CN106910891A - 一种过渡金属氟化物负载硼掺杂纳米碳复合材料的制备方法 - Google Patents
一种过渡金属氟化物负载硼掺杂纳米碳复合材料的制备方法 Download PDFInfo
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Abstract
本发明属于纳米材料技术领域,具体涉及一种过渡金属氟化物负载硼掺杂纳米碳材料的制备方法。本发明方法以过渡金属氟化物、硼氢化物和纳米碳材料作为原材料,通过球磨和加热,即可制得过渡金属氟化物负载硼掺杂纳米碳复合材料。该方法具有低成本,高效率,经济环保,普适性强等特点。
Description
技术领域
本发明属于纳米材料技术领域,具体涉及一种过渡金属氟化物负载硼掺杂纳米碳复合材料的制备方法。
背景技术
锂离子电池具有能量密度高、循环寿命长、转换效率高等优点,被广泛应用于电动汽车、智能电网等高效储能***中。目前商业的锂离子电池的正/负极材料均为插嵌型(例如:石墨负极;LiCoO2正极)。这些插嵌型正负极材料的理论比容量较低(石墨负极的理论比容量仅为:375mAh g-1,LiCoO2正极的理论比容量仅为:140mAh g-1),严重制约了锂离子电池的能量密度。[1,2]因此,开发高比容量的正/负极材料是提高锂离子电池能量密度的关键。
近年来,一系列研究表明过渡金属氟化物(例如: FeF3、FeF2、NiF2、CoF3、CoF2、NiF3、MnF2、CuF2、TiF4等)具有比容量大,能量密度高,廉价无污染等特点,是一类很有潜力的锂离子电池正/负极材料。[3-8] 其中,正极材料以FeF3为代表,其理论比容量高达712mAh g-1,平均工作电压为2.74 V,能量密度可达1951 Wh kg-1;[4,8-10] 负极材料以MnF2为代表,其理论比容量高达577mAh g-1,工作电压为0.8 V。[11,12] 然而,过渡金属氟化物在脱/嵌锂过程中存在着导电性差,体积变化大,电压滞后严重等问题,导致其容量迅速衰减,循环稳定性差。[4,11] 研究工作者们针对这些问题进行了一系列的研究工作。在这之中,将过渡金属氟化物预嵌锂转化成过渡金属/氟化锂,并进一步与纳米碳材料复合是目前普遍采用的解决方案,例如:利用球磨热解法制备的Fe/LiF/石墨烯复合材料在180个循环后仍可保持150 mAh g-1的比容量。[13]过渡金属氟化物脱嵌锂性能的提升归因于:首先,构建碳复合体系可有效缓解其循环过程中的体积变化,并增强体系导电性;其次,预嵌锂后FeF3等正极材料可以直接与石墨、硅等无锂负极组成全电池,MnF2等负极材料在预嵌锂后的首次库仑效率也显著提高。构筑过渡金属/氟化锂/纳米碳复合材料具有以上显著的优点,尚存以下不足:
(1)长循环性能仍难以满足实际应用需求,还需要进一步通过引入杂原子掺杂的碳材料提高其循环性能[14];
(2)过渡金属/氟化锂/纳米碳复合材料的制备一般通过喷雾,球磨热解还原,化学沉积,水热等方法实现,制备成本高,效率低,不利于工业化生产,且难同步实现杂原子的均匀掺杂[15,16];
(3)现有制备方法普遍采用先将氟化锂与过渡金属分别负载至纳米碳材料的载体上,导致氟化锂与过渡金属纳米颗粒之间难以紧密结合,增加了在充电过程中离子/原子扩散距离,严重影响脱/嵌锂电化学反应的可逆程度[13]。
因此,开发一种将氟化锂与过渡金属纳米颗粒同步负载至杂原子掺杂的碳材料,且兼具低成本和高效率的制备方法具有非常重要的意义。
参考文献
[1] Croguennec, L.; Palacin, M. R. J. Am. Chem. Soc. 2015,137, 3140.
[2] Goodenough, J. B.; Kim, Y. Chem. Mater. 2010,22, 587.
[3] Li, H.; Richter, G.; Maier, J. Adv. Mater. 2003,15, 736.
[4]Li, H.; Balaya, P.; Maier, J. J. Electrochem. Soc. 2004,151, 1878.
[5]Amatucci, G. G.; Pereira, N. J. Fluorine Chem. 2007,128, 243.
[6]Teng, Y. T.; Pramana, S. S.; Ding, J.; Wu, T.; Yazami, R. Electrochim. Acta 2013,107, 301.
[7]Hua, X.; Robert, R.; Du, L. S.; Wiaderek, K. M.; Leskes, M.; Chapman,K. W.; Chupas, P. J.; Grey, C. P. J. Phys. Chem. C 2014,118, 15169.
[8]Wang, F.; Robert, R.; Chernova, N. A.; Pereira, N.; Omenya, F.;Badway, F.; Hua, X.; Ruotolo, M.; Zhang, R.; Wu, L.; Volkov, V.; Su, D.; Key,B.; Whittingham, M. S.; Grey, C. P.; Amatucci, G. G.; Zhu, Y.; Graetz, J. J. Am. Chem. Soc. 2011,133, 18828.
[9]Liu, P.; Vajo, J. J.; Wang, J. S.; Li, W.; Liu, J. J. Phys. Chem. C 2012,116, 6467.
[10]Ma, D. L.; Cao, Z. Y.; Wang, H. G.; Huang, X. L.; Wang, L. M.; Zhang,X. B. Energy Environ. Sci. 2012,5, 8538.
[11]Rui, K.; Wen, Z.; Lu, Y.; Jin, J.; Shen, C. Adv. Energy Mater. 2015,5, 1401716.
[12]Rui, K.; Wen, Z.; Huang, X.; Lu, Y.; Jin, J.; Shen, C. Phys. Chem. Chem. Phys. 2016,18, 3780.
[13]Ma, R.; Dong, Y.; Xi, L.; Yang, S.; Lu, Z.; Chung, C. ACS Appl. Mater. Interfaces 2013,5, 892.
[14]Kumagae, K.; Okazaki, K.; Matsui, K.; Horino, H.; Hirai, T.; Yamaki,J.; Ogumi, Z. J. Electrochem. Soc. 2016,163, 1633.
[15]Sun, Y.; Liu, N.; Cui, Y. Nature Energy 2016,1, 16071.
[16] Rui, K.; Wen, Z.; Lu, Y.; Shen, C.; Jin, J. ACS Appl. Mater. Interfaces 2016,8, 1819.。
发明内容
本发明的目的在于提供一种过渡金属氟化物负载硼掺杂纳米碳复合材料的制备方法,使过渡金属与氟化锂的纳米颗粒紧密结合地分散在纳米碳材料基体上,且可同步实现硼掺杂。该方法具有成本低,效率高,经济环保,普适性强等特点。
本发明提供的过渡金属氟化物负载硼掺杂纳米碳复合材料的制备方法,具体步骤如下:
(1)将过渡金属氟化物、硼氢化物(LiBH4)、纳米碳材料加入到球磨罐中,过渡金属氟化物与LiBH4的摩尔比例为1:1~1:4,纳米碳材料的质量占总体质量比为5wt%~80wt%,在保护气氛下球磨2~48 小时;
优选过渡金属氟化物与LiBH4的摩尔比例为1:1~1:2.5,纳米碳材料的质量占总体质量比为5wt%~40wt%,球磨时间为20~48小时;
(2)将球磨产物在动态真空条件下加热至120~500℃,并保温1~48小时,然后降温至室温,收集产物,即得过渡金属氟化物负载硼掺杂纳米碳复合材料。
优选加热温度为320~400℃,保温时间为30~45小时。
步骤(1)中,所述的过渡金属氟化物为FeF3、FeF2、NiF2、NiF3、CoF3、CoF2、MnF2、CuF2、TiF4、ZnF2中的任意一种,或其中的几种。所述的纳米碳材料为石墨、石墨烯、单壁碳纳米管、多壁碳纳米管、碳纳米棒、碳纤维、碳纳米线、碳纳米棍中的任意一种,或其中的几种。所述的保护气氛为氢气、氮气、氩气、氦气中的任意一种。
步骤(2)中,所述的过渡金属为Fe、Ti、Ni、Co、Cu、Mn、Zn中的任意一种,或其中的几种。
本发明方法的积极效果是:
(1)本方法操作简单,所需的球磨和真空脱气装置,均为工业常见生产设备,所需的最高温度仅为500℃,因此本方法效率高,可应用于大规模工业化生产;
(2)本方法制备过程无废液/物排放,且所需的过渡金属氟化物,硼氢化锂和纳米碳材料均为工业常见原材料,因此本方法经济环保,生产成本低廉;
(3)本方法可制备Mn、Fe、Ti、Ni、Co、Cu、Zn等多种过渡金属氟化物负载硼掺杂纳米碳复合材料,在复合材料中氟化锂和过渡金属均以纳米颗粒形式紧密结合地均匀分散在纳米碳载体上,且掺杂元素硼的含量、形貌和分布等可根据制备条件进一步进行调控。
附图说明
图1是所合成的硼掺杂的Mn/LiF/石墨复合材料的X射线衍射图谱。
图2是所合成的硼掺杂的Mn/LiF/石墨复合材料的高倍透射电子显微镜图像。
图3是所合成的硼掺杂的Mn/LiF/石墨复合材料的循环嵌脱锂性能。
图4是所合成的硼掺杂的Fe/LiF/石墨复合材料的扫描电子显微镜图像。
图5是所合成的硼掺杂的Fe/LiF/石墨复合材料的X射线能量分布图谱。
具体实施方式
以下结合示例与附图对本发明的制备方法进行详细的描述。
实施例1:硼掺杂的Mn/LiF/石墨复合材料的制备及其电化学储锂特性
在惰性气体手套箱内,将0.465g MnF2、0.22 g LiBH4和0.2 g 石墨粉末混合装入球磨罐中,在氢气气氛下球磨24 h,球磨转速为400转/分钟,球料比为30:1。将球磨产物持续抽真空,并逐渐升温至140 ℃,保温12 h后自然降至室温,可得到硼掺杂的Mn/LiF/石墨复合材料。所合成的硼掺杂的Mn/LiF/石墨复合材料的X射线衍射图谱和高倍透射电子显微镜图像分别如图1和2所示。图1表明该方法成功制备了LiF。图2中可见Mn和硼的纳米颗粒分散在无定形石墨层上。结合图1和图2说明该方法既可以制备过渡金属/氟化锂/纳米碳复合材料,又可以同步实现硼掺杂。图3给出了所制备的硼掺杂的Mn/LiF/石墨复合材料的长循环性能。在1 A g-1的电流密度下,经过1500个循环,所合成的硼掺杂的Mn/LiF/石墨复合材料仍可以保持的423 mAh g-1的比容量,说明该方法制备的硼掺杂的Mn/LiF/石墨复合材料具有优良的循环性能。
实施例2:硼掺杂的Fe/LiF/石墨复合材料的制备
在惰性气体手套箱内,将0.47 g FeF2、0.25 g LiBH4和0.15 g石墨粉末混合装入球磨罐中,在氩气气氛下球磨48 h,球磨转速为400转/分钟,球料比为40:1。将球磨产物持续抽真空,并逐渐升温至450 ℃,保温12 h后自然降至室温,可得到硼掺杂的Fe/LiF/石墨复合材料。图4和图5分别给出了所制备的硼掺杂的Fe/LiF/石墨复合材料的扫描电子显微镜及其对应的X射线能量分布图谱。图4中可见所制备的Fe/Li/石墨复合材料的颗粒大小为50nm左右。图5中明显可见B、C、F、Fe元素,说明该方法可制备Fe/LiF/石墨复合材料,并同步实现硼掺杂。
实施例3:硼掺杂的Ni/LiF/石墨烯复合材料的制备
在惰性气体手套箱内,将0.485 g NiF2、0.32 g LiBH4和0.1 g石墨烯粉末混合装入球磨罐中,在氮气气氛下球磨6 h,球磨转速为350转/分钟,球料比为40:1。将球磨产物持续抽真空,并逐渐升温至350℃,保温6 h后自然降至室温,可得到硼掺杂的Ni/LiF/石墨烯复合材料。
实施例4:硼掺杂的Co/LiF/多壁碳纳米管复合材料的制备
在惰性气体手套箱内,将0.485 g CoF2、0.25 g LiBH4和0.2 g多壁碳纳米管粉末混合装入球磨罐中,在氢气气氛下球磨4 h,球磨转速为300转/分钟,球料比为30:1。将球磨产物持续抽真空,并逐渐升温至500℃,保温10 h后自然降至室温,可得到硼掺杂的Co/LiF/多壁碳纳米管复合材料。
实施例5:硼掺杂的Mn/LiF/单壁碳纳米管复合材料的制备
在惰性气体手套箱内,将0.47 g MnF2和0.3 g LiBH4和0.25 g单壁碳纳米管粉末混合装入球磨罐中,在氢气气氛下球磨36 h,球磨转速为300转/分钟,球料比为40:1。将球磨产物持续抽真空,并逐渐升温至280 ℃,保温12 h后自然降至室温,可得到硼掺杂的Mn/LiF/单壁碳纳米管复合材料。
Claims (3)
1.一种过渡金属氟化物负载硼掺杂纳米碳复合材料的制备方法,具体步骤如下:
(1)将过渡金属氟化物、LiBH4、纳米碳材料加入到球磨罐中,过渡金属氟化物与LiBH4的摩尔比例为1:1~1:4,纳米碳材料的质量占总体质量比为5wt%~80wt%,在保护气氛下球磨2~48 小时;
(2)将球磨产物在动态真空条件下加热至120~500℃,并保温1~48小时,然后降温至室温,收集产物,即得过渡金属氟化物负载硼掺杂纳米碳复合材料。
2.根据权利要求所述的制备方法,其特征在于,步骤(1)中,所述的过渡金属氟化物为FeF3、FeF2、NiF2、NiF3、CoF3、CoF2、MnF2、CuF2、TiF4、ZnF2中的任意一种,或其中的几种;所述的纳米碳材料为石墨、石墨烯、单壁碳纳米管、多壁碳纳米管、碳纳米棒、碳纤维、碳纳米线、碳纳米棍中的任意一种,或其中的几种;所述的保护气氛为氢气、氮气、氩气、氦气中的任意一种。
3.根据权利要求所述的制备方法,其特征在于,步骤(2)中,所述的过渡金属为Fe、Ti、Ni、Co、Cu、Mn、Zn中的任意一种,或其中的几种。
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