモノステアレート系非イオン界面活性剤 HLB:19.4 分子量:約6800) 花王(株)社製
6)エマノーン1112(ポリエチレングリコールモノラウレート系非イオン界面活性剤 HLB:13.7 分子量:約730) 花王(株)社製
7)アデカミン4MAC−30(カチオン性界面活性剤) (株)ADEKA社製
8)ダイセルCMC#2200 ダイセルファインケム(株)社製
9)VGCF−H(気相成長炭素繊維) 昭和電工(株)社製
10)SP−270(黒鉛粉末) 日本黒鉛工業(株)社製
11)セルシードNMC111(LiNi1/3Co1/3Mn1/3O2) 日本化学工業(株)社製
12)LFP(リン酸鉄リチウム:LiFePO4)
13)NMP(N−メチルピロリドン)
Claims (5)
- 正極活物質と、水分散性高分子バインダー樹脂と、導電助剤と、界面活性剤と、を含有することを特徴とする正極合剤。
- 前記界面活性剤のHLB値が13.0〜20.0である請求項1記載の正極合剤。
- 溶媒として水を含む請求項1または2記載の正極合剤。
- 請求項1〜3のうちいずれか1項記載の正極合剤が集電体に塗布されてなることを特徴とする正極。
- 請求項4に記載の正極を用いたことを特徴とする非水電解質二次電池。
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JP2016122550A (ja) * | 2014-12-24 | 2016-07-07 | トヨタ自動車株式会社 | リチウムイオン二次電池用正極板の製造方法、リチウムイオン二次電池用正極板、及び、リチウムイオン二次電池 |
JP6430472B2 (ja) | 2016-01-15 | 2018-11-28 | 関西ペイント株式会社 | リチウムイオン電池正極用導電ペースト及びリチウムイオン電池正極用合材ペースト |
JP2017183241A (ja) * | 2016-03-31 | 2017-10-05 | 積水化学工業株式会社 | 蓄電デバイス電極用バインダー |
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US10468674B2 (en) | 2018-01-09 | 2019-11-05 | South Dakota Board Of Regents | Layered high capacity electrodes |
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Free format text: JAPANESE INTERMEDIATE CODE: R250 |