CN105264695B - 制备锂二次电池用正极活性材料的方法 - Google Patents
制备锂二次电池用正极活性材料的方法 Download PDFInfo
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- CN105264695B CN105264695B CN201480032440.3A CN201480032440A CN105264695B CN 105264695 B CN105264695 B CN 105264695B CN 201480032440 A CN201480032440 A CN 201480032440A CN 105264695 B CN105264695 B CN 105264695B
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- lithium
- metal oxide
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- positive electrode
- secondary battery
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- 238000000034 method Methods 0.000 title claims abstract description 46
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- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims abstract description 11
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- 150000002641 lithium Chemical class 0.000 claims abstract description 3
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- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
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- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
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- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 125000001841 imino group Chemical group [H]N=* 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- YADSGOSSYOOKMP-UHFFFAOYSA-N lead dioxide Inorganic materials O=[Pb]=O YADSGOSSYOOKMP-UHFFFAOYSA-N 0.000 description 1
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 229910001547 lithium hexafluoroantimonate(V) Inorganic materials 0.000 description 1
- 229910001540 lithium hexafluoroarsenate(V) Inorganic materials 0.000 description 1
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
- 229910001537 lithium tetrachloroaluminate Inorganic materials 0.000 description 1
- HSFDLPWPRRSVSM-UHFFFAOYSA-M lithium;2,2,2-trifluoroacetate Chemical compound [Li+].[O-]C(=O)C(F)(F)F HSFDLPWPRRSVSM-UHFFFAOYSA-M 0.000 description 1
- VROAXDSNYPAOBJ-UHFFFAOYSA-N lithium;oxido(oxo)nickel Chemical compound [Li+].[O-][Ni]=O VROAXDSNYPAOBJ-UHFFFAOYSA-N 0.000 description 1
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- RWHJVIIQVLECOW-UHFFFAOYSA-N lithium;pyridine Chemical compound [Li].C1=CC=NC=C1 RWHJVIIQVLECOW-UHFFFAOYSA-N 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 239000011356 non-aqueous organic solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000379 polypropylene carbonate Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
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- 238000006277 sulfonation reaction Methods 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229920006027 ternary co-polymer Polymers 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1228—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [MnO2]n-, e.g. LiMnO2, Li[MxMn1-x]O2
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- C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
- C01G45/1257—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3 containing lithium, e.g. Li2MnO3, Li2[MxMn1-xO3
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- C01G51/50—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese of the type [MnO2]n-, e.g. Li(CoxMn1-x)O2, Li(MyCoxMn1-x-y)O2
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Abstract
本发明提供了一种制备锂二次电池用正极活性材料的方法，所述方法包括：对选自由以下化合物(1)表示的化合物中的至少一种锂过渡金属氧化物进行预活化的过程；和对所述预活化的锂过渡金属氧化物的表面进行改性的过程：(1‑x)LiM’O2‑yAy‑xLi2MnO3‑y’Ay’(1)，其中M’是MnaMb；M是选自如下的至少一种：Ni、Ti、Co、Al、Cu、Fe、Mg、B、Cr、Zr、Zn和周期表中的第2周期过渡金属；A是选自PO4、BO3、CO3、F和NO3的阴离子中的至少一种；0<x<1；0<y≤0.02；0<y’≤0.02；0.5≤a≤1.0；0≤b≤0.5；且a+b＝1。
Description
技术领域
本发明涉及一种制备锂二次电池用正极活性材料的方法。
背景技术
随着移动装置技术持续发展和对其的需求持续增加，对作为能源的二次电池的需求快速增长。在这些二次电池中，表现出高能量密度和工作电位并具有长循环寿命和低自放电率的锂二次电池是可商购的并被广泛使用。
另外，随着对环境问题关注的增加，对于可以取代作为空气污染主要原因之一的使用化石燃料的车辆如汽油车辆、柴油车辆等的电动车辆(EV)、混合动力电动车辆(HEV)等的研究正在积极进行。作为EV、HEV等的电源，主要使用镍-金属氢化物(Ni-MH)二次电池。然而，对于具有高能量密度、高放电电压和高输出稳定性的锂二次电池的研究在积极进行且一些锂二次电池是可商购的。
锂二次电池具有其中电极组件浸渍有含锂盐的非水电解质的结构，所述电极组件包括：通过将正极活性材料涂布在正极集电器上而制备的正极、通过将负极活性材料涂布在负极集电器上而制备的负极以及设置在所述正极与所述负极之间的多孔隔膜。
作为这种锂二次电池用正极活性材料，主要使用含锂的钴氧化物如LiCoO2。除此之外，也在考虑使用含锂的锰氧化物如具有层状晶体结构的LiMnO2、具有尖晶石结构的LiMn2O4等以及含锂的镍氧化物如LiNiO2。
LiCoO2因优异的总体物理性能如优异的循环性能等而被广泛使用，但安全性低。另外，由于作为原料的钴的资源限制，LiCoO2是昂贵的且其作为诸如电动车辆等领域中的电源的大量使用由此受到限制。由于LiNiO2的制备方法的特性，难以以合理开支大量制造LiNiO2。
另一方面，锂锰氧化物如LiMnO2、LiMn2O4等的优点在于，其包含丰富且环境友好的原料Mn，由此作为可替代LiCoO2的正极活性材料引起了许多关注。然而，这种锂锰氧化物还具有诸如循环特性差等的缺点。
首先，LiMnO2具有诸如初始容量低等的缺点。特别地，LiMnO2在达到恒定容量之前需要数十次的充放电循环。另外，随着循环次数的增加，LiMn2O4的容量减少变得严重，且特别是在50℃以上的高温下，由于电解液的分解、锰的溶出等，循环特性快速劣化。
同时，作为含锂的锰氧化物，除了LiMnO2和LiMn2O4还有Li2MnO3。由于Li2MnO3的结构稳定性是优异的但其是电化学无活性的，所以Li2MnO3自身不能用作二次电池的正极活性材料。因此，一些现有技术提出了使用Li2MnO3与LiMO2(M＝Co、Ni、Ni0.5Mn0.5、Mn)的固溶体作为正极活性材料的技术。在这种正极活性材料固溶体中，Li和O在4.4V的高电压下从晶体结构脱离，并由此显示出电化学活性。然而，存在如下问题，例如在高电压下电解液分解和产生气体的可能性高，需大量使用相对昂贵的材料如LiMO2(M＝Co、Ni、Ni0.5Mn0.5、Mn)等。
另外，含锂的锰氧化物具有低的导电性，由此取决于粒度而具有大的电阻差异。另外，当其在4.4V以上的高电压下实施其活化以便显示高容量时，Li2O从Li2MnO3脱离，由此可能发生结构变化。而且，由于含锂的锰氧化物的晶体结构特性，难以确保期望的稳定性并在预期提高的能量密度方面受到限制。
另外，主要将碳系材料用作锂二次电池用负极。然而，碳系材料具有相对于锂为0V的低电位，由此造成电解质的还原，从而产生气体。为了解决该问题，将具有相对高电位的金属氧化物用作负极活性材料。
然而，在此情况中，在活化和充放电过程期间产生大量气体，并由此促进电解质的副反应，从而降低二次电池的安全性。
因此，需要开发一种能够解决上述问题的技术。
发明内容
技术问题
因此，完成了本发明以解决以上和其它尚未解决的技术问题。
本发明旨在提供通过包括预活化工序而制造可抑制其它副反应的锂二次电池的方法，其中以原料状态进行其中将金属氧化物的氧原子还原至活性气体状态的过程，从而在其中锂从正极活性材料中脱离的充电期间，根据金属的氧化数的增加来调节电荷均衡，由此可以提高电池性能。
技术方案
根据本发明的一个方面，提供一种制备锂二次电池用正极活性材料的方法，所述方法包括：对选自由下式(1)表示的化合物中的至少一种锂过渡金属氧化物进行预活化；和对所述预活化的锂过渡金属氧化物的表面进行改性：
(1-x)LiM’O2-yAy-xLi2MnO3-y’Ay’(1)，
其中M’是MnaMb；
M是选自如下的至少一种：Ni、Ti、Co、Al、Cu、Fe、Mg、B、Cr、Zr、Zn和第II周期过渡金属；
A是选自阴离子如PO4、BO3、CO3、F和NO3中的至少一种；且
0<x<1；0<y≤0.02；0<y’≤0.02；0.5≤a≤1.0；0≤b≤0.5；且a+b＝1。
所述预活化可以包括化学脱锂过程。
在化学脱锂过程中，可以进行与锂吸附剂的反应，所述锂吸附剂包括BF4盐和/或铵盐。所述预活化可以包括高温脱锂过程。
所述高温脱锂过程可以包括在250℃以上的温度下对所述锂过渡金属氧化物进行热处理。
所述高温脱锂过程可以包括在300℃以上的温度下对所述锂过渡金属氧化物进行热处理。
所述高温脱锂过程可以包括在400℃以上的温度下对所述锂过渡金属氧化物进行热处理。
根据选自如下的至少一种方法进行所述改性：原子层沉积(ALD)法、机械研磨法、湿法、化学气相沉积(CVD)法和等离子体化学气相沉积(PCVD)法。
另外，本发明可以提供一种通过所述方法制备的正极活性材料。
另外，本发明可以提供一种包括所述正极活性材料的电池。
电池通常由正极、负极、设置在正极与负极之间的隔膜以及含锂盐的非水电解质构成。下面将对锂二次电池的其它成分进行说明。
通常，通过将包括正极活性材料、导电材料和粘结剂的混合物作为电极混合物涂布到正极集电器上，然后对其干燥来制备正极，根据需要，所述混合物可还包括填料。
除了由式1表示的电极活性材料之外，所述正极活性材料的实例还包括：层状化合物如锂钴氧化物(LiCoO2)和锂镍氧化物(LiNiO2)，或被一种或多种过渡金属取代的化合物；锂锰氧化物如式Li1+xMn2-xO4的化合物，其中0≤x≤0.33，LiMnO3，LiMn2O3，LiMnO2；锂铜氧化物(Li2CuO2)；钒氧化物如LiV3O8、LiV3O4、V2O5和Cu2V2O7；具有式LiNi1-xMxO2的Ni位点型锂镍氧化物，其中M＝Co、Mn、Al、Cu、Fe、Mg、B或Ga，且0.01≤x≤0.3；具有式LiMn2-xMxO2的锂锰复合氧化物，其中M＝Co、Ni、Fe、Cr、Zn或Ta，且0.01≤x≤0.1，或具有式Li2Mn3MO8的锂锰复合氧化物，其中M＝Fe、Co、Ni、Cu或Zn；由LiNixMn2-xO4表示的尖晶石结构的锂锰复合氧化物；其中一些Li原子被碱土金属离子取代的LiMn2O4；二硫化物化合物；以及Fe2(MoO4)3，但本发明不限制于此。
通常将正极集电器制成3～500μm的厚度。正极集电器没有特别限制，只要其在制造的二次电池中不会引起化学变化并具有高导电性即可。例如，正极集电器可以由不锈钢，铝，镍，钛，烧结碳，或经碳、镍、钛、银等表面处理的铝或不锈钢制成。正极集电器在其表面具有微细的不规则处，从而提高正极活性材料与正极集电器之间的粘附性。另外，可以以包括膜、片、箔、网、多孔结构、泡沫和无纺布的各种形式中的任一种使用正极集电器。
相对于包含正极活性材料的混合物的总重量，通常以1～50重量％的量添加导电材料。对导电材料没有特别限制，只要其在制造的电池中不会引起化学变化并具有导电性即可。导电材料的实例包括：石墨如天然石墨或人造石墨；炭黑类如炭黑、乙炔黑、科琴黑、槽法炭黑、炉黑、灯黑和热裂法炭黑；导电纤维如碳纤维和金属纤维；金属粉末如氟化碳粉末、铝粉末和镍粉末；导电晶须如氧化锌和钛酸钾；导电金属氧化物如氧化钛；和聚亚苯基衍生物。
同时，具有弹性的石墨系材料可被用作导电材料，且上面列出的材料可以与石墨系材料一起使用。
粘结剂是有助于活性材料与导电材料之间的粘结并有助于电极活性材料对集电器的粘结的成分。相对于包含正极活性材料的混合物的总重量，通常以1～50重量％的量添加粘结剂。粘结剂的实例包括聚偏二氟乙烯、聚乙烯醇、羧甲基纤维素(CMC)、淀粉、羟丙基纤维素、再生纤维素、聚乙烯基吡咯烷酮、四氟乙烯、聚乙烯、聚丙烯、乙烯-丙烯-二烯三元共聚物(EPDM)、磺化的EPDM、丁苯橡胶、氟橡胶和各种共聚物。
填料任选地用作抑制正极膨胀的成分。填料没有特别限制，只要其是在制造的电池中不引起化学变化的纤维材料即可。填料的实例包括烯烃系聚合物如聚乙烯和聚丙烯；和纤维材料如玻璃纤维和碳纤维。
通过在负极集电器上涂布、干燥并压制负极活性材料来制造负极，根据需要，可还选择性地包括导电材料、粘结剂、填料等。
负极活性材料可以还包括例如：碳如硬碳、石墨系碳；金属复合氧化物如LixFe2O3(0≤x≤1)、LixWO2(其中0≤x≤1)、SnxMe1-xMe’yOz(其中Me：Mn、Fe、Pb或Ge；Me’：Al，B，P，Si，第I族、第II族和第III族元素，或卤素；0<x≤1；1≤y≤3；且1≤z≤8)；锂金属；锂合金；硅系合金；锡系合金；金属氧化物如SnO、SnO2、PbO、PbO2、Pb2O3、Pb3O4、Sb2O3、Sb2O4、Sb2O5、GeO、GeO2、Bi2O3、Bi2O4和Bi2O5；导电聚合物如聚乙炔；Li-Co-Ni系材料；钛氧化物；锂钛氧化物等，特别是碳系材料和/或Si。
典型地将负极集电器制成3～500μm的厚度。负极集电器没有特别限制，只要其在制造的二次电池中不引起化学变化并具有导电性即可。例如，负极集电器可以由铜，不锈钢，铝，镍，钛，烧结碳，经碳、镍、钛或银表面处理的铜或不锈钢，和铝-镉合金制成。与正极集电器类似，负极集电器可还在其表面具有微细的不规则处，从而提高负极集电器与负极活性材料之间的粘附性。另外，可以以包括膜、片、箔、网、多孔结构、泡沫和无纺布的各种形式使用负极集电器。
将隔膜设置在正极与负极之间。作为隔膜，使用具有高离子渗透率和高机械强度的绝缘薄膜。隔膜的孔径通常为0.01～10μm且其厚度通常为5～300μm。这种隔膜的实例包括由具有耐化学性和疏水性的烯烃类聚合物如聚丙烯、玻璃纤维或聚乙烯制成的片或无纺布，牛皮纸等。当固体电解质被用作电解质时，所述固体电解质还起隔膜的作用。
所述含锂盐的非水电解质由非水电解质和锂构成，非水电解质的实例包括非水有机溶剂、有机固体电解质、无机固体电解质等，但本发明不限于此。
非水有机溶剂的实例包括非质子有机溶剂，如N-甲基-2-吡咯烷酮、碳酸亚丙酯、碳酸亚乙酯、碳酸亚丁酯、碳酸二甲酯、碳酸二乙酯、γ-丁内酯、1,2-二甲氧基乙烷、四氢呋喃、2-甲基四氢呋喃、二甲亚砜、1,3-二氧戊环、甲酰胺、二甲基甲酰胺、二氧戊环、乙腈、硝基甲烷、甲酸甲酯、乙酸甲酯、磷酸三酯、三甲氧基甲烷、二氧戊环衍生物、环丁砜、甲基环丁砜、1,3-二甲基-2-咪唑烷酮、碳酸亚丙酯衍生物、四氢呋喃衍生物、醚、丙酸甲酯、丙酸乙酯等。
有机固体电解质的实例包括但不限于聚乙烯衍生物、聚环氧乙烷衍生物、聚环氧丙烷衍生物、磷酸酯聚合物、聚搅拌赖氨酸、聚酯硫化物、聚乙烯醇、聚偏二氟乙烯和含有离子离解基团的聚合物。
无机固体电解质的实例包括但不限于锂(Li)的氮化物、卤化物和硫酸盐如Li3N、LiI、Li5NI2、Li3N-LiI-LiOH、LiSiO4、LiSiO4-LiI-LiOH、Li2SiS3、Li4SiO4、Li4SiO4-LiI-LiOH和Li3PO4-Li2S-SiS2。
锂盐是易溶于非水电解质中的材料且其实例包括但不限于LiCl、LiBr、LiI、LiClO4、LiBF4、LiB10Cl10、LiPF6、LiCF3SO3、LiCF3CO2、LiAsF6、LiSbF6、LiAlCl4、CH3SO3Li、(CF3SO2)2NLi、氯硼烷锂、低级脂肪族羧酸锂、四苯基硼酸锂和亚氨基锂。
另外，为了提高充/放电特性和阻燃性，可以向含锂盐的非水电解质中添加例如吡啶、亚磷酸三乙酯、三乙醇胺、环醚、乙二胺、正甘醇二甲醚、六磷酸三酰胺、硝基苯衍生物、硫、醌亚胺染料、N-取代的唑烷酮、N,N-取代的咪唑烷、乙二醇二烷基醚、铵盐、吡咯、2-甲氧基乙醇和三氯化铝。如果需要，为了赋予不燃性，电解质可还包括含卤素的溶剂如四氯化碳和三氟乙烯。此外，为了提高高温储存特性，所述电解质可还包括二氧化碳气体、氟代碳酸亚乙酯(FEC)、丙烯磺酸内酯(PRS)、氟代碳酸亚丙酯(FPC)等。
在一个具体实施方式中，通过将锂盐如LiPF6、LiClO4、LiBF4或LiN(SO2CF3)2添加到包括作为高介电溶剂和环状碳酸酯的EC或PC与作为低粘度溶剂和线性碳酸酯的DEC、DMC或EMC的混合溶剂，可以制备含锂盐的非水电解质。
本发明提供一种包括所述二次电池作为单元电池的电池模块、包括所述电池模块的电池组以及包括所述电池组作为电源的装置。
此处，所述装置的具体实例包括但不限于电动马达驱动的电动工具；电动车辆(EV)，混合动力电动车辆(HEV)和插电式混合动力电动车辆(PHEV)；电动双轮车辆如电动自行车和电动滑板车；电动高尔夫球车；和用于储电的系统。
具体实施方式
现在，将参考实施例更详细地说明本发明。这些实例仅为了说明目的而提供，且不应解释为限制本发明的范围和主旨。
<实施例1>
正极的制备
将Li(Li1.2Co0.1Ni0.1Mn0.6)O2用作正极活性材料，将包含溶于其中的2.0g BF4的100ml溶液添加到正极活性材料中并混合。将混合溶液在250℃下热处理并然后通过用水洗涤和真空干燥进行脱锂。随后，使用机械研磨进行表面改性过程，由此制备正极活性材料。
将制备的正极活性材料、作为导电材料的炭黑和作为粘结剂的PVdF以90:5:5的重量比添加到N-甲基-2-吡咯烷酮(NMP)，并混合，由此制备正极混合物。在作为正极集电器的厚度为20μm的铝箔上，将制备的正极混合物涂布至40μm的厚度，随后压制并干燥。结果，制备了正极。
负极的制备
将作为负极的天然石墨、作为导电材料的炭黑和作为粘结剂的PVdF以90:5:5的重量比添加到N-甲基-2-吡咯烷酮(NMP)，并混合，由此制备负极混合物。
使用10μm的铜箔，并在负极集电器上将制备的负极混合物涂布至40μm的厚度。随后进行压制和干燥，由此制备负极。
二次电池的制造
通过将隔膜(Toray，厚度：15μm)设置在负极与正极之间制造电极组件。随后，将电极组件容纳在袋型电池壳中，并向其中添加锂非水电解液，所述非水电解液包括以1:1:1的体积比混合的碳酸乙酯:碳酸二甲酯:碳酸甲乙酯和作为锂盐的1M LiPF6的混合物，由此制造锂二次电池。
<实施例2>
以与实施例1中相同的方式制造了锂二次电池，不同之处在于，在正极活性材料的脱锂过程中，在300℃下进行热处理。
<实施例3>
以与实施例1中相同的方式制造了锂二次电池，不同之处在于，在正极活性材料的脱锂过程中，在400℃下进行热处理。
<比较例1>
以与实施例1中相同的方式制造了锂二次电池，不同之处在于，在制备正极活性材料的过程中，不进行脱锂过程和表面改性过程。
<比较例2>
以与实施例1中相同的方式制造了锂二次电池，不同之处在于，在制备正极活性材料的过程中，不进行脱锂过程。
<比较例3>
以与实施例1中相同的方式制造了锂二次电池，不同之处在于，在制备正极活性材料的过程中，不进行表面改性过程。
<实验例1>
将实施例1～3和比较例1～3的二次电池在0.1C和5mA下充电至高达3.35V，并在室温下储存两天和在60℃下储存一天。随后，在93kPa下将副反应气体去除过程进行30秒至1分钟，然后在0.5C下进行充电至高达4.3V。随后，进行恒压充电直至0.05C并在0.5C下进行放电直至2.5V。将这种充放电在45℃下进行250个循环并然后测量气体生成量。将结果总结于下表1中。
<表1>
| 气体生成量(μl) | |
| 实施例1 | 10471 |
| 实施例2 | 10415 |
| 实施例3 | 10350 |
| 比较例1 | 12850 |
| 比较例2 | 12650 |
| 比较例3 | 11030 |
如表1中所示，能够确认，当与比较例1的电池相比时，在根据本发明的实施例1～3的二次电池中的气体生成量更低。因此能够确认，通过在制备正极活性材料的过程中包括脱锂过程和表面改性过程，在电池内的气体生成量下降且电池安全性极大提高。
<实验例2>
根据实施例1和比较例1的二次电池的理论容量15mAh/ea计算为0.5C，且通过其中对电池施加了17.8mA电流的充放电测量了0.5C容量。另外，通过其中对电池施加了与2C对应的100mAh电流的充放电测量了3C容量，并将倍率特性以2C/1C容量表示。将结果总结于下表2中。
<表2>
如表2中所示，能够确认，根据本发明的实施例1的二次电池因脱锂过程和表面改性过程而显示部分容量下降，但当与比较例1的二次电池相比时，倍率特性提高。因此能够确认，通过在电池制造过程的制备正极活性材料的过程中包括脱锂过程和表面改性过程，二次电池的电化学性能提高。
尽管为了示例性目的公开了本发明的优选实施方式，但本领域技术人员应理解，在不背离如在所附权利要求书中公开的本发明的范围和主旨的情况下，各种修改、添加和取代是可能的。
工业实用性
如上所述，根据本发明的制备正极活性材料的方法通过包括预活化过渡金属氧化物的工序，可以提供抑制了其它副反应并显示提高的电池性能的锂二次电池。
Claims (8)
1.一种制备锂二次电池用正极活性材料的方法，所述方法包括：化学脱锂过程，所述化学脱锂过程包括：
通过向其中包含溶解的BF4的溶液添加并混合选自由下式(1)表示的化合物中的至少一种锂过渡金属氧化物，随后对所述锂过渡金属氧化物进行热处理，从而将所述锂过渡金属氧化物预活化；和
使用机械研磨法对预活化的锂过渡金属氧化物的表面进行改性：
(1-x)LiM’O2-xLi2MnO3 (1)，
其中M’是MnaMb；
M是选自如下的至少一种：Ni、Ti、Co、Al、Cu、Fe、Mg、B、Cr、Zr、Zn和第II周期过渡金属；
且
0<x<1；0.5≤a≤1.0；0≤b≤0.5；且a+b＝1。
2.根据权利要求1所述的方法，其中在250℃以上的温度下进行所述热处理。
3.根据权利要求2所述的方法，其中在300℃以上的温度下进行所述热处理。
4.根据权利要求3所述的方法，其中在400℃以上的温度下进行所述热处理。
5.一种正极活性材料，其通过根据权利要求1～4中的任一项所述的方法制备。
6.一种电池，其包含根据权利要求5所述的正极活性材料。
7.一种电池组，其包含根据权利要求6所述的电池。
8.一种装置，其使用根据权利要求7所述的电池组作为电源。
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