CN111704137B - 一种高产率低氟含量的少层MXenes纳米片的制备方法 - Google Patents
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Abstract
一种高产率低氟含量的少层MXenes纳米片的制备方法,属于纳米材料技术领域。将聚乙二醇或烷基酚聚氧乙烯醚等含有羟基或活性氧的有机物、MAX、盐酸、氟化锂混合后,在35℃下搅拌处理24小时,水洗至PH为中性离心即可获得低氟含量的少层MXenes纳米片。本发明有效地解决了少层MXenes纳米片制备过程中产率低和氟含量高的一系列问题,同时制备方法简单,价格低廉、可规模化生产,具有实用前景。
Description
技术领域
本发明属于纳米材料技术领域,特别涉及一种高产率低氟含量的少层MXenes纳米片制备方法。
背景技术
过渡金属碳化物MXenes是一种具有类石墨烯结构的新型二维材料,具有良好的化学稳定性、亲水性、导电性、力学性能以及高比表面积等优点。自2011年由Yury人GogoTsi等人发现以来,已在电化学储能、污水处理、传感器、海水淡化等领域展现出巨大的应用前景。目前,MXenes的制备方法主要通过氢氟酸或氟盐与盐酸的混合溶液刻蚀MAX相中结合较弱的A位元素而得到。这一类方法所制备的MXenes材料常带有F、OH、O等官能团且剥离后所制备的MXenes纳米片的产量极低。更严重的是,其中F官能团的大量存在阻碍了MXenes纳米片的应用,尤其是电化学储能方面。因此,通过改善化学刻蚀探索出一种制备具有高产率低氟含量的MXenes纳米片的方法是其进一步的产业化应用的关键。
发明内容
本发明的目的在于:提供一种简单的改良工艺制备低氟含量的少层MXenes纳米片,并提高少层MXenes的产率,以解决常规制备方法中MXenes纳米片氟含量高,产率低的问题。
本发明将聚乙二醇或烷基酚聚氧乙烯醚等含有羟基或活性氧的有机物、MAX、盐酸、氟化锂混合后,在35℃下搅拌处理24小时,水洗至PH为中性离心即可获得低氟含量的少层MXenes纳米片。搅拌刻蚀过程中,聚乙二醇或烷基酚聚氧乙烯醚等含有羟基或活性氧的有机物分子链上的大量羟基或活性氧会迅速与Ti原子结合形成稳定结构,减少F原子与钛结合的机会,进而实现低氟含量MXenes纳米片的制备。此外,长链的聚乙二醇或烷基酚聚氧乙烯醚等含有羟基或活性氧的有机物分子还同时作为MXenes片层之间的插层剂,减小片与片之间的范德华力,加快片层的剥离速度,从而提高产量。
具体的制备工艺为:
(1)将聚乙二醇或烷基酚聚氧乙烯醚等含有羟基或活性氧的有机物、盐酸、氟化锂混合
其中,聚乙二醇或烷基酚聚氧乙烯醚等含有羟基或活性氧的有机物在混合溶剂中的比例为1-5%;
(2)将MAX缓慢加入到步骤(1)得到的混合溶液在35℃下搅拌处理24小时;
(3)将步骤(2)所得产物机械震荡20-60min,然后水洗至PH为中性后离心即可获得低氟含量的少层MXenes纳米片。
其中含有羟基或活性氧的有机物在混合溶剂中所占比例为1-5wt%。
本发明中的烷基酚聚氧乙烯醚规格包括OP-4、OP-7、OP-10或OP-15,分子式为C34H62O11。
本发明有效地解决了少层MXenes纳米片制备过程中产率低和氟含量高的一系列问题,同时制备方法简单,价格低廉、可规模化生产,具有实用前景。
附图说明
图1为实施例1所制备的少层MXenes纳米片的扫描电镜图。
图2为实施例1所制备的少层MXenes纳米片的XRD。
图3为以实施例1所制备的少层MXenes纳米片F含量与常规样品的对比。
图4为以实施例1所制备的少层MXenes纳米片产量与常规样品的对比。
具体实施方式
实施例1:
(1)将质量为1g聚乙二醇与1g氟化锂加入20ml的9M盐酸中混合均匀;
(2)将质量为1g的MAX缓慢加入步骤(1)得到混合溶液中,并在35℃温度下搅拌处理24小时。
(3)将步骤(2)所得产物机械震荡20-60min,然后水洗至PH为中性后离心即可获得低氟含量的少层MXenes纳米片。
实施例2:
(1)将质量为1gOP-4与1g氟化锂加入20ml的9M盐酸中混合均匀;
(2)将质量为1g的MAX缓慢加入步骤(1)得到混合溶液中,并在35℃温度下搅拌处理24小时。
(3)将步骤(2)所得产物机械震荡20-60min,然后水洗至PH为中性后离心即可获得低氟含量的少层MXenes纳米片。
实施例3:
(1)将质量为1gOP-10与1g氟化锂加入20ml的9M盐酸中混合均匀;
(2)将质量为1g的MAX缓慢加入步骤(1)得到混合溶液中,并在35℃温度下搅拌处理24小时。
(3)将步骤(2)所得产物机械震荡20-60min,然后水洗至PH为中性后离心即可获得低氟含量的少层MXenes纳米片。
对比例1
(1)将质量为1g氟化锂加入20ml的9M盐酸中混合均匀;
(2)将质量为1g的MAX缓慢加入步骤(1)得到混合溶液中,并在35℃温度下搅拌处理24小时。
(3)将步骤(2)所得产物机械震荡20-60min,然后水洗至PH为中性后离心即可获得低氟含量的少层MXenes纳米片。
对上述所得低氟含量的少层MXenes进行SEM、XRD、XPS测试,SEM和XRD结果改良工艺所制备的少层MXenes纳米片与常规工艺所制得的样品无差异,如图1、2所示。但XPS测试表明改良工艺所得样品氟含量明显降低,且产率大幅提高,如图3、4所示。
Claims (2)
1.一种高产率低氟含量的少层MXenes纳米片的制备方法,其特征在于:所述的制备方法为,
(1)将含有羟基或活性氧的有机物、盐酸、氟化锂混合;
(2)将MAX缓慢加入到步骤(1)得到的混合溶液在35℃下搅拌处理24小时;
(3)将步骤(2)所得产物机械震荡20-60min,然后水洗至PH为中性后离心即可获得低氟含量的少层MXenes纳米片;
其中:步骤(1)中所述的含有羟基或活性氧的有机物为聚乙二醇、OP-4、OP-7、OP-10或OP-15。
2.如权利要求1所述的高产率低氟含量的少层MXenes纳米片的制备方法,其特征在于:含有羟基或活性氧的有机物在混合溶剂中所占比例为1-5wt%。
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