CN103682317A - 一种Li2MnO3纳米线及其制备方法和应用 - Google Patents
一种Li2MnO3纳米线及其制备方法和应用 Download PDFInfo
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- 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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- C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
- C01G45/1257—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3 containing lithium, e.g. Li2MnO3, Li2[MxMn1-xO3
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Abstract
本发明公开了一种Li2MnO3纳米线及其制备方法和应用,采用熔盐法在较低温度下合成Li2MnO3纳米线,其直径为5-25nm,长度为几百纳米到几微米。所述的Li2MnO3纳米线作为锂电池正极。一维纳米材料是一种良好的锂电池电极材料,本发明首次提供了一种制备高纯度的Li2MnO3纳米线的方法,其操作简便、成本低、纯度高、性能优异,重现性好。
Description
技术领域
本发明属于锂电池正极材料制备领域,具体涉及一种Li2MnO3纳米线及其制备方法和应用。
背景技术
自上世纪锂电池开发成功以来,锂电池已经得到了广泛的应用,但是要得到循环性能好,比容量高等电化学性能好的锂电池正极材料一直以来是科学家的研究重点。现在工业上常用的正极材料,如LiCoO2、LiNiO2、LiMnO2,他们的容量都不高,只有120 mAh/g左右。随着纳米材料的兴起,一维纳米材料被认为是一种很有前景的锂离子电极材料,而正极材料是锂离子电池的瓶颈。目前还未有制备Li2MnO3纳米线的相关专利报道。
发明内容
本发明的目的在于提供一种Li2MnO3纳米线及其制备方法和应用,首次提供了一种制备高纯度的Li2MnO3纳米线的方法,其操作简便、成本低、纯度高、性能优异,重现性好。
为实现上述目的,本发明采用如下技术方案:
一种Li2MnO3纳米线的直径为5-25nm,长度为几百纳米到几微米。
采用熔盐法在较低温度下合成Li2MnO3纳米线。包括以下步骤:
(1)将0.2g氟化锰与10g硝酸钠混合后磨匀,于540℃煅烧3小时,水洗、无水乙醇过滤各3次,70℃烘干4小时,得到Mn2O3前驱体纳米线;
(2)将0.1gMn2O3前驱体纳米线与5g硝酸锂混合后磨匀,再按步骤(1)的反应条件煅烧、水洗、醇洗和烘干,得到高纯度的Li2MnO3纳米线。
所述的氟化锰是由氢氟酸和碳酸锰反应得到。
所述的Li2MnO3纳米线作为锂电池正极。
锂电池组装:按质量比:Li2MnO3纳米线:聚四氟乙烯:超级碳=7:2:1混合研磨后,均匀地涂在0.25 cm2的铝箔上做正极,参比电极和对电极均为金属锂,电解质由1M LiPF6的EC+DMC+EMC溶液;所有组装过程均在手套箱里进行;所述的EC+DMC+EMC溶液中EC、DMC、EMC的体积比为1:1:1。
本发明的显著优点在于:首次提供了一种制备高纯度的Li2MnO3纳米线的方法,其操作简便、成本低、纯度高、性能优异,重现性好,用此高纯度Li2MnO3纳米线作锂电池正极得到的锂电池具有很高的比容量,在电流密度为0.02 Ag-1下充放电27圈后,放电容量达到了159 mAh/g。
附图说明
图1是Li2MnO3纳米线的SEM图(a)和TEM图(b)。
图2是Li2MnO3纳米线电极材料的放电曲线(c)和放电比容量(d)。
具体实施方式
本发明用简单的熔盐法在较低温度下合成了直径为5-25nm 左右,长度为几百纳米到几微米左右的高纯度的Li2MnO3纳米线。
用此高纯度Li2MnO3纳米线作锂电池正极得到的锂电池具有很高的比容量,在电流密度为0.02 Ag-1下充放电27圈后放电容量达到了159 mAh/g,其他的同行都是在很低的电流密度下呈现更低的比容量。
高纯度Li2MnO3纳米线的制备方法是将0.2g氟化锰(用氢氟酸和碳酸锰反应得到)与10g硝酸钠混合后磨匀,于540℃煅烧3小时,水洗、无水乙醇过滤各3次,70℃烘干4小时,得到Mn2O3前驱体纳米线,然后将其0.1g与5g 硝酸锂混合后磨匀再按上述同样的步骤及反应条件即得到高纯度Li2MnO3纳米线。
锂电池组装:按质量比Li2MnO3纳米线:聚四氟乙烯:超级碳=7:2:1混合研磨后均匀地涂在0.25 cm2的铝箔上做正极,参比电极和对电极均为金属锂,电解质由1M LiPF6的EC+DMC+EMC (EC/DMC/EMC=1/1/1 v/v) 溶液。所有组装过程均在手套箱里进行。
从(a)图中可以看出,Li2MnO3纳米线的长度大概在几百纳米到几微米之间范围内,直径大约5-25纳米;从(b)图中可以看出Li2MnO3纳米线的结晶度很高;从(c)图中可以看出,Li2MnO3纳米线电极材料放电比容量先升后降,首圈放电比容量高达160 mAh/g;从(d)图中可以看出, 在电流密度为0.02 Ag-1下充放电27圈后放电容量达到了159 mAh/g,而且循环性能很好。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (6)
1.一种Li2MnO3纳米线,其特征在于:所述的Li2MnO3纳米线的直径为5-25nm,长度为几百纳米到几微米。
2.一种制备如权利要求1所述的Li2MnO3纳米线的方法,其特征在于:采用熔盐法在较低温度下合成Li2MnO3纳米线。
3.根据权利要求2所述的Li2MnO3纳米线的制备方法,其特征在于:包括以下步骤:
(1)将0.2g氟化锰与10g硝酸钠混合后磨匀,于540℃煅烧3小时,水洗、无水乙醇过滤各3次,70℃烘干4小时,得到Mn2O3前驱体纳米线;
(2)将0.1gMn2O3前驱体纳米线与5g硝酸锂混合后磨匀,再按步骤(1)的反应条件煅烧、水洗、醇洗和烘干,得到高纯度的Li2MnO3纳米线。
4.根据权利要求3所述的Li2MnO3纳米线的制备方法,其特征在于:所述的氟化锰是由氢氟酸和碳酸锰反应得到。
5.一种如权利要求1所述的Li2MnO3纳米线的应用,其特征在于:所述的Li2MnO3纳米线作为锂电池正极。
6.根据权利要求5所述的Li2MnO3纳米线的应用,其特征在于:锂电池组装:按质量比:Li2MnO3纳米线:聚四氟乙烯:超级碳=7:2:1混合研磨后,均匀地涂在0.25 cm2的铝箔上做正极,参比电极和对电极均为金属锂,电解质由1M LiPF6的EC+DMC+EMC溶液;所有组装过程均在手套箱里进行;所述的EC+DMC+EMC溶液中EC、DMC、EMC的体积比为1:1:1。
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Cited By (3)
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CN104022277A (zh) * | 2014-05-16 | 2014-09-03 | 武汉理工大学 | Li2MnO3纳米线及其制备方法和应用 |
CN104084202A (zh) * | 2014-07-14 | 2014-10-08 | 北京工业大学 | 一种Ag/Mn2O3纳米线催化剂的熔融盐原位制备法及应用 |
CN111172743A (zh) * | 2020-01-16 | 2020-05-19 | 浙江大学 | 一种低温快速制备复合金属氧化物纳米薄膜材料的方法 |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104022277A (zh) * | 2014-05-16 | 2014-09-03 | 武汉理工大学 | Li2MnO3纳米线及其制备方法和应用 |
CN104022277B (zh) * | 2014-05-16 | 2016-01-06 | 武汉理工大学 | Li2MnO3纳米线及其制备方法和应用 |
CN104084202A (zh) * | 2014-07-14 | 2014-10-08 | 北京工业大学 | 一种Ag/Mn2O3纳米线催化剂的熔融盐原位制备法及应用 |
CN104084202B (zh) * | 2014-07-14 | 2016-04-13 | 北京工业大学 | 一种Ag/Mn2O3纳米线催化剂的熔融盐原位制备法及应用 |
CN111172743A (zh) * | 2020-01-16 | 2020-05-19 | 浙江大学 | 一种低温快速制备复合金属氧化物纳米薄膜材料的方法 |
CN111172743B (zh) * | 2020-01-16 | 2021-10-19 | 浙江大学 | 一种低温快速制备复合金属氧化物纳米薄膜材料的方法 |
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