CN107265514A - 一种菱形Fe2O3纳米材料及其制备方法 - Google Patents
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- 239000000463 material Substances 0.000 title description 16
- 239000002086 nanomaterial Substances 0.000 claims abstract description 32
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 26
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 14
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- 238000000034 method Methods 0.000 claims abstract description 9
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Abstract
本发明提供了一种菱形Fe2O3纳米材料及其制备方法,包括如下步骤:将无水三氯化铁80~100 mg和阳离子表面活性剂10~15 mg溶解于水10~15mL中,搅拌,使其充分溶解成透明溶液;转入15mL的反应釜中,在130~150℃的条件下反应18~24h,取出,自然冷却;洗涤,50~100℃烘箱干燥30~48 h,即得菱形Fe2O3纳米材料;使用该方法制备的菱形Fe2O3纳米材料具有分散性好、比容量大、循环性能好、使用寿命长等特点;采用一步法,以阳离子表面活性剂(CTAB)为模板,在水热条件下一步合成菱形Fe2O3纳米材料,得到的菱形Fe2O3纳米材料粒径均匀,分散性好,结构稳定。
Description
技术领域
本发明属于纳米材料及其应用技术领域,具体涉及一种Fe2O3纳米材料及其制备方法。
背景技术
随着社会的飞速发展,环境污染和能源危机的挑战日益严峻,绿色能源成为世界各国的研发热点。锂离子电池作为一种新型清洁的可充电电源,具有质量轻、污染小、工作电压高、能量密度大、循环寿命长等优点,在国防、电动车和电子领域展示了广阔的应用前景,被誉为21世纪的理想电源。但是随着电动汽车和混合动力汽车的发展,需要锂离子电池拥有更高容量和更好的倍率放电性能,但是目前的锂离子电池还不能完全达到这些要求。就锂离子电池负极材料而言,目前商业化的碳材料存在比容量低、安全性能欠佳等问题(理论容量仅为372 mAh g-1),已不能满足新一代高比容量电池负极材料的需求。因此,如何用低电压、可嵌锂的化合物替代目前所用的碳材料,以提高锂离子电池的能量密度和安全性能是一个十分重要的课题。为了满足高性能锂离子电池的市场需求,必须寻找能够在低电势下保持高容量的石墨替代材料。
与石墨负极材料相比,过渡金属氧化物为实现具有较高能量密度的锂离子电池提供了更多的选择(Penki T R, Shivakumara S, Minakshi M, Electr℃himica Acta,2015, 167, 330-339; Zhang S, Zhang P, Xie A, et al, Electr℃himica Acta,2016, 212, 912-920.)。在众多的过渡金属氧化物中,Fe2O3由于具有容量高、环境友好、成本较低、安全性能好等优点已引起广泛关注,被认为是锂离子电池商业碳负极材料最有前景的替代材料之一(Qin F, Zhang K, Zhang L, Dalton Transactions, 2015, 44,2150-2156; Jiang T, Bu F, Feng X, ACS Nano, 2017, 11, 5140−5147)。但Fe2O3电极材料在反复嵌/脱锂过程中容易出现大的体积膨胀效应,易造成结构粉化、团聚而失去活性,从而导致Fe2O3电极材料的循环性能及倍率性能变差,极大地限制了Fe2O3作为锂离子电池负极材料的实际应用。众所周知,纳米级的材料与体材料相比有着显著不同的物理与化学性质。在锂离子电池领域,电池电极性质不但与材料的结构有关,而且与电极的形貌有关。最近,虽然有关各种纳米结构的Fe2O3,如纳米颗粒、纳米花、纳米棒和纳米管的制备及其作为锂离电池负极材料相继被报道(Zeng S Y, Tang K B, Li T W. J. Colloid. Interf.Sci, 2007, 312, 513-521;Chen J, Xu L, Li W Y, et a1. Adv. Mater, 2005, 17,582-586; NuLi Y, Zhng P, Guo Z P, et a1. Elctr℃him. Acta, 2008, 53, 4213-4218.)。但粒径均一,分散性好的菱形Fe2O3纳米粒子作为锂离电池的负极还未有报道。
发明内容
本发明目的是提供一种菱形Fe2O3纳米材料及其制备方法,该方法制备的菱形Fe2O3纳米锂电池负极材料具有分散性好、比容量大、循环性能好、使用寿命长等特点。
一种菱形Fe2O3纳米材料,它是由下述方法制备的,包括:
1)将无水三氯化铁80~100 mg和阳离子表面活性剂10~15 mg溶解于水10~15 mL中,搅拌,使其充分溶解成透明溶液;
2)转入15 mL的反应釜中,在130 ~ 150℃的条件下反应18 ~ 24 h,取出,自然冷却;
3)洗涤,50 ~ 100℃烘箱干燥30 ~ 48 h,即得Fe2O3纳米锂电池负极材料;
所述的阳离子表面活性剂为CTAB;所述的洗涤为无水乙醇和蒸馏水交替洗涤;
所述的步骤1)中的无水三氯化铁80mg,CTAB为10mg,水10mL;步骤2)在130℃的条件下反应20h;步骤3)中50℃烘箱干燥48 h;
所述的步骤1)中的无水三氯化铁100mg,CTAB为12mg,水13mL;步骤2)在150℃的条件下反应24h;步骤3)中80℃烘箱干燥30h;
所述的步骤1)中的无水三氯化铁90mg,CTAB为15mg,水15mL;步骤2)在130℃的条件下反应24h;步骤3)中100℃烘箱干燥48h。
一种菱形Fe2O3纳米材料在制备锂离子电池方面的应用。
本发明提供了一种菱形Fe2O3纳米材料及其制备方法,包括如下步骤:将无水三氯化铁80~100 mg和阳离子表面活性剂10~15 mg溶解于水10~15mL中,搅拌,使其充分溶解成透明溶液;转入15mL的反应釜中,在130~150℃的条件下反应18~24h,取出,自然冷却;洗涤,50~100℃烘箱干燥30 ~ 48 h,即得菱形Fe2O3纳米材料;使用该方法制备的菱形Fe2O3纳米材料具有分散性好、比容量大、循环性能好、使用寿命长等特点;采用一步法,以阳离子表面活性剂(CTAB)为模板,在水热条件下一步合成菱形Fe2O3纳米材料,得到的菱形Fe2O3纳米材料粒径均匀,分散性好,结构稳定。
附图说明
图1 菱形Fe2O3纳米材料扫描电镜图;
图2 菱形Fe2O3纳米材料的XRD谱图;
图3 菱形Fe2O3纳米材料的充放电循环曲线。
具体实施方式
实施例1 一种菱形Fe2O3纳米材料制备方法
首先,将80mg无水FeCl3和10mg CTAB(十六烷基三甲基溴化铵),溶解于10mL水中,搅拌使其充分溶解成透明溶液;随后将其转入15mL的反应釜中,在130℃的条件下反应20h;取出自然冷却,用无水乙醇和蒸馏水交替离心分离数次,50℃烘箱干燥48h,即得微米级菱形Fe2O3材料。
实施例2一种菱形Fe2O3纳米材料制备方法
首先,将100 mg无水FeCl3和12 mg CTAB溶解于13 mL水中,搅拌使其充分溶解成透明溶液。随后将其转入15 mL的反应釜中,在150℃的条件下反应24 h,取出自然冷却,用无水乙醇和蒸馏水交替离心分离数次,80℃烘箱干燥30 h,即得微米级菱形Fe2O3材料。
实施例3一种菱形Fe2O3纳米材料制备方法
首先,将90 mg无水FeCl3和15 mg CTAB溶解于15 mL水中,搅拌使其充分溶解成透明溶液。随后将其转入15 mL的反应釜中,在130℃的条件下反应24 h,取出自然冷却,用无水乙醇和蒸馏水交替离心分离数次, 100℃烘箱干燥48 h,即得单分散菱形Fe2O3纳米材料,结果见图1、2。结果表明,得到的菱形Fe2O3纳米材料粒径均匀,分散性好,结构稳定。
实施例4一种菱形Fe2O3纳米材料的应用
单分散菱形Fe2O3纳米材料用于锂离子电池。以合成的单分散菱形Fe2O3纳米材料为活性物质,乙炔黑为导电剂,聚偏氟乙烯(PVDF)为粘结剂,氮甲基吡咯烷酮(NMP)为溶剂。电池的组装过程为:将活性物质 、导电剂、聚偏氟乙烯按70:20:10的重量比准确称量,然后放入玛瑙研钵中充分混合、研磨均匀,然后加入几滴NMP,继续研磨至均匀浆状。将浆料均匀涂于已称量过的铜箔上。然后在真空干燥箱中于120 oC真空干燥12 h至恒重,10 MPa下压片,再继续干燥至少5 h,降到室温后取出称重。
我们用实验半电池来测试合成材料的电化学性能,模拟电池的组装在无水无氧、充有氩气的手套箱中完成。将烘干的极片、电池壳和隔膜放入手套箱。以金属锂片为对电极,Celgard240聚丙烯多孔膜做隔膜,1.0 mol/L LiPF6 的EC-DMC(体积比1:1)溶液做电解液,组装成扣式CR2032模拟电池,进行充放电测试,结果(见图3)。结果表明本发明合成的单分散菱形Fe2O3纳米材料具有很好的循环稳定性。
Claims (6)
1.一种菱形Fe2O3纳米材料,它是由下述方法制备的,包括:
1)将无水三氯化铁80~100 mg和阳离子表面活性剂10~15 mg溶解于水10~15 mL中,搅拌,使其充分溶解成透明溶液;
2)转入15 mL的反应釜中,在130 ~ 150℃的条件下反应18 ~ 24 h,取出,自然冷却;
3)洗涤,50 ~ 100℃烘箱干燥30 ~ 48 h,即得Fe2O3纳米材料。
2.根据权利要求1所述的一种菱形Fe2O3纳米材料,其特征在于:所述的阳离子表面活性剂为CTAB;所述的洗涤为无水乙醇和蒸馏水交替洗涤。
3. 根据权利要求2所述的一种菱形Fe2O3纳米材料,其特征在于:步骤1)中所述的无水三氯化铁80mg,CTAB为10mg,水10mL;步骤2)所述的反应为在130℃的条件下反应20h;步骤3)所述的干燥为50℃烘箱干燥48 h。
4.根据权利要求2所述的一种菱形Fe2O3纳米材料,其特征在于:步骤1)所述的的无水三氯化铁100mg,CTAB为12mg,水13mL;步骤2)所述的反应为在150℃的条件下反应24h;步骤3)所述的干燥为80℃烘箱干燥30h。
5.根据权利要求2所述的一种菱形Fe2O3纳米材料,其特征在于:步骤1)所述的无水三氯化铁90mg,CTAB为15mg,水15mL;步骤2)所述的反应为在130℃的条件下反应24h;步骤3)所述的干燥为100℃烘箱干燥48h。
6.权利要求1所述的一种菱形Fe2O3纳米材料在制备锂离子电池方面的应用。
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