JP6050512B2 - 二次電池用正極活物質コーティング溶液とこの製造方法 - Google Patents
二次電池用正極活物質コーティング溶液とこの製造方法 Download PDFInfo
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- JP6050512B2 JP6050512B2 JP2015539538A JP2015539538A JP6050512B2 JP 6050512 B2 JP6050512 B2 JP 6050512B2 JP 2015539538 A JP2015539538 A JP 2015539538A JP 2015539538 A JP2015539538 A JP 2015539538A JP 6050512 B2 JP6050512 B2 JP 6050512B2
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- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process 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
- 239000002994 raw material Substances 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229940035637 spectrum-4 Drugs 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound 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
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Description
グリコール系溶媒内に金属前駆体及びキレート剤を分散させ混合溶液を製造する段階;
前記混合溶液を1次加熱する段階;及び
前記混合溶液を2次加熱する段階;を含む二次電池用正極活物質コーティング溶液の製造方法を提供する。
グリコール系溶媒内に金属前駆体及びキレート剤を分散させて混合溶液を製造する段階;
前記混合溶液を1次加熱する段階;及び
前記混合溶液を2次加熱する段階を含む二次電池用正極活物質コーティング溶液の製造方法を提供する。
[反応式]
2Mn+ + n(C2H5O2)− + (C6H(8−n)O7)n− → M(C2H5O2)n + M(C6H(8−n)O7)
[化1]
M(C2H5O2)n (1)
[化2]
M(C6H(8−n)O7) (2)
[化3]
M(C6H(8−n)O7)(C2H5O2) (3)
(前記式で、Mは金属前駆体から脱離された金属であって、Mg、Ca、Sr、Ba、Y、Ti、Zr、V、Nb、Ta、Cr、Mo、W、Mn、Fe、Co、Ir、Ni、Zn、Al、Ga、In、Si、Ge、Sn、La及びCeからなる群から選ばれた少なくとも一つの金属であり、nは1から4の整数である。)
M(C2H5O2)n (1)
[化5]
M(C6H(8−n)O7) (2)
[化6]
M(C6H(8−n)O7)(C2H5O2) (3)
(前記式で、Mは金属前駆体から脱離された金属であって、Mg、Ca、Sr、Ba、Y、Ti、Zr、V、Nb、Ta、Cr、Mo、W、Mn、Fe、Co、Ir、Ni、Zn、Al、Ga、In、Si、Ge、Sn、La及びCeからなる群から選ばれた少なくとも一つの金属であり、nは1から4の整数である。)
200gのエチレングリコール(C2H6O2)溶液内に20gのアルミニウムアセテート(Al(C2H3O2)3)と20gのクエン酸(C6H8O7)を分散した後、攪拌して混合溶液を製造した。前記混合溶液を攪拌しつつ141℃の温度で5時間の間1次加熱した後、180℃の温度で混合溶液が濃縮(約1000CPS)されるまで1時間の間2次加熱し、下記式(1a)及び(2a)のように表される金属有機化合物を主成分として含む正極活物質コーティング液(1)を製造した。
[化7]
Al(C2H5O2)3 (1a)
[化8]
Al(C6H5O7) (2a)
200gのエチレングリコール(C2H6O2)溶液内に40gのジルコニウムニトリド(ZrN)と10gのクエン酸(C6H8O7)を分散した後、攪拌して混合溶液を製造した。前記混合溶液を攪拌しつつ150℃の温度で5時間の間1次加熱した後、180℃の温度で混合溶液が濃縮(約1000CPS)されるまで1時間の間2次加熱し、下記式(1b)及び(3a)のように表される金属有機化合物を主成分として含む正極活物質コーティング液(2)を製造した。
[化9]
Zr(C2H5O2)4 (1b)
[化10]
Zr(C6H5O7)(C2H5O2) (3a)
400gのエチレングリコール(C2H6O2)溶液内に70gのマンガンアセテート(Mn(CH3O2)2)と20gのクエン酸(C6H8O7)と5gのホルムアルデヒドを分散した後、攪拌して混合溶液を製造した。前記混合溶液を攪拌しつつ140℃の温度で4時間の間1次加熱した後、180℃の温度で混合溶液が濃縮(約1000CPS)されるまで1時間の間2次加熱し、下記式(1c)及び(2c)のように表される金属有機化合物を主成分として含む正極活物質コーティング液(3)を製造した。
[化11]
Mn(C2H5O2)m (1c)
[化12]
Mn(C6H5O7) (2c)
(前記式で、mは1から3の整数である。)
エタノール8gに前記実施例1で製造した化学式(1)の正極活物質コーティング溶液2gを添加して攪拌しつつ、正極活物質(LiNi0.6Mn0.2Co0.2)O2)50gを添加してペースト状態に撹拌した。攪拌されたペーストを180℃で2時間乾燥した後、800℃の空気中で1時間熱処理し、約0.2重量%のアルミニウムオキシド層が被覆された正極活物質粒子を製造した。
エタノール8gに前記実施例2で製造した正極活物質コーティング溶液2gを添加して攪拌しつつ、正極活物質(LiNi0.6Mn0.2Co0.2)O2)50gを添加してペースト状態に撹拌した。攪拌されたペーストを180℃で2時間乾燥した後、500℃の空気中で1時間熱処理し、約0.2重量%のジルコニウムオキシド層が被覆された正極活物質粒子を製造した。
エタノール8gに前記実施例3で製造した正極活物質コーティング溶液2gを添加して攪拌しつつ、正極活物質(LiNi0.6Mn0.2Co0.2)O2)50gを添加してペースト状態に撹拌した。攪拌されたペーストを180℃で2時間乾燥した後、700℃の空気中で1時間熱処理し、約0.2重量%のマンガンオキシド層が被覆された正極活物質粒子を製造した。
Claims (12)
- グリコール系溶媒内に金属前駆体及びキレート剤を分散させて混合溶液を製造する段階;
前記混合溶液を1次加熱する段階;及び
前記混合溶液を2次加熱する段階を含む二次電池用正極活物質粒子コーティング用溶液の製造方法であって、
前記コーティング溶液は、金属前駆体から脱離された金属とグリコール系溶媒及びキレート剤が結合された金属有機化合物を含む金属グリコレート溶液であり、
前記1次加熱段階は、110から230℃の温度条件下で5から20時間の間実施し、
前記2次加熱段階は、150から300℃の温度で1から5時間の間実施することを特徴とする二次電池用正極活物質粒子コーティング用溶液の製造方法。 - 前記グリコール系溶媒はエチレングリコール、プロピレングリコール、ジエチレングリコール、トリエチレングリコール及びポリエチレングリコールからなる群から選択された単一物または2種以上の混合物を含むことを特徴とする請求項1に記載の二次電池用正極活物質粒子コーティング用溶液の製造方法。
- 前記金属前駆体はMg、Ca、Sr、Ba、Y、Ti、Zr、V、Nb、Ta、Cr、Mo、W、Mn、Fe、Co、Ir、Ni、Zn、Al、Ga、In、Si、Ge、Sn、La及びCeからなる群から選択された金属を少なくとも一つ以上含有するアセテート、ヒドロキシド、ニトラート、ニトリド、スルファート、スルフィド、アルコキシド及びハライドからなる群から選択された単一物または2種以上の混合物を含むことを特徴とする請求項1に記載の二次電池用正極活物質粒子コーティング用溶液の製造方法。
- 前記金属前駆体はアルミニウムアセテート、ジルコニウムニトリドまたはマンガンアセテートであることを特徴とする請求項3に記載の二次電池用正極活物質粒子コーティング用溶液の製造方法。
- 前記キレート剤は、クエン酸、EDTA(ethylenediaminetetraacetic acid)、シュウ酸及びグルコン酸からなる群から選択された単一物または2種以上の混合物を含むことを特徴とする請求項1に記載の二次電池用正極活物質粒子コーティング用溶液の製造方法。
- 前記金属前駆体:グリコール系溶媒:キレート剤の含量比(重量部)は、1:1から500:0.1から20であることを特徴とする請求項1に記載の二次電池用正極活物質粒子コーティング用溶液の製造方法。
- 前記混合溶液の製造時に添加剤をさらに含むことを特徴とする請求項1に記載の二次電池用正極活物質粒子コーティング用溶液の製造方法。
- 前記添加剤は、ホルムアルデヒド、アセトアルデヒド及びグリコ酸からなる群から選択された単一物または2種以上の混合物を含むことを特徴とする請求項7に記載の二次電池用正極活物質粒子コーティング用溶液の製造方法。
- 前記添加剤は、前記金属前駆体の全体1重量部に対し0.1から20重量部で含むことを特徴とする請求項7に記載の二次電池用正極活物質粒子コーティング用溶液の製造方法。
- 前記2次加熱段階は、170から250℃の温度で1から5時間の間実施することを特徴とする請求項1に記載の二次電池用正極活物質粒子コーティング用溶液の製造方法。
- 前記1次及び2次加熱段階は、非活性ガス雰囲気下で実施することを特徴とする請求項1に記載の二次電池用正極活物質粒子コーティング用溶液の製造方法。
- 前記金属グリコレート溶液は、下記化学式(1)から(3)で表される化合物からなる群から選択された少なくとも一つの金属有機化合物を含むことを特徴とする請求項1に記載の二次電池用正極活物質粒子コーティング用溶液の製造方法。
[化1]
M(C2H5O2)n (1)
[化2]
M(C6H(8−n)O7) (2)
[化3]
M(C6H(8−n)O7)(C2H5O2) (3)
(前記式で、Mは金属前駆体から脱離された金属であって、Mg、Ca、Sr、Ba、Y、Ti、Zr、V、Nb、Ta、Cr、Mo、W、Mn、Fe、Co、Ir、Ni、Zn、Al、Ga、In、Si、Ge、Sn、La及びCeからなる群から選ばれた少なくとも一つの金属であり、nは1から4の整数である。)
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