JP6142295B1 - 二次電池用正極活物質 - Google Patents
二次電池用正極活物質 Download PDFInfo
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- 239000007774 positive electrode material Substances 0.000 title claims abstract description 146
- 239000002245 particle Substances 0.000 claims abstract description 79
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 55
- 239000011163 secondary particle Substances 0.000 claims abstract description 42
- 230000001186 cumulative effect Effects 0.000 claims abstract description 23
- 239000011164 primary particle Substances 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 10
- 238000009826 distribution Methods 0.000 claims description 7
- 238000010079 rubber tapping Methods 0.000 claims description 3
- 238000004220 aggregation Methods 0.000 claims description 2
- 230000002776 aggregation Effects 0.000 claims description 2
- 239000006182 cathode active material Substances 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 36
- 239000002994 raw material Substances 0.000 description 24
- 239000012452 mother liquor Substances 0.000 description 22
- 238000004519 manufacturing process Methods 0.000 description 13
- 238000010979 pH adjustment Methods 0.000 description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 11
- 239000003002 pH adjusting agent Substances 0.000 description 11
- 238000012856 packing Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 1
- 229940044175 cobalt sulfate Drugs 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229940053662 nickel sulfate Drugs 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
Description
(1)平均二次粒子径(D99、D50、D2.5)
粒度分布測定装置(堀場製作所社製、LA−950)で測定した(原理はレーザ回折・散乱法)。
X線回折測定は、X線回折装置(リガク社製、RINT2200)を用い、下記条件にて測定を行った。
X線:CuKα/40kV/40mA
スリット:DS/SS=1°,RS=0.3mm
走査モード:FT測定
Sampling Time:0.4秒
Step Width:0.01°
タップデンサー(セイシン社製、KYT−4000)を用いて、JIS R1628に記載の手法のうち、定容積測定法によって測定を行った。
試料を自然落下させて容器に充填し、容器の容積と試料の質量からバルク密度を測定した。
比表面積測定装置(マウンテック社製、Macsorb)を用い、1点BET法によって測定した。
分級装置(日鉄鉱業社製、エルボージェット分級装置EJ−L−3)を用い、分級エッジ距離Mを43.7mm、分級エッジ距離Fを30.0mmで設定し、測定粒子をフィードエアで送り、分級した。
10 pH調整槽
11 pH調整剤供給手段
12 循環経路
13 原料液供給手段
Claims (7)
- 複数の一次粒子が凝集して形成された正極活物質粒子を含有する粒子状正極活物質であって、
前記粒子状正極活物質の、X線回折分析により求められる(101)面の回折ピークの半値幅に対する、前記粒子状正極活物質のうち、累積体積百分率が99体積%の二次粒子径(D99)の正極活物質粒子の、X線回折分析により求められる(101)面の回折ピークの半値幅から、累積体積百分率が2.5体積%の二次粒子径(D2.5)の正極活物質粒子の、X線回折分析により求められる(101)面の回折ピークの半値幅を引いた値の比率が、0以上0.025以下、
前記粒子状正極活物質の、X線回折分析により求められる(001)面の回折ピークの半値幅に対する、前記粒子状正極活物質のうち、累積体積百分率が99体積%の二次粒子径(D99)の正極活物質粒子の、X線回折分析により求められる(001)面の回折ピークの半値幅から、累積体積百分率が2.5体積%の二次粒子径(D2.5)の正極活物質粒子の、X線回折分析により求められる(001)面の回折ピークの半値幅を引いた値の比率が、0以上0.045以下であり、
前記粒子状正極活物質の、X線回折分析により求められる(101)面の回折ピークの半値幅が1.050°以上、X線回折分析により求められる(001)面の回折ピークの半値幅が0.750°以上、
前記累積体積百分率が99体積%の二次粒子径(D99)の正極活物質粒子の、X線回折分析により求められる(101)面の回折ピークの半値幅が1.070°以上、X線回折分析により求められる(001)面の回折ピークの半値幅が0.740°以上、
前記累積体積百分率が2.5体積%の二次粒子径(D2.5)の正極活物質粒子の、X線回折分析により求められる(101)面の回折ピークの半値幅が1.050°以上、X線回折分析により求められる(001)面の回折ピークの半値幅が0.710°以上であり、
前記粒子状正極活物質が、Ni/Co/Zn複合水酸化物、Ni/Co/Mg複合水酸化物、Ni/Al複合水酸化物、Ni/Co/Mn複合水酸化物またはNi/Co/Mn/Al複合水酸化物であり、
前記累積体積百分率が99体積%の二次粒子径(D99)が15μm〜25μm、前記累積体積百分率が2.5体積%の二次粒子径(D2.5)が1.0μm〜5.0μm、累積体積百分率が50体積%の二次粒子径(D50)が8.0μm〜13.5μmであり、二次粒子について粒度分布のピークを一つだけもつ、粒子状正極活物質。 - 粒子円形度が0.85未満である正極活物質粒子の割合が、1.20体積%以下である請求項1に記載の粒子状正極活物質。
- バルク密度が、1.75g/ml以上である請求項1または2に記載の粒子状正極活物質。
- タッピング密度に対するバルク密度の比率が、0.78〜0.90である請求項3に記載の粒子状正極活物質。
- BET比表面積が、10.0〜17.0m2/gである請求項1乃至4のいずれか1項に記載の粒子状正極活物質。
- 請求項1乃至5のいずれか1項に記載の粒子状正極活物質を有する正極板。
- 請求項6に記載の正極板を備えた二次電池。
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JP2016113893A JP6142295B1 (ja) | 2016-06-07 | 2016-06-07 | 二次電池用正極活物質 |
EP17810118.4A EP3467914A4 (en) | 2016-06-07 | 2017-05-25 | POSITIVE ELECTRODE MATERIAL FOR RECHARGEABLE BATTERY |
PCT/JP2017/019554 WO2017212938A1 (ja) | 2016-06-07 | 2017-05-25 | 二次電池用正極活物質 |
CN201780035619.8A CN109314236B (zh) | 2016-06-07 | 2017-05-25 | 二次电池用正极活性物质 |
KR1020187036695A KR102380464B1 (ko) | 2016-06-07 | 2017-05-25 | 이차 전지용 정극 활물질 |
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WO2017212938A1 (ja) | 2017-12-14 |
EP3467914A1 (en) | 2019-04-10 |
JP2017220359A (ja) | 2017-12-14 |
KR20190012187A (ko) | 2019-02-08 |
CN109314236A (zh) | 2019-02-05 |
EP3467914A4 (en) | 2020-02-19 |
KR102380464B1 (ko) | 2022-03-31 |
CN109314236B (zh) | 2021-12-28 |
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