CN1225040C - 一种锂离子电池锂钴氧化物正极材料的制备工艺 - Google Patents
一种锂离子电池锂钴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 19
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 19
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000010406 cathode material Substances 0.000 title 1
- 238000000498 ball milling Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 19
- 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
- 239000000463 material Substances 0.000 claims abstract description 15
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 13
- 239000010941 cobalt Substances 0.000 claims abstract description 13
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 13
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 4
- 239000007774 positive electrode material Substances 0.000 claims description 15
- 230000004520 agglutination Effects 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 9
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 9
- 235000015110 jellies Nutrition 0.000 claims description 9
- 239000008274 jelly Substances 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 2
- 239000010405 anode material Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 238000007873 sieving Methods 0.000 abstract 3
- 239000000084 colloidal system Substances 0.000 abstract 2
- 238000010304 firing Methods 0.000 abstract 2
- 238000000227 grinding Methods 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 230000002441 reversible effect Effects 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
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 239000007772 electrode material Substances 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
- 230000035800 maturation Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 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
- H01M4/13—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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- 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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Abstract
本发明公开了一种锂离子电池锂钴氧化物正极材料的制备工艺，包括固相合成和高温灼烧工序，其特征在于：工序(1)以原子比，锂∶钴＝1-1.1∶1的碳酸锂和氧化钴料混匀后，按此混料的5-10%加入聚丙稀酰胺，搅拌均匀成胶状，工序(2)上述胶状物经干燥箱在150℃下烘干30-80小时，在球磨机中球磨研细，过300目筛，工序(3)上述粉料在400℃-500℃下预烧10小时，自然冷却至室温，工序(4)对预烧的粉料进行球磨研细并过300目筛后，在650-800℃下灼烧，过300目筛即制成锂离子电池锂钴氧化物正极材料。本发明由于在同相合成工序中加入了聚丙稀酰胺，使锂与钴在原子级水平进行混合，可在相对较低温度条件下得到结晶性好纯度较高的锂钴氧化物，因而本发明具有较高的比容量及良好的循环性能的优点。
Description
技术领域：
本发明涉及一种锂离子电池，特别是一种锂离子电池锂钴氧化物正极材料的制备工艺。
背景技术：
锂离子电池的迅猛发展，对电极材料的需求也有大的发展，锂钴氧化物是目前唯一成熟大量使用的锂离子电池的正极材料，但该材料的可逆的嵌入脱嵌晶格的锂离子摩尔百分数55％，在过充电条件下，由于锂含量的减少和平均金属离子氧化水平的升高，降低了材料的稳定性，而且钴资源的稀有，其成本高。
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锂钴氧化物正极材料的制备工艺，所制备的锂钴氧化物正极材料不仅具有优良的电化学性能，且其材料的稳定性有较大提高。本发明的技术方案是，一种锂离子电池锂钴氧化物正极材料的制备工艺，包括固相合成和高温灼烧工序，其特征在于：工序(1)以原子比，锂∶钴为1-1.1∶1的碳酸锂和氧化钴料混匀后，按此混料的5-10％加入聚丙烯酰胺，搅拌均匀成胶状，工序(2)上述胶状物经干燥箱在150℃下烘干30-80小时，在球磨机中球磨研细，过300目筛，工序(3)上述粉料在400℃-500℃下预烧10小时，自然冷却至室温，工序(4)对预烧的粉料进行球磨研细并过300目筛后，在650-800℃下灼烧，过300目筛即制成锂离子电池锂钴氧化物正极材料。
本发明由于在固相合成中加入聚丙烯酰胺，使锂与钴在原子级水平发生混合，可在相对较低温度条件下就能得到结晶性好纯度较高的锂钴氧化物，因而本发明具有较高的可逆比容量及良好的循环性能的优点。
具体实施方式：
实施例1
工序(1)以原子比，锂∶钴＝1∶1的碳酸锂和氧化钴料混匀，按此混料的5％加入聚丙烯酰胺，搅拌均匀成胶状。
工序(2)上述胶状物经干燥箱在150℃下烘干30-80小时，在球磨机中球磨研细，过300目筛。
工序(3)上述粉料在400℃下预烧10小时，自然冷却至室温。
工序(4)对预烧的粉料进行球磨研细并过300目筛后在650℃条件下灼烧3小时，过300目筛即成所要的锂钴氧化物正极材料。
实施例2
工序(1)以原子比，锂∶钴＝1∶1的碳酸锂和氧化钴料混匀，按此混料的5％加入聚丙烯酰胺，搅拌均匀成胶状。
工序(2)上述胶状物径干燥箱在150℃下烘干30-80小时，在球磨机中球磨研细，过300目筛。
工序(3)上述粉料在400℃下预烧10小时，自然冷却至室温。
工序(4)对预烧的粉料进行球磨研细并过300目筛后在650℃条件下灼烧3小时，过300目筛即成所要的锂钴氧化物正极材料。
实施例3
工序(1)以原子比，锂∶钴＝1∶1的碳酸锂和氧化钴料混匀，按此混料的8％加入聚丙烯酰胺，搅拌均匀成胶状。
工序(2)上述胶状物径干燥箱在150℃下烘干30-80小时，在球磨机中球磨研细，过300目筛。
工序(3)上述粉料在400℃下预烧10小时，自然冷却至室温。
工序(4)对预烧的粉料进行球磨研细并过300目筛后在700℃条件下灼烧3小时，过300目筛即成所要的锂钴氧化物正极材料。
实施例4
工序(1)以原子比，锂∶钴＝1.05∶1的碳酸锂和氧化钴料混匀，按此混料的8％加入聚丙烯酰胺，搅拌均匀成胶状。
工序(2)上述胶状物经干燥箱在150℃下烘干30-80小时，在球磨机中球磨研细，过300目筛。
工序(4)对预烧的粉料进行球磨研细并过300目筛后在750℃条件下灼烧3小时，过300目筛即成所要的锂钴氧化物正极材料。
实施例5
工序(1)以原子比，锂∶钴＝1.05∶1的碳酸锂和氧化钴料混匀，按此混料的8％加入聚丙烯酰胺，搅拌均匀成胶状。
工序(2)上述胶状物经干燥箱在150℃下烘干30-80小时，在球磨机中球磨研细，过300目筛。
工序(3)上述粉料在400℃下预烧10小时，自然冷却至室温。
工序(4)对预烧的粉料进行球磨研细并过300目筛后在800℃条件下灼烧3小时，过300目筛即成所要的锂钴氧化物正极材料。
实施例6
工序(1)以原子比，锂∶钴＝1.1∶1的碳酸锂和氧化钴料混匀，按此混料的10％加入聚丙烯酰胺，搅拌均匀成胶状。
工序(2)上述胶状物经干燥箱在150℃下烘干30-80小时，在球磨机中球磨研细，过300目筛。
工序(3)上述粉料在400℃下预烧10小时，自然冷却至室温。
工序(4)对预烧的粉料进行球磨研细并过300目筛后在800℃条件下灼烧3小时，过300目筛即成所要的锂钴氧化物正极材料。
实施例7
工序(1)以原子比，锂∶钴＝1.1∶1的碳酸锂和氧化钴料混匀，按此混料的10％加入聚丙烯酰胺，搅拌均匀成胶状。
工序(2)上述胶状物经干燥箱在150℃下烘干30-80小时，在球磨机中球磨研细，过300目筛。
工序(3)上述粉料在400℃下预烧10小时，自然冷却至室温。
工序(4)对预烧的粉料进行球磨研细并过300目筛后在800℃条件下灼烧3小时，过300目筛即成所要的锂钴氧化物正极材料。
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)
1.一种锂离子电池锂钴氧化物正极材料的制备工艺，包括固相合成和高温灼烧工序，其特征在于：工序(1)以原子比，锂∶钴为1-1.1∶1的碳酸锂和氧化钴料混匀后，按此混料的5-10％加入聚丙烯酰胺，搅拌均匀成胶状，工序(2)上述胶状物经干燥箱在150℃下烘干30-80小时，在球磨机中球磨研细，过300目筛，工序(3)上述粉料在400℃-500℃下预烧10小时，自然冷却至室温，工序(4)对预烧的粉料进行球磨研细并过300目筛后，在650-800℃下灼烧，过300目筛即制成锂离子电池锂钴氧化物正极材料。
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