CN111370666A - 正极材料、其制备方法及应用 - Google Patents
正极材料、其制备方法及应用 Download PDFInfo
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- CN111370666A CN111370666A CN202010194573.8A CN202010194573A CN111370666A CN 111370666 A CN111370666 A CN 111370666A CN 202010194573 A CN202010194573 A CN 202010194573A CN 111370666 A CN111370666 A CN 111370666A
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- 239000007774 positive electrode material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 47
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 30
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000003990 capacitor Substances 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 239000002243 precursor Substances 0.000 claims description 27
- 239000011572 manganese Substances 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000011247 coating layer Substances 0.000 claims description 10
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims description 5
- 229910019142 PO4 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
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 235000021317 phosphate Nutrition 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 3
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910001437 manganese ion Inorganic materials 0.000 claims description 3
- 229910001453 nickel ion Inorganic materials 0.000 claims description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 2
- 150000002222 fluorine compounds Chemical class 0.000 claims description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 claims description 2
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 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
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 2
- 125000005587 carbonate group Chemical group 0.000 claims 1
- 239000010406 cathode material Substances 0.000 abstract description 16
- 230000000087 stabilizing effect Effects 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 229910000473 manganese(VI) oxide Inorganic materials 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 229910017052 cobalt Inorganic materials 0.000 description 8
- 239000010941 cobalt Substances 0.000 description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 8
- 238000000227 grinding Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 238000001354 calcination Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000012452 mother liquor Substances 0.000 description 4
- 230000002572 peristaltic effect Effects 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- 229910013716 LiNi Inorganic materials 0.000 description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 102000020897 Formins Human genes 0.000 description 2
- 108091022623 Formins Proteins 0.000 description 2
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 229910010158 Li2MO3 Inorganic materials 0.000 description 1
- 229910002983 Li2MnO3 Inorganic materials 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
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- H01M4/00—Electrodes
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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
本发明公开一种正极材料，含有具有超晶格结构的晶体，晶体的化学式为xLi2MO3·(1‑x)LiNiaCobMn(1‑a‑b)O2，0<x≤0.1，0.8≤a<1，b≤0.1，所述M选自Mn、Co和Ni中的一种或几种。还公开了该正极材料的制备方法及包含该正极材料的电池或电容器。本发明的正极材料包含具有层状‑层状超晶格结构的晶体，在常规呈层状结构的高镍三元材料基础上穿叉另一种层状结构，利用两种不同层状结构之间的相互齿合，以提升产品的结构稳定性。本发明的正极材料由于锰基富锂相(Li2MnO3)的加入一定程度稀释了产品中镍的含量，镍含量的降低可有效改善电池的产气。因此，本申请可从减少产气和稳定正极结构两方面，提高电池的安全性能。
Description
技术领域
本发明属于化学电源领域，具体涉及一种正极材料、其制备方法及应用。
背景技术
高镍三元正极材料随着镍含量的增加，表面状态异常活跃。在充放电过程中，高镍材料与电解液反应产生大量氧气，进而影响了高镍材料的安全性能；与此同时，镍含量的提高亦会增加Li/Ni混排程度，在锂离子脱嵌过程中晶体结构容易破坏，结构稳定性降低，进而导致高镍材料的循环寿命也随之降低。这两个主要缺陷限制了高镍材料的进一步应用。
目前高镍材料主要靠四价Mn离子起稳定作用，然而随着镍含量的增加，只靠四价Mn离子的骨架支撑作用已经不能达到现在电池体系下，高电压对高镍材料材料稳定性的要求。
发明内容
为了克服上述缺陷，本发明提供一种正极材料及该正极材料的制备方法，和包含该正极材料的锂离子电池或电容器。
本发明的一方面提供一种正极材料，所述正极材料含有具有超晶格结构的晶体，所述晶体的化学式为xLi2MO3·(1-x)LiNiaCobMn(1-a-b)O2，0<x≤0.1，0.8≤a<1，b≤0.1，所述M选自Mn、Co和Ni中的一种或几种。
本发明的另一方面提供一种该正极材料的制备方法，包括：对含有镍离子、锰离子和钴离子的溶液在搅拌条件下将pH值调解至10-12，反应完成后在50-90℃下陈化5-12h，经分离、洗涤、干燥得到前驱体；及将锂源化合物与得到的前驱体混合均匀，并置于600℃-1000℃下烧结6-15h。
本发明的另一方面提供一种包含上述正极材料的锂离子电池或电容器。
本发明的正极材料包含具有层状-层状超晶格结构的晶体，在常规呈层状结构的高镍三元材料基础上穿叉另一种层状结构，利用两种不同层状结构之间的相互齿合，以提升产品的结构稳定性。本发明的正极材料由于富锂相(Li2MO3)的加入一定程度稀释了产品中镍的含量，镍含量的降低可有效改善电池的产气。因此，本申请可从减少产气和稳定正极结构两方面，提高电池的安全性能。
附图说明
通过参照附图详细描述其示例实施方式，本发明的上述和其它特征及优点将变得更加明显。
图1是实施例1中所得正极材料的扫描电镜图。
图2是实施例1中所得正极材料的XRD图谱。
图3是实施例1中所得正极材料与LiNi0.8Co0.1Mn0.1O2的DSC曲线。
图4是实施例1中所得正极材料组装成电池的首次充放电曲线。
具体实施方式
下面结合具体实施方式对本发明作详细说明。
本发明的正极材料，含有具有超晶格结构的晶体，晶体的化学式为xLi2MO3·(1-x)LiNiaCobMn(1-a-b)O2，0<x≤0.1，0.8≤a<1，b≤0.1，所述M选自Mn、Co和Ni中的一种或几种。富锂相Li2MO3是层状材料，具有很稳定的晶体结构。在材料中富锂相Li2MO3的摩尔含量在大于0-10％之间，可以选择在该范围内的任何值，例如1％、2％、3％、4％、5％、6％、7％、8％、9％等。少量的富锂相可以在原子尺度对高镍材料LiNiaCobMn(1-a-b)O2进行纳米尺度掺杂，协同作用可以使高镍材料的晶体结构框架更加的稳定，同时可以降低Li/Ni混排程度，提高镍基材料的结构稳定性。并且富锂相材料具有稳定的表面结构，与高镍材料原位结合形成镍基富锂正极材料可以稳定高镍材料的表面状态，降低高镍三元的风险系数，提高高镍材料的安全性能。
在优选的实施方式中，富锂相Li2MO3为Li2MnO3。
在优选的实施方式中，晶体中还可以包括掺杂元素，包括掺杂元素的晶体的化学式为xLi2MO3·(1-x)LiNiaCobMn(1-a-b-c)M1cO2，c≤0.03。其中掺杂元素M1可以是任何适当的掺杂元素，优选选自Zr、Ti、Al、Mg、Y等过渡金属元素中的一种或多种。
在优选的实施方式中，晶体外存在包覆层，包覆层中所涉及的材料的具体种类并没有特别的限制，可根据需求进行选择。优选，包覆层可以包括氧化物、氟化物、磷酸盐、聚合物中的一种或多种。包覆层的含量可以是任何适当的含量，例如可以是包覆前的整个材料的总重量的0.03～1％。
制备上述正极材料可以包括如下步骤：制备前驱体步骤和烧结步骤。首先形成含有Ni、Co和Mn的前驱体，然后将前驱体与锂源化合物混合烧结得到正极材料。具体而言，正极材料的制备方法包括：对含有镍离子、锰离子和钴离子的溶液在搅拌条件下将pH值调解至10-12，反应完成后在50-90℃下陈化5-12h，经分离、洗涤、干燥得到前驱体。然后进行烧结步骤，将锂源化合物与得到的前驱体混合均匀，并置于600℃-1000℃下烧结6-15h。
在优选的实施方式中，前驱体可以为碳酸盐或氢氧化物。
在优选的实施方式中，锂源化合物可以为LiOH·H2O、Li2CO3、LiNO3、CH3COOLi·2H2O中的一种或几种，锂源化合物的混合量是理论化学剂量的1.05-1.2倍。
在优选的实施方式中，还可以在烧结步骤进行体相掺杂，即将含有掺杂元素的化合物与锂源化合物和前驱体混合均匀进行烧结，掺杂元素选自Zr、Ti、Al、Mg、Y中的一种或多种。
在优选的实施方式中，还可以包括对烧结后的材料进行液相包覆形成包覆层，包覆层包括氧化物、氟化物、磷酸盐、聚合物中的一种或几种。
本发明的正极材料适用于锂离子电池或超级电容器中。
以下通过具体实例进一步描述本申请。不过这些实例仅仅是范例性的，并不对本发明的保护范围构成任何限制。
在下述实施例和对比例中，所使用到的试剂、材料以及仪器如没有特殊的说明，均可商购获得。
实施例1
将一定体积的硫酸镍，钴，锰溶液与过量2％摩尔的氢氧化钠溶液同时通过蠕动泵以580μL·min-1的进料速度滴加到母液中。镍，钴，锰的摩尔比列为72：9：19，物料的反应温度为50℃，pH控制在10，同时顶置搅拌杆以400rmp·min-1的转速剧烈搅拌，反应过程中加入氮气保护。陈化10h后，将得到的氢氧化物前驱体先进行抽滤，然后一定体积蒸馏水中清洗两次，最后在100℃下真空干燥6h，得到的干燥前驱体。将前驱体与一定摩尔比的LiOH充分研磨混合，然后在马弗炉中以5℃·min-1的加热速度先500℃预煅烧5h，而后800℃下煅烧12h，就得到了富锂镍基正极材料0.1Li2MnO3-0.9LiNi0.8Co0.1Mn0.1O2。
图1示出本实施例得到的富锂镍基正极材料的SEM图。从SEM图上可以看出，此富锂镍基正极材料为微米级的单晶颗粒，大小颗粒掺混有利于提高材料的振实和压实密度，适于实际应用。
图2示出本实施例得到富锂镍基正极材料的XRD谱图。从图中可以看出，该材料的绝大部分衍射峰属于空间群为R-3m的α-NaFeO2结构，在20°到23°产生了超晶格衍射峰，表明本实施例得到的正极材料含有超晶格结构。
图3示出本实施例得到的富锂镍基正极材料与高镍LiNi0.8Co0.1Mn0.1O2(NCM811)的DSC曲线。通过DSC曲线可以看出，本实施例得到的富锂镍基材料的起峰温度比NCM11高，峰强和比NCM811低，表明该材料相较于NCM811热稳定性更高。
实施例2
将一定体积的乙酸镍，钴，锰溶液与过量3％摩尔的碳酸钠溶液同时通过蠕动泵以1000μL·min-1的进料速度滴加到装有碳酸钠的母液中。镍，钴，锰的摩尔比列为76：9.5：14.5，物料的反应温度为55℃，pH＝11，同时顶置搅拌杆以500rmp·min-1的转速剧烈搅拌，反应过程中加入氩气保护。陈化5h后得到的碳酸盐前驱体先进行抽滤，然后在800mL蒸馏水中清洗两次，最后在120℃下真空干燥8h，得到的干燥前驱体。将得到的前驱体与一定摩尔比的LiOH充分研磨混合，然后在马弗炉中以5℃·min-1的加热速度先500℃预煅烧5h，而后600℃下煅烧10h，就得到了富锂镍基正极材料0.05Li2MnO3-0.95LiNi0.8Co0.1Mn0.1O2。
实施例3
将一定体积的硫酸镍，钴，锰溶液与过量1％摩尔的氢氧化钠溶液同时通过蠕动泵以780μL·min-1的进料速度滴加到装有氢氧化钠的母液中。镍，钴，锰的摩尔比列为83.6：6.7：9.7，物料的反应温度为60℃，pH＝12，同时顶置搅拌杆以600rmp·min-1的转速剧烈搅拌，反应过程中加入氮气保护。陈化8h后得到的氢氧化物前驱体先进行抽滤，然后在700mL蒸馏水中清洗两次，最后在80℃下真空干燥10h，得到的干燥前驱体。将得到的前驱体与一定摩尔比的Li2CO3充分研磨混合，然后在马弗炉中以5℃·min-1的加热速度先500℃预煅烧5h，而后1000℃下煅烧8h，就得到了富锂正极材料0.05Li2MnO3-0.95LiNi0.88Co0.07Mn0.05O2。
实施例4
将一定量的硫酸镍，钴，锰溶液与过量5％摩尔的碳酸钠溶液同时通过蠕动泵以800μL min-1的进料速度滴加到装有碳酸钠的母液中；镍，钴，锰的摩尔比列为72：19：9，物料的反应温度为45℃，pH＝11，同时顶置搅拌杆以600rmp·min-1的转速剧烈搅拌，反应过程中加入氮气保护。陈化10h后得到的碳酸盐前驱体先进行抽滤，然后在900mL蒸馏水中清洗两次，最后在100℃下真空干燥8h，得到的干燥前驱体。将得到的前驱体与一定摩尔比的CH3COOLi充分研磨混合，然后在马弗炉中以5℃·min-1的加热速度先500℃预煅烧5h，而后800℃下煅烧15h，就得到了富锂正极材料0.1Li2CoO3-0.9LiNi0.8Co0.1Mn0.1O2。
将实施例1-4得到的富锂镍基正极材料制作成电极片并组装成纽扣电池。具体过程为：首先把富锂正极材料、乙炔黑、PVDF按质量比8:1:1充分研磨混合后，而后加入NMP使混合物溶解，持续搅拌6h；然后使用刮刀涂布在干净的铝箔上。在120℃真空干燥12h，使用冲片机冲出直径为14mm的电极片。在布劳恩手套箱中将其组装成型号为2032的纽扣半电池。以锂片作对电极和参比电极，电解液为1摩尔的LiPF6溶解到重量比为3:5:2的碳酸乙烯酯、碳酸二甲酯和氟代碳酸乙烯酯中。将组装成的电池在深圳新威测试仪上进行充放电测试
图3示出实施例1得到富锂镍基正极材料的首次充放电曲线。通过该曲线可以得出，在充放电电压窗口为3.0-4.25V下同时充放电电流为1/3C的情况下，首次充电比容量和放电比容量分别为205.4mAh·g–1和186.4mAh·g–1，首次效率为90.75％，表现出不错的首次充放电性能。实施例1-4得到富锂镍基正极材料的首次充放电比容量和效率如表1所示。
表1
从表1可以看出实施例1-4的正极材料首次充放电比容量和首次充放电效率较好。并且实施例2-4得到的正极材料也具有超晶格结构且与没有超晶格结构的NCM811相比具有更好的热稳定性。
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节，也不限制该发明仅为所述的具体实施方式。显然，根据本说明书的内容，可作很多的修改和变化。本说明书选取并具体描述这些实施例，是为了更好地解释本发明的原理和实际应用，从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。
Claims (10)
1.一种正极材料，其特征在于，所述正极材料含有具有超晶格结构的晶体，所述晶体的化学式为xLi2MO3·(1-x)LiNiaCobMn(1-a-b)O2，0<x≤0.1，0.8≤a＜1，b≤0.1，所述M选自Mn、Co和Ni中的一种或几种。
2.如权利要求1所述的正极材料，其特征在于，所述M为Mn。
3.如权利要求1所述的正极材料，其特征在于，所述晶体还包括掺杂元素，包括掺杂元素的晶体的化学式为xLi2MO3·(1-x)LiNiaCobMn(1-a-b-c)M1cO2，c≤0.03，所述M1选自Zr、Ti、Al、Mg、Y中的一种或多种。
4.如权利要求1所述的正极材料，其特征在于，所述晶体外存在包覆层，所述包覆层包括氧化物、氟化物、磷酸盐、聚合物中的一种或多种。
5.一种权利要求1所述的正极材料的制备方法，其特征在于，包括：
制备前驱体步骤，对含有镍离子、锰离子和钴离子的溶液在搅拌条件下将pH值调解至10-12，反应完成后在50-90℃下陈化5-12h，经分离、洗涤、干燥得到前驱体；及
烧结步骤，将锂源化合物与得到的前驱体混合均匀，并置于600℃-1000℃下烧结6-15h。
6.根据权利要求5所述的制备方法，其特征在于，所述前驱体为碳酸盐或氢氧化物。
7.根据权利要求5所述的制备方法，其特征在于，所述锂源化合物为LiOH·H2O、Li2CO3、LiNO3、CH3COOLi·2H2O中的一种或几种，所述锂源化合物的混合量是理论化学剂量的1.05-1.2倍。
8.根据权利要求5所述的制备方法，其特征在于，所述烧结步骤中，还添加含掺杂元素的化合物与锂源化合物和所述前驱体一起烧结，掺杂元素选自Zr、Ti、Al、Mg、Y中的一种或多种。
9.根据权利要求5所述的制备方法，其特征在于，还包括对烧结后的材料进行液相包覆形成包覆层，所述包覆层包括氧化物、氟化物、磷酸盐、聚合物中的一种或几种。
10.一种锂离子电池或电容器，其特征在于，包括权利要求1-4任一所述的正极材料。
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| CN104966833A (zh) * | 2015-07-28 | 2015-10-07 | 宁德时代新能源科技有限公司 | 正极材料、其制备方法及包含该正极材料的锂离子电池 |
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| CN111987297A (zh) * | 2020-08-26 | 2020-11-24 | 北京理工大学重庆创新中心 | 表面铝掺杂及磷酸钛铝锂包覆的富锂锰基正极材料及制备 |
| CN112151798A (zh) * | 2020-09-16 | 2020-12-29 | 天目湖先进储能技术研究院有限公司 | 一种氟化物/氧化物共包覆正极材料及其制备方法 |
| CN112151798B (zh) * | 2020-09-16 | 2022-03-15 | 天目湖先进储能技术研究院有限公司 | 一种氟化物/氧化物共包覆正极材料及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP3882216A1 (en) | 2021-09-22 |
| US20210296644A1 (en) | 2021-09-23 |
| US11569505B2 (en) | 2023-01-31 |
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