JP6890874B2 - 二次電池用正極活物質の製造方法、このように製造された正極活物質及びこれを含むリチウム二次電池 - Google Patents
二次電池用正極活物質の製造方法、このように製造された正極活物質及びこれを含むリチウム二次電池 Download PDFInfo
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- JP6890874B2 JP6890874B2 JP2020506194A JP2020506194A JP6890874B2 JP 6890874 B2 JP6890874 B2 JP 6890874B2 JP 2020506194 A JP2020506194 A JP 2020506194A JP 2020506194 A JP2020506194 A JP 2020506194A JP 6890874 B2 JP6890874 B2 JP 6890874B2
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- positive electrode
- active material
- secondary battery
- electrode active
- lithium
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- 239000007774 positive electrode material Substances 0.000 title claims description 75
- 229910052744 lithium Inorganic materials 0.000 title claims description 32
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 30
- 238000004519 manufacturing process Methods 0.000 title claims description 18
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- 239000011247 coating layer Substances 0.000 claims description 37
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims description 34
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- 239000002033 PVDF binder Substances 0.000 claims description 25
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- 239000011572 manganese Substances 0.000 claims description 19
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- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
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- QEXMICRJPVUPSN-UHFFFAOYSA-N lithium manganese(2+) oxygen(2-) Chemical class [O-2].[Mn+2].[Li+] QEXMICRJPVUPSN-UHFFFAOYSA-N 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
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- ACFSQHQYDZIPRL-UHFFFAOYSA-N lithium;bis(1,1,2,2,2-pentafluoroethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)C(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)C(F)(F)F ACFSQHQYDZIPRL-UHFFFAOYSA-N 0.000 description 1
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
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Description
本出願は、2017年9月29日付韓国特許出願第10−2017−0127757号及び2018年9月27日付韓国特許出願第10−2018−0115214号に基づく優先権の利益を主張し、当該韓国特許出願の文献に開示された全ての内容は本明細書の一部として含まれる。
[化学式1]
LipNi1−x−yCoxMa yMb zO2
前記式で、MaはMn、Al及びZrからなる群から選択される一つ以上の元素であり、MbはAl、Zr、Ti、Mg、Ta、Nb、Mo、W及びCrからなる群から選択される一つ以上の元素であり、0.9≦p≦1.5、0≦x≦0.5、0≦y≦0.5、0≦z≦0.1である。より好ましくは、0≦x+y≦0.7であってもよく、最も好ましくは0<x+y≦0.4であり、遷移金属全体中のニッケル(Ni)の含量が60モル%以上の高濃度ニッケル(High‐Ni)NCM系正極活物質であってもよい。例えば、前記正極活物質は、より好ましくは、LiNi0.8Co0.1Mn0.1O2、LiNi0.9Co0.05Mn0.05O2、またはLiNi0.6Co0.2Mn0.2O2などの高濃度ニッケル(High‐Ni)NCM系リチウム遷移金属酸化物であってもよい。
LiNi0.6Co0.2Mn0.2O2とポリビニリデンフルオライド(PVDF)、カーバイド(carbide)としてB4Cを100:2:0.1の重量比で混合し、酸素雰囲気下、400℃で3時間ほど熱処理することで、前記LiNi0.6Co0.2Mn0.2O2の粒子表面にコーティング層を形成した。
カーバイド(carbide)としてB4Cの代わりにAl4C3を混合して製造することを除いては、実施例1と同様に実施して製造した。
コーティング用ポリマーとしてポリビニリデンフルオライド(PVDF)の代わりにポリビニルピロリドン(PVP)を混合して製造することを除いては、実施例1と同様に実施して製造した。
LiNi0.6Co0.2Mn0.2O2とポリビニリデンフルオライド(PVDF)、カーバイド(carbide)としてB4Cを100:0.2:0.5の重量比で混合し、酸素雰囲気下、400℃で3時間ほど熱処理することで、前記LiNi0.6Co0.2Mn0.2O2の粒子表面にコーティング層を形成した。
コーティング層を形成していないLiNi0.6Co0.2Mn0.2O2を準備した。
LiNi0.6Co0.2Mn0.2O2とH3BO3を100:0.1の重量比で混合し、酸素雰囲気下、400℃で3時間ほど熱処理することで、前記LiNi0.6Co0.2Mn0.2O2の粒子表面をコーティングした。
LiNi0.6Co0.2Mn0.2O2とポリビニリデンフルオライド(PVDF)、カーボンブラックを100:2:0.1の重量比で混合し、酸素雰囲気下、400℃で3時間ほど熱処理することで、前記LiNi0.6Co0.2Mn0.2O2の粒子表面にコーティング層を形成した。
LiNi0.6Co0.2Mn0.2O2とB4Cを100:0.1の重量比で混合し、酸素雰囲気下、400℃で3時間ほど熱処理することで、前記LiNi0.6Co0.2Mn0.2O2の粒子表面をコーティングした。
LiNi0.6Co0.2Mn0.2O2とポリビニリデンフルオライド(PVDF)を100:2の重量比で混合し、酸素雰囲気下、400℃で3時間ほど熱処理することで、前記LiNi0.6Co0.2Mn0.2O2の粒子表面をコーティングした。
前記実施例1及び比較例2により製造された正極活物質を走査型電子顕微鏡(SEM)で拡大して観察した写真を、図1、図2(実施例1)及び図3、図4(比較例2)に示した。
実施例1から4及び比較例1から5で製造された正極活物質を用い、カーボンブラック、PVDFバインダをN‐メチルピロリドン溶媒中に重量比として96:2:2の割合で混合して正極形成用組成物を製造し、これをアルミニウム集電体の片面に塗布した後、130℃で乾燥して圧延し、それぞれ正極を製造した。
前記のように製造された各リチウム二次電池セル(full cell)に対し、それぞれ25℃及び45℃でCCCVモードで0.7C、4.4Vになるまで充電し、0.55C条件でカットオフし、0.5Cの定電流で3.0Vになるまで放電して100回の充放電を実施しながら、抵抗増加率(DCIR[%])を測定した。その結果を表2に示した。
Claims (15)
- リチウム遷移金属酸化物を設ける段階と、
前記リチウム遷移金属酸化物、コーティング用ポリマー及びカーバイドを混合して混合物を形成する段階と、
前記混合物を熱処理し、前記リチウム遷移金属酸化物の粒子表面に炭化されたコーティング用ポリマー及びカーバイドを含むコーティング層を形成する段階と、
を含み、
前記カーバイドは、B 4 C、Al 4 C 3 、TiC、TaC、WC、NbC、HfC、VC及びZrCからなる群から選択される一つ以上である、二次電池用正極活物質の製造方法。 - 前記コーティング用ポリマーは、ポリビニリデンフルオライド(PVDF)、ポリビニルピロリドン、ポリエチレン、ポリスチレン、ポリエチレンテレフタレート、ポリ塩化ビニル、ポリ塩化ビニリデン、エポキシ樹脂、アミノ樹脂、フェノール樹脂、ポリエステル樹脂からなる群から選択される一つ以上である、請求項1に記載の二次電池用正極活物質の製造方法。
- 前記混合物は、リチウム遷移金属酸化物100重量部に対し、前記コーティング用ポリマーを0.001から10重量部含む、請求項1又は2に記載の二次電池用正極活物質の製造方法。
- 前記混合物は、リチウム遷移金属酸化物100重量部に対し、前記カーバイドを0.001から10重量部含む、請求項1から3のいずれか一項に記載の二次電池用正極活物質の製造方法。
- 前記混合物は、前記コーティング用ポリマーと前記カーバイドを1:99から99:1の重量比で含む、請求項1から4のいずれか一項に記載の二次電池用正極活物質の製造方法。
- 前記リチウム遷移金属酸化物は、リチウムコバルト酸化物(LiCoO2)、リチウムニッケル酸化物(LiNiO2)、リチウムマンガン酸化物(LiMn2O4)、リン酸鉄リチウム化合物(LiFePO4)、及び下記化学式1で表されるリチウム複合遷移金属酸化物からなる群から選択される一つ以上を含み、
[化学式1]
LipNi1−x−yCoxMa yMb zO2
前記化学式1で、MaはMn、Al及びZrからなる群から選択される一つ以上の元素であり、MbはAl、Zr、Ti、Mg、Ta、Nb、Mo、W及びCrからなる群から選択される一つ以上の元素であり、0.9≦p≦1.5、0≦x≦0.5、0≦y≦0.5、0≦z≦0.1である、請求項1から5のいずれか一項に記載の二次電池用正極活物質の製造方法。 - 前記熱処理は、200から800℃で行われる、請求項1から6のいずれか一項に記載の二次電池用正極活物質の製造方法。
- リチウム遷移金属酸化物と、
前記リチウム遷移金属酸化物の粒子表面に形成されたコーティング層と、を含み、
前記コーティング層は膜形態からなり、
前記コーティング層は、コーティング用ポリマーの炭化物及びカーバイドを含み、
前記カーバイドは、B 4 C、Al 4 C 3 、TiC、TaC、WC、NbC、HfC、VC及びZrCからなる群から選択される一つ以上である、二次電池用正極活物質。 - 前記コーティング用ポリマーは、ポリビニリデンフルオライド(PVDF)、ポリビニルピロリドン、ポリエチレン、ポリスチレン、ポリエチレンテレフタレート、ポリ塩化ビニル、ポリ塩化ビニリデン、エポキシ樹脂、アミノ樹脂、フェノール樹脂、ポリエステル樹脂からなる群から選択される一つ以上である、請求項8に記載の二次電池用正極活物質。
- 前記コーティング用ポリマーは、ポリビニリデンフルオライド(PVDF)及びポリビニルピロリドン、ポリエチレンテレフタレート及びポリ塩化ビニリデンからなる群から選択される一つ以上である、請求項8に記載の二次電池用正極活物質。
- 前記カーバイドは、B4CまたはAl4C3である、請求項8から10のいずれか一項に記載の二次電池用正極活物質。
- 前記コーティング層は、5nmから2,000nmの厚さを有する、請求項8から11のいずれか一項に記載の二次電池用正極活物質。
- 前記コーティング層は、リチウム遷移金属酸化物粒子100重量部に対し、前記カーバイドを0.001から10重量部含む、請求項8から12のいずれか一項に記載の二次電池用正極活物質。
- 請求項8から13のいずれか一項に記載の二次電池用正極活物質を含む二次電池用正極。
- 請求項14に記載の二次電池用正極を含むリチウム二次電池。
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Application Number | Priority Date | Filing Date | Title |
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KR20170127757 | 2017-09-29 | ||
KR10-2017-0127757 | 2017-09-29 | ||
KR1020180115214A KR102143101B1 (ko) | 2017-09-29 | 2018-09-27 | 이차전지용 양극 활물질의 제조방법, 이와 같이 제조된 양극 활물질 및 이를 포함하는 리튬 이차전지 |
KR10-2018-0115214 | 2018-09-27 | ||
PCT/KR2018/011579 WO2019066585A1 (ko) | 2017-09-29 | 2018-09-28 | 이차전지용 양극 활물질의 제조방법, 이와 같이 제조된 양극 활물질 및 이를 포함하는 리튬 이차전지 |
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US11271210B2 (en) | 2019-12-04 | 2022-03-08 | Apple Inc. | Cathode active material with silicon carbide additive |
US20220109136A1 (en) * | 2020-10-01 | 2022-04-07 | GM Global Technology Operations LLC | Electrode assembly and method of making the same |
CN112670514B (zh) * | 2020-12-28 | 2022-05-06 | 天津巴莫科技有限责任公司 | 一种双包覆型锂电池正极材料及其制备方法 |
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