JP7442915B2 - リチウム二次電池用電極の設計方法およびこれを含むリチウム二次電池用電極の製造方法 - Google Patents
リチウム二次電池用電極の設計方法およびこれを含むリチウム二次電池用電極の製造方法 Download PDFInfo
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- JP7442915B2 JP7442915B2 JP2022109759A JP2022109759A JP7442915B2 JP 7442915 B2 JP7442915 B2 JP 7442915B2 JP 2022109759 A JP2022109759 A JP 2022109759A JP 2022109759 A JP2022109759 A JP 2022109759A JP 7442915 B2 JP7442915 B2 JP 7442915B2
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- 239000011267 electrode slurry Substances 0.000 description 18
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- 230000007423 decrease Effects 0.000 description 17
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- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 2
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 description 2
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 2
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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
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Images
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/041—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/34—Generating the ultrasonic, sonic or infrasonic waves, e.g. electronic circuits specially adapted therefor
- G01N29/348—Generating the ultrasonic, sonic or infrasonic waves, e.g. electronic circuits specially adapted therefor with frequency characteristics, e.g. single frequency signals, chirp signals
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/44—Processing the detected response signal, e.g. electronic circuits specially adapted therefor
- G01N29/4409—Processing the detected response signal, e.g. electronic circuits specially adapted therefor by comparison
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4285—Testing apparatus
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/48—Accumulators combined with arrangements for measuring, testing or indicating the condition of cells, e.g. the level or density of the electrolyte
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Description
実施例1
<正極1~14の製造>
正極活物質として粒径10μmのLi(Ni0.6Co0.2Mn0.2)O2 98.38重量%、導電材としてカーボンナノチューブ(CNT)0.35重量%、バインダーとしてポリビニリデンフルオライド(PVdF)1.2重量%、N-メチル-2-ピロリドン(NMP)溶媒にポリビニリデンフルオライド(PVdF)が0.07重量%混合された分散剤とともに、溶媒としてはN-メチル-2-ピロリドン(NMP)を使用した。
負極活物質として天然黒鉛96重量%、デンカブラック(Denka black)(導電剤)1重量%およびSBR(結合剤)2重量%、およびCMC(増粘剤)1重量%を水に添加し、負極混合物スラリーを製造した。
特定の周波数Fcを確認した前記14種の正極それぞれと前記製造された負極との間に厚さ17μmのポリエチレン製の多孔膜を介在させた後、エチレンカーボネート(EC)およびジエチルカーボネート(DEC)を30:70の体積比で混合した溶媒に1M LiPF6が溶解された電解質を注入し、パウチ型二次電池をそれぞれ製造した。
<正極i~ivの製造>
正極活物質として粒径10μmのLi(Ni0.6Co0.2Mn0.2)O2 96.25重量%、導電材としてカーボンブラック1.5重量%、バインダーとしてポリビニリデンフルオライド(PVdF)2.025重量%、N-メチル-2-ピロリドン(NMP)溶媒にポリビニリデンフルオライド(PVdF)が0.225重量%混合された分散剤とともに、溶媒としてはN-メチル-2-ピロリドン(NMP)を使用した。
<正極aの製造>
正極活物質として粒径5μmのLi(Ni0.6Co0.2Mn0.2)O2 97.1重量%、導電材としてカーボンブラック1重量%、バインダーとしてポリビニリデンフルオライド(PVdF)1.8重量%、N-メチル-2-ピロリドン(NMP)溶媒にポリビニリデンフルオライド(PVdF)が0.225重量%混合された分散剤を溶媒であるN-メチル-2-ピロリドン(NMP)に添加し、正極スラリーを製造した。前記正極スラリーを厚さ20μm程度の正極集電体であるアルミニウム(Al)薄膜に塗布し、乾燥して正極を製造した後、ロールプレス(roll press)を施して正極を製造した。
正極活物質の重量をそれぞれ96.6重量%、96.1重量%および95.1重量%に変更し、これに合わせて導電材の含量を、それぞれ1.5重量%、2重量%および3重量%に変更した以外は、前記正極aの製造と同様の方法で正極を製造した。
<正極Aの製造>
正極活物質として粒径12μmのLi(Ni0.6Co0.2Mn0.2)O2 99.3重量%、導電材としてカーボンブラック0.4重量%、バインダーとしてポリビニリデンフルオライド(PVdF)0.17重量%、およびN-メチル-2-ピロリドン(NMP)溶媒にポリビニリデンフルオライド(PVdF)が0.1重量%混合された分散剤を溶媒であるN-メチル-2-ピロリドン(NMP)に添加し、正極スラリーを製造した。前記正極スラリーを厚さ20μm程度の正極集電体であるアルミニウム(Al)薄膜に塗布し、乾燥して正極を製造した後、ロールプレス(roll press)を施して正極を製造した。
正極活物質の重量をそれぞれ99重量%、98.7重量%、97.3重量%および96.3重量%に変更し、これに合わせて導電材の含量をそれぞれ0.7重量%、1重量%、2重量%および3重量%に変更した以外は、前記正極Aの製造と同様の方法で正極を製造した。
Claims (9)
- (1)活物質、バインダーおよび導電材を含み、導電材の含量のみを異ならせた複数個の電極を製造するステップと、
(2)広帯域誘電分光計(BDS)を用いて、前記製造された複数個の電極それぞれに周波数を変更しながら交流電流を加え、それぞれの電極の伝導度を測定するステップと、
(3)前記それぞれの電極の伝導度がDC伝導度からAC伝導度に変化する点の特定の周波数Fcを確認するステップと、
(4)前記確認された特定の周波数Fcと予め設定された基準周波数Frとを比較し、前記基準周波数Frと前記特定の周波数Fcとの偏差が基準偏差以内に相当する電極に含まれた導電材の含量を適正値として判定するステップとを含み、
前記基準周波数Frを設定するステップは、
(i)組成または製造過程を異ならせた複数個の電極を製造するステップと、
(ii)広帯域誘電分光計(BDS)を用いて、前記製造された複数個の電極それぞれに105Hzから109Hzまで周波数を変更しながら交流電流を加え、それぞれの電極の伝導度を測定するステップと、
(iii)前記それぞれの電極の伝導度がDC伝導度からAC伝導度に変化する点の特定の周波数Fcを確認するステップと、
(iv)前記それぞれの電極を含む複数個のリチウム二次電池を製造し、それぞれの前記リチウム二次電池の前記特定の周波数Fcでの物質移動抵抗Rmの値を確認するステップと、
(v)前記特定の周波数Fcによる前記物質移動抵抗Rmの値の挙動を観察し、前記物質移動抵抗Rmの値が最低値を示した特定の周波数Fcを基準周波数Frとして設定するステップとを含む、リチウム二次電池用電極の設計方法。 - 前記ステップ(2)における電極の伝導度を測定するステップは、前記交流電流の変化に伴う電極の伝導度の変化を観察する過程を含む、請求項1に記載のリチウム二次電池用電極の設計方法。
- 前記予め設定された基準周波数Frは、5×106Hz~5×107Hzの範囲で設定された周波数の値である、請求項1または2に記載のリチウム二次電池用電極の設計方法。
- 前記予め設定された基準周波数Frは、107Hzである、請求項1から3のいずれか一項に記載のリチウム二次電池用電極の設計方法。
- 前記基準周波数Frと前記特定の周波数Fcとの偏差が基準偏差以内に相当する電極が複数個であるときに、より低い特定の周波数Fcを有する電極に含まれた導電材の含量を最適値として判定するステップをさらに含む、請求項1から4のいずれか一項に記載のリチウム二次電池用電極の設計方法。
- 前記ステップ(4)において、基準偏差は、3×106Hzである、請求項1から5のいずれか一項に記載のリチウム二次電池用電極の設計方法。
- 前記ステップ(v)において、前記物質移動抵抗Rmの値が最低値を示した特定の周波数Fcが複数個であるときに、最も低い周波数の値を示した特定の周波数Fcを基準周波数Frとして設定するステップをさらに含む、請求項1から6のいずれか一項に記載のリチウム二次電池用電極の設計方法。
- 前記リチウム二次電池用電極は、リチウム二次電池用正極である、請求項1から7のいずれか一項に記載のリチウム二次電池用電極の設計方法。
- 請求項1から8のいずれか一項に記載の設計方法によって電極の組成を決定する過程を含む、リチウム二次電池用電極の製造方法。
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