WO2022131573A1 - 리튬 이차 전지용 양극 활물질, 이의 제조방법 및 이를 포함하는 리튬 이차 전지 - Google Patents
리튬 이차 전지용 양극 활물질, 이의 제조방법 및 이를 포함하는 리튬 이차 전지 Download PDFInfo
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- WO2022131573A1 WO2022131573A1 PCT/KR2021/016671 KR2021016671W WO2022131573A1 WO 2022131573 A1 WO2022131573 A1 WO 2022131573A1 KR 2021016671 W KR2021016671 W KR 2021016671W WO 2022131573 A1 WO2022131573 A1 WO 2022131573A1
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- WIPO (PCT)
- Prior art keywords
- active material
- lithium
- mol
- based compound
- positive electrode
- Prior art date
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- 239000007774 positive electrode material Substances 0.000 title claims abstract description 106
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 64
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 119
- 239000002245 particle Substances 0.000 claims abstract description 68
- 150000001875 compounds Chemical class 0.000 claims abstract description 44
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims description 91
- 239000006182 cathode active material Substances 0.000 claims description 83
- 239000002243 precursor Substances 0.000 claims description 77
- 239000000203 mixture Substances 0.000 claims description 56
- 238000000975 co-precipitation Methods 0.000 claims description 49
- 239000011572 manganese Substances 0.000 claims description 46
- 229910052759 nickel Inorganic materials 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 28
- 229910052751 metal Inorganic materials 0.000 claims description 24
- 229910017052 cobalt Inorganic materials 0.000 claims description 21
- 239000010941 cobalt Substances 0.000 claims description 21
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 21
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 18
- 229910052748 manganese Inorganic materials 0.000 claims description 18
- 229910052782 aluminium Inorganic materials 0.000 claims description 17
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- 230000000052 comparative effect Effects 0.000 description 66
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- -1 for example Inorganic materials 0.000 description 20
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- 229910052739 hydrogen Inorganic materials 0.000 description 3
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Images
Classifications
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- 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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- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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Abstract
Description
a(Å) | c(Å) | c/a | 결정립 크기(nm) | I(003)/I(104) | R-factor | GOF | ||
비교예 1 | Li(M)O2 (Ni=0.80) | 2.8741 | 14.1985 | 4.9401 | 113.9 | 1.24 | 0.526 | 1.149 |
비교예 2 | Li(M)0.995Al0.005O2 | 2.8740 | 14.1980 | 4.9401 | 98.5 | 1.26 | 0.515 | 1.148 |
비교예 3 | Li(M)0.995Al0.01O2 | 2.8745 | 14.1986 | 4.9395 | 94.3 | 1.22 | 0.521 | 1.146 |
비교예 4 | Li(M)0.995Al0.015O2 | 2.8735 | 14.1989 | 4.9413 | 85.4 | 1.23 | 0.520 | 1.152 |
실시예 1 | Li(M)0.995Al0.005O2 | 2.8745 | 14.2009 | 4.9403 | 102.7 | 1.22 | 0.521 | 1.142 |
실시예 2 | Li(M)0.995Al0.01O2 | 2.8742 | 14.2055 | 4.9424 | 95.6 | 1.23 | 0.519 | 1.146 |
실시예 3 | Li(M)0.995Al0.02O2 | 2.8740 | 14.2054 | 4.9427 | 86.3 | 1.24 | 0.511 | 1.151 |
비교예 5 | Li(M)O2 (Ni=0.92) | 2.8745 | 14.1966 | 4.9388 | 94.3 | 1.22 | 0.528 | 1.158 |
비교예 6 | Li(M)0.995Al0.005O2 | 2.8745 | 14.2029 | 4.9409 | 89.7 | 1.22 | 0.519 | 1.150 |
실시예 4 | Li(M)0.995Al0.005O2 | 2.8740 | 14.2067 | 4.9431 | 90.0 | 1.22 | 0.521 | 1.149 |
실시예 5 | Li(M)0.99Al0.01O2 | 2.8739 | 14.2107 | 4.9447 | 84.3 | 1.21 | 0.520 | 1.151 |
비교예 7 | Li(M)O2 (Ni=0.96) | 2.8735 | 14.2009 | 4.9420 | 85.3 | 1.23 | 0.520 | 1.138 |
비교예 8 | Li(M)0.995Al0.005O2 | 2.8744 | 14.2015 | 4.9406 | 78.6 | 1.24 | 0.515 | 1.145 |
실시예 6 | Li(M)0.995Al0.005O2 | 2.8739 | 14.2098 | 4.9444 | 80.6 | 1.22 | 0.512 | 1.151 |
실시예 7 | Li(M)0.99Al0.01O2 | 2.8750 | 14.2091 | 4.9422 | 65.3 | 1.22 | 0.514 | 1.146 |
방전용량 (mAh/g) |
초기 효율(%) |
상온 사이클 수명(%) | 고온 사이클 수명(%) | 상온초기 저항(Ω) |
저항 증가율(%) |
평균누설 전류(mA) |
DSC peak 온도(℃) |
|
비교예 1 | 210.1 | 93.8 | 96.5 | 92.8 | 23.4 | 113.7 | 0.51 | 225.2 |
비교예 2 | 208.5 | 93.9 | 96.6 | 93.3 | 23.1 | 96.8 | 0.45 | 228.5 |
비교예 3 | 205.6 | 94.0 | 96.9 | 94.1 | 22.2 | 88.2 | 0.43 | 230.9 |
비교예 4 | 202.8 | 93.8 | 98.1 | 96.3 | 22.6 | 64.2 | 0.38 | 234.5 |
비교예 9 | 160.1 | 95.1 | 97.2 | 95.2 | 15.8 | 61.2 | 0.42 | 275.1 |
비교예 10 | 208.7 | 93.8 | 96.9 | 94.1 | 26.1 | 98.1 | 0.55 | 218.6 |
실시예 1 | 210.8 | 94.0 | 96.8 | 93.6 | 22.5 | 65.8 | 0.48 | 227.9 |
실시예 2 | 209.7 | 94.1 | 97.8 | 95.2 | 21.1 | 46.8 | 0.25 | 231.5 |
실시예 3 | 205.1 | 93.9 | 99.5 | 97.2 | 21.5 | 35.7 | 0.15 | 236.7 |
방전용량 (mAh/g) |
초기효율 (%) |
상온수명 (%) |
고온수명 (%) |
상온초기 저항(Ω) |
저항 증가율(%) |
평균누설전류 (mA) | DSC peak 온도(℃) |
|
비교예 5 | 223.5 | 93.6 | 85.2 | 80.8 | 38.2 | 385.1 | 0.98 | 210.8 |
비교예 6 | 222.4 | 93.5 | 88.6 | 82.7 | 32.3 | 258.7 | 0.85 | 215.9 |
실시예 4 | 222.3 | 93.9 | 95.9 | 93.9 | 27.2 | 141.8 | 0.62 | 219.7 |
실시예 5 | 221.2 | 93.6 | 97.1 | 94.7 | 26.5 | 122.5 | 0.35 | 225.2 |
방전용량 (mAh/g) |
초기효율 (%) |
상온수명 (%) |
고온수명 (%) |
상온초기 저항(Ω) |
저항 증가율(%) |
평균누설 전류(mA) |
DSC peak 온도(℃) |
|
비교예7 | 228.2 | 94.5 | 40.6 | 35.1 | 49.6 | 550.6 | 1.97 | 200.1 |
비교예8 | 227.2 | 94.8 | 60.8 | 52.7 | 41.8 | 323.1 | 1.51 | 208.7 |
실시예6 | 227.3 | 94.6 | 71.4 | 64.0 | 35.2 | 204.2 | 1.15 | 210.1 |
실시예7 | 224.3 | 95.2 | 88.7 | 84.9 | 28.9 | 157.9 | 0.87 | 215.8 |
Al 평균 함량(몰%) | 중심부와 표면부에서 Al 농도 차이 | ||
표면부(반지름의 약 30% 이에 해당) | 중심부 | ||
비교예 1 | 0 | 0 | 0 |
비교예 2 | 1.6 | 0.24 | 1.36 |
비교예 3 | 2.29 | 0.97 | 1.32 |
비교예 4 | 2.87 | 1.5 | 1.37 |
실시예 1 | 0.45 | 0.52 | 0.07 |
실시예 2 | 0.87 | 0.96 | 0.09 |
실시예 3 | 1.4 | 1.4 | 0 |
비교예 5 | 0 | 0 | 0 |
비교예 6 | 1.72 | 0.31 | 1.41 |
실시예 4 | 0.36 | 0.57 | 0.21 |
실시예 5 | 0.97 | 0.92 | 0.05 |
비교예 7 | 0 | 0 | 0 |
비교예 8 | 1.51 | 0.18 | 1.33 |
실시예 6 | 0.51 | 0.48 | 0.03 |
실시예 7 | 0.97 | 0.89 | 0.08 |
Claims (10)
- Ni 함량이 75 몰% 이상인 리튬 니켈계 화합물 입자이고,상기 리튬 니켈계 화합물 입자의 중심부와 표면부에서 Al의 농도 차이가 1 mol% 이하인리튬 이차 전지용 양극 활물질.
- 제1항에 있어서,상기 리튬 니켈계 화합물 입자의 평균 입경(D50)은10 ㎛내지 20㎛인 리튬 이차 전지용 양극 활물질.
- 제1항에 있어서,상기 리튬 니켈계 화합물 입자는 하기 화학식 1로 표현되는 것인 리튬 이차 전지용 양극 활물질.[화학식 1]LiaNixCoyMnzAl1-(x+y+z)O2(상기 화학식 1에서,a는 0.95 ≤ a ≤ 1.15, x는 0.75 ≤ x ≤ 0.98, y는 0 < y < 0.2이고, z는 0 < z <0.2이고, y+z≤0.25임)
- 제1항에 있어서,상기 표면부는 상기 리튬 니켈계 화합물 입자의 최표면부터 깊이 방향으로 리튬 니켈계 화합물 입자 평균 반지름의 30% 이하의 길이에 해당하는 영역인 리튬 이차 전지용 양극 활물질.
- 제3항에 있어서,상기 화학식 1에서 x+y+z는 0.98 내지 0.999 범위인 리튬 이차 전지용 양극 활물질.
- 니켈 원료 물질, 코발트 원료 물질, 망간 원료 물질, 및 알루미늄 원료 물질을 용매 중에서 공침하여, 전구체 화합물을 제조하는 단계;상기 전구체 화합물 및 리튬 원료 물질을 혼합하여 혼합물을 생성하는 단계; 및상기 혼합물을 소성하는 단계를 포함하는 리튬 이차 전지용 양극 활물질의 제조 방법으로서,상기 리튬 이차 전지용 양극 활물질은 Ni 함량이 80 몰% 이상인 리튬 니켈계 화합물 입자이고, 상기 리튬 니켈계 화합물 입자의 중심부와 표면부에서 Al의 농도 차이가 1 mol% 이하인리튬 전지용 양극 활물질의 제조방법.
- 제6항에 있어서,상기 공침하는 단계는 11.0 내지 12.0의 pH에서 실시하는 것인 리튬 이차 전지용 양극 활물질의 제조방법.
- 제6항에 있어서,상기 리튬 니켈계 화합물 내의 Al 함량은,상기 리튬 니켈계 화합물 입자 내의 리튬을 제외한 금속 원소 전체를 기준으로, 0.1몰% 내지 2몰%인 리튬 이차 전지용 양극 활물질의 제조방법.
- 제6항에 있어서,상기 표면부는 상기 리튬 니켈계 화합물 입자의 최표면부터 깊이 방향으로 리튬 니켈계 화합물 입자 평균 반지름의 30% 이하의 깊이에 해당하는 영역인 리튬 이차 전지용 양극 활물질의 제조방법.
- 제1항 내지 제5항 중 어느 한항의 양극 활물질을 포함하는 양극;음극; 및비수 전해질을 포함하는 리튬 이차 전지.
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KR20190132633A (ko) * | 2017-03-31 | 2019-11-28 | 스미또모 가가꾸 가부시끼가이샤 | 리튬니켈 복합 산화물의 제조 방법 |
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