JP6048711B2 - 多結晶リチウムマンガン酸化物粒子、その製造方法及びこれを含む正極活物質、正極、およびリチウム二次電池 - Google Patents
多結晶リチウムマンガン酸化物粒子、その製造方法及びこれを含む正極活物質、正極、およびリチウム二次電池 Download PDFInfo
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- JP6048711B2 JP6048711B2 JP2015528424A JP2015528424A JP6048711B2 JP 6048711 B2 JP6048711 B2 JP 6048711B2 JP 2015528424 A JP2015528424 A JP 2015528424A JP 2015528424 A JP2015528424 A JP 2015528424A JP 6048711 B2 JP6048711 B2 JP 6048711B2
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- Prior art keywords
- manganese oxide
- oxide particles
- lithium manganese
- polycrystalline
- polycrystalline lithium
- Prior art date
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- 239000002245 particle Substances 0.000 title claims description 137
- 229910002102 lithium manganese oxide Inorganic materials 0.000 title claims description 100
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 title claims description 99
- 238000004519 manufacturing process Methods 0.000 title claims description 37
- 229910052744 lithium Inorganic materials 0.000 title claims description 29
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 26
- 239000007774 positive electrode material Substances 0.000 title claims description 18
- 239000011572 manganese Substances 0.000 claims description 86
- 239000002243 precursor Substances 0.000 claims description 37
- 239000013078 crystal Substances 0.000 claims description 34
- 229910052748 manganese Inorganic materials 0.000 claims description 34
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 33
- 239000011734 sodium Substances 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 30
- 238000005245 sintering Methods 0.000 claims description 28
- -1 aluminum compound Chemical class 0.000 claims description 18
- 239000011164 primary particle Substances 0.000 claims description 18
- 239000011163 secondary particle Substances 0.000 claims description 16
- 238000002441 X-ray diffraction Methods 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 12
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 10
- 150000003388 sodium compounds Chemical class 0.000 claims description 9
- 150000001639 boron compounds Chemical class 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 claims description 3
- 150000001869 cobalt compounds Chemical class 0.000 claims description 3
- 150000002259 gallium compounds Chemical class 0.000 claims description 3
- 150000002604 lanthanum compounds Chemical class 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 150000003682 vanadium compounds Chemical class 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 150000003755 zirconium compounds Chemical class 0.000 claims description 3
- 229910013553 LiNO Inorganic materials 0.000 claims description 2
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 229910052810 boron oxide Inorganic materials 0.000 claims description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 2
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical group [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 2
- 229910001386 lithium phosphate Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 claims description 2
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 150000003748 yttrium compounds Chemical class 0.000 claims description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims 4
- 229910018119 Li 3 PO 4 Inorganic materials 0.000 claims 1
- KLARSDUHONHPRF-UHFFFAOYSA-N [Li].[Mn] Chemical compound [Li].[Mn] KLARSDUHONHPRF-UHFFFAOYSA-N 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 16
- 238000000034 method Methods 0.000 description 14
- 238000010828 elution Methods 0.000 description 13
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 11
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 10
- 239000002002 slurry Substances 0.000 description 9
- 239000003792 electrolyte Substances 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 7
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- 230000008859 change Effects 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 7
- 239000007773 negative electrode material Substances 0.000 description 7
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- 238000006243 chemical reaction Methods 0.000 description 5
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
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- 239000000126 substance Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229920000049 Carbon (fiber) Polymers 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000004917 carbon fiber Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
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- 239000010936 titanium Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
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- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000011244 liquid electrolyte Substances 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 229910001437 manganese ion Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 2
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- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- AJELVSDAOKZZHZ-UHFFFAOYSA-N calcium;dioxido(oxo)silane;zirconium(4+) Chemical compound [Ca+2].[Zr+4].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O AJELVSDAOKZZHZ-UHFFFAOYSA-N 0.000 description 1
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- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical group 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Description
実施例1
Li2CO3 37.50g、10μmの平均粒径を有する(Mn0.95Al0.05)3O4 141.88g、焼結補助剤としてNa2CO3 0.62g(0.01mol)をミキサー(Waring blender)に入れ、前記ミキサーの中心部rpmが18000rpmで、1分間混合した。前記混合された粉末を500ccのアルミナるつぼに入れて約800℃で4時間の間、大気(Air)雰囲気で焼成を行った。焼成後得たケーキ(cake)を乳ばちで粉砕した後、400メッシュ篩(sieve)を利用して分級を実施しLi(1.09)Mn1.80Al0.1Na0.01O4を得た。前記Li(1.09)Mn1.80Al0.1Na0.01O4は200nmの結晶の大きさを有する二つ以上の結晶粒子(一次粒子)が集まってなる二次粒子であって、前記二次粒子の平均粒径は1.05μmであった。
Na2CO3の量を0.62g(0.01mol)に代えて1.24g(0.02mol)を用いたことを除き、前記実施例1と同様の方法で行ってLi(1.09)Mn1.80Al0.1Na0.01O4を得た。
焼結補助剤としてNa2CO3を添加しないことを除き、前記実施例1と同様の方法で行ってLi(1.09)Mn1.81Al0.1O4を得た。
10μmの平均粒径を有する(Mn0.995Al0.005)3O4に代えて5μmの平均粒径を有する(Mn0.995Al0.005)3O4を用い、焼結補助剤としてNa2CO3を添加しないことを除き、前記実施例1と同様の方法で行ってLi(1.09)Mn1.81Al0.1O4を得た。
10μmの平均粒径を有する(Mn0.995Al0.005)3O4に代えて5μmの平均粒径を有する(Mn0.995Al0.005)3O4を用いたことを除き、前記実施例1と同様の方法で行ってLi(1.09)Mn1.80Al0.1Na0.01O4を得た。
マンガン前駆体として多結晶(Mn0.995Al0.005)3O4を用いる代わりに単結晶Mn3O4を用いたことを除き、前記実施例1と同様の方法で行ってLi(1.09)Mn1.9Na0.01O4を得た。
前記Li(1.09)Mn1.9Na0.01O4は一次粒子の形態で粒径が10μmであった。
実施例3
正極の製造
前記実施例1で製造された多結晶リチウムマンガン酸化物粒子を正極活物質として用いた。
負極活物質として炭素粉末96.3重量%、導電剤としてsuper−p 1.0重量%及びバインダとしてスチレンブタジエンゴム(SBR)及びカルボキシメチルセルロース(CMC)を1.5重量%と1.2重量%で混合し、溶媒であるNMPに添加して負極活物質スラリーを製造した。前記負極活物質スラリーを厚さが10μmの負極集電体である銅(Cu)薄膜に塗布し、乾燥して負極を製造した後、ロールプレス(roll press)を行って負極を製造した。
一方、電解質としてエチレンカーボネート及びジエチルカーボネートを30:70の体積比で混合して製造された非水電解液溶媒にLiPF6を添加して、1MのLiPF6非水性電解液を製造した。
このように製造された正極と負極を、ポリエチレンとポリプロピレンの混合セパレータを介在させ、通常の方法でポリマー型電池を製作した後、製造された前記非水性電解液を注液してリチウム二次電池の製造を完成した。
前記実施例2で製造された多結晶リチウムマンガン酸化物粒子をそれぞれ正極活物質として用いたことを除き、実施例3と同様の方法でリチウム二次電池を製造した。
前記比較例1から4で製造されたリチウムマンガン酸化物粒子をそれぞれ正極活物質として用いたことを除き、実施例3と同様の方法でリチウム二次電池を製造した。
前記実施例1で製造された多結晶リチウムマンガン酸化物粒子、及び比較例4で製造されたリチウムマンガン酸化物粒子に対しそれぞれSEM顕微鏡写真を確認し、その結果をそれぞれ図1及び図2に示した。
実施例1と2、及び比較例1から3で製造された多結晶リチウムマンガン酸化物粒子に対しX線回折分析(D4 Endeavor、Bruker)を行った。その結果を下記表1及び図3に示した。
実施例3と4、及び比較例5から8で製造されたリチウム二次電池を定電流/定電圧(CC/CV)条件で、(電池容量3.4mAh)を2Cの定電流(CC)で充電し、その後、定電圧(CV)で充電して充電電流が0.17mAhになるまで1回目の充電を行った。その後20分間放置した後、0.1Cの定電流で10mVになるまで放電して1サイクル目の放電容量を測定した。引続き、各電池に対して前記充電及び放電を繰り返して行って容量を測定し、これを下記表2に示した。
実施例1と2、及び比較例1から3の多結晶リチウムマンガン酸化物粒子に対し、XRD結晶分析により粒子の結晶の大きさを測定した。
Claims (29)
- 前記式(1)において、前記fの範囲は0.001≦f≦0.03である請求項1に記載の多結晶リチウムマンガン酸化物粒子。
- 前記式(1)において、前記混合元素はB、Co、V、La、Ti、Ni、Zr、Y及びGaからなる群より選択されたいずれか一つ、またはこれらのうち2種以上の混合元素を含む請求項1または請求項2に記載の多結晶リチウムマンガン酸化物粒子。
- 前記式(1)において、前記MはNa、またはNa及びBの混合元素である請求項3に記載の多結晶リチウムマンガン酸化物粒子。
- 前記二次粒子の平均粒径D50は、5μmから20μmの範囲である請求項1から請求項4の何れか一項に記載の多結晶リチウムマンガン酸化物粒子。
- 前記多結晶リチウムマンガン酸化物粒子のうちNaの元素の量は、700ppmから3000ppmである請求項1から請求項5の何れか一項に記載の多結晶リチウムマンガン酸化物粒子。
- 前記リチウムマンガン酸化物粒子は、X線回折分析(X−ray diffraction)測定時にI(111)/I(111)ピーク強度比を100%に定義する場合、I(311)/I(111)が40%以上である請求項1から請求項6の何れか一項に記載の多結晶リチウムマンガン酸化物粒子。
- 前記リチウムマンガン酸化物粒子は、X線回折分析(X−ray diffraction)測定時にI(111)/I(111)ピーク強度比を100%に定義する場合、I(400)/I(111)が40%以上で、I(440)/I(111)が20%以上である請求項1から請求項7の何れか一項に記載の多結晶リチウムマンガン酸化物粒子。
- 前記リチウムマンガン酸化物粒子は、X線回折分析(X−ray diffraction)測定時に(311)ピークの半値幅(Full Width at Half−Maximum;FWHM)が0.3度以下である請求項1から請求項8の何れか一項に記載の多結晶リチウムマンガン酸化物粒子。
- 前記リチウムマンガン酸化物粒子の比表面積(BET)は、0.5m2/g以下である請求項1から請求項9の何れか一項に記載の多結晶リチウムマンガン酸化物粒子。
- 前記多結晶マンガン前駆体は100nmから300nm範囲の平均の結晶の大きさを有する二つ以上の一次粒子が凝集されて形成された二次粒子の形態である請求項11に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記二次粒子の平均粒径D50は、9μmから25μmである請求項12に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記二次粒子の平均粒径D50は、9μmから15μmである請求項13に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記多結晶マンガン前駆体は、Alを0.01重量%から10重量%で含む請求項11から請求項14の何れか一項に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記多結晶マンガン前駆体は、(Mn(1−y)Aly)3O4 (0<y≦0.2)を含む請求項15に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記多結晶マンガン前駆体は、MnCO3、Mn3O4、MnSO4及びMn2O3からなる群より選択されたいずれか一つ、またはこれらのうち2種以上の混合物をアルミニウム化合物とともに共沈させて形成されたものである請求項16に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記アルミニウム化合物は、Al 2 (SO4 ) 3 、AlCl 3 及びAl(NO3 ) 3 からなる群より選択されたいずれか一つ、またはこれらのうち2種以上の混合物である請求項17に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記焼結補助剤は、ナトリウム化合物を含む請求項11から請求項18の何れか1項に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記焼結補助剤は、ホウ素化合物、コバルト化合物、バナジウム化合物、ランタン化合物、ジルコニウム化合物、イットリウム化合物及びガリウム化合物からなる群より選択されたいずれか一つ、またはこれらのうち2種以上の混合物をさらに含む請求項19に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記焼結補助剤は、ナトリウム化合物、またはナトリウム化合物とホウ素化合物の混合物である請求項19に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記ナトリウム化合物は、炭酸ナトリウム、珪酸ナトリウム、水酸化ナトリウムまたはこれらの2種以上の混合物である請求項19から請求項21の何れか一項に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記ホウ素化合物はホウ酸、四ホウ酸リチウム、酸化ホウ素及びホウ酸アンモニウムからなる群より選択されたいずれか一つ、またはこれらのうち2種以上の混合物である請求項21に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記焼結補助剤は、多結晶マンガン前駆体の総重量に対して0.2重量%から2重量%の量で用いられる請求項11から請求項23の何れか一項に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記焼成は、700℃から1000℃の温度で行われる請求項11から請求項24の何れか一項に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 前記リチウム前駆体は塩化リチウム(LiCl)、炭酸リチウム(Li2CO3)、水酸化リチウム(LiOH)、リン酸リチウム(Li3PO4)及び硝酸リチウム(LiNO3)からなる群より選択されたいずれか一つ、またはこれらのうち2種以上の混合物である請求項11から請求項25の何れか一項に記載の多結晶リチウムマンガン酸化物粒子の製造方法。
- 請求項1から請求項10の何れか一項に記載の多結晶リチウムマンガン酸化物粒子を含む正極活物質。
- 請求項27に記載の正極活物質を含む正極。
- 請求項28に記載の正極を含むリチウム二次電池。
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