JP5612854B2 - ゲルポリマー層を含む電池用分離膜 - Google Patents
ゲルポリマー層を含む電池用分離膜 Download PDFInfo
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- JP5612854B2 JP5612854B2 JP2009507595A JP2009507595A JP5612854B2 JP 5612854 B2 JP5612854 B2 JP 5612854B2 JP 2009507595 A JP2009507595 A JP 2009507595A JP 2009507595 A JP2009507595 A JP 2009507595A JP 5612854 B2 JP5612854 B2 JP 5612854B2
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- gel polymer
- solvent
- separation membrane
- polymer layer
- battery
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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
- 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
- H01M50/411—Organic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
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- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
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- H—ELECTRICITY
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- 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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- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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- H—ELECTRICITY
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- 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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
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- 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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
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- H—ELECTRICITY
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- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
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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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Cell Separators (AREA)
- Secondary Cells (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
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Description
二次電池は、化学エネルギー及び電気エネルギーの可逆的相互変換を用いて、充放電の繰返しが可能な化学電池であって、Ni−MH二次電池及びリチウム二次電池に分けられる。
使用可能な基材材料の非制限的な例としては、ポリオレピン系列、ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリエステル、ポリアセタール、ポリアミド、ポリカーボネート、ポリイミド、ポリエーテルエーテルケトン、ポリエーテルスルホン、ポリフェニレンオキシド、ポリフェニレンサルファイド、ポリエチレンナフタリン又はこれらの混合体などが挙げられ、その他、耐熱性エンジニアリングプラスチックを制限なく使用できる。
1−1.分離膜の製造
PVdF−CTFE(フッ化ポリビニリデン−クロロトリフルオロエチレン共重合体.)高分子をアセトンに約5wt%添加した後、50℃で約12時間以上溶解させ、高分子溶液を製造した。このように製造された高分子溶液に、非溶媒であるメタノールをアセトンに基づいて30vol%で添加した。このように製造された溶液をディップコーティング法により厚さ12μm程度のトウネン社のF12BMS分離膜多孔性基材(気孔率50%)にコートし、コーティング厚さは約2μm程度に調節した。その後、ゲルポリマー上に開放型気孔が形成及び連結されるように、上記コーティング層を90℃で1分間乾燥した。
通気度の測定装置で測定した結果、F12BMS基材の通気度は、約240〜260秒内外であり、コートされたゲルポリマー層を含む場合の通気度は、約350〜400秒内外であった。
(正極の製造)
正極活物質としてLiCoO2 92wt%、導電剤としてカーボンブラック4wt%、結合剤としてPVdF 4wt%を、溶剤であるN−メチル−2−ピロリドン(NMP)に添加して、正極混合物スラリーを製造した。正極混合物スラリーを、厚さが20μmの正極集電体であるアルミニウム(Al)薄膜に塗布及び乾燥して正極を製造した後、ロールプレスを施した。
負極活物質として炭素粉末、結合剤としてPVdF、導電剤としてカーボンブラックを、それぞれ96wt%、3wt%、1wt%として、溶剤であるNMPに添加して負極混合物スラリーを製造した。負極混合物スラリーを厚さが10μmの負極集電体である銅(Cu)薄膜に塗布及び乾燥して負極を製造した後、ロールプレスを施した。
前記正極、負極及び実施例1−1で製造された分離膜を積層方式により組み立て、組み立てられた電池に1Mの六フッ化リン酸リチウム(LiPF6)が溶解されたエチレンカーボネート/エチルメチルカーボネート(EC/EMC=1:2、体積比)系電解液を注入して、リチウム二次電池を製造した。
PVdF−CTFE(フッ化ポリビニリデン−クロロトリフルオロエチレン共重合体.)高分子をアセトンに約5wt%添加した後、50℃で約12時間以上溶解させ、高分子溶液を製造した。このように製造された溶液をディップコーティング法により厚さ12μm程度のトウネン社のF12BMS分離膜多孔性基材(気孔率50%)にコートし、コーティング厚さは約2μm程度に調節した。その後、ゲルポリマー上に開放型気孔が形成及び連結されるように、上記コーティング層を90℃で1分間乾燥しながら、非溶媒である水を蒸気状で噴射した。
通気度の測定装置で測定した結果、非溶媒蒸気噴射法により形成されたゲルポリマー層を含む場合の通気度は、約400〜450秒内外であって、実施例1の非溶媒添加法と類似している通気度を示した。
PVdF−CTFE(フッ化ポリビニリデン−クロロトリフルオロエチレン共重合体.)高分子をアセトンに約5wt%添加した後、50℃で約12時間以上溶解させ、高分子溶液を製造した。このように製造された溶液をディップコーティング法により厚さ12μm程度のトウネン社のF12BMS分離膜多孔性基材(気孔率50%)にコートし、コーティング厚さは約2μm程度に調節した。このとき、分離膜上に緻密なゲルポリマー層が形成された。通気度の測定装置で測定した結果、F12BMS基材の通気度は約240〜260秒内外であり、緻密にコートされたゲルポリマー層を含む場合の通気度は5,000秒以上であった。
非溶媒であるメタノール添加量をアセトンに基づいて5vol%で添加した以外は、実施例1と同様な方法によりゲルポリマー層が形成された分離膜及びリチウム二次電池を製造した。このように製造されたゲルポリマーがコートされた分離膜の通気度を測定した結果、1,500〜1,700秒内外であった。
非溶媒であるメタノール添加量をアセトンに基づいて15vol%で添加した以外は、実施例1と同様な方法によりゲルポリマー層が形成された分離膜及びリチウム二次電池を製造した。このように製造されたゲルポリマーがコートされた分離膜の通気度を測定した結果、800〜900秒内外であった。
実施例1〜実施例4及び比較例1で製造されたゲルポリマー層が形成された分離膜の表面を分析するために、走査電子顕微鏡(SEM)で表面を確認した。比較例1の分離膜は、表面が緻密なゲルポリマー層により覆われて多孔性構造を確認できなかった。これとは異なり、本発明により製造された実施例1及び実施例2の分離膜は、互いに連結している開放型3次元気孔を多数含むゲルポリマー層が基材上に形成されていることを確認できた(図3、図7参照)。非溶媒をゲルポリマー溶液に添加して製造された実施例1及び非溶媒を蒸気噴射して製造された実施例2の場合は、類似している形態の開放型多孔性を有する形態を示し、通気度の値も類似している特性を示す。また、非溶媒の量を異なるようにした場合(実施例3、実施例4)は、非溶媒の量の減少に従って気孔率が減少して、通気度の測定値が増加することが確認できた(図3、図9、図10参照)。
表面形態に従う電解液の沈積差を確認するために、実施例1及び比較例1の分離膜上に、一般的に電解液として用いられるEC:EMC=1:2、LiPF6 1M造成の溶液を注射針で一滴ずつ表面上に沈積し、電解液の侵透性を観察した。図4から分かるように、緻密な表面構造を有する既存の比較例1の場合は、沈積後に時間が経過しても電解液に大きい変化がなかったが、実施例1の場合は、3次元気孔を有する多孔性のゲルポリマー構造であるため、30秒以内に電解液が全面に拡散しながら、電解液の濡れ性が大きく増加したことを確認できた。
本発明で製造された分離膜を含むリチウム二次電池の高率放電特性及びサイクル特性を評価するために、下記のように行った。
1C電池容量が1350mAhである実施例1及び比較例1の電池を、0.5C充電に0.2C、0.5C、1C、2Aの放電速度でサイクリングを行い、これらの放電容量をC−レート特性別に図5に示した。
実施例1、実施例2及び比較例1のリチウム二次電池を、23℃の温度、1Cの電流及び4.2〜3V区間において、充電及び放電を400サイクル繰返しで実施した。
Claims (10)
- 電池用分離膜の製造方法であって、
ゲルポリマーを溶媒に溶解させたゲルポリマー溶液を基材上に適用する段階と、及び、
乾燥時に非溶媒蒸気を噴射して相分離する段階を含んでなり、
前記基材上に互いに連結している開放型3次元気孔を含むことを特徴とする、ゲルポリマー層を備えた電池用分離膜の製造方法。 - 前記乾燥温度が、50〜130℃であることを特徴とする、請求項1に記載の製造方法。
- 前記ゲルポリマーの溶解度指数が15〜45MPa1/2である、請求項1又は2に記載の製造方法。
- 前記ゲルポリマーの分子量が、10,000〜1,000,000であることを特徴とする、請求項1〜3の何れか一項に記載の製造方法。
- 前記ゲルポリマーを溶解させる溶媒が、アセトン、テトラヒドロフラン、塩化メチレン、クロロホルム、ジメチルホルムアミド、N−メチル−2−ピロリドン、シクロヘキサン又はこれらの混合物であることを特徴とする、請求項1〜4の何れか一項に記載の製造方法。
- 前記ゲルポリマーに対する非溶媒が、アルコール類、水又はこれらの混合物であることを特徴とする、請求項1〜5の何れか一項に記載の製造方法。
- 前記溶媒に対する前記ゲルポリマーの濃度が、0.1〜30wt%であることを特徴とする、請求項1〜6の何れか一項に記載の製造方法。
- 前記溶媒に対する前記非溶媒の比率が、0.1〜50vol%であることを特徴とする、請求項1〜7の何れか一項に記載の製造方法。
- 前記気孔の平均直径が、0.01〜10μmであることを特徴とする、請求項1〜8の何れか一項に記載の製造方法。
- 前記基材の厚さが1〜100μmであり、
前記ゲルポリマー層の厚さが0.1〜10μmであることを特徴とする、請求項1〜9の何れか一項に1に記載の製造方法。
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2007
- 2007-04-25 EP EP14158052.2A patent/EP2741345B1/en active Active
- 2007-04-25 EP EP12175275.2A patent/EP2541645B1/en active Active
- 2007-04-25 US US12/226,582 patent/US20090311589A1/en not_active Abandoned
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- 2007-04-25 JP JP2009507595A patent/JP5612854B2/ja active Active
- 2007-04-25 EP EP07746178A patent/EP2025020A4/en not_active Withdrawn
- 2007-04-25 CN CN200780015291XA patent/CN101432906B/zh active Active
- 2007-04-25 KR KR1020070040290A patent/KR100925643B1/ko active IP Right Grant
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EP2541645B1 (en) | 2014-08-27 |
JP2015028942A (ja) | 2015-02-12 |
JP2022071878A (ja) | 2022-05-16 |
CN101432906B (zh) | 2011-06-15 |
WO2007126242A1 (en) | 2007-11-08 |
JP2017103241A (ja) | 2017-06-08 |
TW200816545A (en) | 2008-04-01 |
CN101432906A (zh) | 2009-05-13 |
JP2009535764A (ja) | 2009-10-01 |
KR100925643B1 (ko) | 2009-11-06 |
EP2541645A3 (en) | 2013-08-28 |
EP2741345B1 (en) | 2017-09-13 |
EP2541645A2 (en) | 2013-01-02 |
EP2025020A4 (en) | 2011-07-20 |
EP2741345A3 (en) | 2014-12-17 |
JP7109384B2 (ja) | 2022-07-29 |
KR20070106416A (ko) | 2007-11-01 |
TWI348779B (en) | 2011-09-11 |
US20090311589A1 (en) | 2009-12-17 |
EP2741345A2 (en) | 2014-06-11 |
JP2019079822A (ja) | 2019-05-23 |
EP2025020A1 (en) | 2009-02-18 |
JP6463785B2 (ja) | 2019-02-06 |
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