CN110085859A - 一种锂离子电池正极材料及其制备方法 - Google Patents
一种锂离子电池正极材料及其制备方法 Download PDFInfo
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 32
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000010405 anode material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011572 manganese Substances 0.000 claims abstract description 30
- 229910013716 LiNi Inorganic materials 0.000 claims abstract description 21
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 11
- 230000008020 evaporation Effects 0.000 claims abstract description 11
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- IAQLJCYTGRMXMA-UHFFFAOYSA-M lithium;acetate;dihydrate Chemical compound [Li+].O.O.CC([O-])=O IAQLJCYTGRMXMA-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000010792 warming Methods 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 abstract description 6
- 229910002099 LiNi0.5Mn1.5O4 Inorganic materials 0.000 description 20
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- NLTSCOZQKALPGZ-UHFFFAOYSA-N acetic acid;dihydrate Chemical compound O.O.CC(O)=O NLTSCOZQKALPGZ-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/54—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [Mn2O4]-, e.g. Li(NixMn2-x)O4, Li(MyNixMn2-x-y)O4
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Abstract
本发明公开一种锂离子电池正极材料及其制备方法,该锂离子电池正极材料为具有微米尺度空心长方体结构的LiNi0.5Mn1.5O4材料,其在具有高能量密度的同时,还具有良好的循环性能和倍率性能。其制备方法包括如下步骤:(1)将四水醋酸锰和四水醋酸镍依次加入无水乙醇中,水浴条件下溶解;将溶解完成后所得溶液倒入水热釜中,通过溶剂热反应得到前驱体;(2)将二水醋酸锂溶于前驱体溶液中,加热、搅拌蒸发,煅烧所得产物,得到具有微米尺度空心长方体结构的LiNi0.5Mn1.5O4。该方法通过控制反应原料比和反应温度,最终可制得尺寸均匀、结晶度高的空心长方体结构的LiNi0.5Mn1.5O4,另外,该方法简单、易于操作、成本低。
Description
技术领域
本发明涉及一种锂离子电池正极材料,特别涉及一种具备空心长方体结构的锂离子电池正极材料LiNi0.5Mn1.5O4及其制备方法,属于锂离子电池技术领域。
背景技术
锂离子电池是一种二次电池,在生产生活过程中有着广泛的应用。随着便携式电子器件,尤其是电动汽车的快速发展,人们对锂离子电池的能量密度、循环寿命和倍率性能提出了更高的要求。
LiNi0.5Mn1.5O4有较高的能量密度,然而其倍率性能和循环性能还有待提高。基于此,提高其倍率性能和循环性能具有重要的现实意义和商业价值。
发明内容
发明目的:针对现有技术中存在的问题,本发明提供一种锂离子电池正极材料,并提供了一种该锂离子电池正极材料的制备方法。
技术方案:本发明所述的一种锂离子电池正极材料,为具有微米尺度空心长方体结构的LiNi0.5Mn1.5O4材料,该结构的LiNi0.5Mn1.5O4材料在拥有高能量密度的同时,还表现出良好的倍率性能和循环寿命。
本发明所述的一种锂离子电池正极材料的制备方法,包括如下步骤:
(1)将四水醋酸锰和四水醋酸镍依次加入无水乙醇中,水浴条件下溶解;将溶解完成后所得溶液倒入水热釜中,通过溶剂热反应得到前驱体;
(2)将二水醋酸锂溶于前驱体溶液中,加热、搅拌蒸发,对所得产物进行煅烧,得到具有微米尺度空心长方体结构的LiNi0.5Mn1.5O4。
该方法中,原料的加入量满足如下关系:四水醋酸锰、四水醋酸镍与二水醋酸锂的摩尔比为3:1:2。
步骤(1)中,四水醋酸锰和四水醋酸镍溶解的水浴温度越高,所得前驱体越容易团聚,且尺度越小,不利于空心长方体结构的形成,较优的,控制四水醋酸锰和四水醋酸镍溶解的水浴温度≤35℃,该温度范围内均可制备出微米尺度空心长方体结构的LiNi0.5Mn1.5O4;该温度最好为35℃,随水浴温度的降低,溶剂热反应所得到的产物的量会相应降低。
进一步的,溶解后,溶剂热反应条件优选为:反应温度85~120℃,反应时间12小时;其中,反应温度最好为115℃。
上述步骤(2)中,相应的,二水醋酸锂溶于前驱体溶液中后,加热、搅拌蒸发的温度最好为60℃。进一步的,煅烧条件最好为:先升温至450℃保温1小时,然后升温至750℃保温10小时,煅烧温度过低将导致LiNi0.5Mn1.5O4结晶性不足,过高将导致LiNi0.5Mn1.5O4结构破坏。更进一步的,煅烧升温过程中,升温速率最好控制在2℃/min。
有益效果:与现有的LiNi0.5Mn1.5O4材料相比,本发明的优点在于:1)本发明的微米尺度空心长方体结构LiNi0.5Mn1.5O4锂离子电池正极材料在具有高能量密度的同时,还具有良好的循环性能和倍率性能;2)本发明的制备方法通过反应原料比和反应温度(包括四水醋酸锰和四水醋酸镍的溶解温度,溶剂热反应温度和煅烧温度)的有效控制,最终可制得空心长方体结构的LiNi0.5Mn1.5O4,该空心长方体LiNi0.5Mn1.5O4锂离子电池正极材料样品尺寸均匀,结晶度高;且该制备方法简单、易于操作、成本低。
附图说明
图1为实施例1制得的空心长方体LiNi0.5Mn1.5O4的XRD图谱;
图2为实施例1制得的空心长方体LiNi0.5Mn1.5O4在不同放大倍率下的SEM图片;
图3为实施例1制得的前驱体以及LiNi0.5Mn1.5O4材料的TEM图片,其中,(a)为实心长方体前驱体的TEM图片,(b)为空心长方体LiNi0.5Mn1.5O4的TEM图片,(c)为空心长方体LiNi0.5Mn1.5O4的HRTEM图片;
图4为实施例1制得的空心长方体LiNi0.5Mn1.5O4的元素分布图片;
图5为实施例1制得的空心长方体LiNi0.5Mn1.5O4的循环性能图片;
图6为实施例1制得的空心长方体LiNi0.5Mn1.5O4的倍率性能图片。
具体实施方式
以下结合附图对本发明的技术方案作进一步说明。
本发明的一种锂离子电池正极材料,为具有微米尺度空心长方体结构的LiNi0.5Mn1.5O4材料,该结构的LiNi0.5Mn1.5O4材料在拥有高能量密度的同时,还表现出良好的倍率性能和循环寿命。
实施例1
先将0.3676g的四水醋酸锰和0.1244g的四水醋酸镍依次加入70ml的无水乙醇中,并在35℃的水浴条件下进行溶解。溶解完成后,将所得的溶液转移至100ml的水热釜内,在115℃下保温12小时。之后,将所得前驱体转移至100ml的烧杯中,加入0.102g的二水醋酸锂,并在60℃下进行搅拌蒸发;将搅拌蒸发得到的粉末放入马弗炉内,先以2℃/min的速率升温至450℃,并保温一小时,然后以2℃/min的速率升温至750℃,保温10小时,即得锂离子电池正极材料LiNi0.5Mn1.5O4。
图1为本实施例制得的锂离子电池正极材料LiNi0.5Mn1.5O4的XRD图谱,可以看到,其结晶度很高,没有杂相。其SEM图片如图2,包括在低倍、中倍和高倍几种不同放大倍率下的SEM图,可以看到,该LiNi0.5Mn1.5O4材料为具有微米尺度的空心长方体结构。图3为本实施例制得的前驱体和最终产物LiNi0.5Mn1.5O4的TEM图片,该图片进一步证明了本实施例制得的LiNi0.5Mn1.5O4材料为空心长方体结构,具有微米尺度;图4为本实施例制得的空心长方体LiNi0.5Mn1.5O4材料的元素分布图片,该图证实了Mn、Ni、O三种元素在空心长方体LiNi0.5Mn1.5O4材料中均匀分布。
将本实施例制得的空心长方体LiNi0.5Mn1.5O4作为锂离子电池正极,进行循环性能和倍率性能测试;其循环性能曲线如图5,可以看到,该电极在30C的放电电流密度下,首次放电容量为109.26mAh/g,在经过800次充放电循环后,其放电容量为104.37mAh/g,容量保有率为95.5%,显示了空心长方体LiNi0.5Mn1.5O4作为锂离子电池正极具备较好的循环性能。其倍率性能如图6,该曲线给出了在1C、2C、5C、10C、20C、30C的充放电电流密度下,容量变化平缓,显示了空心长方体LiNi0.5Mn1.5O4作为锂离子电池正极具备较好的倍率性能。
实施例2
先将0.3676g的四水醋酸锰和0.1244g的四水醋酸镍依次加入70ml的无水乙醇中,并在35℃的水浴条件下进行溶解。溶解完成后,将所得的溶液转移至100ml的水热釜内,在85℃下保温12小时。之后,将所得前驱体转移至100ml的烧杯中,加入0.102g的二水醋酸锂,并在60℃下进行搅拌蒸发;将搅拌蒸发得到的粉末放入马弗炉内,先以2℃/min的速率升温至450℃,并保温一小时,然后以2℃/min的速率升温至750℃,保温10小时,即得锂离子电池正极材料LiNi0.5Mn1.5O4。
本实施例制得的锂离子电池正极材料LiNi0.5Mn1.5O4的微观形貌结构与实施例1中相近,为具有微米尺度的空心长方体结构。
实施例3
先将0.3676g的四水醋酸锰和0.1244g的四水醋酸镍依次加入70ml的无水乙醇中,并在35℃的水浴条件下进行溶解。溶解完成后,将所得的溶液转移至100ml的水热釜内,在120℃下保温12小时。之后,将所得前驱体转移至100ml的烧杯中,加入0.102g的二水醋酸锂,并在60℃下进行搅拌蒸发;将搅拌蒸发得到的粉末放入马弗炉内,先以2℃/min的速率升温至450℃,并保温一小时,然后以2℃/min的速率升温至750℃,保温10小时,即得锂离子电池正极材料LiNi0.5Mn1.5O4。
本实施例制得的锂离子电池正极材料LiNi0.5Mn1.5O4的微观形貌结构也与实施例1中相近,为具有微米尺度的空心长方体结构。
Claims (8)
1.一种锂离子电池正极材料,其特征在于,该锂离子电池正极材料是具有微米尺度空心长方体结构的LiNi0.5Mn1.5O4材料。
2.一种权利要求1所述的锂离子电池正极材料的制备方法,其特征在于,包括如下步骤:
(1)将四水醋酸锰和四水醋酸镍依次加入无水乙醇中,水浴条件下溶解;将溶解完成后所得溶液倒入水热釜中,通过溶剂热反应得到前驱体;
(2)将二水醋酸锂溶于前驱体溶液中,加热、搅拌蒸发,对所得产物进行煅烧,得到具有微米尺度空心长方体结构的LiNi0.5Mn1.5O4。
3.根据权利要求2所述的锂离子电池正极材料的制备方法,其特征在于,原料的加入量满足如下关系:四水醋酸锰、四水醋酸镍与二水醋酸锂的摩尔比为3:1:2。
4.根据权利要求2所述的锂离子电池正极材料的制备方法,其特征在于,步骤(1)中,所述水浴条件为:水浴温度≤35℃。
5.根据权利要求2所述的锂离子电池正极材料的制备方法,其特征在于,步骤(1)中,所述溶剂热反应条件为:反应温度85~120℃,反应时间12小时。
6.根据权利要求2所述的锂离子电池正极材料的制备方法,其特征在于,步骤(2)中,所述加热搅拌蒸发的温度为60℃。
7.根据权利要求2所述的锂离子电池正极材料的制备方法,其特征在于,步骤(2)中,所述煅烧条件为:先升温至450℃保温1小时,然后升温至750℃保温10小时。
8.根据权利要求7所述的锂离子电池正极材料的制备方法,其特征在于,所述煅烧过程中,升温速率为2℃/min。
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