CN1324731C - 一种锂离子电池用锂锰氧化物正极材料的制备工艺 - Google Patents
一种锂离子电池用锂锰氧化物正极材料的制备工艺 Download PDFInfo
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 14
- 229910002102 lithium manganese oxide Inorganic materials 0.000 title claims abstract description 10
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000010406 cathode material Substances 0.000 title 1
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000010405 anode material Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 6
- 239000011572 manganese Substances 0.000 claims abstract description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 4
- 229920002401 polyacrylamide Polymers 0.000 claims abstract 2
- 238000005516 engineering process Methods 0.000 claims description 9
- 239000003292 glue Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 abstract description 3
- 238000007873 sieving Methods 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 238000010304 firing Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 230000006911 nucleation Effects 0.000 abstract 1
- 238000010899 nucleation Methods 0.000 abstract 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 14
- 239000003795 chemical substances by application Substances 0.000 description 9
- 229920002521 macromolecule Polymers 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 7
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 7
- 229910052808 lithium carbonate Inorganic materials 0.000 description 7
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 7
- 239000007772 electrode material Substances 0.000 description 2
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
Classifications
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Complex oxides containing manganese and at least one other metal element
- C01G45/1221—Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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
- H01M4/50—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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
本发明公开了一种锂离子电池用锂锰氧化物正极材料的制备工艺，包括有固相合成和灼烧工序，其特征在于：工序(1)按锂∶锰的原子比值为0.5-0.55的锂源和锰源物料混匀，按此混料的5-10%的比例加入聚丙烯酰胺，混匀成胶状，在球磨机内球磨、研细，过300目筛，工序(2)将工序(1)的粉料置于微波炉内进行微波造核后，在400-450℃干燥箱中进行预烧8小时，自然冷却至室温，工序(3)对预烧后的料进行第二次球磨后，放入干燥箱中进行550-700℃灼烧10小时后，过300目筛即成。本发明与现行技术比具有充放电效率高的显著优点。
Description
技术领域：
本发明属于一种电池，特别是一种锂离子电池用锂锰氧化物正极材料的制备工艺。
背景技术：
目前已商品化的锂离子电池金属氧化物类电极材料中，锂锰氧化物电极材料由于其在价格、材料的环境兼容性及后处理方面所具有的明显特点，被普遍看好的下一代锂离子电池正极材料。但是，由于现行的固相合成技术中的温度高达800℃，容易造成锂的损失，此外现行的工艺所制备的锂锰氧化物正极材料，其充放电容量只有110mAh/g，有效率不足80％。
发明内容：
本发明需要解决的技术问题是设计一种锂离子电池用锂锰氧化物正极材料的制备工艺，所制取的正极材料具有充放电效率高，且工艺成本低的优点。本发明的技术方案是，一种锂离子电池用锂锰氧化物正极材料的制备工艺，包括有固相合成和灼烧工序，其特征在于：工序(1)按锂：锰的原子比值为0.5-0.55的锂源和锰源物料混匀，按此混料的5-10％的比例加入高分子网络剂，混匀成胶状，在球磨机内球磨、研细，过300目筛。工序(2)将工序(1)的粉料置于微波炉内进行微波造核后，在400-450℃干燥箱中进行预烧8小时，自然冷却至室温，工序(3)对预烧后的料进行第二次球磨后，放入干燥箱中进行550-700℃灼烧10小时后，过300目筛即成。本发明由于改变了原料的配比，增加了球磨和过筛工序和预热处理工序，设置了微波造核及加入高分子网络剂工序，降低了灼烧温度，因而本发明制备的锂锰氧化物正极材料，其晶体结构不受锂的嵌入、脱嵌而损坏，因而本发明具有充放电效率高(95％)，且工艺成本低的显著优点。
具体实施方式：
实施例1
工序(1)将锂与锰的原子比值为0.50的碳酸锂和电解二氧化锰物料混匀，按此混合料的5％加高分子网络剂，混匀成胶状，经球磨机球磨，过300目筛。
工序(2)将上述粉料置于微波炉内进行微波造核后，进行400℃预烧8小时，自然冷却至常温。
工序(3)对预烧后的料进行再次球磨后，在550℃灼烧10小时，过300目筛即成。
实施例2
工序(1)将锂与锰的原子比值为0.51的碳酸锂和电解二氧化锰物料混匀，按此混合料的5％加高分子网络剂，混匀成胶状，经球磨机球磨，过300目筛。
工序(2)将上述粉料置于微波炉内进行微波造核后，进行400℃预烧8小时，自然冷却至常温。
工序(3)对预烧后的料进行再次球磨后，在600℃灼烧10小时，过300目筛即成。
实施例3
工序(1)将锂与锰的原子比值为0.52的碳酸锂和电解二氧化锰物料混匀，按此混合料的5％加高分子网络剂，混匀成胶状，经球磨机球磨，过300目筛。
工序(2)将上述粉料置于微波炉内进行微波造核后，进行400℃预烧8小时，自然冷却至常温。
工序(3)对预烧后的料进行再次球磨后，在650℃灼烧10小时，过300目筛即成。
实施例4
工序(1)将锂与锰的原子比值为0.53的碳酸锂和电解二氧化锰物料混匀，按此混合料的8％加高分子网络剂，混匀成胶状，经球磨机球磨，过300目筛。
工序(2)将上述粉料置于微波炉内进行微波造核后，进行450℃预烧8小时，自然冷却至常温。
工序(3)对预烧后的料进行再次球磨后，在650℃灼烧10小时，过300目筛即成。
实施例5
工序(1)将锂与锰的原子比值为0.55的碳酸锂和电解二氧化锰物料混匀，按此混合料的8％加高分子网络剂，混匀成胶状，经球磨机球磨，过300目筛。
工序(2)将上述粉料置于微波炉内进行微波造核后，进行450℃预烧8小时，自然冷却至常温。
工序(3)对预烧后的料进行再次球磨后，在650℃灼烧10小时，过300目筛即成。
实施例6
工序(1)将锂与锰的原子比值为0.52的碳酸锂和电解二氧化锰物料混匀，按此混合料的8％加高分子网络剂，混匀成胶状，经球磨机球磨，过300目筛。
工序(2)将上述粉料置于微波炉内进行微波造核后，进行450℃预烧8小时，自然冷却至常温。
工序(3)对预烧后的料进行再次球磨后，在700℃灼烧10小时，过300目筛即成。
实施例7
工序(1)将锂与锰的原子比值为0.53的碳酸锂和电解二氧化锰物料混匀，按此混合料的10％加高分子网络剂，混匀成胶状，经球磨机球磨，过300目筛。
工序(2)将上述粉料置于微波炉内进行微波造核后，进行450℃预烧8小时，自然冷却至常温。
工序(3)对预烧后的料进行再次球磨后，在700℃灼烧10小时，过300目筛即成。
将上述方法制备的锂离子电池正极材料与锂离子电池负极材料石墨，以偏氟乙烯为极板粘结剂，分别制成锂离子电池的正极片与负极片，以聚丙烯微孔膜为电极隔膜，以体积比为碳酸二甲酯∶碳酸二乙酯∶碳酸乙烯酯＝1∶1∶1的1M六氟磷酸锂为电解液组装成锂离子电池。
各实施例制备的锂离子电池的性能表
Claims (1)
1.一种锂离子电池用锂锰氧化物正极材料的制备工艺，包括有固相合成和灼烧工序，其特征在于：工序(1)按锂：锰的原子比值为0.5-0.55的锂源和锰源物料混匀，按此混料的5-10％的比例加入聚丙烯酰胺，混匀成胶状，在球磨机内球磨、研细，过300目筛，工序(2)将工序(1)的粉料置于微波炉内进行微波造核后，在400-450℃干燥箱中进行预烧8小时，自然冷却至室温，工序(3)对预烧后的料进行第二次球磨后，放入干燥箱中进行550-700℃灼烧10小时后，过300目筛即成。
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| CN101746829B (zh) * | 2008-12-15 | 2013-08-07 | 山东神工海特电子科技有限公司 | 可充锂锰电池用复合MnO2正极材料制备方法 |
| CN104843795B (zh) * | 2015-04-30 | 2016-08-24 | 昆明理工大学 | 一种微波辅助制备锰氧化物晶须的方法 |
| CN112216815B (zh) * | 2019-07-11 | 2021-12-07 | 深圳市比亚迪锂电池有限公司 | 锂锰电池正极和锂锰电池 |
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| CN1395335A (zh) * | 2002-06-14 | 2003-02-05 | 中山大学 | 低温燃料电池纳米催化剂的制备方法 |
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- 2003-07-15 CN CNB031262570A patent/CN1324731C/zh not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1126380A (zh) * | 1994-11-03 | 1996-07-10 | 北京有色金属研究总院 | 用于锂二次电池的阴极材料及制法 |
| CN1042377C (zh) * | 1996-05-10 | 1999-03-03 | 中国科学院物理研究所 | 一种合成锂离子电池中正极材料的方法 |
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| CN1395335A (zh) * | 2002-06-14 | 2003-02-05 | 中山大学 | 低温燃料电池纳米催化剂的制备方法 |
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| CN1538541A (zh) | 2004-10-20 |
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