CN116544392A - 一种锂离子电池正极材料的制备方法 - Google Patents
一种锂离子电池正极材料的制备方法 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
- 239000010405 anode material Substances 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002270 dispersing agent Substances 0.000 claims abstract description 46
- 239000006185 dispersion Substances 0.000 claims abstract description 40
- 239000011162 core material Substances 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 35
- 239000007774 positive electrode material Substances 0.000 claims abstract description 35
- 238000003756 stirring Methods 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 125000002091 cationic group Chemical group 0.000 claims abstract description 23
- 125000000129 anionic group Chemical group 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- LTYBJDPMCPTGEE-UHFFFAOYSA-N (4-benzoylphenyl) prop-2-enoate Chemical compound C1=CC(OC(=O)C=C)=CC=C1C(=O)C1=CC=CC=C1 LTYBJDPMCPTGEE-UHFFFAOYSA-N 0.000 claims description 2
- RQGWOIYIEIOALO-UHFFFAOYSA-N 2-prop-1-enylisoindole-1,3-dione Chemical compound C1=CC=C2C(=O)N(C=CC)C(=O)C2=C1 RQGWOIYIEIOALO-UHFFFAOYSA-N 0.000 claims description 2
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 2
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 claims description 2
- CSCBZXDYYKIKTH-UHFFFAOYSA-N [O-2].[Al+3].[Ni+2].[Mn+2].[Co+2] Chemical compound [O-2].[Al+3].[Ni+2].[Mn+2].[Co+2] CSCBZXDYYKIKTH-UHFFFAOYSA-N 0.000 claims description 2
- FBDMTTNVIIVBKI-UHFFFAOYSA-N [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] Chemical compound [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] FBDMTTNVIIVBKI-UHFFFAOYSA-N 0.000 claims description 2
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 claims description 2
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 2
- 229910002102 lithium manganese oxide Inorganic materials 0.000 claims description 2
- DVATZODUVBMYHN-UHFFFAOYSA-K lithium;iron(2+);manganese(2+);phosphate Chemical compound [Li+].[Mn+2].[Fe+2].[O-]P([O-])([O-])=O DVATZODUVBMYHN-UHFFFAOYSA-K 0.000 claims description 2
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 claims description 2
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 claims description 2
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 claims description 2
- SQSAJLXDUSFNKX-UHFFFAOYSA-M sodium;3-(prop-2-enoylamino)butane-2-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)C(C)C(C)NC(=O)C=C SQSAJLXDUSFNKX-UHFFFAOYSA-M 0.000 claims description 2
- FZGFBJMPSHGTRQ-UHFFFAOYSA-M trimethyl(2-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCOC(=O)C=C FZGFBJMPSHGTRQ-UHFFFAOYSA-M 0.000 claims description 2
- 238000007086 side reaction Methods 0.000 abstract description 6
- 239000003792 electrolyte Substances 0.000 abstract description 5
- 230000004888 barrier function Effects 0.000 abstract description 3
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 14
- 229910021641 deionized water Inorganic materials 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 238000000576 coating method Methods 0.000 description 6
- 239000011247 coating layer Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
本发明公开了一种锂离子电池正极材料的制备方法,包括以下步骤:将阳离子型分散剂溶解于溶剂中,再加入正极内核材料,超声处理30~60min,继续搅拌1~5h,得到正极内核材料分散液;将阴离子型分散剂溶解于溶剂中,再加入无机包覆剂,超声处理30~60min,继续搅拌1~5h,得到无机包覆剂分散液;将正极内核材料分散液和无机包覆剂分散液混合搅拌均匀,在100~150℃下干燥12~24h,再进行热处理,得到正极材料。本发明利用异种电荷互相吸引的原理使得无机包覆剂点对点均匀地包覆在正极内核材料表面,在正极表面形成物理阻挡层,防止其与电解质发生副反应,提高正极材料的热稳定性、离子导电率及循环稳定性。
Description
技术领域
本发明涉及正极材料技术领域,具体涉及一种锂离子电池正极材料的制备方法。
背景技术
锂离子电池因其具有高比能量和长循环性能,在新能源汽车、移动设备、储能电站等领域受到广泛应用。随着技术的不断发展,人们对锂离子电池也提出更高的要求,设计研发具有更高容量、高功率、高比能量、循环稳定性好的电极材料已经成为新能源领域的研究热点之一。正极材料作为锂离子电池最重要的组件之一,其性能对锂离子电池的发展和应用有着关键作用。但是正极材料的结构相变及电解液副反应等不利因素制约着电池的性能,通常采用包覆的手段来解决上述问题。
包覆是一个简单、经济的方法,但包覆的均匀性及包覆层的厚度对正极材料性能起着关键的因素,因为大部分包覆材料是电化学惰性且绝缘的,当包覆层太薄无法完整包覆正极材料时,包覆层无法阻止内部过渡金属的溶解以及电极的副反应;当包覆层太厚时,会影响正极材料的导电性和锂离子扩散速度,从而影响材料的循环容量和速率性能,当包覆不均匀时,正极材料会出现嵌锂不均匀,导致材料颗粒内部的应力分布不均匀,从而正极材料内部产生裂纹,引起电解液与材料发生副反应,加速电池衰减。
发明内容
有鉴于此,本发明的目的是针对现有技术的不足,提供一种包覆均匀、性能稳定的锂离子电池正极材料的制备方法。
为达到上述目的,本发明采用以下技术方案:
一种锂离子电池正极材料的制备方法,包括以下步骤:
(1)将阳离子型分散剂溶解于溶剂中,再加入正极内核材料,超声处理30~60min,继续搅拌1~5h,得到正极内核材料分散液;
(2)将阴离子型分散剂溶解于溶剂中,再加入无机包覆剂,超声处理30~60min,继续搅拌1~5h,得到无机包覆剂分散液;
(3)将步骤(1)所制备的正极内核材料分散液和步骤(2)所制备的无机包覆剂分散液混合搅拌均匀,在100~150℃下干燥12~24h,再进行热处理,得到正极材料。
优选的,所述阳离子型分散剂由N-丙烯基邻苯二甲酰亚胺和丙烯酰氧乙基三甲基氯化铵聚合而成,其化学结构式为式I所示,
其中p,q=10~100。
优选的,所述正极内核材料为镍钴锰酸锂、镍钴锰酸铝、钴酸锂、锰酸锂、镍酸锂、磷酸铁锂、磷酸铁锰锂中的一种或多种。
优选的,所述阴离子型分散剂由4-丙烯酰氧基二苯甲酮和2-丙烯酰胺基-甲基丙磺酸钠盐聚合而成,其化学结构式如式II,
其中n,m=10~100。
优选的,所述无机包覆剂为Li2O·Al2O3·B2O3。
优选的,所述阳离子型分散剂与正极内核材料干粉的质量比为(0.001~0.02):1。
优选的,所述阴离子型分散剂与无机包覆剂干粉的质量比为(0.005~0.03):1。
优选的,步骤(3)中所述热处理的温度为400~600℃,热处理时间为5~12h。
本发明的有益效果是:
本发明采用阳离子型分散剂包覆在正极内核材料表面带正电荷,阴离子型分散剂包覆在无机包覆剂表面带负电荷,利用带有异种电荷的物体之间互相吸引的作用,使得无机包覆剂点对点均匀地包覆在正极内核材料表面,在正极表面形成物理阻挡层,防止其与电解质发生副反应,提高正极材料的热稳定性、离子导电率及循环稳定性;同时阳离子型分散剂和阴离子分散剂本身均匀地包覆在正极内核材料表面,起到分散作用,在高温热处理后,碳化形成薄薄的碳导电包覆层,进一步形成物理屏障,防止副反应,提高正极材料电子导电性及电化学稳定性,另外分散剂中的氮元素掺杂在正极材料的表面,形成空位,导致局部电子缺陷,进一步改善正极材料的导电率及电性能。
附图说明
图1为本发明循环容量保持率测试结果示意图。
具体实施方式
下面结合实施例对本发明作进一步描述。
实施例1:
阳离子型分散剂结构式为p和q=20;阴离子型分散剂结构式为/>n和m=20。
(1):取0.1g上述阳离子型分散剂溶解于30mL去离子水中,添加10gNCM811正极内核材料,超声处理30min,继续搅拌2h,得到正极内核材料分散液;
(2):取上述0.004g阴离子型分散剂溶解于5mL去离子水中,添加0.2gLi2O·Al2O3·B2O3,超声处理30min,继续搅拌2h,得到无机包覆剂分散液;
(3):将步骤(1)所制备的正极内核材料分散液和步骤(2)所制备的无机包覆剂分散液混合搅拌均匀,在120℃环境中干燥12h,升温至400℃热处理12h,得到正极材料。
实施例2:
阳离子型分散剂结构式为p和q=10;阴离子型分散剂结构式为/>n和m=10。
(1):取0.01g上述阳离子型分散剂溶解于30mL去离子水中,添加10gNCM811正极内核材料,超声处理30min,继续搅拌2h,得到正极内核材料分散液;
(2):取上述0.002g阴离子型分散剂溶解于5mL去离子水中,添加0.1gLi2O·Al2O3·B2O3,超声处理30min,继续搅拌2h,得到无机包覆剂分散液;
(3):将步骤(1)所制备的正极内核材料分散液和步骤(2)所制备的无机包覆剂分散液混合搅拌均匀,在120℃环境中干燥12h,升温至550℃热处理5h,得到正极材料。
实施例3:
阳离子型分散剂结构式为p和q=20;阴离子型分散剂结构式为/>n和m=20。
步骤(一):取0.1g上述阳离子型分散剂溶解于30mL去离子水中,添加10g NCM811正极内核材料,超声处理30min,继续搅拌2h,得到正极内核材料分散液;
步骤(二):取上述0.01g阴离子型分散剂溶解于5mL去离子水中,添加0.5gLi2O·Al2O3·B2O3,超声处理30min,继续搅拌2h,得到无机包覆剂分散液;
步骤(三):将步骤(一)所制备的正极内核材料分散液和步骤(二)所制备的无机包覆剂分散液混合搅拌均匀,在120℃环境中干燥12h,升温至550℃热处理10h,得到正极材料。
实施例4:
阳离子型分散剂结构式为p和q=30;阴离子型分散剂结构式为/>n和m=30。
步骤(一):取0.05g上述阳离子型分散剂溶解于30mL去离子水中,添加10g NCM811正极内核材料,超声处理30min,继续搅拌2h,得到正极内核材料分散液;
步骤(二):取上述0.004g阴离子型分散剂溶解于5mL去离子水中,添加0.2gLi2O·Al2O3·B2O3,超声处理30min,继续搅拌2h,得到无机包覆剂分散液;
步骤(三):将步骤(一)所制备的正极内核材料分散液和步骤(二)所制备的无机包覆剂分散液混合搅拌均匀,在120℃环境中干燥12h,升温至550℃热处理12h,得到正极材料。
实施例5:
阳离子型分散剂结构式为p和q=90;阴离子型分散剂结构式为/>n和m=90。
步骤(一):取0.2g上述阳离子型分散剂溶解于30mL去离子水中,添加10g NCM811正极内核材料,超声处理30min,继续搅拌2h,得到正极内核材料分散液;
步骤(二):取上述0.004g阴离子型分散剂溶解于5mL去离子水中,添加0.2gLi2O·Al2O3·B2O3,超声处理30min,继续搅拌2h,得到无机包覆剂分散液;
步骤(三):将步骤(一)所制备的正极内核材料分散液和步骤(二)所制备的无机包覆剂分散液混合搅拌均匀,在120℃环境中干燥12h,升温至550℃热处理12h,得到正极材料。
实施例6:
阳离子型分散剂结构式为p和q=50;阴离子型分散剂结构式为/>n和m=50。
步骤(一):取0.1g上述阳离子型分散剂溶解于30mL去离子水中,添加10g NCM811正极内核材料,超声处理30min,继续搅拌2h,得到正极内核材料分散液;
步骤(二):取上述0.004g阴离子型分散剂溶解于5mL去离子水中,添加0.2gLi2O·Al2O3·B2O3,超声处理30min,继续搅拌2h,得到无机包覆剂分散液;
步骤(三):将步骤(一)所制备的正极内核材料分散液和步骤(二)所制备的无机包覆剂分散液混合搅拌均匀,在120℃环境中干燥12h,升温至550℃热处理12h,得到正极材料。
对比例1
(1)取10g NCM811正极内核材料分散于30mL去离子水中,超声处理30min,继续搅拌2h,得到正极内核材料分散液;
(2)取0.2gLi2O·Al2O3·B2O3分散于10mL去离子水中,超声处理30min,继续搅拌2h,得到无机包覆剂分散液;
(3)将步骤(1)所制备的正极内核材料分散液和步骤(2)所制备的无机包覆剂分散液混合搅拌均匀,在120℃环境中干燥12h,升温至550℃热处理12h,得到正极材料。
将实施例1、4和对比例1所制备的正极活性材料分别与PVDF、SP按照95:3:2的比值进行匀浆混合,再进行涂布、冲片得到正电极,负极片以石墨、SP、CMC和SBR按照95:1:1.5:2.5的比例进行匀浆混合,再进行涂布、冲片得到负电极,以LiPF6/EC+DEC+DMC作为电解液(体积比为1:1:1),隔膜为商业化陶瓷隔膜,组装成软包电池,以1/3C充电,1/3C放电进行循环测试,结果如图1所示。从图1中可以看出,本发明制备的正极材料具有较好的电化学稳定性。
最后说明的是,以上实施例仅用以说明本发明的技术方案而非限制,本领域普通技术人员对本发明的技术方案所做的其他修改或者等同替换,只要不脱离本发明技术方案的精神和范围,均应涵盖在本发明的权利要求范围当中。
Claims (8)
1.一种锂离子电池正极材料的制备方法,其特征在于,包括以下步骤:
(1)将阳离子型分散剂溶解于溶剂中,再加入正极内核材料,超声处理30~60min,继续搅拌1~5h,得到正极内核材料分散液;
(2)将阴离子型分散剂溶解于溶剂中,再加入无机包覆剂,超声处理30~60min,继续搅拌1~5h,得到无机包覆剂分散液;
(3)将步骤(1)所制备的正极内核材料分散液和步骤(2)所制备的无机包覆剂分散液混合搅拌均匀,在100~150℃下干燥12~24h,再进行热处理,得到正极材料。
2.根据权利要求1所述的锂离子电池正极材料的制备方法,其特征在于,所述阳离子型分散剂由N-丙烯基邻苯二甲酰亚胺和丙烯酰氧乙基三甲基氯化铵聚合而成,其化学结构式为式I所示,
其中p,q=10~100。
3.根据权利要求1所述的锂离子电池正极材料的制备方法,其特征在于,所述正极内核材料为镍钴锰酸锂、镍钴锰酸铝、钴酸锂、锰酸锂、镍酸锂、磷酸铁锂、磷酸铁锰锂中的一种或多种。
4.根据权利要求1所述的锂离子电池正极材料的制备方法,其特征在于,所述阴离子型分散剂由4-丙烯酰氧基二苯甲酮和2-丙烯酰胺基-甲基丙磺酸钠盐聚合而成,其化学结构式如式II,
其中n,m=10~100。
5.根据权利要求1所述的锂离子电池正极材料的制备方法,其特征在于,所述无机包覆剂为Li2O·Al2O3·B2O3。
6.根据权利要求1所述的锂离子电池正极材料的制备方法,其特征在于,所述阳离子型分散剂与正极内核材料干粉的质量比为(0.001~0.02):1。
7.根据权利要求1所述的锂离子电池正极材料的制备方法,其特征在于,所述阴离子型分散剂与无机包覆剂干粉的质量比为(0.005~0.03):1。
8.根据权利要求1所述的锂离子电池正极材料的制备方法,其特征在于,步骤(3)中所述热处理的温度为400~600℃,热处理时间为5~12h。
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