JP2020515012A - 二次電池正極用スラリーの製造方法 - Google Patents
二次電池正極用スラリーの製造方法 Download PDFInfo
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- JP2020515012A JP2020515012A JP2019551448A JP2019551448A JP2020515012A JP 2020515012 A JP2020515012 A JP 2020515012A JP 2019551448 A JP2019551448 A JP 2019551448A JP 2019551448 A JP2019551448 A JP 2019551448A JP 2020515012 A JP2020515012 A JP 2020515012A
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- Prior art keywords
- positive electrode
- slurry
- mixture
- secondary battery
- producing
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Links
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Images
Classifications
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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Abstract
Description
Li1+aFe1−xMxPO4−bAb
1(%)≦HBDwt%/(BD+HBD)wt%×100≦30(%)
正極活物質として平均粒径(D50)1.2μmのLiFePO4、導電材としてカーボンブラック、バインダーとしてPVDFを、N‐メチルピロリドン溶媒に、93:3:4の割合(重量比)でホモディスパー(Homo‐disper)を用いて3000rpmで60分間混合することで、第1混合物を製造した。この際、第1混合物の固形分の含量は68重量%であった。このように製造されたペースト状の第1混合物にN‐メチルピロリドン溶媒をさらに投入しながら、ホモミキサー(Homo mixer)を用いて3,000rpmで20分間混合(mixing)して正極用スラリー(固形分の含量48重量%)を製造した。
正極活物質として平均粒径(D50)1.2μmのLiFePO4、導電材としてカーボンブラック、バインダーとしてPVDFを、N‐メチルピロリドン溶媒に93:3:4の割合(重量比)で混合し、さらにHNBR分散剤(AN37重量%、HBDの割合21%)を前記正極活物質100重量部に対して1重量部で混合することで第1混合物(固形分の含量68重量%)を製造したことを除き、実施例1と同様に行って正極用スラリー(固形分の含量48重量%)を製造した。
第1混合物の固形分の含量を79重量%とし、このように製造された凝集体状態の第1混合物にN−メチルピロリドン溶媒をさらに投入しながら混合したことを除き、実施例1と同様に行って正極用スラリーを製造した。
第1混合物の固形分の含量を48重量%とし、このように形成された液状の第1混合物をホモミキサー(Homo mixer)を用いて3,000rpmで80分間混合したことを除き、実施例1と同様に行って正極用スラリーを製造した。
前記実施例1、2、および比較例1、2の正極用スラリーの製造時に、混合物の23℃でのせん断粘性率(shear viscosity)を測定した。TAインスツルメント社のレオメーター(DHR2)を用いてせん断粘性率を測定した。測定方法としては、DHR2装備の二重円筒(Concentric cylinder)タイプのアクセサリを用いて、前記混合物10mlを投入した後、せん断粘性率を測定した。その結果を下記表1に示した。
前記実施例1、2、および比較例1、2で製造された正極用スラリー中の粒子の粒度分布を確認するために、粒ゲージ(Grind gauge)を用いて粒子の粒サイズを測定した。その結果を下記表2に示した。
前記実施例1および比較例1、2で製造された正極スラリーをそれぞれアルミニウム集電体に塗布し、130℃で乾燥した後、圧延することで正極を製造した。
Claims (11)
- リン酸鉄リチウム系正極活物質、導電材、バインダー、および溶媒を投入してペースト状の第1混合物を形成するステップと、
前記ペースト状の第1混合物に溶媒をさらに投入しながら混合することで、正極用スラリーを製造するステップと、を含む、二次電池正極用スラリーの製造方法。 - 前記第1混合物の固形分の含量が50〜75重量%である、請求項1に記載の二次電池正極用スラリーの製造方法。
- 前記第1混合物の固形分の含量が60〜70重量%である、請求項1に記載の二次電池正極用スラリーの製造方法。
- 前記第1混合物のせん断速度10−1/sでのせん断粘性率が1,000〜5,000Pa・s(23℃)である、請求項1から3のいずれか一項に記載の二次電池正極用スラリーの製造方法。
- 前記第1混合物のせん断速度1/sでのせん断粘性率が100〜500Pa・s(23℃)である、請求項1から4のいずれか一項に記載の二次電池正極用スラリーの製造方法。
- 前記第1混合物のせん断速度10−1/sでのせん断粘性率が2,000〜3,000Pa・s(23℃)であり、前記第1混合物のせん断速度1/sでのせん断粘性率が200〜300Pa・s(23℃)である、請求項1から3のいずれか一項に記載の二次電池正極用スラリーの製造方法。
- 前記リン酸鉄リチウム系正極活物質は、平均粒径(D50)が1μm未満の一次粒子である、請求項1から6のいずれか一項に記載の二次電池正極用スラリーの製造方法。
- 前記リン酸鉄リチウム系正極活物質が下記化学式1で表され、
[化学式1]
Li1+aFe1−xMxPO4−bAb
前記化学式1中、Mは、Mn、Ni、Co、Cu、Sc、Ti、Cr、V、およびZnからなる群から選択される何れか一つ以上であり、Aは、S、Se、F、Cl、およびIからなる群から選択される何れか一つ以上であり、−0.5<a<0.5、0≦x<0.5、0≦b≦0.1である、請求項1から7のいずれか一項に記載の二次電池正極用スラリーの製造方法。 - 前記第1混合物の形成時に分散剤をさらに投入する、請求項1から8のいずれか一項に記載の二次電池正極用スラリーの製造方法。
- 前記分散剤が、水素化ニトリルブタジエンゴム(HNBR)を含む、請求項9に記載の二次電池正極用スラリーの製造方法。
- 前記分散剤は、リン酸鉄リチウム系正極活物質100重量部に対して0.8〜1.5重量部で混合される、請求項9又は10に記載の二次電池正極用スラリーの製造方法。
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