CN104218234B - 一种高循环性能的锂离子电池复合正极材料及其制备方法 - Google Patents
一种高循环性能的锂离子电池复合正极材料及其制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 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
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000010406 cathode material Substances 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 48
- 239000011149 active material Substances 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 238000007873 sieving Methods 0.000 claims abstract description 12
- PFYQFCKUASLJLL-UHFFFAOYSA-N [Co].[Ni].[Li] Chemical compound [Co].[Ni].[Li] PFYQFCKUASLJLL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- OVAQODDUFGFVPR-UHFFFAOYSA-N lithium cobalt(2+) dioxido(dioxo)manganese Chemical compound [Li+].[Mn](=O)(=O)([O-])[O-].[Co+2] OVAQODDUFGFVPR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 229910013716 LiNi Inorganic materials 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 4
- 238000004381 surface treatment Methods 0.000 claims description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000010405 anode material Substances 0.000 claims description 2
- 239000011164 primary particle Substances 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052744 lithium Inorganic materials 0.000 abstract description 5
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 abstract description 3
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 6
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910002991 LiNi0.5Co0.2Mn0.3O2 Inorganic materials 0.000 description 2
- 229910002995 LiNi0.8Co0.15Al0.05O2 Inorganic materials 0.000 description 2
- 229910015866 LiNi0.8Co0.1Al0.1O2 Inorganic materials 0.000 description 2
- 229910001228 Li[Ni1/3Co1/3Mn1/3]O2 (NCM 111) Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 229910021161 Co0.1Al0.1O2 Inorganic materials 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 229910015760 LiNi0.8Co0.18Al0.02O2 Inorganic materials 0.000 description 1
- 229910015872 LiNi0.8Co0.1Mn0.1O2 Inorganic materials 0.000 description 1
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical group [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000013500 performance material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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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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Abstract
本发明涉及一种高循环性能的锂离子电池复合正极材料及其制备方法，由LiNi1‑m‑ nComAlnO2和LiNiaCo1‑a‑bMnbO2两种活性物质组成，其中0.1<m<0.3，0.01<n<0.2，0<1‑m‑n<1，0<a<1，0<b<1，0<1‑a‑b<1，镍钴铝酸锂占镍钴铝酸锂和镍钴锰酸锂质量总和的10%～90%。它是将LiNi1‑m‑nComAlnO2和LiNiaCo1‑a‑bMnbO2两种活性物质按一定的比例混合均匀，经煅烧后冷却、粉碎、过筛或者经表面处理后煅烧、冷却、粉碎、过筛而得到。本发明复合材料的比容量相对于镍钴锰酸锂有了较大幅的提高，热稳定性及安全性能相对于镍钴铝酸锂材料有所提高，特别是循环性能良好。
Description
技术领域
本发明涉及一种锂离子电池，特别是涉及一种高循环性能的锂离子电池复合正极材料及其制备方法。
技术背景
作为一种新型绿色二次电池，锂电池具有体积小、质量轻、比容量大、循环寿命长、自放电小和无记忆效应等优点，目前已经广泛应用于便携式移动电子产品和电动交通工具等领域。随着科技的进步，锂离子电池的应用领域将越来越广，对其尺寸、重量、使用寿命等的要求也越来越高，目前市场上应用的钴酸锂、磷酸铁锂、锰酸锂等正极材料已经难以满足市场对锂离子电池高能量密度的需求。
用于锂离子电池正极材料的镍钴铝酸锂材料具有电压平台高、比容量大、能量密度高等优点而备受关注，但由于含镍量高，材料稳定性差，安全性能差。与镍钴锰酸锂三元材料相比，镍钴铝酸锂最大缺点是热稳定性差，同时镍钴铝酸锂对环境水分比较敏感，制浆过程中容易出现“果冻”现象。将两种材料混合后进行表面处理以及煅烧处理，使得整体材料的比容量得到改善，同时对混合材料进行表面处理，减少表面杂质，降低材料pH值，使材料的电化学性能、循环性能及材料加工性能均得到改善。
发明内容
本发明的目的在于提供一种高循环性能的低成本的锂离子电池复合正极材料，克服现有正极材料的不足，同时对混合后的材料进行表面处理，提高材料的循环性能。
为了实现上述目的，本发明采用了以下技术方案：
第一个方面，一种高循环性能的锂离子电池复合正极材料，所述的复合正极材料由LiNi1-m-nComAlnO2和LiNiaCo1-a-bMnbO2两种活性物质组成，其中0.1<m<0.3，0.01<n<0.2，0<1-m-n<1，0<a<1，0<b<1，0<1-a-b<1。
作为优选，所述的镍钴铝酸锂占镍钴铝酸锂和镍钴锰酸锂质量总和的10%～90%。
第二个方面，一种如第一个方面所述的高循环性能的锂离子电池复合正极材料的制备方法，其特征在于，包括以下步骤：
⑴ 将一定量的LiNi1-m-nComAlnO2和LiNiaCo1-a-bMnbO2两种活性物质按一定的比例混合均匀；
⑵ 将混合材料在一定温度下煅烧一段时间后，冷却、粉碎、过筛得到复合正极材料；或者，将混合后的材料进行表面处理，然后将处理后的混合材料在一定温度下煅烧一段时间后，冷却、粉碎、过筛得到复合正极材料。
作为优选，所述的LiNi1-m-nComAlnO2的D50为5～20μm，LiNiaCo1-a-bMnbO2的D50为5～20μm。
作为进一步优化，所述的LiNi1-m-nComAlnO2为一次颗粒团聚而成的二次颗粒，D50为10～16μm，D10≥5μm，D90≤30μm，所述的LiNiaCo1-a-bMnbO2的D50为10～16μm，D10≥5μm，D90≤30μm。
作为优选，所述的LiNi1-m-nComAlnO2包括纯的LiNi1-m-nComAlnO2材料以及采用任何表面改性或结构掺杂改性等手段处理过的LiNi1-m-nComAlnO2；所述的LiNiaCo1-a-bMnbO2包括纯的LiNiaCo1-a-bMnbO2材料以及采用任何表面改性或结构掺杂改性等手段处理过的LiNi1-m-nComAlnO2材料。
作为优选，所述的表面处理包括任何能减少混合材料表面残留的碳酸锂、氧化锂杂质的处理方法。
作为优选，所述的表面处理还包括任何对混合后材料表面进行包覆改性的处理方法。
作为优选，所述的煅烧温度为300～900℃，煅烧时间为3～24h。
与现有的技术相比，本发明的最大优点和有益效果如下：
⑴ 将两种材料按照一定比例进行混合均匀后进行烧结的制备方法，使所得的复合材料的比容量相对于镍钴锰酸锂有了较大幅的提高，热稳定性及安全性能相对于镍钴铝酸锂材料有所提高。
⑵ 对混合后的材料进行表面处理，使复合材料表面残留的碳酸锂、氧化锂等杂质得到进一步清除，提高了材料的导电性能。
⑶ 通过对复合材料进行表面处理，降低材料的pH值，同时对材料进行低温处理，可以提高材料的加工性能，保证极片的一致性。
⑷ 对混合后的材料进行表面包覆，使得包覆层在隔绝电解液与正极材料的同时使锂离子自由通过，从而在完成充放电的同时避免电解液在高电压下的分解，提高了离子电池的循环寿命以及稳定性。
附图说明
图1是实施例1的复合正极材料的首次充放电曲线图。
图2是实施例1的复合正极材料的循环充放电曲线图。
具体实施方式
为了对本发明有更深的了解，下面结合实施例对技术方案进行清楚、完整地描述，但是本发明的实施例仅仅是为了解释本发明，并非限制本发明，本领域技术人员在没有做出创造性劳动的前提下所获得的所有其他实施案例，均属于本发明的保护范围。
实施例1：
将LiNi0.8Co0.15Al0.05O2和LiNi1/3Co1/3Mn1/3O2两种活性物质按5:5的比例进行干混，混料时间为2h。
将混合后的混合材料放入炉中进行焙烧处理，以4℃/min的升温速率升至500℃，并在500℃保温7h，冷却、粉碎、过筛后得到复合正极材料。
材料的电化学性能测试采用蓝电电池测试系统在25℃下进行测试，测试电压范围为3V～4.3V；倍率性能测试条件：0.2C充放电一次，0.2C充电1C放电一次；循环性能测试条件：以1C倍率进行充放电，循环100周，考察容量保持率。0.2C倍率下放电比容量为189.7mAh/g，1C倍率下的放电比容量为177.8mAh/g，1C/0.2C放电比率为94.3%，倍率性能较好。1C充放电循环100周容量保持率大于98%，循环性能较好。
实施例2：
将LiNi0.8Co0.15Al0.05O2和LiNi0.5Co0.2Mn0.3O2两种活性物质按6:4的比例进行干混，混料时间为2h。
将混合后的混合材料放入炉中进行焙烧处理，以5℃/min的升温速率升至700℃，并在700℃保温8h，冷却、粉碎、过筛后得到复合正极材料。
实施例3：
将LiNi0.8Co0.1Al0.1O2和表面包覆质量分数为1%氧化铝的LiNi0.5Co0.2Mn0.3O2两种活性物质按4:6的比例进行干混，混料时间为2h。
将混合后混合材料放入炉中进行焙烧处理，以5℃/min的升温速率升至800℃，并在800℃保温6h，冷却、粉碎、过筛后得到复合正极材料。
实施例4：
将LiNi0.8Co0.1Al0.1O2和LiNi1/3Co1/3Mn1/3O2两种活性物质按3:7的比例进行干混，混料时间为2h。
将硝酸铝在室温下配制成硝酸铝溶液，将上述混合后的活性物质加入到硝酸铝溶液中搅拌形成固液混合物，使硝酸铝溶液均匀包覆在活性物质颗粒表面；由硝酸铝煅烧后形成Al2O3的质量占混合后活性物质质量的1%。
将上述固液混合物进行干燥，将干燥后的固体材料放入炉中进行焙烧处理，以4℃/min的升温速率升至600℃，并在600℃保温5h，冷却、粉碎、过筛后得到复合正极材料。
实施例5：
将LiNi0.8Co0.18Al0.02O2和LiNi0.8Co0.1Mn0.1O2两种活性物质按4:6的比例进行干混，混料时间为2h。
将上述混合后的活性物质进行酸洗，然后水洗。
将上述固液混合物进行喷雾干燥，将干燥后的固体材料放入炉中进行焙烧处理，以4℃/min的升温速率升至600℃，并在600℃保温5h，冷却、粉碎、过筛后得到复合正极材料。
实施例6：
将表面包覆质量分数为0.5%氧化镁的LiNi0.8Co0.1Al0.1O2和LiNi0.5Co0.2Mn0.3O2两种活性物质按4:6的比例进行干混，混料时间为2h。
将混合后混合材料放入炉中进行焙烧处理，以5℃/min的升温速率升至800℃，并在800℃保温6h，冷却、粉碎、过筛后得到复合正极材料。
Claims (6)
1.一种高循环性能的锂离子电池复合正极材料的制备方法，所述锂离子电池复合正极材料由LiNi1-m-nComAlnO2和LiNiaCo1-a-bMnbO2两种活性物质组成，其中0.1<m<0.3，0.01<n<0.2，0<1-m-n<1，0<a<1，0<b<1，0<1-a-b<1；其特征在于，所述制备方法包括以下步骤：
⑴ 将一定量的LiNi1-m-nComAlnO2和LiNiaCo1-a-bMnbO2两种活性物质按一定的比例混合均匀；所述的LiNi1-m-nComAlnO2为一次颗粒团聚而成的二次颗粒，D50为10～16μm，D10≥5μm，D90≤30μm，所述的LiNiaCo1-a-bMnbO2的D50为10～16μm，D10≥5μm，D90≤30μm；
⑵ 将混合材料在一定温度下煅烧一段时间后，冷却、粉碎、过筛得到复合正极材料；或者，将混合后的材料进行表面处理，然后将处理后的混合材料在一定温度下煅烧一段时间后，冷却、粉碎、过筛得到复合正极材料。
2.根据权利要求1所述的高循环性能的锂离子电池复合正极材料的制备方法，其特征在于，所述的镍钴铝酸锂占镍钴铝酸锂和镍钴锰酸锂质量总和的10%～90%。
3.根据权利要求1所述的高循环性能的锂离子电池复合正极材料的制备方法，其特征在于，所述的LiNi1-m-nComAlnO2包括纯的LiNi1-m-nComAlnO2材料以及采用任何表面改性或结构掺杂改性手段处理过的LiNi1-m-nComAlnO2；所述的LiNiaCo1-a-bMnbO2包括纯的LiNiaCo1-a- bMnbO2材料以及采用任何表面改性或结构掺杂改性手段处理过的LiNi1-m-nComAlnO2材料。
4.根据权利要求1所述的高循环性能的锂离子电池复合正极材料的制备方法，其特征在于，所述的表面处理包括任何能减少混合材料表面残留的碳酸锂、氧化锂杂质的处理方法。
5.根据权利要求1所述的高循环性能的锂离子电池复合正极材料的制备方法，其特征在于，所述的表面处理还包括任何对混合后材料表面进行包覆改性的处理方法。
6.根据权利要求1所述的高循环性能的锂离子电池复合正极材料的制备方法，其特征在于，所述的煅烧温度为300～900℃，煅烧时间为3～24h。
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