JP6581096B2 - 黒鉛/ケイ素/炭素繊維複合材料を含有する電気エネルギー蓄電池用の電極 - Google Patents
黒鉛/ケイ素/炭素繊維複合材料を含有する電気エネルギー蓄電池用の電極 Download PDFInfo
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Description
i)炭素繊維及びケイ素粒子を溶媒の存在下で機械的に粉砕し、
ii)工程i)で得られた混合物を溶媒が完全に消失するまで乾燥し、
iii)工程ii)で得られた乾燥した粉砕生成物を黒鉛状炭素の粒子に加え、
iv)少なくとも1種類の結合剤及び任意選択的に水の存在下で、全体を混合し、
v)工程iv)で得られた混合物を電流コレクタの上に塗布し、
vi)乾燥する、
各工程を含む、本発明に従った電極の調製方法に関する。
i)炭素繊維及びケイ素粒子を溶媒の存在下で機械的に粉砕し、
ii)工程i)で得られた混合物を溶媒が完全に消失するまで乾燥し、
iii)工程ii)で得られた乾燥した粉砕生成物を黒鉛状炭素の粒子に加え、
iv)少なくとも1種類の結合剤及び任意選択的に水の存在下で、全体を混合し、
v)工程iv)で得られた混合物を電流コレクタの上に塗布し、
vi)乾燥する、
各工程を含む、本発明に従った電極の調製方法に関する。
実施例1:脱挿入における比容量
複合材料の調製
本発明に従った複合材料A及び同一の組成を有する比較複合材料Bを、以下の手順に従って、下記表1に与えられる割合で調製する。
粉砕(工程i)
機械的粉砕は、炭素繊維とケイ素の混合物7gを含む、瑪瑙ボールを備えた、レッチェ社製の遊星型粉砕ミル(planetary grinding mill)を使用して行われる。瑪瑙ボールの量は150gである。よって構成される混合物は、シクロヘキサンまたはヘキサン型の長鎖アルカン中で、500回/分で1.5時間、粉砕される;炭素繊維は、2〜20μmの寸法及び150nm以下の直径を有していてよく、ケイ素粒子は、4μm以下の寸法を有しうる。
粉砕後、炭素繊維及びケイ素からなる混合物は、抽出器を備えた換気ストーブ内で、55℃で24〜48時間乾燥される。
次に、粉砕生成物は、精密天秤で重量測定され、次いで、10gの水を含む二重ジャケットのビーカー中で、ディスパーマット社製の直径30mmのプロペラ式分散ミキサを使用して、6000回/分で15分間、分散される。
粉砕工程は使用されない。
本発明に従った電極A(複合材料A)及び同一の組成を有する比較電極B(複合材料B)は、以下の手順及び表2に示す成分及び含量を用いて調製される。
結合剤1(CMC)が複合材料に添加される。
電極は、10μmの厚さを有する銅電流コレクタ上に前もって調製されたインクの約90〜120μm厚のフィルムを塗布することによって調製される。次に、電極は、50〜60ミクロンの厚さになるまで乾燥される。
「ボタン電池」型のリチウム電池は、 リチウム負極、上記のように調製された正極、及びセルガード(Celgard)型のポリマーセパレータの積層によって作製され、上記のように調製された電極の表面は金属リチウム負極とは反対側にある。
本発明に従った電池A(電極Aに対応)及び比較電池B(電極Bに対応)は、以下の手順に従い、20℃の温度で試験された。
− Li+/Liカップルに対し、0.01Vの電位に達するまで、定電流モード(一定の電流強度)において0.1Cのレジームで充電し、続いて、挿入電流が0.001C以下になるまで、0.01Vの電圧での定電圧モード(電流の一定電位)において単相とし、次に、
− Li+/Liカップルに対し、1.2Vの電位に達するまで、定電流モードにおいて0.1Cのレジームで放電し、
− 脱挿入における比容量(Liイオン電池の放電中に負極に含まれる容量に対応する)が測定され、次に該手順が再び開始される。
2つの比較電極C及びD並びに本発明に従った電極Eは、下記表3に示す各電極の特徴を伴って調製される。
対応する複合材料(C、D及びE)は、以下の手順及び下記表4に与えられる割合で調製される。
ケイ素は、単に黒鉛状炭素と混合される。
複合材料Dの調製は、上述の複合材料Bの調製と同一である。
複合材料Eの調製は、上述の複合材料Aの調製と同一である。
3つの電極C、D及びEは、電極A及びBですでに述べた手順に従い、下記表5に示される成分及び含量を用いて調製される。
リチウムイオン電池は、上記のように調製された負極(C、D又はE)、LiNi1/3Mn1/3Co1/3O2をベースとし、10.2cm2の表面積を有する正極、及びセルガード型のポリマーセパレータを積層することにより調製され、負極の表面は正極の反対側にある。
本発明に従った電池E(電極Eに対応)及び比較電池C及びD(電極C及びDに対応)は、以下の手順に従い、20℃の温度で試験された:
− 4.15Vの電位に達するまで定電流モードにおける0.1Cのレジームで充電し、その後、定電流モードにおいて2.8Vまで放電することによる電池の形成。
Claims (16)
- 黒鉛状炭素をベースとした複合電極材料であって、炭素繊維とケイ素との密接な混合物の、黒鉛状炭素内に分散された粉砕生成物を含み、
黒鉛状炭素が、複合材料の全重量に対して、89〜99重量%を占めることと、
ケイ素が、複合材料の全重量に対して、0.1〜8重量%を占めることと、
を特徴とする複合電極材料。 - 黒鉛状炭素が、複合材料の全重量に対して、89〜97重量%を占めることを特徴とする請求項1に記載の材料。
- 黒鉛状炭素が、1〜100μmの平均サイズを有する粒子の形態をしていることを特徴とする請求項1又は2に記載の材料。
- ケイ素が、複合材料の全重量に対して、1〜8重量%を占めることを特徴とする請求項1から3のいずれか一項に記載の材料。
- ケイ素が、4μm以下の平均サイズを有する粒子の形態をしていることを特徴とする請求項1から4のいずれか一項に記載の材料。
- 炭素繊維が気相(VGCF)中で成長した炭素繊維であることを特徴とする請求項1から5のいずれか一項に記載の材料。
- 炭素繊維が、複合材料の全重量に対して、0.1〜3重量%を占めることを特徴とする請求項1から6のいずれか一項に記載の材料。
- 炭素繊維が、1〜40μmの平均長を有することを特徴とする請求項1から7のいずれか一項に記載の材料。
- ケイ素の量の炭素繊維の量に対する重量比が、1〜10であることを特徴とする請求項1から8のいずれか一項に記載の材料。
- 請求項1〜9のいずれか一項に記載の材料、及び1種類以上の結合剤を含有する、電気エネルギー蓄電池用の電極。
- 前記1種類以上の結合剤が、ポリブタジエン−スチレン、ポリブタジエン−ニトリル及び有機ポリマーのラテックスから選択されることを特徴とする請求項10に記載の電極。
- 1種類以上の結合剤が、電極の全重量に対して0.1〜10重量%を占めることを特徴とする請求項11記載の電極。
- 請求項10から12のいずれか一項に記載の電極である負極と、正極と、を備えた電気エネルギーを貯蔵するためのリチウムイオン電池。
- 請求項13に記載の電池を1つ以上備えた電気エネルギー蓄電池。
- 請求項10から12のいずれか一項に記載の電極を調製する方法であって、以下:
i)溶媒の存在下で炭素繊維及びケイ素粒子を機械的に粉砕し、
ii)工程i)で得られた混合物を溶媒が完全に消失するまで乾燥し、
iii)工程ii)で得られた乾燥粉砕生成物を黒鉛状炭素の粒子に加え、
iv)少なくとも1種類の結合剤及び任意選択的に水の存在下で、全体を混合し、
v)工程iv)で得られた混合物を電流コレクタの上に塗布し、
vi)乾燥する、
各工程を含む方法。 - 工程i)の粉砕が、瑪瑙ボールを備えた遊星型粉砕ミルを使用して行われることを特徴とする請求項15に記載の方法。
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PCT/FR2014/052456 WO2015044618A1 (fr) | 2013-09-30 | 2014-09-30 | Electrode pour batterie de stockage d'energie electrique comprenant un materiau composite graphite/silicium/fibres de carbone |
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CN110943203B (zh) | 2019-12-12 | 2022-05-24 | 中创新航技术研究院(江苏)有限公司 | 硅-石墨复合物、其制备方法及包含该硅-石墨复合物的锂电池负极、锂电池 |
US20240128440A1 (en) | 2021-02-25 | 2024-04-18 | Panasonic Intellectual Property Management Co., Ltd. | Negative electrode for lithium ion secondary battery, lithium ion secondary battery, method for manufacturing cnt-si paste, method for manufacturing negative electrode for lithium ion secondary battery, and method for manufacturing lithium ion secondary battery |
KR20220159587A (ko) * | 2021-05-26 | 2022-12-05 | 주식회사 엘지에너지솔루션 | 리튬 이차전지용 음극 및 이를 포함하는 리튬 이차전지 |
CN114335553B (zh) * | 2022-03-15 | 2022-05-27 | 湖南金阳烯碳新材料有限公司 | 一种硅碳-石墨负极材料及其制备方法与应用 |
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