JP7352900B2 - 非水電解質二次電池 - Google Patents
非水電解質二次電池 Download PDFInfo
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- JP7352900B2 JP7352900B2 JP2020502915A JP2020502915A JP7352900B2 JP 7352900 B2 JP7352900 B2 JP 7352900B2 JP 2020502915 A JP2020502915 A JP 2020502915A JP 2020502915 A JP2020502915 A JP 2020502915A JP 7352900 B2 JP7352900 B2 JP 7352900B2
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- negative electrode
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- lithium
- secondary battery
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- 150000003376 silicon Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000000279 solid-state nuclear magnetic resonance spectrum Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Description
負極は、例えば、負極集電体と、負極集電体の表面に形成され、かつ負極活物質を含む負極合剤層とを具備する。負極合剤層は、負極合剤を分散媒に分散させた負極スラリーを、負極集電体の表面に塗布し、乾燥させることにより形成できる。乾燥後の塗膜を、必要により圧延してもよい。負極合剤層は、負極集電体の一方の表面に形成してもよく、両方の表面に形成してもよい。
プローブ:Varian 7mm CPMAS-2
MAS:4.2kHz
MAS速度:4kHz
パルス:DD(45°パルス+シグナル取込時間1Hデカップル)
繰り返し時間:1200sec
観測幅:100kHz
観測中心:-100ppm付近
シグナル取込時間:0.05sec
積算回数:560
試料量:207.6mg
リチウムシリケート相LiySiOzの組成は、例えば、以下の方法により分析することができる。
正極は、例えば、正極集電体と、正極集電体の表面に形成された正極合剤層とを具備する。正極合剤層は、正極合剤を分散媒に分散させた正極スラリーを、正極集電体の表面に塗布し、乾燥させることにより形成できる。乾燥後の塗膜を、必要により圧延してもよい。正極合剤層は、正極集電体の一方の表面に形成してもよく、両方の表面に形成してもよい。
電解液は、非水溶媒と、非水溶媒に溶解したリチウム塩と、を含み、リチウム塩は、LFSIを含む。
通常、正極と負極との間には、セパレータを介在させることが望ましい。セパレータは、イオン透過度が高く、適度な機械的強度および絶縁性を備えている。セパレータとしては、微多孔薄膜、織布、不織布などを用いることができる。セパレータの材質としては、ポリプロピレン、ポリエチレンなどのポリオレフィンが好ましい。
[負極材料LSXの調製]
二酸化ケイ素と炭酸リチウムとを原子比:Si/Liが1.05となるように混合し、混合物を950℃空気中で10時間焼成することにより、式:Li2Si2O5(u=0.5)で表わされるリチウムシリケートを得た。得られたリチウムシリケートは平均粒径10μmになるように粉砕した。
導電層を有するLSX粒子と黒鉛とを混合し、負極活物質として用いた。導電層を有するLSX粒子と黒鉛との合計に占める黒鉛の割合を94質量%とした。負極活物質と、カルボキシメチルセルロースのナトリウム塩(CMC-Na)と、ポリアクリル酸(PAA)と、スチレン-ブタジエンゴム(SBR)と、を混合し、水を添加した後、混合機(プライミクス社製、T.K.ハイビスミックス)を用いて攪拌し、負極スラリーを調製した。
リチウムニッケル複合酸化物(LiNi0.8Co0.18Al0.02O2)と、アセチレンブラックと、ポリフッ化ビニリデンとを、95:2.5:2.5の質量比で混合し、N-メチル-2-ピロリドン(NMP)を添加した後、混合機(プライミクス社製、T.K.ハイビスミックス)を用いて攪拌し、正極スラリーを調製した。次に、アルミニウム箔の表面に正極スラリーを塗布し、塗膜を乾燥させた後、圧延して、アルミニウム箔の両面に、密度3.6g/cm3の正極合剤層が形成された正極を作製した。
非水溶媒にリチウム塩を溶解させて電解液を調製した。非水溶媒には、エチレンカーボネート(EC)と、ジメチルカーボネート(DMC)と、酢酸メチル(MA)とを、20:40:40の体積比で含む混合溶媒を用いた。リチウム塩には、LFSIおよびLiPF6を用いた。電解液中のLFSIの濃度と、電解液中のLiPF6の濃度とを、それぞれ、表1に示す値とした。
各電極にタブをそれぞれ取り付け、タブが最外周部に位置するように、セパレータを介して正極および負極を渦巻き状に巻回することにより電極群を作製した。電極群をアルミニウムラミネートフィルム製の外装体内に挿入し、105℃で2時間真空乾燥した後、非水電解液を注入し、外装体の開口部を封止して、電池A1を得た。
負極の作製において、導電層を有するLSX粒子と黒鉛との合計に占める黒鉛の割合を表1に示す値とし、負極活物質100質量部あたりのCMC-Naの添加量を表1に示す値とした。電解液の調製において、電解液中のLFSIの濃度と、電解液中のLiPF6の濃度とを、それぞれ、表1に示す値とした。上記以外、実施例1と同様にして電池A2~A9を作製した。
負極の作製において、導電層を有するLSX粒子と黒鉛との合計に占める黒鉛の割合を91質量%とし、CMC-Naを用いなかった。電解液の調製において、リチウム塩にLiPF6のみを用い、電解液中のLiPF6の濃度を1.2mol/Lとした。上記以外、実施例1と同様にして電池B1を作製した。
電解液の調製において、リチウム塩にLiPF6のみを用い、電解液中のLiPF6の濃度を1.2mol/Lとしたこと以外、実施例1と同様にして電池B2を作製した。
負極の作製においてCMC-Naを用いないこと以外、実施例1と同様にして電池B3を作製した。
負極の作製において、負極活物質に黒鉛のみを用い、CMC-Naの添加量を負極活物質100質量部あたり0.5質量部とした。電解液の調製において、リチウム塩にLiPF6のみを用い、電解液中のLiPF6の濃度を1.0mol/Lとした。上記以外、実施例1と同様にして電池B4を作製した。
0.3It(990mA)の電流で電圧が4.2Vになるまで定電流充電を行い、その後、4.2Vの定電圧で電流が0.015It(50mA)になるまで定電圧充電した。その後、0.3It(990mA)の電流で電圧が2.75Vになるまで定電流放電を行った。充電と放電との間の休止期間は10分とした。充放電は25℃の環境下で行った。このときの放電容量D1を、初期容量として求めた。
上記の評価1と同じ条件で充電および放電を行い、さらに、上記の評価1と同じ条件で充電を行った。充電完了後60分間休止し、0.3It(990mA)の電流で10秒間定電流放電を行った。放電開始前の電圧と放電開始から10秒経過後の電圧との差を0.3Itの電流値で除した値を、初期の内部抵抗(DC-IR)とした。
0.3It(990mA)の電流で電圧が4.2Vになるまで定電流充電を行い、その後、4.2Vの定電圧で電流が0.015It(50mA)になるまで定電圧充電した。その後、0.3It(990mA)の電流で電圧が2.75Vになるまで定電流放電を行った。充電と放電との間の休止期間は10分とした。充放電は25℃の環境下で行った。
5:封口板
6:電池ケース
9:電極群
11:正極リード
13:負極端子
14:負極リード
Claims (11)
- 正極と、負極と、電解液と、を備え、
前記負極は、電気化学的にリチウムを吸蔵および放出可能な負極活物質と、結着剤と、を含み、
前記負極活物質は、Si含有材料および炭素材料を含み、
前記Si含有材料と前記炭素材料との合計に占める前記炭素材料の割合は、70質量%以上98質量%以下であり、
前記Si含有材料は、リチウムシリケート相および前記リチウムシリケート相内に分散しているシリコン粒子を含有する複合材料を含み、
前記リチウムシリケート相の組成式は、Li2uSiO2+u(0<u≦2)であり、
前記結着剤は、カルボキシアルキルセルロースおよびその塩よりなる群から選択される少なくとも1種のセルロース化合物を含み、
前記電解液は、非水溶媒と、前記非水溶媒に溶解したリチウム塩と、を含み、
前記リチウム塩は、リチウムビス(フルオロスルホニル)イミド:LFSIを含む、非水電解質二次電池。 - 前記カルボキシアルキルセルロースは、カルボキシメチルセルロースである、請求項1に記載の非水電解質二次電池。
- 前記セルロース化合物は、前記カルボキシアルキルセルロースのナトリウム塩であって、前記カルボキシアルキルセルロースに含まれるカルボキシル基のうち、水素原子がナトリウム原子で置換される割合は、30%以上である、請求項1または2に記載の非水電解質二次電池。
- 前記負極中の前記セルロース化合物は、カルボキシアルキルセルロースのナトリウム塩であって、その含有量は、前記負極活物質100質量部あたり0.4質量部以上1.5質量部以下である、請求項1~3のいずれか1項に記載の非水電解質二次電池。
- 前記非水溶媒に溶解したリチウム塩は、さらに、LiPF6を含む、請求項1~4のいずれか1項に記載の非水電解質二次電池。
- 前記電解液中の前記LFSIおよび前記LiPF6の合計濃度が1mol/L以上2mol/L以下である、請求項5に記載の非水電解質二次電池。
- 前記LFSIと前記LiPF6との合計に占める前記LFSIの割合は、7mol%以上79mol%以下である、請求項5または6に記載の非水電解質二次電池。
- 前記LFSIと前記LiPF6との合計に占める前記LFSIの割合は、15mol%上50mol%以下である、請求項5または6に記載の非水電解質二次電池。
- 前記電解液中の前記LFSIの濃度が、0.1mol/L以上1.1mol/L以下であり、
前記電解液中の前記LiPF6の濃度が、0.3mol/L以上1.3mol/L以下である、請求項5~8のいずれか1項に記載の非水電解質二次電池。 - 前記非水溶媒が、鎖状カルボン酸エステルを含む、請求項1~9のいずれか1項に記載の非水電解質二次電池。
- 正極と、負極と、電解液と、を備え、
前記負極は、電気化学的にリチウムを吸蔵および放出可能な負極活物質と、結着剤と、を含み、
前記負極活物質は、Si含有材料および炭素材料を含み、
前記Si含有材料と前記炭素材料との合計に占める前記炭素材料の割合は、70質量%以上98質量%以下であり、
前記結着剤は、カルボキシアルキルセルロースおよびその塩よりなる群から選択される少なくとも1種のセルロース化合物を含み、
前記セルロース化合物は、前記カルボキシアルキルセルロースのナトリウム塩を含み、
前記負極中の前記セルロース化合物の含有量は、前記負極活物質100質量部あたり0.4質量部以上1.5質量部以下であり、
前記電解液は、非水溶媒と、前記非水溶媒に溶解したリチウム塩と、を含み、
前記リチウム塩は、リチウムビス(フルオロスルホニル)イミド:LFSIを含む、非水電解質二次電池。
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US11916237B2 (en) | 2024-02-27 |
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