JP2015527714A - 二次電池用正極活物質及びそれを含む二次電池 - Google Patents
二次電池用正極活物質及びそれを含む二次電池 Download PDFInfo
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- JP2015527714A JP2015527714A JP2015525377A JP2015525377A JP2015527714A JP 2015527714 A JP2015527714 A JP 2015527714A JP 2015525377 A JP2015525377 A JP 2015525377A JP 2015525377 A JP2015525377 A JP 2015525377A JP 2015527714 A JP2015527714 A JP 2015527714A
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- positive electrode
- active material
- electrode active
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- coating
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 229910021470 non-graphitizable carbon Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 229920005608 sulfonated EPDM Polymers 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- MDCWDBMBZLORER-UHFFFAOYSA-N triphenyl borate Chemical compound C=1C=CC=CC=1OB(OC=1C=CC=CC=1)OC1=CC=CC=C1 MDCWDBMBZLORER-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
Description
5〜10μmのLi1.11Mn0.53Ni0.36O2粉末を準備した。また、NH4FとC9H12O3Alを質量比を基準として1:1.18で混合した後、Li1.11Mn0.53Ni0.36O2粉末と混合した。このとき、Li1.11Mn0.53Ni0.36O2粉末に対するF量は0.08wt%であり、Al量は0.04wt%である。その後、混合物を400℃で5時間熱処理した後、粉砕してふるいにかけた。
5〜10μmのLi1.11Mn0.53Ni0.36O2粉末を準備した。
実施例1及び比較例1で製造された正極活物質をSEMイメージを撮影して、図1及び図2にそれぞれ示した。
実施例1及び比較例1で製造された正極活物質を活物質:導電材:バインダーの比率(wt%)が95:2.5:2.5になるようにNMPによく混ぜた後、20μmのAl foilに塗布した後、130℃で乾燥させることで正極電極を得た。負極活物質として黒鉛を使用し、EC:DMC:DEC=1:2:1である溶媒に1MのLiPF6が入っている電解液を使用して電池を得た。得られた電池は、2.5〜4.65Vで0.1C充放電したときの放電容量を得て、下記表1及び図3に示した。
実験例2で製造された電池を3.0〜4.4Vで0.5Cで充放電テストを行った。このとき、寿命特性を、30サイクル進行後の初期容量に対する維持率で評価し、下記表2及び図4に示した。
実験例2で製造された電池を3.0〜4.4Vでレート特性テストを行って、0.1Cの容量に対する各C−rateによる容量で計算して下記表3に示した。
Claims (20)
- 下記化学式1で表されるリチウム遷移金属酸化物の表面に、コーティング前駆体との反応により、下記Mを含む複合体コーティング層が形成されていることを特徴とする、正極活物質:
LixMO2(1)
上記式中、
Mが、MnaM’1−bで表され、M’が、Al、Mg、Ni、Co、Cr、V、Fe、Cu、Zn、Ti及びBからなる群から選択される1つ以上であり、0.95≦x≦1.5であり、0.5≦a≦1である。 - 前記複合体コーティング層が、Li−M−X、Li−M−m及びLi−M−X−mからなる群から選択される1つ以上の結合構造を有しており、前記Xが、第1コーティング前駆体に由来したハロゲン元素であり、前記mが、第2コーティング前駆体に由来した金属元素であることを特徴とする、請求項1に記載の正極活物質。
- 前記第1コーティング前駆体が、ハロゲン元素Xを含む有機化合物又は無機化合物であり、前記Xが、前記有機化合物又は無機化合物に由来したF、Cl、BrまたはIであることを特徴とする、請求項2に記載の正極活物質。
- 前記有機化合物が、PVdF、PVdF−HFP、PVF、PTFE及びETFEからなる群から選択されるいずれか1つであり、前記無機化合物が、ハロゲン元素を含むリチウム塩またはアンモニウム塩であることを特徴とする、請求項3に記載の正極活物質。
- 前記第1コーティング前駆体がPVdFであることを特徴とする、請求項3に記載の正極活物質。
- 前記第2コーティング前駆体が、金属mを含む酸化物であり、前記金属mが、前記酸化物に由来したAl、Ba、Ca、Mg、Si、Ti、Zr、Zn、及びSrからなる群から選択される1つ以上であることを特徴とする、請求項2に記載の正極活物質。
- 前記第2コーティング前駆体がAl2O3であることを特徴とする、請求項6に記載の正極活物質。
- 前記第2コーティング前駆体が、金属mを含むカーボネート系列の物質であり、前記金属mが、前記カーボネート系列の物質に由来したAl、Ba、Ca、Mg、Si、Ti、Zr、Zn、及びSrからなる群から選択される1つ以上であることを特徴とする、請求項2に記載の正極活物質。
- 前記第2コーティング前駆体がCaCO3であることを特徴とする、請求項8に記載の正極活物質。
- 前記第2コーティング前駆体が、金属mを含む有機物であり、前記金属mが、前記有機物に由来したAl、Ba、Ca、Mg、Si、Ti、Zr、Zn、及びSrからなる群から選択される1つ以上であることを特徴とする、請求項2に記載の正極活物質。
- 前記第2コーティング前駆体がC9H12O3Alであることを特徴とする、請求項10に記載の正極活物質。
- 前記複合体コーティング層が、リチウム遷移金属酸化物の表面積を基準として、60〜100%のコーティング面積で形成されたことを特徴をする、請求項2に記載の正極活物質。
- 前記複合体コーティング層において前記Xの含量が、正極活物質の全重量に対して0.01〜1.00wt%であり、前記mの含量が、正極活物質の全重量に対して0.01〜0.50wt%であることを特徴とする、請求項2に記載の正極活物質。
- 請求項1に記載の正極活物質を製造する方法であって、
(a)化学式1のリチウム遷移金属酸化物を準備する過程と、
(b)前記リチウム遷移金属酸化物に、第1コーティング前駆体及び第2コーティング前駆体を同時にコーティングする過程と、
(c)段階(b)のコーティング後、熱処理する過程と、
を含むことを特徴とする、正極活物質の製造方法。 - 前記コーティングが、高エネルギーミリングまたは混合による乾式法で形成されたことを特徴とする、請求項14に記載の正極活物質の製造方法。
- 段階(b)において第1コーティング前駆体及び第2コーティング前駆体が、重量比を基準として2:3〜5:2の混合比で使用されることを特徴とする、請求項14に記載の正極活物質の製造方法。
- 請求項1に記載の正極活物質を含むことを特徴とする、正極合剤。
- 請求項17に記載の正極合剤が集電体上に塗布されていることを特徴とする、二次電池用正極。
- 請求項18に記載の二次電池用正極を含むことを特徴とする、二次電池。
- 請求項19に記載の二次電池がリチウム二次電池であることを特徴とする、二次電池。
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WO2014073833A1 (ko) | 2014-05-15 |
US20180248183A1 (en) | 2018-08-30 |
EP2869369A1 (en) | 2015-05-06 |
KR101658503B1 (ko) | 2016-09-21 |
US20150132651A1 (en) | 2015-05-14 |
CN104521040B (zh) | 2017-04-26 |
CN104521040A (zh) | 2015-04-15 |
EP2869369A4 (en) | 2015-12-30 |
US10573888B2 (en) | 2020-02-25 |
US10014521B2 (en) | 2018-07-03 |
KR20140058165A (ko) | 2014-05-14 |
JP6100901B2 (ja) | 2017-03-22 |
EP2869369B1 (en) | 2018-01-03 |
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