CN113562781A - 一种高镍锂离子电池正极材料的改性方法 - Google Patents
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 28
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 20
- 239000007774 positive electrode material Substances 0.000 title claims abstract description 16
- 238000002715 modification method Methods 0.000 title description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 20
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 229920002620 polyvinyl fluoride Polymers 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 239000010406 cathode material Substances 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 229910013716 LiNi Inorganic materials 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims abstract description 7
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
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- 229910052782 aluminium Inorganic materials 0.000 description 1
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Abstract
一种高镍锂离子电池正极材料的改性方法,包括将高镍正极材料(LiNi0.8Co0.1Mn0.1O2)置于反应器内,反应器内抽真空,加入乙醇和环己醇的混合液,快速搅拌1~2h,过滤,在管式炉中进行煅烧0.5~2h,冷却后备用;将聚氟乙烯加入到丙酮中,升温至75~80℃进行搅拌并将步骤S1中的产物加入其中,搅拌2~5h,然后过滤,球磨,干燥后得到所述正极材料。
Description
技术领域
本发明属于锂离子电池正极材料技术领域,具体涉及一种高镍锂离子电池正极材料的改性方法。
背景技术
锂离子电池因具有高能量密度、高工作电压等优势而被广泛应用于各类电动储能装置。其中,正极材料的成本约占总体成本40%,因而,制备出高容量、高循环稳定性以及低成本的正极材料对于降低电池成本而言是至关重要的。近年来,高镍系三元材料由于具有较高的能量密度而成为动力型锂离子电池首选的正极材料。但高镍材料在实际应用过程中存在的容量衰减问题使其大规模的商用受到限制。其中,高镍材料二次颗粒内部产生的微裂纹是造成材料容量衰减的一个重要原因。这主要是因为组成二次球颗粒的一次颗粒在空间取向上呈现无序性,因而,在充放电过程中二次颗粒内部晶界处存在各向异性的应力应变,这容易引发颗粒晶界处微裂纹的产生;并且,随着材料在脱/嵌锂的过程中晶格的伸缩,更进一步地促使了微裂纹的增生并向一次颗粒内部延伸,最后致使一次颗粒的破碎与粉化。
发明内容
本发明的目的是提供一种高镍锂离子电池正极材料的改性方法,所述制备方法包括以下步骤:
S1:将高镍正极材料(LiNi0.8Co0.1Mn0.1O2)置于反应器内,反应器内抽真空,加入乙醇和环己醇的混合液,快速搅拌1~2h,过滤,在管式炉中进行煅烧0.5~2h,冷却后备用。
S2:将聚氟乙烯加入到丙酮中,升温至75~80℃进行搅拌并将步骤S1中的产物加入其中,搅拌2~5h,然后过滤,球磨,干燥后得到所述正极材料。
优选的,所述步骤S1中乙醇和环己醇的混合液中乙醇和环己醇的体积比为(1~1.5):(1.2~2.6)。
优选的,所述步骤S1中管式炉煅烧的温度为500~550℃。
优选的,所述步骤S2中聚氟乙烯和丙酮的质量体积比为(3~5)g:(110~140)mL。
优选的,所述步骤S2中丙酮和步骤S1中的产物的质量体积比为(5.2~8.4)mL:(120~160)g。
优选的,所述步骤S2中干燥的温度为100~105℃,干燥时间为2~3h。
与现有技术相比,本发明具有如下有益效果:
本发明中,在高镍材料表面形成了一个稳定界面,减少了活性物质在电解液中的暴露,减缓了电极材料的腐蚀,减少了界面副反应,减少了分解的电解液在电极表面的沉积;所得锂离子电池高镍三元正极材料具有稳定的晶界修饰层,可大大提高晶界对应力的承受能力,抑制循环过程中晶间裂纹的产生;晶界修饰层可以阻止前驱体一次颗粒之间的融合,防止二次再结晶,有利于提高正极材料的循环稳定性。
附图说明
图1为本发明实施例1改性正极材料的SEM图谱;
具体实施方式
下面对本发明实施例作具体详细的说明,本实施例在本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
实施例1
一种高镍锂离子电池正极材料的改性方法,具体包括以下步骤:
S1:将高镍正极材料(LiNi0.8Co0.1Mn0.1O2)置于反应器内,反应器内抽真空,加入乙醇和环己醇的混合液,快速搅拌1h,过滤,在管式炉中进行煅烧0.5h,冷却后备用;其中乙醇和环己醇的体积比为1:1.2,管式炉煅烧的温度为500℃。
S2:将聚氟乙烯加入到丙酮中,升温至75℃进行搅拌并将步骤S1中的产物加入其中,搅拌2h,然后过滤,球磨,干燥后得到所述正极材料;其中聚氟乙烯和丙酮的质量体积比为3g:110mL;丙酮和步骤S1中的产物的质量体积比为5.2mL:120g;干燥的温度为100℃,干燥时间为2h。
实施例2
一种高镍锂离子电池正极材料的改性方法,具体包括以下步骤:
S1:将高镍正极材料(LiNi0.8Co0.1Mn0.1O2)置于反应器内,反应器内抽真空,加入乙醇和环己醇的混合液,快速搅拌2h,过滤,在管式炉中进行煅烧2h,冷却后备用;其中乙醇和环己醇的体积比为1.5:2.6,管式炉煅烧的温度为550℃。
S2:将聚氟乙烯加入到丙酮中,升温至80℃进行搅拌并将步骤S1中的产物加入其中,搅拌5h,然后过滤,球磨,干燥后得到所述正极材料;其中聚氟乙烯和丙酮的质量体积比为5g:140mL;丙酮和步骤S1中的产物的质量体积比为8.4mL:160g;干燥的温度为105℃,干燥时间为3h。
实施例3
一种高镍锂离子电池正极材料的改性方法,具体包括以下步骤:
S1:将高镍正极材料(LiNi0.8Co0.1Mn0.1O2)置于反应器内,反应器内抽真空,加入乙醇和环己醇的混合液,快速搅拌1.5h,过滤,在管式炉中进行煅烧1h,冷却后备用;其中乙醇和环己醇的体积比为1.2:1.8,管式炉煅烧的温度为520℃。
S2:将聚氟乙烯加入到丙酮中,升温至77℃进行搅拌并将步骤S1中的产物加入其中,搅拌3h,然后过滤,球磨,干燥后得到所述正极材料;其中聚氟乙烯和丙酮的质量体积比为4g:120mL;丙酮和步骤S1中的产物的质量体积比为5.9mL:140g;干燥的温度为102℃,干燥时间为2.5h。
实施例4
一种高镍锂离子电池正极材料的改性方法,具体包括以下步骤:
S1:将高镍正极材料(LiNi0.8Co0.1Mn0.1O2)置于反应器内,反应器内抽真空,加入乙醇和环己醇的混合液,快速搅拌2h,过滤,在管式炉中进行煅烧1.5h,冷却后备用;其中乙醇和环己醇的体积比为1.4:2.3,管式炉煅烧的温度为540℃。
S2:将聚氟乙烯加入到丙酮中,升温至78℃进行搅拌并将步骤S1中的产物加入其中,搅拌4h,然后过滤,球磨,干燥后得到所述正极材料;其中聚氟乙烯和丙酮的质量体积比为4.6g:130mL;丙酮和步骤S1中的产物的质量体积比为8.1mL:150g;干燥的温度为104℃,干燥时间为2.8h。
实验例
电池组装:将活性物质、super-P和PVDF(聚偏氟乙烯)按88:7:5的质量比溶解于N-甲基吡络烷酮溶液中,充分混合均匀后涂覆于铝箔上,经过烘干、压片、冲片制成直径13mm电极片,最后在120℃真空干燥16h。所组装的锂离子电池均为2032型扣式电池,所有电池均在高纯氩气保护的手套箱内(水氧含量低于1×10-6)组装,半电池均采用金属锂作为对电极,隔膜型号为Celgard-2500,本实验中采用的电解液为1mol/LLiPF6,其中溶剂为EC+DMC+EMC(体积比为1:1:1)。
性能测试:采用扫描电子显微镜和高分辨透射电镜对材料进行形貌分析;采用蓝电电池测试***进行恒流充放电测试,电压范围是2.8~4.3V;交流阻抗图谱通过IM6电化学工作站进行测试获得,其中设置扰动正弦电压振幅为5mV,测试频率范围控制在0.01Hz~100kHz,其测试结果如表1所示,
表1.测试结果:
从表1中可以看出,实施例1~4中改性的正极材料具有良好的循环稳定性和较低电荷转移电阻。
Claims (6)
1.一种高镍锂离子电池正极材料的改性方法,其特征在于,所述制备方法包括以下步骤:
S1:将高镍正极材料(LiNi0.8Co0.1Mn0.1O2)置于反应器内,反应器内抽真空,加入乙醇和环己醇的混合液,快速搅拌1~2h,过滤,在管式炉中进行煅烧0.5~2h,冷却后备用;
S2:将聚氟乙烯加入到丙酮中,升温至75~80℃进行搅拌并将步骤S1中的产物加入其中,搅拌2~5h,然后过滤,球磨,干燥后得到所述正极材料。
2.根据权利要求1所述的一种高镍锂离子电池正极材料的改性方法,其特征在于,所述步骤S1中乙醇和环己醇的混合液中乙醇和环己醇的体积比为(1~1.5):(1.2~2.6)。
3.根据权利要求1所述的一种高镍锂离子电池正极材料的改性方法,其特征在于,所述步骤S1中管式炉煅烧的温度为500~550℃。
4.根据权利要求1所述的一种高镍锂离子电池正极材料的改性方法,其特征在于,所述步骤S2中聚氟乙烯和丙酮的质量体积比为(3~5)g:(110~140)mL。
5.根据权利要求1所述的一种高镍锂离子电池正极材料的改性方法,其特征在于,所述步骤S2中丙酮和步骤S1中的产物的质量体积比为(5.2~8.4)mL:(120~160)g。
6.根据权利要求1所述的一种高镍锂离子电池正极材料的改性方法,其特征在于,所述步骤S2中干燥的温度为100~105℃,干燥时间为2~3h。
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