CN108264092A - 一种高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法 - Google Patents
一种高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法 Download PDFInfo
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Abstract
本发明公开了一种高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法,具体步骤如下:(1)取硝酸亚铁溶液,加入十二烷基苯磺酸钠调节硝酸亚铁溶液的pH=1.5~3.5,然后加入氢氧化钾溶液,继续搅拌10 h~13h;(2)将步骤(1)搅拌好的溶液转入水热反应釜中,加入十二烷基硫酸钠调节溶液pH=8~10,进行水热反应;(3)反应结束后,抽滤,干燥得到样品,将样品煅烧后得高循环性能锂离子电池负极材料Fe2O3纳米针叶。本发明制备的针状的Fe2O3在用于锂离子电池负极材料时,其独特的结构对于在充放电过程中,缩短了离子的传输路径,对于电池的循环性能有着极大的好处。
Description
技术领域
本发明属于新能源材料制备技术领域,具体涉及一种高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法。
背景技术
氧化铁(Fe2O3),一种n型半导体材料,其禁带宽度较窄(2.2eV左右),具有良好耐候性、耐光性、无毒性和对紫外线具有良好的吸收和屏蔽作用,可广泛应用于涂料、油墨、吸附、催化、气敏和湿敏材料、电化学、生物医学工程等领域。由于纳米氧化铁具有诸多的优点和广泛的应用前景,近年来国内外研究者对其投入了大量的研究,包括应用于锂离子电池领域。通常认为扩散电阻、电导率、电荷传递电阻对LIB负极的电化学性能具有重要影响,使用纳米尺寸的负极材料不仅可以降低锂离子在电极体内的扩散长度,而且可以大大地增加表面反应活化位,因而,使用纳米尺寸Fe2O3作为LIB的电极活性材料,将极大地降低负极反应的过电位,提高其倍率性能。我们所采用的就是减小氧化铁的粒度,进而提高其电化学性能。通过以上方案制备的纳米针叶状的Fe2O3,直径极小,能够有效减短粒子传输路径,增大粒子的传输速度,进而改善其比容量性能。
发明内容
针对现有技术中存在的问题,本发明提供一种高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法,这种材料具有极好的比容量性能,同其他同类材料相比,性能更加优越。
为解决上述技术问题,本发明采用以下技术方案:
一种高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法,具体步骤如下:
(1)取硝酸亚铁溶液,加入十二烷基苯磺酸钠调节硝酸亚铁溶液的pH=1.5 ~ 3.5,然后加入氢氧化钾溶液,继续搅拌10 h ~13h;
(2)将步骤(1)搅拌好的溶液转入水热反应釜中,加入十二烷基硫酸钠调节溶液pH=8~10,进行水热反应;
(3)反应结束后,抽滤,干燥得到样品,将样品煅烧后得高循环性能锂离子电池负极材料Fe2O3纳米针叶。
所述步骤(1)中硝酸亚铁溶液的浓度为(3.5-4.6) mol/L,氢氧化钾溶液的浓度为(4.2-5.7)mol/L,硝酸亚铁溶液与氢氧化钾溶液的体积比1:1-3。
所述步骤(2)中水热反应的温度为110℃~150℃,水热反应的时间为3 h-5h;
所述步骤(3)中的煅烧温度为300℃-400℃,煅烧时间为2h~6h。
本发明的有益效果:1、本发明制备的针状的Fe2O3在用于锂离子电池负极材料时,其独特的结构对于在充放电过程中,缩短了离子的传输路径,对于电池的循环性能有着极大的好处;2、该制备工艺下,十二烷基苯磺酸钠调节表面活性剂的加入不仅对产物的晶型、结晶度等产生了影响,同样对合成样品的相貌也有不同的影响;3、十二烷基硫酸钠表面活性剂的加入,对溶液体系的离子强度和溶液的粘度都有一定程度的改变,从而对反应离子的移动性和晶核的形成速度产生了影响,为了促进生成α-FeOOH,最终形成的产物具有相同的尺寸和形貌;4、α-FeOOH会在反应过程中形成的胶体表面进行吸附,从而改变形核与结晶长大的动力学过程,同时离子的选择性吸附还会引起各向异性生长;纳米粒胶体表面会发生吸附,由于带有同性的电荷,相互排斥作用使得纳米粒子不易团聚,具有更好的分散性,晶粒会沿着特定的取向进行排列,随着结晶的进一步长大,形成的纳米粒子会定向排列为针叶状α-FeOOH,通过煅烧反应形成针状结构的 α-Fe2O3。此外,该方法制备的样品晶型完好,并且几乎没有杂质,成本较低,适合大范围推广。
附图说明
图1为本发明实施例1所制备的纳米针叶状Fe2O3的XRD图。
图2为本发明实施例1所制备的纳米针叶状Fe2O3的SEM图。
图3为本发明实施例1所制备的纳米针叶状Fe2O3在0.2 C条件下的循环性能图。
具体实施方式
下面结合具体实施例,对本发明做进一步说明。应理解,以下实施例仅用于说明本发明而非用于限制本发明的范围,该领域的技术熟练人员可以根据上述发明的内容作出一些非本质的改进和调整。
实施例1
本实施例的高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法,步骤如下:
(1)取浓度为4.2 mol/L的硝酸亚铁溶液,采用十二烷基苯磺酸钠调节至pH=3,然后加入浓度为5.3 mol/L氢氧化钾溶液,继续搅拌10h,硝酸亚铁溶液和氢氧化钾溶液的体积比为1:1.5;
(2)将上述搅拌好的溶液转入150mL的水热反应釜中,然后采用十二烷基硫酸钠将溶液pH调节至9,在温度为150℃条件下,水热反应3 h;
(3)将上述所得产品抽滤,干燥之后将样品在350℃煅烧4h后得到针叶状结构纳米氧化铁。
图1为实施例1所制备的针叶状纳米氧化铁的XRD图,对比后发现制备的产品晶型优异,纯度较高,结晶度较好。
图2为实施例1所制备的针叶状纳米氧化铁的SEM图,图中的产物都为纳米针叶状,纳米针叶状直径为50nm,表面光滑。
图3为实施例1所制备的针叶状纳米氧化铁电化学循环性能图,在0.2 C下,电压窗口在0 ~ 3.0V之间,经过100次的循环性能图,在0.2 C倍率下,初始容量为998.6 mAh/g,经过100次循环后,电化学容量为990.9 mAh/g,容量保持率为99.2%。
实施例2
本实施例的高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法,步骤如下:
(1)取浓度为3.5 mol/L的硝酸亚铁溶液,采用十二烷基苯磺酸钠调节至pH=3.5,然后加入浓度为4.2 mol/L氢氧化钾溶液,继续搅拌12h,硝酸亚铁溶液和氢氧化钾溶液的体积比为1:3;
(2)将上述搅拌好的溶液转入150mL的水热反应釜中,然后采用十二烷基硫酸钠将溶液pH调节至10,在温度为110℃条件下,水热反应5h;
(3)将上述所得产品抽滤,干燥之后将样品在300℃煅烧6h后得到针叶状结构纳米氧化铁。
实施例3
本实施例的高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法,步骤如下:
(1)取浓度为4.6 mol/L的硝酸亚铁溶液,采用十二烷基苯磺酸钠调节至pH=1.5,然后加入浓度为5.7 mol/L氢氧化钾溶液,继续搅拌13h,硝酸亚铁溶液和氢氧化钾溶液的体积比为1:3;
(2)将上述搅拌好的溶液转入150mL的水热反应釜中,然后采用十二烷基硫酸钠将溶液pH调节至8,在温度为130℃条件下,水热反应4h;
(3)将上述所得产品抽滤,干燥之后将样品在400℃煅烧2h后得到针叶状结构纳米氧化铁。
以上显示和描述了本发明的基本原理和主要特征以及本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (4)
1.一种高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法,其特征在于步骤如下:
(1)取硝酸亚铁溶液,加入十二烷基苯磺酸钠调节硝酸亚铁溶液的pH=1.5 ~ 3.5,然后加入氢氧化钾溶液,继续搅拌10 h ~13h;
(2)将步骤(1)搅拌好的溶液转入水热反应釜中,加入十二烷基硫酸钠调节溶液pH=8~10,进行水热反应;
(3)反应结束后,抽滤,干燥得到样品,将样品煅烧后得高循环性能锂离子电池负极材料Fe2O3纳米针叶。
2.根据权利要求1所述的高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法,其特征在于:所述步骤(1)中硝酸亚铁溶液的浓度为(3.5-4.6) mol/L,氢氧化钾溶液的浓度为(4.2-5.7)mol/L,硝酸亚铁溶液与氢氧化钾溶液的体积比1:1-3。
3.根据权利要求1所述的高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法,其特征在于:所述步骤(2)中水热反应的温度为110℃~150℃,水热反应的时间为3 h-5h。
4.根据权利要求1所述的高循环性能锂离子电池负极材料Fe2O3纳米针叶的制备方法,其特征在于:所述步骤(3)中的煅烧温度为300℃-400℃,煅烧时间为2h~6h。
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JPS5820733A (ja) * | 1981-07-29 | 1983-02-07 | Kanto Denka Kogyo Kk | 極微小な非針状鉄酸化物の製造方法 |
CN103204550A (zh) * | 2013-04-12 | 2013-07-17 | 陕西科技大学 | 一种微米级Fe2O3 的可控制备方法 |
CN106328930A (zh) * | 2016-10-13 | 2017-01-11 | 河南理工大学 | 高容量锂离子电池负极材料α‑Fe2O3的制备方法 |
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JPS5820733A (ja) * | 1981-07-29 | 1983-02-07 | Kanto Denka Kogyo Kk | 極微小な非針状鉄酸化物の製造方法 |
CN103204550A (zh) * | 2013-04-12 | 2013-07-17 | 陕西科技大学 | 一种微米级Fe2O3 的可控制备方法 |
CN106328930A (zh) * | 2016-10-13 | 2017-01-11 | 河南理工大学 | 高容量锂离子电池负极材料α‑Fe2O3的制备方法 |
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