JP5681703B2 - 電気化学素子用セパレータおよびそれを用いた電気化学素子、並びにその電気化学素子用セパレータの製造方法 - Google Patents
電気化学素子用セパレータおよびそれを用いた電気化学素子、並びにその電気化学素子用セパレータの製造方法 Download PDFInfo
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- JP5681703B2 JP5681703B2 JP2012510602A JP2012510602A JP5681703B2 JP 5681703 B2 JP5681703 B2 JP 5681703B2 JP 2012510602 A JP2012510602 A JP 2012510602A JP 2012510602 A JP2012510602 A JP 2012510602A JP 5681703 B2 JP5681703 B2 JP 5681703B2
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- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 150000005621 tetraalkylammonium salts Chemical class 0.000 description 1
- 229920006259 thermoplastic polyimide Polymers 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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Description
有機バインダであるSBRのエマルジョン(固形分比率40質量%):300gと、水:4000gとを容器に入れ、均一に分散するまで室温で攪拌した。この分散液に耐熱温度が150℃以上の耐熱性微粒子であるベーマイト粉末(板状、平均粒径1μm、アスペクト比10):4000gを4回に分けて加え、増粘剤としてカルボキシメチルセルロース水溶液(固形分として、耐熱性微粒子100質量部に対して1質量部)を添加し、ディスパーにより2800rpmで5時間攪拌して均一なスラリーを調製した。このスラリーにフッ素系界面活性剤であるパーフルオロオクタンスルフォン酸を、水100質量部に対して0.1質量部添加して、耐熱多孔質層形成用スラリーを得た。この耐熱多孔質層形成用スラリーを、樹脂多孔質膜であるPE製多孔質膜(厚み12μm)上にグラビアコーターを用いて塗布した後、乾燥して、樹脂多孔質膜と耐熱多孔質層との2層構造の厚み16μmのセパレータを得た。ここで、樹脂多孔質膜として使用したPE製多孔質膜の表面張力(濡れ指数)Aは30mN/mであり、耐熱多孔質層形成用スラリーの表面張力Bは21.5mN/mであった。
界面活性剤をシリコーン系界面活性剤であるジメチルポリシロキサンポリオキシアルキレン共重合体に変更した以外は、実施例1と同様にして耐熱多孔質層形成用スラリーを調製し、このスラリーを用いた以外は実施例1と同様にしてセパレータを作製した。
界面活性剤の添加量を水100質量部に対して2.5質量部に変更した以外は、実施例1と同様にして耐熱多孔質層形成用スラリーを調製し、このスラリーを用いた以外は実施例1と同様にしてセパレータを作製した。
界面活性剤を使用しない以外は、実施例1と同様にして耐熱多孔質層形成用スラリーを調製し、このスラリーを用いた以外は実施例1と同様にしてセパレータを作製した。
界面活性剤の添加量を水100質量部に対して0.005質量部に変更した以外は、実施例1と同様にして耐熱多孔質層形成用スラリーを調製し、このスラリーを用いた以外は実施例1と同様にしてセパレータを作製した。
<正極の作製>
正極活物質であるLiCoO2:90質量部、導電助剤であるアセチレンブラック:7質量部、およびバインダであるPVDF:3質量部を、N−メチル−2−ピロリドン(NMP)を溶剤として均一になるように混合して正極合剤含有ペーストを調製した。このペーストを、集電体となる厚さ15μmのアルミニウム箔の両面に、塗布長が表面280mm、裏面210mmになるように間欠塗布し、乾燥した後、カレンダー処理を行って、全厚が150μmになるように正極合剤層の厚みを調整し、幅43mmになるように切断して正極を作製した。更に、この正極におけるアルミニウム箔の露出部に正極リード部を溶接した。
負極活物質である黒鉛:95質量部と、バインダであるPVDF:5質量部とを、NMPを溶剤として均一になるように混合して負極合剤含有ペーストを調製した。このペーストを、集電体となる厚さ10μmの銅箔の両面に、塗布長が表面290mm、裏面230mmになるように間欠塗布し、乾燥した後、カレンダー処理を行って、全厚が142μmになるように負極合剤層の厚みを調整し、幅45mmになるように切断して負極を作製した。更に、この負極における銅箔の露出部に負極リード部を溶接した。
前記のようにして得た正極と負極とを、実施例1のセパレータを、その耐熱多孔質層が負極側に向くように介在させて重ね合わせ、渦巻状に巻回して巻回電極体を作製した。得られた巻回電極体を押しつぶして扁平状にした後にラミネートフィルム製の外装体に入れ、非水電解液(エチレンカーボネートとエチルメチルカーボネートを体積比で1対2に混合した溶媒に、LiPF6を濃度1.2mol/Lで溶解した溶液)を注入した後に、外装体の開口部を封止して電池を作製した。
セパレータを実施例2のセパレータに変更した以外は、実施例4と同様にして電池を作製した。
セパレータを実施例3のセパレータに変更した以外は、実施例4と同様にして電池を作製した。
セパレータを比較例2のセパレータに変更した以外は、実施例4と同様にして電池を作製した。
2 ダイヘッド
3 セパレータ
3a 樹脂多孔質膜
3b 耐熱多孔質層
4 バックロール
5 ターンロール
6 乾燥ゾーン
7 粘着テープ
Claims (14)
- 熱可塑性樹脂を主成分とし親水化処理されていない樹脂多孔質膜の少なくとも片面に、耐熱性微粒子を主成分とし有機バインダを含む耐熱多孔質層を有する電気化学素子用セパレータであって、
前記樹脂多孔質膜の表面張力(濡れ指数)Aが、35mN/m以下であり、
前記耐熱多孔質層が、水系の媒体を含み、かつ表面張力Bが29mN/m未満の耐熱多孔質層形成用組成物を乾燥させることにより形成されたものであり、
前記耐熱多孔質層形成用組成物は、界面活性剤を含有しており、
前記表面張力(濡れ指数)Aと前記表面張力Bとの関係が、A>Bであり、前記樹脂多孔質膜と前記耐熱多孔質層との180°での剥離強度が、1.0N/cm以上であることを特徴とする電気化学素子用セパレータ。 - 前記耐熱性微粒子の含有量が、前記耐熱多孔質層の構成成分の全体積中、80体積%以上である請求項1に記載の電気化学素子用セパレータ。
- 前記耐熱多孔質層形成用組成物は、前記媒体100質量部に対して0.01〜1質量部の界面活性剤を含有している請求項1に記載の電気化学素子用セパレータ。
- 前記界面活性剤が、炭化水素系界面活性剤、フッ素系界面活性剤およびシリコーン系界面活性剤よりなる群から選択される少なくとも1種である請求項1または3に記載の電気化学素子用セパレータ。
- 前記界面活性剤が、前記樹脂多孔質膜の、前記耐熱多孔質層が形成された面とは反対側の表面には存在していない請求項1、3または4に記載の電気化学素子用セパレータ。
- 前記耐熱多孔質層形成用組成物を塗布した前記樹脂多孔質膜の表面の領域の面積のうち、95%以上において前記耐熱多孔質層が形成されている請求項1〜5のいずれかに記載の電気化学素子用セパレータ。
- 前記耐熱多孔質層に存在する直径3mm以上のピンホールが、前記耐熱多孔質層の形成部分100cm2あたり1個以下である請求項1〜6のいずれかに記載の電気化学素子用セパレータ。
- 前記熱可塑性樹脂は、融点が100〜140℃のポリオレフィンである請求項1〜7のいずれかに記載の電気化学素子用セパレータ。
- 正極、負極、セパレータおよび非水電解液を含む電気化学素子であって、
前記セパレータが、請求項1〜8のいずれかに記載の電気化学素子用セパレータであることを特徴とする電気化学素子。 - 熱可塑性樹脂を主成分とし親水化処理されていない樹脂多孔質膜の少なくとも片面に、耐熱性微粒子を主成分とし有機バインダを含む耐熱多孔質層を有する電気化学素子用セパレータを製造する方法であって、
表面張力(濡れ指数)Aが35mN/m以下の樹脂多孔質膜を準備する工程と、
水系の媒体を含み、前記媒体100質量部に対して0.01〜1質量部の界面活性剤を含有し、かつ表面張力Bが29mN/m未満の耐熱多孔質層形成用組成物を、前記樹脂多孔質膜の表面に塗布し、乾燥して耐熱多孔質層を形成する工程とを含み、
前記表面張力(濡れ指数)Aと前記表面張力Bとの関係を、A>Bとすることを特徴とする電気化学素子用セパレータの製造方法。 - 前記耐熱多孔質層形成用組成物は、前記媒体100質量部に対して0.5質量部以下の界面活性剤を含有している請求項10に記載の電気化学素子用セパレータの製造方法。
- 前記界面活性剤が、炭化水素系界面活性剤、フッ素系界面活性剤およびシリコーン系界面活性剤よりなる群から選択される少なくとも1種である請求項10または11に記載の電気化学素子用セパレータの製造方法。
- 前記界面活性剤が、前記樹脂多孔質膜の、前記耐熱多孔質層が形成された面とは反対側の表面には存在していない請求項10〜12のいずれかに記載の電気化学素子用セパレータの製造方法。
- 前記熱可塑性樹脂は、融点が100〜140℃のポリオレフィンである請求項10〜13のいずれかに記載の電気化学素子用セパレータの製造方法。
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JP6109467B2 (ja) | 2011-06-28 | 2017-04-05 | 日産自動車株式会社 | 耐熱絶縁層付セパレータ |
CN103314044A (zh) * | 2011-12-02 | 2013-09-18 | 三菱树脂株式会社 | 叠层多孔膜的制造方法 |
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JP2013203894A (ja) * | 2012-03-28 | 2013-10-07 | Asahi Kasei E-Materials Corp | ポリオレフィン微多孔膜 |
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JP6094542B2 (ja) | 2014-07-29 | 2017-03-15 | 住友化学株式会社 | 多孔質膜 |
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JP2017059769A (ja) * | 2015-09-18 | 2017-03-23 | ニッポン高度紙工業株式会社 | アルミニウム電解コンデンサ用セパレータ及びアルミニウム電解コンデンサ |
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JP2019016436A (ja) * | 2017-07-03 | 2019-01-31 | 宇部マクセル株式会社 | 積層膜ロールおよびその製造方法 |
JP7301508B2 (ja) * | 2018-08-08 | 2023-07-03 | キヤノン株式会社 | 接合レンズ、およびそれを有する光学系、および光学機器、および接合レンズの製造方法 |
US20210280947A1 (en) * | 2018-08-28 | 2021-09-09 | Shenzhen Senior Technology Material Co., Ltd. | Coating Liquid for Use in Lithium Ion Battery, Lithium Ion Battery Separator, and Lithium Ion Battery |
CN111208136B (zh) * | 2020-01-16 | 2023-04-07 | 东莞维科电池有限公司 | 一种在线检查涂层隔膜朝向的方法及装置 |
CN114361714A (zh) * | 2021-12-06 | 2022-04-15 | 惠州市旭然新能源有限公司 | 一种涂覆浆料、其制备方法和应用涂覆浆料制成的复合多孔性隔膜、锂离子电池 |
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KR101485387B1 (ko) | 2015-01-23 |
WO2011129169A1 (ja) | 2011-10-20 |
CN102844909A (zh) | 2012-12-26 |
CN102844909B (zh) | 2016-03-02 |
KR20130026444A (ko) | 2013-03-13 |
JPWO2011129169A1 (ja) | 2013-07-11 |
US20120328929A1 (en) | 2012-12-27 |
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