CN104112853B - 一种锂离子电池层状正极材料及其制备方法 - Google Patents
一种锂离子电池层状正极材料及其制备方法 Download PDFInfo
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- 239000010406 cathode material Substances 0.000 title claims abstract description 39
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 31
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 26
- 238000000576 coating method Methods 0.000 claims abstract description 26
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 15
- -1 thio ammonium molybdate Chemical compound 0.000 claims abstract description 12
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 11
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 11
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 11
- 238000000137 annealing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 8
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 8
- 239000010409 thin film Substances 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910032387 LiCoO2 Inorganic materials 0.000 claims description 5
- 229910001228 Li[Ni1/3Co1/3Mn1/3]O2 (NCM 111) Inorganic materials 0.000 claims description 5
- 229910016722 Ni0.5Co0.2Mn0.3 Inorganic materials 0.000 claims description 5
- 229910016771 Ni0.5Mn0.5 Inorganic materials 0.000 claims description 4
- 238000005253 cladding Methods 0.000 abstract description 9
- 229910052723 transition metal Inorganic materials 0.000 abstract description 5
- 150000003624 transition metals Chemical class 0.000 abstract description 5
- 238000009831 deintercalation Methods 0.000 abstract description 3
- 230000002687 intercalation Effects 0.000 abstract description 3
- 238000009830 intercalation Methods 0.000 abstract description 3
- 230000035800 maturation Effects 0.000 abstract description 3
- 239000011572 manganese Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910002998 Li(Ni0.5Mn0.5)O2 Inorganic materials 0.000 description 1
- 229910006247 ZrS2 Inorganic materials 0.000 description 1
- QTHKJEYUQSLYTH-UHFFFAOYSA-N [Co]=O.[Ni].[Li] Chemical compound [Co]=O.[Ni].[Li] QTHKJEYUQSLYTH-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- VGYDTVNNDKLMHX-UHFFFAOYSA-N lithium;manganese;nickel;oxocobalt Chemical compound [Li].[Mn].[Ni].[Co]=O VGYDTVNNDKLMHX-UHFFFAOYSA-N 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- CPABIEPZXNOLSD-UHFFFAOYSA-N lithium;oxomanganese Chemical compound [Li].[Mn]=O CPABIEPZXNOLSD-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- 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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Abstract
本发明所述的一种锂离子电池层状正极材料及其制备方法,该材料是在层状锂电池正极材料的表面包覆MoS2/WS2薄膜。方法为1)将四硫代钼酸铵或四硫代钨酸铵加入到乙醇水溶液中,搅拌溶解;再将锂离子电池层状正极材料加入到上述溶液中,在80~100℃条件下加热搅拌,干燥后得到包覆后的前驱体;3)将前驱体研磨后置于管式炉中,在一定气氛下400~600℃温度下退火处理2~5h,得到表面包覆0.5wt%~6wt% MoS2或WS2的目标产物。本发明采用的包覆物层状过渡金属二硫化物具有类石墨烯结构,其有利于该材料中Li+ 嵌入/脱出,使得包覆后的正极材料表面包覆薄膜均匀,且采用的包覆方法技术成熟可靠。
Description
技术领域
本发明涉及锂离子电池层状正极材料制备领域,特别是涉及锂离子电池层状正极材料的表面包覆改性及其制备方法。
背景技术
由于锂离子电池具有能量密度高、重量轻、无记忆效应、倍率性能好、循环寿命长等一系列突出优点,被公认为下一代电动汽车、混合动力电动汽车的理想能源。锂离子电池的能量密度主要取决于正极材料的能量密度,所以,开发出高能量密度的正极材料成为人们关注的焦点。
对于锂离子电池,由于正极材料与电解液发生反应(如氧化还原反应),会造成正极材料中的金属元素溶解(如Mn)、固体电解质界面膜的增加等问题,从而导致电池的容量衰减,并导致安全性下降。因此,需要采用表面包覆等技术手段来改进锂离子电池层状正极材料的电化学性能。现今的包覆方式大体可以分为两种:干法包覆和湿法包覆。相比较来说,湿法包覆均匀,且得到的正极材料的电化学性能更优越。如中国发明专利申请“锂离子电池正极材料及其制备方法”(公开号CN1627550)中使用湿法在锂钴氧、锂镍钴氧、锂镍钴锰氧、锂锰氧材料表面包覆金属Al、Mg、Zn、Ca、Ba、Ti、V、Sn或非金属Si、B中某一种元素的氧化物来改善材料的循环性能、高温稳定性、倍率性能和安全性能。
由于层状过渡金属二硫化物,如MoS2, SnS2,
WS2,ZrS2等,具有石墨烯相同的结构,因此,他们被广泛用作锂离子电池负极材料。而层状过渡金属二硫化物的类石墨烯结构将有利于该材料中Li+ 嵌入/脱出。到目前为止,层状过渡金属二硫化物包覆改性锂离子电池层状正极材料的研究还未见报道。
发明内容
本发明所要解决的技术问题是提供一种表面包覆改性锂离子电池层状正极材料及其制备方法,采用该方法包覆的正极材料表面包覆均匀、技术成熟可靠。
本发明所述的一种锂离子电池层状正极材料,是在层状锂电池正极材料的表面包覆MoS2/WS2薄膜。
该锂离子电池层状正极材料的制备方法有两种,对于包覆MoS2薄膜,其制备过程为:
1)将一定量的四硫代钼酸铵加入到乙醇水溶液中,搅拌溶解;
2)再将锂离子电池层状正极材料加入到上述溶液中,在80~100℃条件下加热搅拌,干燥后得到包覆后的前驱体;
3)将前驱体研磨后置于管式炉中,在一定气氛下400~600℃温度下退火处理2~5h,得到表面包覆0.5wt%~6wt% MoS2的目标产物。
上述步骤1)中所述的四硫代钼酸铵与乙醇的摩尔比为 1:500~5000,乙醇水溶液中去离子水与乙醇的体积比为1:0.5~2。
上述步骤2)中所述的层状正极材料包括:一元层状正极材料如LiCoO2;二元层状正极材料如Li[Ni0.5Mn0.5]O2;三元层状正极材料如Li[Ni0.5Co0.2Mn0.3]O2、Li[Ni1/3Co1/3Mn1/3]O2、Li1.2[Mn0.51Ni0.19Co0.1]O2、Li1.2[Mn0.54Ni0.13Co0.13]O2。
上述步骤3)中所述的气氛为Ar或N2。
对于包覆WS2薄膜,其制备过程为:
1)将一定量的四硫代钨酸铵加入到乙醇水溶液中,搅拌溶解;
2)再将锂离子电池层状正极材料加入到上述溶液中,在80~100℃条件下加热搅拌,干燥后得到包覆后的前驱体;
3)将前驱体研磨后置于管式炉中,在一定气氛下400~600℃温度下退火处理2~5h,得到表面包覆0.5wt%~6wt% WS2的目标产物。
上述步骤1)中所述的四硫代钨酸铵与乙醇的摩尔比为1:500~5000,乙醇水溶液中去离子水与乙醇的体积比为1:0.5~2。
上述步骤2)中所述的层状正极材料包括:一元层状正极材料如LiCoO2;二元层状正极材料如Li[Ni0.5Mn0.5]O2;三元层状正极材料如Li[Ni0.5Co0.2Mn0.3]O2、Li[Ni1/3Co1/3Mn1/3]O2、Li1.2[Mn0.51Ni0.19Co0.1]O2、Li1.2[Mn0.54Ni0.13Co0.13]O2。
上述步骤3)中所述的气氛为Ar或N2。
本发明采用的包覆物层状过渡金属二硫化物具有类石墨烯结构,其有利于该材料中Li+ 嵌入/脱出,使得包覆后的正极材料表面包覆薄膜均匀,且采用的包覆方法技术成熟可靠。
附图说明
图1是本发明实施例1的2wt% MoS2包覆Li1.2[Mn0.54Ni0.13Co0.13]O2/Li扣式电池的XRD图;
图2是本发明实施例1的2wt% MoS2包覆Li1.2[Mn0.54Ni0.13Co0.13]O2/Li扣式电池的循环曲线。
具体实施方式
以下结合实施例对本发明进行具体说明。
实施例1
将0.163克四硫代钼酸铵加入到乙醇水溶液中,搅拌溶解,其中四硫代钼酸铵与乙醇的摩尔比为 1:1000,去离子水与乙醇的体积比为1:1;再将4.90克层状正极材料Li1.2[Mn0.54Ni0.13Co0.13]O2加入到上述溶液中,在90℃条件下加热搅拌,干燥后得到包覆后的前驱体;将前驱体研磨后置于管式炉中,在Ar气氛下500℃温度下退火处理2h,得到表面包覆2wt% MoS2的目标产物。由图1和图2可见,包覆后的电池性能得到了明显改善。
实施例2
将0.81克四硫代钼酸铵加入到乙醇水溶液中,搅拌溶解,其中四硫代钼酸铵与乙醇的摩尔比为 1:500,去离子水与乙醇的体积比为1:0.5;再将99.5克锂离子电池层状正极材料Li[Ni0.5Co0.2Mn0.3]O2加入到上述溶液中,在100℃条件下加热搅拌,干燥后得到包覆后的前驱体;将前驱体研磨后置于管式炉中,在N2气氛下400℃温度下退火处理5h,得到表面包覆0.5wt%MoS2的目标产物。
实施例3
将0.49克四硫代钼酸铵加入到乙醇水溶液中,搅拌溶解,其中四硫代钼酸铵与乙醇的摩尔比为 1:5000,去离子水与乙醇的体积比为1:2;再将4.7克锂离子电池层状正极材料LiCoO2加入到上述溶液中,在80℃条件下加热搅拌,干燥后得到包覆后的前驱体;将前驱体研磨后置于管式炉中,在Ar气氛下600℃温度下退火处理2h,得到表面包覆6wt% MoS2的目标产物。
实施例4
将1.4克四硫代钨酸铵加入到乙醇水溶液中,搅拌溶解,其中四硫代钨酸铵与乙醇的摩尔比为1:500,去离子水与乙醇的体积比为1:2;再将49克锂离子电池层状正极材料Li(Ni0.5Mn0.5)O2加入到上述溶液中,在90℃条件下加热搅拌,干燥后得到包覆后的前驱体;将前驱体研磨后置于管式炉中,在Ar气氛下400℃温度下退火处理3h,得到表面包覆2wt% WS2的目标产物。
实施例5
将0.07克四硫代钨酸铵加入到乙醇水溶液中,搅拌溶解,其中四硫代钨酸铵与乙醇的摩尔比为 1:1000,去离子水与乙醇的体积比为1:1;再将9.95克锂离子电池层状正极材料Li[Ni1/3Co1/3Mn1/3]O2加入到上述溶液中,在100℃条件下加热搅拌,干燥后得到包覆后的前驱体;将前驱体研磨后置于管式炉中,在N2气氛下400℃温度下退火处理4h,得到表面包覆0.5wt% WS2的目标产物。
实施例6
将4.21克四硫代钨酸铵加入到乙醇水溶液中,搅拌溶解,其中四硫代钨酸铵与乙醇的摩尔比为1:5000,去离子水与乙醇的体积比为1:0.5;再将47克层状正极材料Li1.2[Mn0.51Ni0.19Co0.1]O2加入到上述溶液中,在90℃条件下加热搅拌,干燥后得到包覆后的前驱体;将前驱体研磨后置于管式炉中,在Ar气氛下500℃温度下退火处理2h,得到表面包覆6wt% WS2的目标产物。
本发明具体应用途径很多,以上所述仅是本发明的优选实施方式,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,还可以作出若干改进,这些改进也应视为本发明的保护范围。
Claims (6)
1.一种锂离子电池层状正极材料,其特征在于,在层状锂电池正极材料的表面包覆MoS2薄膜,制备的具体过程包括以下步骤:
1)将一定量的四硫代钼酸铵加入到乙醇水溶液中,搅拌溶解,所述的四硫代钼酸铵与乙醇的摩尔比为 1:500~5000,乙醇水溶液中去离子水与乙醇的体积比为1:0.5~2;
2)再将锂离子电池层状正极材料加入到上述溶液中,在80~100℃条件下加热搅拌,干燥后得到包覆后的前驱体;
3)将前驱体研磨后置于管式炉中,在一定气氛下400~600℃温度下退火处理2~5h,得到表面包覆0.5wt%~6wt% MoS2的目标产物。
2.根据权利要求1所述锂离子电池层状正极材料,其特征在于,所述步骤2)中所述的层状正极材料为:一元层状正极材料LiCoO2、二元层状正极材料Li[Ni0.5Mn0.5]O2、三元层状正极材料Li[Ni0.5Co0.2Mn0.3]O2、Li[Ni1/3Co1/3Mn1/3]O2或Li1.2[Mn0.51Ni0.19Co0.1]O2。
3.根据权利要求1或2所述锂离子电池层状正极材料,其特征在于,所述步骤3)中的气氛为Ar或N2。
4.一种锂离子电池层状正极材料,其特征在于,在层状锂电池正极材料的表面包覆WS2薄膜,制备的具体过程包括以下步骤:
1)将一定量的四硫代钨酸铵加入到乙醇水溶液中,搅拌溶解,所述的四硫代钨酸铵与乙醇的摩尔比为 1:500~5000,乙醇水溶液中去离子水与乙醇的体积比为1:0.5~2;
2)再将锂离子电池层状正极材料加入到上述溶液中,在80~100℃条件下加热搅拌,干燥后得到包覆后的前驱体;
3)将前驱体研磨后置于管式炉中,在一定气氛下400~600℃温度下退火处理2~5h,得到表面包覆0.5wt%~6wt% WS2的目标产物。
5.根据权利要求4所述锂离子电池层状正极材料,其特征在于,所述步骤2)中所述的层状正极材料为:一元层状正极材料LiCoO2、二元层状正极材料Li[Ni0.5Mn0.5]O2、三元层状正极材料Li[Ni0.5Co0.2Mn0.3]O2、Li[Ni1/3Co1/3Mn1/3]O2或Li1.2[Mn0.51Ni0.19Co0.1]O2。
6.权利要求4或5所述锂离子电池层状正极材料,其特征在于,所述步骤3)中的气氛为Ar或N2。
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