CN108281623A - 一种包覆有四氧化三钴保护层的富锂正极材料 - Google Patents
一种包覆有四氧化三钴保护层的富锂正极材料 Download PDFInfo
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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 title claims abstract description 82
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 37
- 239000011241 protective layer Substances 0.000 title claims abstract description 36
- 239000010406 cathode material Substances 0.000 title 1
- 239000010405 anode material Substances 0.000 claims abstract description 39
- 150000007524 organic acids Chemical class 0.000 claims abstract description 19
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims abstract description 14
- 229940011182 cobalt acetate Drugs 0.000 claims abstract description 12
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 5
- 239000011975 tartaric acid Substances 0.000 claims description 5
- 235000002906 tartaric acid Nutrition 0.000 claims description 5
- NIONDZDPPYHYKY-SNAWJCMRSA-N (2E)-hexenoic acid Chemical compound CCC\C=C\C(O)=O NIONDZDPPYHYKY-SNAWJCMRSA-N 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 4
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 4
- 239000004310 lactic acid Substances 0.000 claims description 4
- 235000014655 lactic acid Nutrition 0.000 claims description 4
- 239000001630 malic acid Substances 0.000 claims description 4
- 235000011090 malic acid Nutrition 0.000 claims description 4
- PGMYKACGEOXYJE-UHFFFAOYSA-N pentyl acetate Chemical compound CCCCCOC(C)=O PGMYKACGEOXYJE-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 claims 1
- 239000010941 cobalt Substances 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- 239000010410 layer Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 19
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 10
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract 2
- 238000000576 coating method Methods 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000002243 precursor Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 235000015165 citric acid Nutrition 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- SVMCDCBHSKARBQ-UHFFFAOYSA-N acetic acid;cobalt Chemical compound [Co].CC(O)=O SVMCDCBHSKARBQ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 description 2
- -1 pentyl ester Chemical class 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- 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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Abstract
本发明涉及一种包覆有四氧化三钴保护层的富锂正极材料。本发明属于锂离子电池正极材料技术领域。一种包覆有四氧化三钴保护层的富锂正极材料,其特点是:包覆有四氧化三钴保护层的富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2表面包覆有四氧化三钴保护层,保护层Co3O4与Li1.2Ni0.176Co0.1Mn0.524O2的摩尔比为0.1‑10:99.9‑90;包覆四氧化三钴保护层采用的原料乙酸钴、有机酸的质量比为1‑5:40‑200,乙酸钴、有机酸和Li1.2Ni0.176Co0.1Mn0.524O2的总质量与有机溶剂的配比是1g:10‑20ml。本发明具有产品稳定性好,循环性能高,包覆效果好,有效提高了材料的电化学性能,制备工艺简单,操作方便,适用范围广等优点。
Description
技术领域
本发明属于锂离子电池正极材料技术领域,特别是涉及一种包覆有四氧化三钴保护层的富锂正极材料。
背景技术
目前,新能源和可再生能源技术被公认是21世纪最重要的高新技术产业,其中电化学电源体系的发展方向为大容量、高功率和长寿命。锂离子电池体系是近些年出现的新型化学电源体系,具有重量轻、储能大、功率大、安全性能好、寿命长、自放电系数小等优点,已深入到人们生活的方方面面,广泛应用于手机、笔记本电脑、数码相机、摄像机、玩具、电动工具等等,是目前具有最高比能量的实用化二次电池体系。如今,随着电子产品功能的日新月异以及锂离子电池在电动车上的大规模应用,巨大、高速增长的市场对锂离子电池提出高比能、长寿命的迫切要求,锂离子电池性能的提高成为行业发展的关键,而限制锂离子电池发展的最大瓶颈就是锂离子电池正极材料。传统锂离子电池正极材料钴酸锂、锰酸锂、磷酸铁锂、三元材料等的比容量一般都在200mAh/g以下,因此迫切要求开发出新的高比能锂离子电池正极材料,通过研究发现Li1.2Ni0.176Co0.1Mn0.524O2是一种非常好的高比能富锂正极材料,其实际放电比容量可以达到250mAh/g以上,但是其稳定性以及循环性能还有待于进一步提高。
发明内容
本发明为解决公知技术中存在的技术问题而提供一种包覆有四氧化三钴保护层的富锂正极材料。
本发明的目的是提供一种具有产品稳定性好,循环性能高,包覆效果好,有效提高了材料的电化学性能,制备工艺简单,操作方便,适用范围广等特点的包覆有四氧化三钴保护层的富锂正极材料。
一种包覆有四氧化三钴保护层的富锂正极材料,Li1.2Ni0.176Co0.1Mn0.524O2表面包覆有四氧化三钴(Co3O4)保护层,其中保护层Co3O4与Li1.2Ni0.176Co0.1Mn0.524O2的摩尔比为0.1-10:99.9-90;原料乙酸钴、有机酸的质量比为1-5:40-200,乙酸钴、有机酸和Li1.2Ni0.176Co0.1Mn0.524O2的总质量与有机溶剂的配比是1g:10-20ml,原料经混合搅拌形成溶胶,60-120℃恒温干燥成干态凝胶,研磨后以5-10℃/min的升温速度加热至400-1000℃,在空气气氛下恒温煅烧2-24h,随后停止加热,自然冷却后即得到表面包覆有Co3O4的富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2。
本发明包覆有四氧化三钴保护层的富锂正极材料所采取的技术方案是:
一种包覆有四氧化三钴保护层的富锂正极材料,其特点是:包覆有四氧化三钴保护层的富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2表面包覆有四氧化三钴保护层,保护层Co3O4与Li1.2Ni0.176Co0.1Mn0.524O2的摩尔比为0.1-10:99.9-90;包覆四氧化三钴保护层采用的原料乙酸钴、有机酸的质量比为1-5:40-200,乙酸钴、有机酸和Li1.2Ni0.176Co0.1Mn0.524O2的总质量与有机溶剂的配比是1g:10-20ml。
本发明包覆有四氧化三钴保护层的富锂正极材料还可以采用如下技术方案:
所述的包覆有四氧化三钴保护层的富锂正极材料,其特点是:有机酸为柠檬酸、苹果酸、乙烯酸、乳酸或者酒石酸中的一种或几种的混合物。
所述的包覆有四氧化三钴保护层的富锂正极材料,其特点是:有机溶剂为乙醇、乙酸戊酯、乙二醇、异丙醇中的一种或几种的混合物。
本发明具有的优点和积极效果是:
包覆有四氧化三钴保护层的富锂正极材料由于采用了本发明全新的技术方案,与现有技术相比,本发明具有以下特点:
(1)本发明采用在含有有机酸的有机溶液中加入乙酸钴和富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2,得到了表面包覆了Co3O4的富锂正极材料。经过理化及电性能测试表明,包覆了Co3O4的富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2的基体结构没有改变,只是在其表面形成了Co3O4包覆保护层,保持富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2原有高比能性能的同时,具有有效阻止电解液与电极材料接触的作用,增加了材料在充放电过程中的稳定性,使得富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2的循环性能得到了明显提升,进一步提高了材料的电化学性能;
(2)本发明采用溶胶-凝胶法进行富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2的表面包覆,得到的包覆层更加均匀、致密,极大地提高了包覆效果。
附图说明
图1是本发明富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2包覆Co3O4前后XRD的比较图;
图2是本发明富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2包覆Co3O4前后循环性能曲线比较图。
具体实施方式
为能进一步了解本发明的发明内容、特点及功效,兹例举以下实施例,并配合附图详细说明如下:
参阅附图1和图2。
一种包覆有四氧化三钴保护层的富锂正极材料,富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2表面包覆有Co3O4保护层;保护层Co3O4与Li1.2Ni0.176Co0.1Mn0.524O2的摩尔比为0.1-10:99.9-90;原料乙酸钴、有机酸的质量比为1-5:40-200;所述乙酸钴、有机酸和Li1.2Ni0.176Co0.1Mn0.524O2的总质量与有机溶剂的配比是1g:10-20ml;所述有机酸为柠檬酸、苹果酸、乙烯酸、乳酸或者酒石酸中的一种或几种的混合物;所述有机溶剂为乙醇、乙酸戊酯、乙二醇、异丙醇中的一种或几种的混合物。
一种包覆有四氧化三钴保护层的富锂正极材料,制备步骤:
(1)将乙酸钴溶解在含有有机酸(作为螯合剂)的有机溶剂中,搅拌混合均匀,然后加入富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2,常温下持续搅拌8-24h,使其在分子水平上充分混合均匀形成溶胶;然后在继续搅拌的同时将溶胶加热至60-120℃,恒温持续搅拌至挥发掉溶剂,形成干燥的凝胶前躯体;
(2)将步骤(1)中的干燥的凝胶前躯体研磨均匀,然后放入马弗炉中,以5-10℃/min的升温速度加热至400-1000℃,在空气气氛下恒温煅烧2-24h,随后停止加热,自然冷却后即得到表面包覆有Co3O4的富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2。
有机酸为柠檬酸、苹果酸、乙烯酸、乳酸或者酒石酸中的一种或几种的混合物;有机溶剂为乙醇、乙酸戊酯、乙二醇、异丙醇中的一种或几种的混合物;乙酸钴、有机酸的质量比为1-5:40-200;所述干燥的凝胶前躯体中Co3O4与Li1.2Ni0.176Co0.1Mn0.524O2的物质的量比为0.1-10:99.9-90;所述乙酸钴、有机酸和Li1.2Ni0.176Co0.1Mn0.524O2的总质量与有机溶剂的配比是1g:10-20ml。
实施例1:
一种包覆有四氧化三钴保护层的富锂正极材料,Li1.2Ni0.176Co0.1Mn0.524O2表面包覆有Co3O4保护层,其制备过程:将1.255g乙酸钴,加入到380ml乙醇中,然后再加入10g柠檬酸,搅拌使其溶解,然后加入20g Li1.2Ni0.176Co0.1Mn0.524O2搅拌12h,使它们在分子水平上充分混合均匀形成溶胶;然后在80℃条件下加热搅拌使乙醇溶液慢慢挥发,形成干燥的凝胶前躯体;将前躯体研磨均匀后,放入马弗炉中,以5℃/min的速度升温至800℃,空气气氛下恒温煅烧5h;在此高温煅烧过程中在Li1.2Ni0.176Co0.1Mn0.524O2材料表面形成Co3O4晶体,自然冷却后即得到表面包覆Co3O4的Li1.2Ni0.176Co0.1Mn0.524O2正极材料。
实施例2:
一种包覆有四氧化三钴保护层的富锂正极材料,Li1.2Ni0.176Co0.1Mn0.524O2表面包覆有Co3O4保护层,其制备过程:将2.536g乙酸钴,加入到450ml乙醇中,然后再加入21g苹果酸,搅拌使其溶解,然后加入20g Li1.2Ni0.176Co0.1Mn0.524O2搅拌12h,使它们在分子水平上充分混合均匀形成溶胶;然后在80℃条件下加热搅拌使乙醇溶液慢慢挥发,形成干燥的凝胶前躯体;将前躯体研磨均匀后,放入马弗炉中,以5℃/min的速度升温至700℃,空气气氛下恒温煅烧6h;在此高温煅烧过程中在Li1.2Ni0.176Co0.1Mn0.524O2材料表面形成Co3O4晶体,自然冷却后即得到表面包覆Co3O4的Li1.2Ni0.176Co0.1Mn0.524O2正极材料。
根据图1的测试结果得出,Li1.2Ni0.176Co0.1Mn0.524O2材料包覆Co3O4前后,其XRD图没有明显的变化,说明在Li1.2Ni0.176Co0.1Mn0.524O2材料表面形成的包覆层没有改变Li1.2Ni0.176Co0.1Mn0.524O2材料的基体结构,只是在其表面形成了保护层。
根据图2的测试结果得出,本发明制备的Li1.2Ni0.176Co0.1Mn0.524O2材料包覆Co3O4后与未进行包覆的Li1.2Ni0.176Co0.1Mn0.524O2材料相比较,包覆层能够有效的阻止了电解液与电极材料的接触,增加了材料在充放电过程中的稳定性,材料的循环性能得到了明显的提升,有效提高了材料的电化学性能。
本实施例具有所述的产品稳定性好,循环性能高,包覆效果好,有效提高了材料的电化学性能,制备工艺简单,操作方便,适用范围广等积极效果。
Claims (3)
1.一种包覆有四氧化三钴保护层的富锂正极材料,其特征是:包覆有四氧化三钴保护层的富锂正极材料Li1.2Ni0.176Co0.1Mn0.524O2表面包覆有四氧化三钴保护层,保护层Co3O4与Li1.2Ni0.176Co0.1Mn0.524O2的摩尔比为0.1-10:99.9-90;包覆四氧化三钴保护层采用的原料乙酸钴、有机酸的质量比为1-5:40-200,乙酸钴、有机酸和Li1.2Ni0.176Co0.1Mn0.524O2的总质量与有机溶剂的配比是1g:10-20ml。
2.根据权利要求1所述的包覆有四氧化三钴保护层的富锂正极材料,其特征是:有机酸为柠檬酸、苹果酸、乙烯酸、乳酸或者酒石酸中的一种或几种的混合物。
3.根据权利要求1所述的包覆有四氧化三钴保护层的富锂正极材料,其特征是:有机溶剂为乙醇、乙酸戊酯、乙二醇、异丙醇中的一种或几种的混合物。
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