JP2021528813A - 電気化学素子用分離膜及びこれを製造する方法 - Google Patents
電気化学素子用分離膜及びこれを製造する方法 Download PDFInfo
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Abstract
Description
1)分離膜の構造
本発明による分離膜は、多孔性高分子基材、及び前記多孔性高分子基材の少なくとも一面に形成された無機コーティング層を含む。前記無機コーティング層は、無機物粒子及びバインダー樹脂を含み、前記バインダー樹脂は、PVdF系高分子を含む第1バインダー樹脂及び酸価1以下のアクリル系高分子を含む第2バインダー樹脂を含む。また、本発明の一実施形態において、前記無機コーティング層は、表層部におけるバインダー樹脂の含量が高くて分離膜と電極との接着力に優れる。
前記多孔性高分子基材は、負極と正極との電気的接触を遮断しながら、イオンを通過させるイオン伝導性バリア(porous ion−conducting barrier)であって、内部に複数の気孔が形成された基材を意味する。複数の気孔が相互連結された構造になっており、基材の一面から他面へと気体または液体が通過可能である。
a)高分子樹脂を溶融/押出して成膜した多孔性フィルム
b)a)の多孔性フィルムが2層以上積層された多層膜
c)高分子樹脂を溶融/紡糸して得られたフィラメントを集積して製造された不織布ウェブ
d)b)の不織布ウェブが2層以上積層された多層膜
e)a)〜d)のうち二つ以上を含む多層構造の多孔性複合膜
本発明において、前記分離膜は、前記多孔性高分子基材の少なくとも一面に形成された無機コーティング層を含む。前記無機コーティング層は、バインダー樹脂及び無機物粒子を含む混合物を含む。本発明の一実施形態において、前記無機コーティング層は、層の内部に無機物粒子が密集した状態で充填され得、無機物粒子同士の間に形成されたインタースティシャルボリュームによる多数の微細気孔を有し得る。これら微細気孔が互いに連結された構造になって、一面から他面へと気体または液体が通過可能な多孔性構造を有し得る。本発明の一実施形態において、前記無機物粒子はバインダー樹脂によって表面の全部または少なくとも一部がコーティングされ、前記バインダー樹脂を介して粒子同士が面結着及び/または点結着され得る。本発明の一実施形態において、前記無機物粒子は、バインダー樹脂と無機物粒子との総量100重量%に対して50重量%以上の比率で無機コーティング層に含まれ得、望ましくは無機物粒子は60重量%以上、70重量%または80重量%以上で含まれ得る。また、上記の範囲内で95重量%以下または90重量%以下で含まれ得る。
B1.バインダー樹脂
本発明の一実施形態において、前記無機コーティング層は、第1バインダー樹脂であるPVdF系高分子及び第2バインダー樹脂であるアクリル系高分子を含み、ここで前記アクリル系高分子は酸価が1以下のものである。
(数1)
酸価=A×N×f×KOH消費量(mL)/S
本発明の具体的な一実施形態において、前記無機物粒子は、電気化学的に安定さえすれば特に制限されない。すなわち、本発明で使用可能な無機物粒子は、適用される電気化学素子の作動電圧範囲(例えば、Li/Li+基準で0〜5V)で酸化及び/または還元反応が起きないものであれば特に制限されない。特に、無機物粒子として誘電率の高い無機物粒子を使用する場合、液体電解質内の電解質塩、例えばリチウム塩の解離度増加に寄与して電解液のイオン伝導度を向上させることができる。
まず、バインダー樹脂を溶媒に溶解して高分子バインダー溶液を用意する。その後、無機物粒子及び溶媒を含む混合物に前記高分子バインダー溶液を投入し混合して無機コーティング層形成用スラリーを用意する。前記混合物及び/またはスラリーには、必要に応じて分散剤のような補助剤をさらに投入してもよい。次いで、これを多孔性高分子基材上に塗布し、加湿条件下で所定時間静置してバインダー樹脂を固化(乾燥)させる。加湿条件で固化しながら前記スラリー中のバインダー樹脂の相分離が誘発される。本発明の一実施形態において、前記加湿条件は相対湿度約40%〜80%の条件であり得る。このような相分離の過程で、溶媒が無機コーティング層の表面部に移動し、溶媒の移動とともにバインダー樹脂が無機コーティング層の表面部に移動されながら、表層部にバインダー樹脂の含量の高い電極接着部が形成される。本発明の一実施形態において、加湿相分離を通じてPVdF系高分子とともにアクリル系高分子も一緒に表層部に移動する。これによって、電極接着部内のPVdF系高分子とアクリル系高分子との含量比は最初スラリー製造時に投入された含量比と類似した水準を維持し、これらの含量比は無機コーティング層の全体厚さにおいて均一に維持される。このように本発明は、PVdF系高分子によって表層部にバインダーの含量の高い電極接着部が効果的に形成され、前記電極接着部にアクリル系高分子が適正量含まれることで電極と分離膜との間の高い接着力が発揮される。
一方、本発明は、上述した分離膜を含む二次電池を提供する。前記電池は、負極、正極及び前記負極と正極との間に介在された分離膜を含み、前記分離膜は、上述した特徴を備えた低抵抗分離膜である。
分離膜の製造
アセトン200gにバインダー樹脂及び分散剤(シアノエチレンポリビニルアルコール)を溶解させて高分子溶液を製造した。ここに無機物粒子(日本軽金属製、LS235、平均粒径0.5μm)を投入し、ボールミル方式で分散させて無機コーティング層用スラリーを用意した。多孔性高分子基材(東レ製、B12PA1)を用意し、ディップコーティング(dip coating)法で前記スラリーを前記基材の表面にコーティングして、相対湿度(RH)約50%の条件で2分間静置してバインダー樹脂の加湿相分離を誘導した。それぞれの実施例及び比較例で使用されたバインダー樹脂などの成分と含量比は、下記表1及び表2のようである。表1に示されたようにそれぞれの実施例で使用されたPMMAは酸価1未満のものが使用された。一方、表1は、図5にも同じ内容を図面として再度示した。
抵抗の測定方法
それぞれの実施例及び比較例の分離膜に対し、以下のような方法で抵抗を測定した。エチレンカーボネート、プロピレンカーボネート及びプロピルプロピオネートを25:10:65の比率(体積比)で混合した溶媒に、LiPF6を1モル濃度で溶解して電解液を用意した。それぞれの分離膜を直径15mmの円形に切断し、前記電解液を含浸させた後、二枚のステンレス電極の間に前記分離膜を介在させて電極形態のコインセル(Wellcos社製)を製作した。前記コインセルをEIS分析装置(ソーラトロン社製)を使用して電気抵抗を測定した。
それぞれの実施例または比較例(例えば、実施例1)で収得した分離膜サンプルを70mm(長さ)×15mm(幅)の大きさで切断して両面テープを張り付けたガラス板上に接着した試片を用意した。それぞれの試片を接着強度測定機(LLOYDインストルメント製、LF plus)に固定し、上側の分離膜試験片を25℃で25mm/分の速度で180゜の角度で剥離し、このときの強度を測定した。
天然黒鉛、SBR(スチレンブタジエンゴム)、CMC及び導電材(重量比で90:2.5:2.5:5)を水に投入して負極スラリーを収得した。前記負極スラリーを銅薄膜(厚さ20μm)上に5mg/cm2のローディング量で塗布して乾燥した。次いで、これを90℃、8.5MPaの条件で圧延し、60mm(長さ)×25mm(幅)に切断して負極を収得した。それぞれの実施例及び比較例で収得した分離膜を70mm(長さ)×25mm(幅)に切断し、用意した負極と分離膜をプレスを用いて70℃、4MPaの条件でラミネートして試片を製作した。用意した試片を両面テープを用いてガラス板に張り付けて固定し、このとき、負極がガラス板に対面するように配置した。試片の分離膜部分を25℃で25mm/minの速度で180゜の角度で剥離し、このときの強度を測定した。
一方、アクリル系高分子であるPMMAの含量比に応じた加湿相分離の効果を確認するため、下記のように参照例1a〜参照例1dを行った。
アセトン200gにバインダー樹脂を溶解させて高分子溶液を製造した。多孔性高分子基材(東レ製、B12PA1)を用意し、ディップコーティング法で前記高分子溶液を前記多孔性高分子基材の表面にコーティングして、相対湿度(RH)約50%の条件で2分間静置してバインダー樹脂の加湿相分離を誘導した。それぞれの参照例で使用されたバインダー樹脂などの成分と含量比は下記表6のようである。
Claims (16)
- 多孔性高分子基材、及び前記多孔性高分子基材の少なくとも一面に形成された無機コーティング層を含み、
前記無機コーティング層は、無機物粒子及びバインダー樹脂を含み、
前記バインダー樹脂は、PVdF系高分子を含む第1バインダー樹脂及びアクリル系高分子を含む第2バインダー樹脂を含み、
前記アクリル系樹脂は、酸価が1以下であって、ガラス転移温度(Tg)が90℃〜130℃である、電気化学素子用分離膜。 - 前記アクリル系高分子は、分子量(Mw)が100,000〜200,000である、請求項1に記載の電気化学素子用分離膜。
- 前記アクリル系高分子は、(メタ)アクリル酸エステル含む(メタ)アクリル系重合体を含み、単量体は、ブチル(メタ)アクリレート、2−エチルへキシル(メタ)アクリレート、エチル(メタ)アクリレート、メチル(メタ)アクリレート、n−プロピル(メタ)アクリレート、イソプロピル(メタ)アクリレート、t−ブチル(メタ)アクリレート、ペンチル(メタ)アクリレート、n−オキシル(メタ)アクリレート、イソオクチル(メタ)アクリレート、イソノニル(メタ)アクリレート、ラウリル(メタ)アクリレート及びテトラデシル(メタ)アクリレートから選択された一つ以上を含む、請求項1に記載の電気化学素子用分離膜。
- 前記アクリル系高分子は、PMMAを含む、請求項1に記載の電気化学素子用分離膜。
- 前記アクリル系高分子は、PMMAを含み、前記PMMAは、分子量(Mw)が100,000〜200,000であり、酸価が1以下であり、Tgが90℃〜130℃である、請求項1に記載の電気化学素子用分離膜。
- 前記アクリル系高分子は、前記バインダー樹脂100重量%のうち10重量%〜80重量%の含量で含まれる、請求項1に記載の電気化学素子用分離膜。
- 前記アクリル系高分子は、前記バインダー樹脂100重量%のうち10重量%〜50重量%の含量で含まれる、請求項1に記載の電気化学素子用分離膜。
- 前記PVdF高分子は、フッ化ビニリデンの単独重合体、フッ化ビニリデンと共重合可能な単量体との共重合体及びこれらの混合物のうち一つ以上を含む、請求項1に記載の電気化学素子用分離膜。
- 前記PVdF高分子は、分子量(Mw)が300,000以上1,000,000以下である、請求項8に記載の電気化学素子用分離膜。
- 前記フッ化ビニリデンと共重合可能な単量体は、フッ化ビニル、トリフルオロエチレン、クロロフルオロエチレン、1,2−ジフルオロエチレン、テトラフルオロエチレン、ヘキサフルオロプロピレン、ペルフルオロ(アルキルビニル)エーテル、ペルフルオロ(1,3−ジオキソール)及びペルフルオロ(2,2−ジメチル−1,3−ジオキソール)から選択された1種以上である、請求項8に記載の電気化学素子用分離膜。
- 前記分離膜の無機コーティング層の表面にバインダー樹脂の含量の高い接着性表層部が配置されている、請求項1に記載の電気化学素子用分離膜。
- 前記分離膜は、加湿条件下の相分離工程を通じて分離膜の無機コーティング層の表面にバインダー樹脂の含量の高い接着性表層部が配置される、請求項11に記載の電気化学素子用分離膜。
- 前記加湿条件は、相対湿度40%〜80%の条件である、請求項12に記載の電気化学素子用分離膜。
- 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に記載のものである、電気化学素子用電極組立体。
- 請求項1に記載の分離膜を製造する方法であって、
多孔性高分子基材を用意し、前記多孔性高分子基材の少なくとも一面に無機コーティング層用スラリーを塗布し、前記スラリーを加湿条件で相分離するように維持して分離膜の無機コーティング層の表面にバインダー樹脂の含量の高い接着性表層部を配置させる、電気化学素子用分離膜の製造方法。 - 前記加湿条件は、相対湿度40%〜80%の条件である、請求項14に記載の電気化学素子用分離膜の製造方法。
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WO2020067778A1 (ko) | 2020-04-02 |
US11990642B2 (en) | 2024-05-21 |
KR102437371B1 (ko) | 2022-08-26 |
EP3848997A1 (en) | 2021-07-14 |
CN112424991A (zh) | 2021-02-26 |
EP3848997A4 (en) | 2021-11-10 |
CN112424991B (zh) | 2023-09-19 |
KR20200036648A (ko) | 2020-04-07 |
US20210280945A1 (en) | 2021-09-09 |
JP7374134B2 (ja) | 2023-11-06 |
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