CN104466113B - 一种具有核壳结构的镍掺杂钴酸锂复合正极材料的制备方法 - Google Patents
一种具有核壳结构的镍掺杂钴酸锂复合正极材料的制备方法 Download PDFInfo
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002131 composite material Substances 0.000 title claims abstract description 13
- 239000010406 cathode material Substances 0.000 title abstract 3
- 239000011258 core-shell material Substances 0.000 title abstract 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 27
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 18
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 5
- 239000010439 graphite Substances 0.000 claims abstract description 5
- 238000005253 cladding Methods 0.000 claims abstract description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 19
- 239000010941 cobalt Substances 0.000 claims description 19
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims description 8
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims description 4
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims description 4
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 claims description 4
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 150000002815 nickel Chemical class 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- -1 Graphite compound Chemical class 0.000 claims description 2
- 229910012713 LiCo1-xNixO2 Inorganic materials 0.000 claims description 2
- 229910012964 LiCo1−xNixO2 Inorganic materials 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 6
- 239000011149 active material Substances 0.000 abstract description 2
- 229920000620 organic polymer Polymers 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 150000001868 cobalt Chemical class 0.000 description 2
- 229940011182 cobalt acetate Drugs 0.000 description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229940078494 nickel acetate Drugs 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910032387 LiCoO2 Inorganic materials 0.000 description 1
- 229910014405 LiNi1/2Co1/2O2 Inorganic materials 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—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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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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Abstract
本发明涉及一种具有核壳结构的镍掺杂钴酸锂复合正极材料的制备方法，该方法包括如下步骤：（1）镍掺杂钴酸锂的制备，（2）制备包覆材料，（3）包覆形成核壳结构。本发明制备的正极材料，采用高镍掺杂的钴酸锂材料作为活性材料，以提高材料的能量密度，采用使用有机聚合物和Si/石墨作为包覆材料，提高该材料的导电性和电化学稳定性。因此该复合材料在用于锂离子电池时，具有高比容量和长使用寿命。
Description
技术领域
本发明涉一种具有核壳结构的镍掺杂钴酸锂复合正极材料的制备方法。
背景技术
人们对能量存储技术产生了日益增加的兴趣。已经广泛地将电化学装置用作便携式电话、便携式摄像机、笔记本电脑、PC和电动汽车的能源，从而导致深入的研究和开发。就此而言，电化学装置是至关重要的主题。特别地，开发可充电二次电池成为了关注的焦点。此外，在开发这类电池期间，最近已经对新型电极和新型电池的设计进行了研究，从而提高容量密度和比能量。
锂离子二次电池具有高能量密度、重量轻、不污染环境、无记忆效应、工作性能稳定、安全可靠等特点，自问世以来应用广泛，已成为目前主要的便携式电源，也是大功率动电池的开发重点。 层状锂离子电池正极材料是领域内研究的热点。理论上具有层状结构和尖晶石结构的材料，都可以作为锂离子电池的正极材料，其中LiCoO2用作锂离子电池正极材料具有如下特点：1、安全性好；2、容量一般；3、循环性能一般。
在锂离子蓄电池电化学体系中，碳材料是帮助化学能直接向电能成功转化的关键组分。碳表面积和孔隙率对该电化学体系的性能是重要的。高表面积碳通常导致和锂离子储存的高容量，同时高度多孔的碳促进气态和液态反应物及产物的质量传递。
然而，在锂二次电池中，存在的问题是在充电/放电期间，在电池内因在电极表面上充当电解质的非水电解质溶液、特别是碳酸酯有机溶剂发生分解而发生副反应。此外，当具有大分子量的电解质溶剂如碳酸亚乙酯(EC)、碳酸亚丙酯(PC)等共同插入在碳基阳极的石墨层之间时，阳极的结构可能会坍塌。
发明内容
本发明提供一种具有核壳结构的镍掺杂钴酸锂复合正极材料的制备方法，使用该方法制备的正极材料，具有较高比容量的同时，还具良好的电化学稳定性。
为了实现上述目的，本发明提供一种具有核壳结构的镍掺杂钴酸锂复合正极材料的制备方法，该方法包括如下步骤：
（1）镍掺杂钴酸锂的制备
该镍掺杂钴酸锂的化学式为LiCo1-xNixO2，其中： x=0.45-0.55；
将草酸锂、氢氧化钴和氢氧化镍按比例混合，其中Li∶Co：Ni的摩尔比为1.02∶1-x：x，将混合物混磨均匀后放入加热炉中，热处理气氛为空气，升温速率为5-10℃／分钟，至550-650℃预处理，预处理时间为2-4h，然后升温至850-900℃，热处理时间为4-6h，然后降至室温，并将合成物料粉碎筛分，得到粒径为10-20μm的镍掺杂钴酸锂；
（2）制备包覆材料
将0.2-0.3重量份的聚乙二醇甲基醚溶于100重量份的丙酮中得到聚乙二醇甲基醚溶液，并以相对于每100重量份溶液5-8重量份的量向所述溶液中添加直径为50-100nm的Si/石墨复合粒子，超声分散得到包覆材料体系；
（3）包覆形成核壳结构
将上述镍掺杂钴酸锂和上述包覆材料体系按照质量比（10-15）:100混合，以350-400r/min的速度搅拌6-10h后，对混合溶液进行过滤，从而得到核壳结构的复合正极材料。
本发明制备的正极材料，采用高镍掺杂的钴酸锂材料作为活性材料，以提高材料的能量密度，采用使用有机聚合物和Si/石墨作为包覆材料，提高该材料的导电性和电化学稳定性。因此该复合材料在用于锂离子电池时，具有高比容量和长使用寿命。
具体实施方式
实施例一
本实施例的活性物质为LiCo0.55Ni0.45O2。
将草酸锂、氢氧化钴和氢氧化镍按比例混合，其中Li∶Co：Ni的摩尔比为1.02∶0.55：0.45，将混合物混磨均匀后放入加热炉中，热处理气氛为空气，升温速率为5℃／分钟，至550℃预处理，预处理时间为4h，然后升温至850℃，热处理时间为6h，然后降至室温，并将合成物料粉碎筛分，得到粒径为10-20μm的镍掺杂钴酸锂。
将0.2重量份的聚乙二醇甲基醚溶于100重量份的丙酮中得到聚乙二醇甲基醚溶液，并以相对于每100重量份溶液5重量份的量向所述溶液中添加直径为50-100nm的Si/石墨复合粒子，超声分散得到包覆材料体系。
将上述镍掺杂钴酸锂和上述包覆材料体系按照质量比10:100混合，以350r/min的速度搅拌10h后，对混合溶液进行过滤，从而得到核壳结构的复合正极材料。
实施例二
本实施例的活性物质为LiCo0.45Ni0.55O2。
将草酸锂、氢氧化钴和氢氧化镍按比例混合，其中Li∶Co：Ni的摩尔比为1.02∶0.45：0.55，将混合物混磨均匀后放入加热炉中，热处理气氛为空气，升温速率为10℃／分钟，至650℃预处理，预处理时间为2h，然后升温至900℃，热处理时间为4h，然后降至室温，并将合成物料粉碎筛分，得到粒径为10-20μm的镍掺杂钴酸锂。
将0.3重量份的聚乙二醇甲基醚溶于100重量份的丙酮中得到聚乙二醇甲基醚溶液，并以相对于每100重量份溶液8重量份的量向所述溶液中添加直径为50-100nm的Si/石墨复合粒子，超声分散得到包覆材料体系。
将上述镍掺杂钴酸锂和上述包覆材料体系按照质量比15:100混合，以400r/min的速度搅拌6h后，对混合溶液进行过滤，从而得到核壳结构的复合正极材料。
比较例
将乙酸镍、乙酸钴、乙酸锂按摩尔比为1/2∶1/2∶1溶于去离子水中，乙酸镍、乙酸钴、乙酸钴和乙酸锂的总浓度为0.4mol/L，混合均匀后加入浓度为0.5mol/L的柠檬酸水溶液，再加入质量百分浓度为15％的氨水溶液调节pH值为10；所述镍盐、钴盐和钴盐的总量与螯合剂的摩尔比为1∶1； 将得到的混合溶液于50℃的水浴中加热以蒸发水分，加热时间为18小时，并不断搅拌，搅拌速度为200转/分钟，得到凝胶体； 将凝胶体于鼓风干燥箱中烘干，烘干温度为80℃，烘干时间为30小时，得到干燥的凝胶体； 将干燥的凝胶体进行预烧，预烧温度为200℃，预烧时间为20小时，得到前驱体；前驱体自然冷却至室温后于球磨机中研磨0.5小时，将研磨后的前驱体在650℃下进行煅烧，煅烧时间为30小时，煅烧后自然冷却至室温后再次在球磨机上研磨0.5小时，即得到所述的锂离子电池多元正极材料LiNi1/ 2Co1/2O2。
将上述实施例一、二以及比较例所得产物分别和导电碳黑、粘结剂PVDF(聚偏氟乙烯)按质量比80∶10∶10混合，涂覆在铜箔上，以金属锂片为对极，电解液为1mol/L的LiPF6溶液，溶剂为EC、DEC和EMC的混合溶剂，体积比为1∶1∶1。在氩气保护的手套箱内将正极、负极、电解液、隔离膜与电池壳组装成扣式电池。在测试温度为25℃下进行电性能测试，经测试该实施例一和二的材料与比较例的产物相比，首次比容量提高了25-28%，使用寿命提高了50%以上。
Claims (1)
1.一种具有核壳结构的镍掺杂钴酸锂复合正极材料的制备方法，该方法包括如下步骤：
（1）镍掺杂钴酸锂的制备
该镍掺杂钴酸锂的化学式为LiCo1-xNixO2，其中： x=0.45-0.55；
将草酸锂、氢氧化钴和氢氧化镍按比例混合，其中Li∶Co：Ni的摩尔比为1.02∶1-x：x，将混合物混磨均匀后放入加热炉中，热处理气氛为空气，升温速率为5-10℃／分钟，至550-650℃预处理，预处理时间为2-4h，然后升温至850-900℃，热处理时间为4-6h，然后降至室温，并将合成物料粉碎筛分，得到粒径为10-20μm的镍掺杂钴酸锂；
（2）制备包覆材料
将0.2-0.3重量份的聚乙二醇甲基醚溶于100重量份的丙酮中得到聚乙二醇甲基醚溶液，并以相对于每100重量份溶液5-8重量份的量向所述溶液中添加直径为50-100nm的Si/石墨复合粒子，超声分散得到包覆材料体系；
（3）包覆形成核壳结构
将上述镍掺杂钴酸锂和上述包覆材料体系按照质量比（10-15）:100混合，以350-400r/min的速度搅拌6-10h后，对混合溶液进行过滤，从而得到核壳结构的复合正极材料。
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