JP7531613B2 - リチウム二次電池用分離膜、その製造方法及びそれを含むリチウム二次電池 - Google Patents
リチウム二次電池用分離膜、その製造方法及びそれを含むリチウム二次電池 Download PDFInfo
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- JP7531613B2 JP7531613B2 JP2022568471A JP2022568471A JP7531613B2 JP 7531613 B2 JP7531613 B2 JP 7531613B2 JP 2022568471 A JP2022568471 A JP 2022568471A JP 2022568471 A JP2022568471 A JP 2022568471A JP 7531613 B2 JP7531613 B2 JP 7531613B2
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- separator
- coating layer
- secondary battery
- lithium secondary
- porous coating
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- 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
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
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Description
通気時間増加率≦100%、
熱収縮率≦10%、
電極接着力≧70gf/25mm、
多孔性コーティング層形成用スラリーの粘度≦20cP。
(この際、通気時間増加率と熱収縮率は、下記式で定義され、熱収縮率は、横方向(TD)熱収縮率と縦方向(MD)熱収縮率とのうち小さな値で算定する。
通気時間増加率(%)=[(多孔性高分子基材の通気時間-分離膜の通気時間)/(多孔性高分子基材の通気時間)]×100、
熱収縮率(%)=[(最初長さ-150℃/分間熱収縮処理後の長さ)/(最初長さ)]×100)
-カラム:PL MiniMixed Bx2
-溶媒:DMF
-流速:0.3ml/min
-試料濃度:2.0mg/ml
-注入量:10μl
-カラム温度:40℃
-検出器:アジレント製 RI検出器
-標準:ポリスチレン(3次関数で補正)
-データ処理:ChemStation
前記板状型無機物粒子は、長径(横幅)が0.5μm以上、0.6μm以上、0.7μm以上であり、1.5μm以下、1.3μm以下、または1.2μm以下である。
本発明において、「アスペクト比」とは、厚さの算術平均に対する長径の算術平均の比率(長径の算術平均/厚さの算術平均)を言うものである。この際、長径及び厚さは、前述した方法で求めうる。
本発明において、板状型無機物粒子の含量は、多孔性コーティング層形成用スラリー100重量部を基準に20重量部以上、25重量部以上、または30重量部以上であり、50重量部以下、45重量部以下、または40重量部以下である。
本発明の具体的な一実施形態において、前記板状型無機物粒子は、Al(OH)3、AlO(OH)、Mg(OH)2、BaTiO3、またはこれらのうち2以上を含みうる。
熱収縮率≦10%、
電極接着力≧70gf/25mm、
多孔性コーティング層形成用スラリーの粘度≦20cP。
(この際、通気時間増加率と熱収縮率は、下記式で定義され、熱収縮率は、横方向(TD)熱収縮率と縦方向(MD)熱収縮率とのうち小さな値で算定する。
通気時間増加率(%)=[(多孔性高分子基材の通気時間-分離膜の通気時間)/(多孔性高分子基材の通気時間)]×100、
熱収縮率(%)=[(最初長さ-150℃/分間熱収縮処理後の長さ)/(最初長さ)]×100)
無機物粒子として板状型の水酸化アルミニウム(平均粒径:800nm、Huber社)、分散剤としてポリ(エチレングリコール)-ブロック-ポリ(アクリル酸)(poly(ethylene glycol)-block-poly(acrylic acid)、BYK社)を常温で水に投入して均一に撹拌した後、粒子型バインダー高分子としてアクリル系粒子型バインダー(Zeon社)を順次に投入して多孔性コーティング層形成用スラリーを準備した。前記スラリーのうち、無機物粒子と粒子型バインダー高分子との重量比は、70:30にした。また、前記無機物粒子と前記分散剤との重量比は、99.5:0.5であった。ドクターブレードを用いて、前記スラリーをポリエチレン多孔性基材の一面に塗布し、乾燥して多孔性コーティング層が形成された分離膜を準備した。それを表1に示した。実施例1によって製造された分離膜のSEM写真を図1に記載した。
分散剤としてポリ(エチレングリコール)-ブロック-ポリ(アクリル酸)の代わりに、カルボキシメチルセルロース(CMC、GL chem社)を使用したことを除いては、実施例1と同じ方法で分離膜を製造した。それを表1に示した。比較例1によって製造された分離膜のSEM写真を図2に記載した。
板状型の無機物粒子の代わりに、球状の無機物粒子であるアルミナ(Al2O3、平均粒径:600nm、Alteo社)を使用し、分散剤としてポリ(エチレングリコール)-ブロック-ポリ(アクリル酸)の代わりに、カルボキシメチルセルロース(CMC、GL chem社)を使用したことを除いては、実施例1と同じ方法で分離膜を製造した。それを表1に示した。比較例2によって製造された分離膜のSEM写真を図3に記載した。
分散剤としてポリ(エチレングリコール)-ブロック-ポリ(アクリル酸)の代わりに、グリコール基の官能基のみを有するポリエチレングリコール(Poly ethylene glycol、Aldrich社)を使用したことを除いては、実施例1と同じ方法で分離膜を製造した。それを表1に示した。
分散剤としてポリ(エチレングリコール)-ブロック-ポリ(アクリル酸)の代わりに、カルボキシル基の官能基のみを有するポリアクリル酸(Poly acrylic acid、Aldrich社)を使用したことを除いては、実施例1と同じ方法で分離膜を製造した。それを表1に示した。
1)厚さ測定方法
分離膜の厚さは、厚さ測定器(Mitutoyo社、VL-50S-B)を用いて測定した。
25℃で多孔性コーティング層形成用スラリー100ccをDV 2T Viscometer(Brookfield viscometer)装置を通じて測定した。
通気時間測定器(製造社:Asahi Seiko、製品名:EG01-55-1MR)を用いて一定の圧力(0.05MPa)で100mlの空気が分離膜を通過するのにかかる時間(sec)を測定した。サンプルの左/中/右の各1pointずつ総3point測定して平均を記録した。
電極と分離膜との接着力を測定するために、次のように負極を準備した。
前記熱収縮率は、(最初長さ-150℃/分間熱収縮処理後の長さ)/(最初長さ)×100で算定する。
スラリーに含まれた無機物粒子の平均粒径は、Particle Size Analyzer(製品名:MASTERSIZER 3000;製造社:Malvern)を用いて測定した。
多孔性コーティング層内の粒子型バインダーの組成比は、X線回折分析及びX線分光学組成分析(EDX)を通じて測定した。
10:多孔性高分子基材
20:多孔性コーティング層
21:無機物粒子
22:粒子型バインダー高分子
Claims (17)
- 多孔性高分子基材と、
前記多孔性高分子基材の少なくとも一側表面に形成され、無機物粒子、粒子型バインダー高分子及び分散剤を含む多孔性コーティング層と、を備え、
前記分散剤は、カルボキシ基とグリコール基とを含み、
前記多孔性コーティング層が、厚さ方向に上層、中層、及び下層に区分される時、
前記上層は、前記多孔性コーティング層を厚さ方向にn等分した時、最外郭層であり、
前記下層は、前記多孔性コーティング層を厚さ方向にn等分した時、前記多孔性高分子基材と対面する層であり、
前記中層は、前記多孔性コーティング層で前記上層と下層とを除いた残りの層であり、
前記nは、3~10のうち何れか1つの整数であり、
前記上層内の粒子型バインダー高分子の含量は、前記下層内の粒子型バインダー高分子の含量よりも大きなことを特徴とする、リチウム二次電池用分離膜。 - 前記粒子型バインダー高分子の含量が、前記多孔性コーティング層の厚さ方向基準に下層から上層に行くほど増加する濃度勾配を有し、
前記無機物粒子の含量が、前記多孔性コーティング層の厚さ方向基準に上層から下層に行くほど増加する濃度勾配を有することを特徴とする、請求項1に記載のリチウム二次電池用分離膜。 - 前記多孔性コーティング層において、前記中層は、前記粒子型バインダー高分子が漸進的な濃度勾配を有するか、または特異的な濃度勾配がないことを特徴とする、請求項1に記載のリチウム二次電池用分離膜。
- 前記無機物粒子と前記分散剤との重量比は、99.5:0.5~95:5であることを特徴とする、請求項1から3の何れか一項に記載のリチウム二次電池用分離膜。
- 前記粒子型バインダー高分子の含量は、多孔性コーティング層100重量部を基準に10~50重量部であることを特徴とする、請求項1から4の何れか一項に記載のリチウム二次電池用分離膜。
- 前記分散剤は、グリコール基の当量数/カルボキシ基の当量数の値が0.05~0.25であることを特徴とする、請求項1から5の何れか一項に記載のリチウム二次電池用分離膜。
- 前記分散剤の重量平均分子量は、100~10,000であることを特徴とする、請求項1から6の何れか一項に記載のリチウム二次電池用分離膜。
- 前記分散剤は、ポリアクリル酸及びポリエチレングリコールの共重合体であることを特徴とする、請求項1から7の何れか一項に記載のリチウム二次電池用分離膜。
- 前記分散剤は、ポリアクリル酸とポリエチレングリコールとのブロック共重合体であることを特徴とする、請求項8に記載のリチウム二次電池用分離膜。
- 前記多孔性コーティング層の厚さは、2~10μmであることを特徴とする、請求項1から9の何れか一項に記載のリチウム二次電池用分離膜。
- 前記無機物粒子は、板状型無機物粒子であることを特徴とする、請求項1から10の何れか一項に記載のリチウム二次電池用分離膜。
- 前記板状型無機物粒子は、アスペクト比が3.5以上であることを特徴とする、請求項11に記載のリチウム二次電池用分離膜。
- 前記板状型無機物粒子は、Al(OH)3、AlO(OH)、Mg(OH)2、BaTiO3またはこれらのうち1以上を含むことを特徴とする、請求項11または12に記載のリチウム二次電池用分離膜。
- 請求項1に記載のリチウム二次電池用分離膜の製造方法であって、
多孔性高分子基材の少なくとも一側表面に溶媒、無機物粒子、粒子型バインダー高分子及び分散剤を含む多孔性コーティング層形成用スラリーを塗布及び乾燥する段階を含み、
前記多孔性コーティング層形成用スラリーの粘度は、200cP以下であり、
前記多孔性コーティング層形成用スラリー内の固形分の含量は、前記スラリー100重量部を基準に10~40重量部であることを特徴とする、分離膜の製造方法。 - 前記溶媒は、水であり、
前記粒子型バインダー高分子は、溶媒に分散されている粒子状であり、
前記乾燥段階で相分離が行われることを特徴とする、請求項14に記載の分離膜の製造方法。 - 前記分離膜は、下記3つの式を満足することを特徴とする、請求項14または15に記載のリチウム二次電池用分離膜の製造方法:
通気時間増加率≦100%、
電極接着力≧70gf/25mm、
多孔性コーティング層形成用スラリーの粘度≦20cP。
(この際、通気時間増加率は、下記式で定義される。
通気時間増加率(%)=[(分離膜の通気時間-多孔性高分子基材の通気時間)/(多孔性高分子基材の通気時間)]×100 - 正極、負極及び前記正極と負極との間に介在された分離膜を含み、
前記分離膜は、請求項1から13のうち何れか一項に記載のものである、リチウム二次電池。
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US10096810B2 (en) * | 2012-05-10 | 2018-10-09 | Samsung Sdi Co., Ltd. | Separator and method of manufacturing the same and rechargeable lithium battery including the same |
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