CN109694074B - 一种电化学法制备MXenes及其衍生物纳米片的方法 - Google Patents
一种电化学法制备MXenes及其衍生物纳米片的方法 Download PDFInfo
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Abstract
本发明属于MXenes及其衍生物纳米片的制备技术领域,涉及一种电化学法制备MXenes及其衍生物纳米片的方法,先称取1.43g氟化氢铵粉末、0.93g氟化铵粉末、1.55g氟化氢钠粉末分别放到50mL烧杯中,取50mL的去离子水加入到盛有粉末的烧杯中,放到磁力搅拌器上将氟化氢铵粉末彻底溶解;再将大块Ti3AlC2MAX固定到夹片电极上作为阳极,Pt片电极(面积>1.0cm2)作为阴极,并施加3V的直流恒电压,反应6‑24小时;最后离心制得产品,本发明与现有技术相比,制备过程中使用低浓度的氟化氢铵避免了高浓度的氢氟酸或者盐酸和氟化物的混合物,无毒,危害低,消除了潜在危险工艺过程绿色环保;采用电化学方法电解大块MAX过程缩短了反应时间,提高了剥离。
Description
技术领域:
本发明属于MXenes及其衍生物纳米片的制备技术领域,涉及一种自下而上的基于电化学法剥离制备MXenes及其衍生物纳米片的工艺,特别是一种以低浓度氟氢化物为电解液制备MXenes及其衍生物纳米片的方法,并将制备的MXenes及其衍生物纳米片应用到仿生酶领域。
背景技术:
二维材料定义为具有非常高的纵横比和相当于几个原子层的厚度的晶体,最近在国际上引起了人们的极大关注。而MXenes是一类新兴的二维(2D)过渡金属碳化物,氮化物或碳氮化物材料。到目前为止,研究最多的MXene是Ti3C2Tx,T代表表面终止基团,如=O,-OH,-F,x代表表面终止基团的个数。
Ti3C2Tx MXene由于其优异的化学性能被广泛的应用于生物传感器,电磁波吸收,催化剂,锂离子电池以及超级电容器等方面,因此引起了人们广泛的关注。但是由于Ti3C2TxMXene表面的Ti原子不稳定,可以氧化成为二氧化钛,这为制备TiO2/Ti3C2Tx及其衍生物提供了可能。然而,大多数MXenes的剥离需要高浓度的氢氟酸或者高浓度氟化锂和盐酸的混合溶液去除前驱体中的铝或硅相,继而用过氧化氢等氧化剂或者通过溶剂热的方法形成Ti3C2Tx MXene或其衍生物上负载有二氧化钛的复合物。但是,高浓度的氢氟酸和盐酸非常危险,对健康有害,且极易造成环境污染。此外,这些传统的剥离MXene的方法需要较长的蚀刻时间,以及后续插层,分层和离心等繁琐的步骤。因此,现在迫切的需要探索简单且环境友好的方法制备基于MXene的纳米材料,因此本发明寻求设计一种电化学法制备MXenes及其衍生物纳米片的方法,无毒且制备过程安全环保。
发明内容:
本发明的目的在于克服现有技术存在的缺点,寻求设计一种工艺简单、制备成本低、绿色环保的制备Ti3C2Tx MXene及其衍生物纳米片的方法,该方法通过电化学方法剥离得到的Ti3C2Tx MXene及其衍生物纳米片具有过氧化物酶和超氧化物歧化酶的双酶性质且能应用到仿生酶领域。相对于现有技术来说,此制造工艺简单、制备成本低、绿色环保地制备Ti3C2Tx MXene及其衍生物纳米片。
为了实现上述目的,本发明涉及的电化学法制备MXenes及其衍生物纳米片的方法的工艺具体包括以下步骤:
S1、称取1.43g氟化氢铵粉末、0.93g氟化铵粉末、1.55g氟化氢钠粉末分别放到50mL烧杯中,取50mL的去离子水加入到盛有粉末的烧杯中,放到磁力搅拌器上将氟化氢铵粉末彻底溶解;
S2、将大块Ti3AlC2 MAX固定到夹片电极上作为阳极,Pt片电极(面积>1.0cm2)作为阴极,并施加3V的直流恒电压,反应6-24小时;
S3、反应结束后将烧杯里的电解液取出后放入离心管中,将离心管对称放置于离心机内,以大于7000转/分钟的转速离心10分钟以上,取上层清液,离心结束后的电解液由于生成了Ti3C2Tx MXene及其衍生物纳米片而由无色变成为淡黄色再变为深棕色后再变为淡黄色。
本发明通过对所得的Ti3C2Tx MXene及其衍生物纳米片采用不同手段进行表征,所采用的手段包括原子力显微镜(AFM)、X射线衍射(XRD)、红外、X射线光电子能谱仪(XPS)和透射电镜(TEM)中的一种或两种以上。
本发明制备的Ti3C2Tx MXene及其衍生物纳米片粒径均匀且大约在230±30nm,平均尺寸为3.0±0.56nm;采用不同的电解质以及电解时间,所得到的Ti3C2Tx MXene及其衍生物纳米片的过氧化物酶性质有较大的差异,采用氟化氢铵为电解液电解16h得到的Ti3C2TxMXene及其衍生物纳米片具有最强的过氧化物酶的性质,同时被证明具有超氧化物歧化酶的性质,且通过电化学方法制备得到的Ti3C2Tx MXene及其衍生物纳米片能够用来进行胆固醇的检测,且其检测最低限可达到15.2μM。
本发明与现有技术相比,制备过程中使用低浓度的氟化氢铵避免了高浓度的氢氟酸或者盐酸和氟化物的混合物,无毒,危害低,消除了潜在危险工艺过程绿色环保;采用电化学方法电解大块MAX过程缩短了反应时间,提高了剥离,同时电化学提供了一个电氧化的作用,使MXene在无额外氧化剂的条件下快速得到二氧化钛,操作简单,原料易得,制备成本低。通过一步电化学法,生成负载有二氧化钛的MXenes纳米材料,并被发现有过氧化物酶和超氧化物歧化酶等纳米酶的性质,同时结合胆固醇酶建立双酶体系成功用于胆固醇的灵敏检测。
附图说明:
图1为本发明涉及的制备Ti3C2Tx MXene及其衍生物纳米片的机理图。
图2为本发明涉及的Ti3C2Tx MXene及其衍生物纳米片的透射电镜图、粒子尺寸分布图和原子力显微镜示意图。
图3为本发明使用实施例1中制备的Ti3C2Tx MXene及其衍生物纳米片,在不同的反应体系中,测试了波长为652nm处3,3',5,5'-四甲基联苯胺的紫外吸光度随时间变化原理示意图。
图4为本发明使用实施例1中制备的Ti3C2Tx MXene及其衍生物纳米片下消除超氧自由基的状态原理示意图。
图5为本发明使用实施例1中制备的Ti3C2Tx MXene及其衍生物纳米片检测胆固醇的紫外图和线性关系原理示意图。
具体实施方式:
下面通过具体实施例并结合附图对本发明作进一步说明。
实施例1:
本实施例涉及的电化学法制备MXenes及其衍生物纳米片的方法的工艺步骤具体如下:
S1、称取1.43g粉末放到50mL烧杯中,取50mL的去离子水加入到盛有粉末的烧杯中,放到磁力搅拌器上将氟化氢铵粉末彻底溶解;
S2、将大块Ti3AlC2 MAX固定到夹片电极上作为阳极,Pt片电极(面积>1.0cm2)作为阴极,并施加3V的直流恒电压,反应6-24小时;
S3、反应结束后将烧杯里的电解液取出后放入离心管中,将离心管对称放置于离心机内,以大于7000转/分钟的转速离心10分钟以上,取上层清液,离心结束后的电解液由无色变成为淡黄色再变为深棕色后再变为淡黄色。
实施例2:
本实施例对实施例1制备的Ti3C2Tx MXene及其衍生物纳米片在不同的反应体系中,测试了波长为652nm处3,3',5,5'-四甲基联苯胺的紫外吸光度随时间变化,如图3所示,在含有3,3',5,5'-四甲基联苯胺、过氧化氢和纳米片的体系中,反应溶液逐渐变成蓝色,证明该纳米片具有过氧化物酶的活性。
实施例3:
本实施例对实施例1制备的Ti3C2Tx MXene及其衍生物纳米片消除超氧自由基的情况,如图4A所示,在含有核黄素、蛋氨酸和硝基四氮唑蓝的混合溶液中加入纳米片,在有光照照射的情况下,其在560nm处的紫外吸光度有所下降,说明其消除了超氧自由基;如图4B所示,随着纳米片的浓度的增加,560nm处的紫外吸光度逐渐降低,说明消除超氧自由基的含量逐渐增多,证明该纳米片具有超氧化物歧化酶的活性。
实例4:
本实施例对实施例1制备的Ti3C2Tx MXene及其衍生物纳米片应用于胆固醇的检测,如图5所示,其检测最低限可达到15.2μM。
Claims (3)
1.一种电化学法制备MXenes及其衍生物纳米片的方法,其特征在于工艺具体包括以下步骤:
S1、称取1.43g氟化氢铵粉末放到50mL烧杯中,取50mL的去离子水加入到盛有粉末的烧杯中,放到磁力搅拌器上将氟化氢铵粉末彻底溶解;
S2、将大块Ti3AlC2 MAX固定到夹片电极上作为阳极,Pt片电极作为阴极,其中Pt片电极的面积>1.0cm2,并施加3V的直流恒电压,反应6-24小时;
S3、反应结束后将烧杯里的电解液取出后放入离心管中,将离心管对称放置于离心机内,以大于7000转/分钟的转速离心10分钟以上,取上层清液,离心结束后的电解液由于生成了Ti3C2TxMXene及其衍生物纳米片而由无色变成为淡黄色再变为深棕色后再变为淡黄色。
2.根据权利要求1所述的一种电化学法制备MXenes及其衍生物纳米片的方法,其特征在于上述制备的Ti3C2TxMXene及其衍生物纳米片粒径均匀且在230±30nm,平均尺寸为3.0±0.56nm。
3.如权利要求1-2中任一权利要求所述方法制备得到MXenes及其衍生物纳米片的应用,其特征在于制备得到的Ti3C2TxMXene及其衍生物纳米片能够用来进行胆固醇的检测,且其检测最低限可达到15.2μM。
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