JP6431249B1 - 電極用バインダー、電極用組成物及び電極 - Google Patents
電極用バインダー、電極用組成物及び電極 Download PDFInfo
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- JP6431249B1 JP6431249B1 JP2018535435A JP2018535435A JP6431249B1 JP 6431249 B1 JP6431249 B1 JP 6431249B1 JP 2018535435 A JP2018535435 A JP 2018535435A JP 2018535435 A JP2018535435 A JP 2018535435A JP 6431249 B1 JP6431249 B1 JP 6431249B1
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- electrode
- binder
- copolymer latex
- monomer
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- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- NJRXVEJTAYWCQJ-UHFFFAOYSA-N thiomalic acid Chemical compound OC(=O)CC(S)C(O)=O NJRXVEJTAYWCQJ-UHFFFAOYSA-N 0.000 description 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-L thiosulfate(2-) Chemical compound [O-]S([S-])(=O)=O DHCDFWKWKRSZHF-UHFFFAOYSA-L 0.000 description 1
- 229960002447 thiram Drugs 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- H—ELECTRICITY
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- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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Abstract
【選択図】なし
Description
また、本実施形態における電極用バインダーに含まれる共重合体ラテックスの電解液(エチレンカーボネート/ジエチルカーボネート=1/2(体積比))膨潤度は1.3〜10であることが好ましく、より好ましくは、1.5以上、さらに好ましくは2.0以上、より好ましくは9.5以下、さらに好ましくは9.0以下である。上記範囲となるように調整することにより、活物質を包み込んだバインダー中をイオンが透過しやすくなり、入出力特性に優れる電池を提供することができる。電解液膨潤度は、エチレン性不飽和カルボン酸単量体、不飽和カルボン酸アルキルエステル単量体及びシアン化ビニル単量体の種類や量を変更すること、分子量調整剤の種類や量を変更することにより共重合体のゲル含有量を調整すること、等により調整することができる。電解液膨潤度は、下記実施例の方法にて測定することができる。
正極活物質としては、特に限定されないが、リチウムイオン二次電池の場合、例えば、MnO2、MoO3、V2O5、V6O13、Fe2O3、Fe3O4等の遷移金属酸化物、LiCoO2、LiMnO2、LiNiO2、LMO2(ここでMはNi,Mn,Co,Alなどを2種あるいは3種以上含む)等の層状構造、LiMn2O4、LiM2O4(ここで、MはNi,Mn,Co,Alなどを2種あるいは3種以上含む)のスピネル構造、LiFePO4等のオリビン構造を有する複合金属酸化物、Li2MnO3等のリチウム過剰系複合酸化物、TiS2、TiS3、MoS3、FeS2等の遷移金属硫化物、CuF2、NiF2等の金属フッ化物などが挙げられる。これらは、1種を単独でまたは2種以上を組み合わせて使用することができる。
<共重合ラテックスの製造>
(実施例1)
耐圧性の重合反応機に、窒素雰囲気下で、t−ドデシルメルカプタン0.2部と、表1記載の各単量体、ドデシルベンゼンスルホン酸ナトリウム、純水を加えて70℃に昇温した後に、過硫酸カリウム1部を加えて重合を開始した。重合開始から8時間後に重合を停止し、水酸化ナトリウム水溶液でpHを調整した。その後に、水蒸気蒸留により未反応単量体および他の低沸点化合物を除去することで、共重合体ラテックスAを得た。
(実施例2〜13、比較例1〜10)
表1〜4に示す配合部数で各単量体、ドデシルベンゼンスルホン酸ナトリウム、純水を仕込んだ以外は、実施例1と同様にして、共重合体ラテックスB〜Wを得た。
<重合体ラテックスの光子相関法による平均粒子径の測定>
FPAR−1000(大塚電子製)を使用し、JIS Z8826に準拠した方法で測定した。結果を表1〜4に示す。
<重合体ラテックスのガラス転移温度の測定>
共重合体ラテックスをガラス板に0.5g程度塗り、70℃×4時間乾燥することでフィルムを作製した。乾燥後のフィルムをDSC試験用のアルミニウムパンにセットし、再度加熱によりサンプルを均一化し、その後、測定温度を−100〜150℃まで速度10℃/分で昇温して、相変化の吸熱の開始点を読み取って共重合体ラテックスのガラス転移温度とした。結果を表1〜4に示す。
<重合体ラテックスの電解液膨潤度の測定>
共重合体ラテックスを80℃×24時間減圧乾燥することでフィルムを作製し、5mm角に裁断した。裁断したフィルム片を電解液(エチレンカーボネート/ジエチルカーボネート=1/2(体積比))に60℃、72時間浸漬し、その後フィルム片を取り出し、電解液に膨潤した状態のフィルム片重量を測定した(この時の重量を「膨潤フィルム重量」と呼ぶ)。その後、フィルム片を100℃×72時間減圧乾燥し、乾燥後のフィルム片重量を測定した(この時の重量を「乾燥フィルム重量」と呼ぶ)。下記式より膨潤度を算出した。結果を表1〜4に示す。
膨潤度 = 膨潤フィルム重量 / 乾燥フィルム重量
<負極用組成物の調整>
負極活物質として天然黒鉛100質量部、増粘剤としてカルボキシメチルセルロース水溶液を固形分換算で1質量部をプラネタリーミキサー(プライミクス社製 2P−1型)へ投入し、40rpmで20分間撹拌した。次いで、全固形分が50%となるように適量の純水を加え、40rpmで20分間撹拌した。その後、電極用バインダーとして各実施例および各比較例の共重合体ラテックスを固形分換算で1質量部、全固形分が45質量%となるように適量の純水を加えて40rpmで10分間撹拌し、負極用組成物を調製した。
<負極の作製>
上記のようにして得られた負極用組成物を集電体となる厚さ20μmの銅箔に塗布し、80℃で10分間乾燥後、室温でロールプレスして、塗工層の厚みが70μmの負極を得た。電極用バインダーの活物質への被覆性を評価する際には、ロールプレスによる圧延を行う前の状態のものを用いた。
<負極の電極用バインダーの活物質への被覆性の評価>
電極用バインダーが活物質の表面をより多く被覆することにより、充放電を繰り返した際のサイクル特性が向上することから、上記の方法で得られた各負極シートにおいて、下記の方法により電極用バインダーの活物質への被覆性を評価した。すなわち、上記で得られた各負極シート(圧延前のもの)を1cm四方に切り、四酸化オスミウム雰囲気下で染色した後、走査型電子顕微鏡(日本電子製、商品名:JSM−6510LA)を用いて、5000倍にて観察した。SEM観察画像において、活物質の面積に対し、活物質上に電極用バインダーが付着している面積を目視で確認し、下記のとおり評価した。なお、SEM観察画像8画面のうち、最も平均的な画像を選び、評価した。結果を表1〜4に示す。
A:活物質表面の80%以上を電極用バインダーが被覆している。
B:活物質表面の60%以上80%未満を電極用バインダーが被覆している。
C:活物質表面の40%以上60%未満を電極用バインダーが被覆している。
D:活物質表面の40%未満しか電極用バインダーが被覆していない。
<正極用組成物の調整>
予め、正極活物質としてLiCoO2を100質量部、導電剤としてアセチレンブラックを5質量部をドライブレンドし、プラネタリーミキサー(プライミクス社製 2P−1型)へ投入した。次いで、ポリフッ化ビニリデン(PVdF)のN−メチル−2−ピロリドン(NMP)溶液をPVdF固形分換算で5質量部投入し、50rpmで30分撹拌した。その後、さらにPVdFのNMP溶液をPVdF固形分換算で5質量部投入し、50rpmで30分撹拌した。全固形分が65質量%となるように適量のNMP溶媒を加えてさらに50rpmで30分間撹拌し、正極用組成物を調製した。
<正極の作製>
上記のようにして得られた正極用組成物を集電体となる厚さ20μmのアルミニウム箔に塗布し、130℃で20分間乾燥後、室温でロールプレスして、塗工層の厚みが70μmの正極を得た。
<ラミネートセル作製>
得られた正極を電極部の長辺が103mm、短辺が60mm、タブ溶接部が15mm四方となるよう押切り、タブ溶接部にアルミ製タブを溶接した。得られた負極は電極部の長辺が107mm、短辺が62mm、タブ溶接部が15mm四方となるように押切り、タブ溶接部にニッケル製タブを溶接した。また、ポリプロピレン製セパレータを長辺117mm、短辺66mmの長方形に裁断し、成形した正負極間に設置した。この電極組みをアルミラミネートシートで包埋し、電解液を注入した後密封することで、ラミネートセルを作製した。この際、電解液は1M LiPF6 を含む エチレンカーボネート(EC):ジエチルカーボネート(DEC)=1:1(体積比)を用いた。
<入出力特性の評価>
得られたラミネートセルをCCCV条件 定電流レート0.1C、4.2V到達後電流レート0.01Cとなるまで充電し、休止時間10分を設けた後、CC条件、定電流レート0.1Cで3V到達時まで放電した。この操作を3回繰り返した。4回目の充電はCCCV条件 定電流レート0.2C、4.2V到達後電流レート0.02Cとなるまで充電し、休止時間10分を設けた後、CC条件、定電流レート1Cで3V到達時まで放電した。5回目の充電、休止時間は4回目と同条件で行い、放電時に定電流レートを3Cとすることで放電容量を測定した。入出力特性の評価は1Cでの放電容量に対する3Cの放電容量の割合で評価し、容量維持率が70%を超える場合はA、70%未満の場合はBと評価した。結果を表1〜4に示す。
<型保持性の評価>
入出力特性試験後のラミネートセルをCCCV条件、定電流レート0.2C、4.2V到達後電流レート0.02Cとなるまで充電し、休止時間10分を設けた後、CC条件、定電流レート1Cで3V到達時まで放電する操作を100サイクル繰り返した。100サイクル後、ラミネートセルを解体し、取り出した負極合剤層表面を指でこすり、合剤層の状態を目視で下記の通り評価した。結果を表1〜4に示す。
A:合剤層の剥がれが見られない。
B:合剤層の内部から剥がれた。
C:合剤層が銅箔表面から剥がれた。
Claims (4)
- 共重合体ラテックスを含む電極用バインダーであって、
前記共重合体ラテックスがエチレン性不飽和カルボン酸単量体に由来する構造単位を2〜25質量%、及び前記エチレン性不飽和カルボン酸単量体と共重合可能な単量体に由来する構造単位を75〜98質量%含有し、
前記共重合体ラテックスのガラス転移温度が25℃以下であり、
前記共重合体ラテックスの光子相関法による平均粒子径が140nm以下であり、
前記共重合体ラテックスのpHが7〜10であり、
前記共重合体ラテックスの電解液(エチレンカーボネート/ジエチルカーボネート=1/2(体積比))膨潤度が1.3〜10である、電極用バインダー。 - 前記共重合体ラテックスは、前記エチレン性不飽和カルボン酸単量体と共重合可能な単量体に由来する構造単位であり、かつ、単独重合体のガラス転移温度が80℃以上の単量体に由来する構造単位を、25質量%以上含有する、請求項1に記載の電極用バインダー。
- 請求項1または2に記載の電極用バインダーと、活物質と、を含有する、電極用組成物。
- 集電体と、
前記集電体上に設けられ、請求項3に記載の電極用組成物から形成される電極合剤層と、
を備える、電極。
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KR20210111337A (ko) | 2021-09-10 |
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KR102413750B1 (ko) | 2022-06-27 |
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