JP2015092463A - 蓄電素子 - Google Patents
蓄電素子 Download PDFInfo
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- JP2015092463A JP2015092463A JP2014184624A JP2014184624A JP2015092463A JP 2015092463 A JP2015092463 A JP 2015092463A JP 2014184624 A JP2014184624 A JP 2014184624A JP 2014184624 A JP2014184624 A JP 2014184624A JP 2015092463 A JP2015092463 A JP 2015092463A
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- 239000004816 latex Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 description 1
- IRDCEJVOXCGYAV-UHFFFAOYSA-M lithium;2-dodecylbenzenesulfonate Chemical compound [Li+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O IRDCEJVOXCGYAV-UHFFFAOYSA-M 0.000 description 1
- ACFSQHQYDZIPRL-UHFFFAOYSA-N lithium;bis(1,1,2,2,2-pentafluoroethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)C(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)C(F)(F)F ACFSQHQYDZIPRL-UHFFFAOYSA-N 0.000 description 1
- NTWKDFWKALPPII-UHFFFAOYSA-M lithium;octadecane-1-sulfonate Chemical compound [Li+].CCCCCCCCCCCCCCCCCCS([O-])(=O)=O NTWKDFWKALPPII-UHFFFAOYSA-M 0.000 description 1
- JFNAJRJKQQEFNH-UHFFFAOYSA-M lithium;octane-1-sulfonate Chemical compound [Li+].CCCCCCCCS([O-])(=O)=O JFNAJRJKQQEFNH-UHFFFAOYSA-M 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- UUIQMZJEGPQKFD-UHFFFAOYSA-N n-butyric acid methyl ester Natural products CCCC(=O)OC UUIQMZJEGPQKFD-UHFFFAOYSA-N 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002627 poly(phosphazenes) Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910021484 silicon-nickel alloy Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 150000008053 sultones Chemical class 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- VOVUARRWDCVURC-UHFFFAOYSA-N thiirane Chemical compound C1CS1 VOVUARRWDCVURC-UHFFFAOYSA-N 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Images
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Abstract
Description
まず、蓄電素子10の製造方法について説明する。具体的には、以下のようにして、後述する実施例1〜33及び比較例1〜37における蓄電素子としての電池の作製を行った。なお、実施例1〜33は、いずれも、上述した実施の形態に係る蓄電素子10に関するものである。
正極活物質として、LiNiMnCoO2を用いた。また、導電助剤にはアセチレンブラック、バインダにはPVDFを用い、正極活物質が90質量%、導電助剤が5質量%、バインダが5質量%となるように配合した。また、正極基材層には厚み20μmのアルミニウム箔を用い、当該アルミニウム箔上にアンダーコート層を形成した。そして、アンダーコート層を形成した正極基材層に、正極活物質、導電助剤、バインダから成るコート剤を箔状に塗布乾燥後、正極合剤層の密度が下記の表1〜4に記載の密度になるようにプレスを行った。なお、比較例5、27〜37については、正極基材層にアンダーコート層を形成せずに、正極の作製を行った。
負極活物質として、ハードカーボン(難黒鉛化性炭素)を用いた。また、バインダにはPVDFを用い、負極活物質が95質量%、バインダが5質量%となるように配合した。また、負極基材層には、厚み10μmの銅箔を用い、負極活物質、導電助剤、バインダにN−メチル−2−ピロリドン(NMP)を加え混練し箔状に塗布乾燥後、プレスを行った。
セパレータ基材層として、透気度が120秒/100ccのポリオレフィン製微多孔膜を使用した。また、無機粒子(アルミナ粒子)、バインダ(アクリル酸)等を混合し、コート剤を作製した。そして、コート剤をセパレータ基材層上にグラビア法にてコートし塗工後、80℃で乾燥させることにより、無機フィラー層を備えた無機層含有セパレータを作製した。
非水電解質としては、プロピレンカーボネート(PC):ジメチルカーボネート(DMC):エチルメチルカーボネート(EMC)=3:2:5(体積比)の混合溶媒に、電解質塩としてLiPF6を調整後に1mol/Lとなるように溶解した。なお、これに添加剤として公知の添加剤を加えることにしてもよい。
正極、負極及びセパレータを、セパレータの無機フィラー層が正極に対向するように積層して巻回後、容器に挿入し、非水電解質を注入して封口した。
電池を放電状態(2V)にて解体し、正極を取り出してDMCにて十分洗浄を行い、25℃で真空乾燥を実施した。以下の試験においては、全て洗浄乾燥後のサンプルを用いて実施した。
マイクロメータにて、正極合剤塗布部分の厚みLを測定した。その後、アセトンもしくはNMPにて合剤を剥離し、剥離後の箔厚みLbを測定した。そして、(L−Lb)/2にて、正極合剤層の片面の塗布厚みを求めた。なお、合剤を剥離するために用いる溶剤は、正極基材層(箔)を侵食しなければ特に制限されない。また、測定は、1サンプルあたり5回実施してその平均値を1サンプルの正極合剤層の片面の厚みとし、10サンプルの正極合剤層の片面の厚みを平均したものを、正極合剤層片面厚みとした。
正極を2×2cm2のサイズに切り出し、2端子表面抵抗計(三菱化学アナリテック、ロレスタEP、プローブは2探針のMCP−TPAPを使用)にて、25℃±10℃、露点0℃以下の環境で表面抵抗を測定した。測定は、1サンプル片面あたり5回実施し、計10回の平均値を1サンプルの表面抵抗とした。なお、片面塗工の場合には、合剤塗工側の5回の平均値を1サンプルの表面抵抗とするものとする。10サンプルについて表面抵抗を測定し、平均したものを正極表面抵抗とした。
正極を2×2cm2のサイズに切り出し、プロピレンカーボネート:ジメチルカーボネート:エチルメチルカーボネート=6:7:7となるよう調製した混合溶媒中に浸漬させ、容器をラミネート封止した状態で65℃の恒温層にて2日間保管を行った。そして、保管後、容器から取り出しDMCにて十分洗浄を行い、25℃で真空乾燥を実施した。そして、正極溶媒浸漬試験(正極膨潤試験)後に正極表面抵抗を測定し、表面抵抗上昇率=(溶媒浸漬試験後正極表面抵抗/溶媒浸漬試験前正極表面抵抗)×100−100にて、下記の表1〜4における表面抵抗上昇率を算出した。
正極を2×2cm2のサイズに切り出し、重量Maを測定した。その後、アセトンもしくはNMPにて合剤を剥離し、剥離後の箔重量Mbを測定した。そして、(Ma−Mb)/8にて、単位面積当たりの正極合剤層の片面塗布重量を求めた。なお、合剤を剥離するために用いる溶剤は、正極基材層(箔)を侵食しなければ特に制限されない。また、測定は、1サンプルあたり5回実施してその平均値を1サンプルの正極合剤層の片面の重量とし、10サンプルの正極合剤層の片面の重量を平均したものを、正極合剤層片面重量とした。
単位面積当たりの正極合剤密度=正極合剤層片面重量/正極合剤層片面厚みにて、下記の表1〜4における正極合剤密度を算出した。
クロスセクションポリッシャ(CP)加工にて断面出しを行った正極を走査型電子顕微鏡(SEM)で観察し、アンダーコート層の厚みを求め、下記の表1〜3におけるアンダーコート層厚みとした。
25℃の恒温層内で以下の試験を実施した。まず、(3−1a)下限電圧2.4Vにて4Aの定電流放電試験を実施し、次に、(3−1b)上限電圧4.1Vにて4Aの定電流定電圧充電を3時間実施後、下限電圧2.4Vにて放電試験4Aの定電流放電を実施した。そして、(3−1b)の放電時の電流容量を電池容量とした。
直前の容量確認試験により1C(A)を定め、放電状態から25℃、0.5C(A)、充電時間1時間にて、SOC(State of Charge)を50%に調整した。そして、温度25℃、電流40C(A)で放電を実施し、1秒目の抵抗D1=(1秒目の電圧と通電前の電圧との差)/電流にて1秒目の抵抗D1を算出し、1秒目の出力W1=(通電前電圧−下限電圧)/D1×下限電圧にて1秒目の出力W1を算出した。また、同様に、10秒目の抵抗D2=(10秒目の電圧と通電前の電圧との差)/電流にて10秒目の抵抗D2を算出し、10秒目の出力W2=(通電前電圧−下限電圧)/D2×下限電圧にて10秒目の出力W2を算出した。
まず、(3−3a)直前の25℃、4A放電試験(上限4.1V、下限2.4V)にて放電した電流容量により1C(A)を定め、放電状態から25℃、0.5C(A)、充電時間1.6時間にて、SOCを80%に調整した。そして、(3−3b)60℃の恒温層に30日保管し、取り出し室温に冷却後、容量確認試験及び25℃出力試験を実施した。そして、上記(3−3a)〜(3−3b)を累積放置日数が360日に到達するまで実施した。なお、電池は膨れ防止のため、金属板で初期電池厚み+1mm以下に緊圧して試験を実施した。そして、試験後の1秒目の出力W1を下記の表1〜4における劣化後出力(1秒目)とし、10秒目の出力W2を下記の表1〜4における劣化後出力(10秒目)とした。
100 容器
110 ふた板
120 正極集電体
130 負極集電体
200 正極端子
300 負極端子
400 電極体
410 正極
411 正極基材層
412 アンダーコート層
413 正極合剤層
420 負極
421 負極基材層
422 負極合剤層
430 セパレータ
431 セパレータ基材層
432 無機フィラー層
Claims (8)
- 正極と、負極と、前記正極と前記負極との間に配置されるセパレータと、非水電解質とを有する蓄電素子であって、
前記正極は、
正極基材層と、
正極活物質を含む正極合剤層と、
前記正極基材層と前記正極合剤層との間に配置されるアンダーコート層とを有し、
前記正極合剤層の密度は、2.1g/cm3以上2.7g/cm3以下であり、
前記正極は、溶媒浸漬試験後の表面抵抗上昇率が30%以下であり、
前記アンダーコート層は、キトサン誘導体、セルロース誘導体及びアクリル酸誘導体から選択される少なくとも一種のバインダを含む
蓄電素子。 - 前記正極合剤層の密度は、2.2g/cm3以上2.6g/cm3以下である
請求項1に記載の蓄電素子。 - 前記正極は、溶媒浸漬試験後の表面抵抗上昇率が−50%以上である
請求項1または2に記載の蓄電素子。 - 前記アンダーコート層は、厚みが0.1μm以上3.0μm以下である
請求項1〜3のいずれか1項に記載の蓄電素子。 - 前記アンダーコート層は、厚みが0.2μm以上2.0μm以下である
請求項4に記載の蓄電素子。 - 前記アンダーコート層は、さらに導電助剤を含み、前記バインダの質量が前記導電助剤の質量の2倍以上3倍以下である
請求項1〜5のいずれか1項に記載の蓄電素子。 - 前記正極活物質は、LiaNibM1cM2dWxNbyZrzO2(但し、式中、a、b、c、d、x、y、zは、0≦a≦1.2、0≦b≦1、0≦c≦0.5、0≦d≦0.5、0≦x≦0.1、0≦y≦0.1、0≦z≦0.1、b+c+d=1を満たし、M1、M2はMn、Ti、Cr、Fe、Co、Cu、Zn、Al、Ge、Sn及びMgからなる群から選択される少なくとも1種の元素である)で表される化合物を有する
請求項1〜6のいずれか1項に記載の蓄電素子。 - 前記負極は、負極活物質として難黒鉛化性炭素を含む
請求項1〜7のいずれか1項に記載の蓄電素子。
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KR20180057345A (ko) * | 2016-11-22 | 2018-05-30 | 주식회사 엘지화학 | 전극의 평가 방법 |
JP2022543417A (ja) * | 2020-06-25 | 2022-10-12 | エルジー エナジー ソリューション リミテッド | バインダー層が形成された電極及びその製造方法 |
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JP6428612B2 (ja) | 2013-10-15 | 2018-11-28 | 株式会社村田製作所 | 電池、電池パック、電子機器、電動車両、蓄電装置および電力システム |
CN107611448A (zh) * | 2017-09-07 | 2018-01-19 | 湖北金泉新材料有限责任公司 | 一种新型电极及包含该电极的锂离子电池 |
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JP6350150B2 (ja) | 2018-07-04 |
KR20150037556A (ko) | 2015-04-08 |
US20150092320A1 (en) | 2015-04-02 |
US9455091B2 (en) | 2016-09-27 |
CN104518220A (zh) | 2015-04-15 |
CN104518220B (zh) | 2019-02-05 |
EP2863456B1 (en) | 2019-11-13 |
EP2863456A1 (en) | 2015-04-22 |
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