JP7439284B2 - 正極活物質前駆体および正極活物質前駆体の製造方法 - Google Patents
正極活物質前駆体および正極活物質前駆体の製造方法 Download PDFInfo
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- JP7439284B2 JP7439284B2 JP2022550990A JP2022550990A JP7439284B2 JP 7439284 B2 JP7439284 B2 JP 7439284B2 JP 2022550990 A JP2022550990 A JP 2022550990A JP 2022550990 A JP2022550990 A JP 2022550990A JP 7439284 B2 JP7439284 B2 JP 7439284B2
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- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 1
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 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
- 239000000571 coke Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 230000001687 destabilization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 150000004862 dioxolanes Chemical class 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000003759 ester based solvent Substances 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Chemical group CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000004210 ether based solvent Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000011357 graphitized carbon fiber Substances 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 150000002430 hydrocarbons Chemical group 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000002461 imidazolidines Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000011254 layer-forming composition Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical class [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 229910000686 lithium vanadium oxide Inorganic materials 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
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011656 manganese carbonate Substances 0.000 description 1
- 235000006748 manganese carbonate Nutrition 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- 239000011564 manganese citrate Substances 0.000 description 1
- 235000014872 manganese citrate Nutrition 0.000 description 1
- 229940097206 manganese citrate Drugs 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(II) nitrate Inorganic materials [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 description 1
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002931 mesocarbon microbead Substances 0.000 description 1
- 239000011302 mesophase pitch Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 description 1
- 229910001453 nickel ion Inorganic materials 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
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011301 petroleum pitch Substances 0.000 description 1
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229920001384 propylene homopolymer Polymers 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002153 silicon-carbon composite material Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 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
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000002733 tin-carbon composite material Substances 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
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Images
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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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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- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- 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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Description
[化学式1]
[Nix1Coy1Mnz1M1 a](OH)2
[化学式2]
[Nix2Coy2Mnz2M2 b](OH)2
前記化学式1および化学式2中、
M1およびM2は、それぞれ独立して、Zr、B、W、Mo、Cr、Al、Ti、Mg、TaおよびNbから選択される1種以上であり、
0.6≦x1≦1.0、0≦y1≦0.4、0≦z1≦0.4、0≦a<0.1、x1+y1+z1+a=1であり、
0.6≦x2≦1.0、0≦y2≦0.4、0≦z2≦0.4、0≦b<0.1、x2+y2+z2+b=1であり、
aとbのうち少なくとも一つは0超である。
先ず、本発明によるバイモーダル型正極活物質前駆体の製造方法について説明する。
前記第1ステップは、第1遷移金属水溶液および前記第1遷移金属水溶液とは金属元素の組成が相違する第2遷移金属水溶液を準備するステップである。前記第1遷移金属水溶液と前記第2遷移金属水溶液のうち少なくとも一つは、Zr、B、W、Mo、Cr、Al、Ti、Mg、TaおよびNbから選択される1種以上のドーピング元素を含む。
前記第2ステップは、反応器内に前記第1遷移金属水溶液、アンモニウムカチオン錯体形成剤および塩基性水溶液を含む第1反応原料物質を投入し、pH12以上で沈殿反応により第1正極活物質前駆体粒子の核を形成した後、pH12未満で沈殿反応により第1正極活物質前駆体粒子を成長させるステップである。
前記第3ステップは、前記第1正極活物質前駆体粒子を含む反応器に前記第2遷移金属水溶液、アンモニウムカチオン錯体形成剤および塩基性水溶液を含む第2反応原料物質を投入し、pH12以上で沈殿反応により第2正極活物質前駆体粒子の核を形成した後、pH12未満で沈殿反応により前記第1正極活物質前駆体粒子と第2正極活物質前駆体粒子を同時に成長させ、平均粒径(D50)が相違する第1正極活物質前駆体粒子と第2正極活物質前駆体粒子を含むバイモーダル型正極活物質前駆体を製造するステップである。
次に、本発明によるバイモーダル型正極活物質前駆体について説明する。
[Nix1Coy1Mnz1M1 a](OH)2
[Nix2Coy2Mnz2M2 b](OH)2
M1およびM2は、それぞれ独立して、Zr、B、W、Mo、Cr、Al、Ti、Mg、TaおよびNbから選択される1種以上であり、
0.6≦x1≦1.0、0≦y1≦0.4、0≦z1≦0.4、0≦a<0.1、x1+y1+z1+a=1であり、
0.6≦x2≦1.0、0≦y2≦0.4、0≦z2≦0.4、0≦b<0.1、x2+y2+z2+b=1であり、
aとbのうち少なくとも一つは0超である。
次に、本発明によるバイモーダル型正極活物質前駆体とリチウム原料物質の焼成品である正極活物質について説明する。
次に、上述の本発明の正極活物質を含む正極について説明する。
次に、上述の正極を含む電気化学素子について説明する。
実施例1
NiSO4、CoSO4、MnSO4をニッケル:コバルト:マンガンのモル比が73:7:20のモル比になるようにする量で水の中で混合し、濃度2.4Mの第1遷移金属水溶液を準備した。また、NiSO4、CoSO4、MnSO4をニッケル:コバルト:マンガンのモル比が68:12:20のモル比になるようにする量で、ZrSO4を第2遷移金属水溶液に含まれる金属元素の全含有量に対して0.2モル%の量で水の中で混合し、濃度2.4Mの第2遷移金属水溶液を準備した。
コアシェル構造を有する大粒子の正極活物質前駆体と小粒子の正極活物質前駆体をそれぞれ製造した後、これを混合して、バイモーダル前駆体を製造した。
大粒子の正極活物質前駆体と小粒子の正極活物質前駆体をそれぞれ製造した後、これを混合し、バイモーダル前駆体を製造した。
前記実施例1および比較例1~2で製造した正極活物質前駆体の粒子特性を評価した。
100mLの容器に実施例1および比較例1~2でそれぞれ取得した正極活物質前駆体50gを充填した後、所定の条件で振動させて得られる粒子の見掛け密度を測定した。具体的には、タップ密度試験機(KYT-4000、Seishin社製)を用いて前記正極活物質前駆体のタップ密度を測定した。測定結果は、下記表1に示した。
前記実施例1および比較例1~2で製造した正極活物質前駆体粒子をそれぞれ2.5kgf/cm2の圧延密度で圧縮してペレット状にした後、密度測定装置(4350L、Carver社製)を用いて正極活物質前駆体のペレット密度を測定した。測定結果は、下記表1に示した。
前記実施例1および比較例1~2で製造した正極活物質前駆体の表面特性を走査電子顕微鏡を用いて確認した。
前記実施例1および比較例1~2で製造した正極活物質前駆体粒子の粒度分布を確認するために、粒度分布測定装置(S-3500、Microtrac社製)を用いて実施例1および比較例1~2で生成した正極活物質前駆体の粒度を測定し、その結果を下記表2および図4に示した。
前記実施例1および比較例1~2で製造した正極活物質前駆体を用いて製造した正極活物質の焼成均一度を確認するために、前記実施例1および比較例1~2でそれぞれ製造した正極活物質前駆体をそれぞれLiOHと1:1.03の比率(重量%)で混合し、830℃で10時間焼成して、バイモーダル型正極活物質を製造した。前記で製造した正極活物質を用いて、二次電池を製造した後、前記二次電池の初期容量および容量維持率を確認した。
Claims (13)
- 第1遷移金属水溶液および前記第1遷移金属水溶液とは金属元素の組成が相違する第2遷移金属水溶液を準備する第1ステップと、
反応器内に前記第1遷移金属水溶液、アンモニウムカチオン錯体形成剤および塩基性水溶液を含む第1反応原料物質を投入し、pH12以上で沈殿反応により第1正極活物質前駆体粒子の核を形成した後、pH12未満で沈殿反応により第1正極活物質前駆体粒子を成長させる第2ステップと、
前記第1正極活物質前駆体粒子を含む反応器に前記第2遷移金属水溶液、アンモニウムカチオン錯体形成剤および塩基性水溶液を含む第2反応原料物質を投入し、pH12以上で沈殿反応により第2正極活物質前駆体粒子の核を形成した後、pH12未満で沈殿反応により前記第1正極活物質前駆体粒子と第2正極活物質前駆体粒子を同時に成長させ、平均粒径(D50)が相違する第1正極活物質前駆体粒子と第2正極活物質前駆体粒子を含むバイモーダル型正極活物質前駆体を製造する第3ステップとを含み、
前記第1遷移金属水溶液と前記第2遷移金属水溶液のうち少なくとも一つは、Zr、B、W、Mo、Cr、Al、Ti、Mg、TaおよびNbから選択される1種以上のドーピング元素を含む、バイモーダル型正極活物質前駆体の製造方法。 - 前記反応器は、濾過装置をさらに含み、
前記反応器が満液になると、前記反応器内に含まれた濾過装置を介して反応が完了した反応母液を反応器の外部に排出しながら、反応原料物質を投入する、請求項1に記載のバイモーダル型正極活物質前駆体の製造方法。 - 前記ドーピング元素は、Zr、Al、BおよびWから選択される1種以上である、請求項1に記載のバイモーダル型正極活物質前駆体の製造方法。
- 前記ドーピング元素は、前記第1遷移金属水溶液または前記第2遷移金属水溶液に含まれる金属元素の全含有量に対して0.01モル%~0.5モル%の含有量で含まれる、請求項1に記載のバイモーダル型正極活物質前駆体の製造方法。
- コアシェル構造を有する第1正極活物質前駆体粒子および前記第1正極活物質前駆体粒子より平均粒径(D50)が小さい第2正極活物質前駆体粒子を含み、
前記第1正極活物質前駆体粒子のコア部は、下記化学式1で表される組成を有し、
前記第1正極活物質前駆体粒子のシェル部と前記第2正極活物質前駆体粒子は下記化学式2で表される組成を有し、
化学式1で表される組成と化学式2で表される組成は相違し、
[化学式1]
[Nix1Coy1Mnz1M1 a](OH)2
[化学式2]
[Nix2Coy2Mnz2M2 b](OH)2
前記化学式1および前記化学式2中、
M1およびM2は、それぞれ独立して、Zr、B、W、Mo、Cr、Al、Ti、Mg、TaおよびNbから選択される1種以上であり、
0.6≦x1≦1.0、0≦y1≦0.4、0≦z1≦0.4、0≦a<0.1、x1+y1+z1+a=1であり、
0.6≦x2≦1.0、0≦y2≦0.4、0≦z2≦0.4、0≦b<0.1、x2+y2+z2+b=1であり、
aとbのうち少なくとも一つは0超である、バイモーダル型正極活物質前駆体。 - 前記化学式1および前記化学式2中、M1およびM2は、それぞれ独立して、Zr、Al、BおよびWから選択される1種以上である、請求項5に記載のバイモーダル型正極活物質前駆体。
- 前記化学式1中、aは0であり、前記化学式2中、bは0.0001≦b≦0.05である、請求項5に記載のバイモーダル型正極活物質前駆体。
- 前記第1正極活物質前駆体粒子の平均粒径(D50)が8μm~15μmであり、前記第2正極活物質前駆体粒子の平均粒径(D50)が1μm以上8μm未満である、請求項5に記載のバイモーダル型正極活物質前駆体。
- 前記バイモーダル型正極活物質前駆体のタップ密度が2.0g/cc~2.5g/ccである、請求項5に記載のバイモーダル型正極活物質前駆体。
- 前記バイモーダル型正極活物質前駆体を1.0kgf/cm2~5.0kgf/cm2の圧延密度で圧縮してペレット状に製造してから測定したペレット密度が2.0g/cc~3.0g/ccである、請求項5に記載のバイモーダル型正極活物質前駆体。
- 請求項5から10のいずれか一項に記載のバイモーダル型正極活物質前駆体とリチウム原料物質の焼成品である正極活物質。
- 請求項11に記載の正極活物質を含む正極。
- 請求項12に記載の正極を含む電気化学素子。
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