CN115385309A - 一种二维氧掺杂GaSe纳米片的制备方法及应用 - Google Patents
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Abstract
本发明涉及材料制备技术领域,公开了一种二维氧掺杂GaSe纳米片的制备方法及应用,包括以下步骤:步骤1:将GaSe粉末置于溶剂中,超声处理;步骤2:在步骤1得到的溶液中滴加H2O2;其中GaSe粉末和H2O2的比例为4:1;步骤3:滴加完成后超声处理,离心得到含二维氧掺杂GaSe纳米片;本发明得到的氧掺杂GaSe纳米片制备得到的气敏传感器件,在UV光激发条件下实现了室温下的可逆传感,其具有较低的NO2检测极限,较快的气敏响应和恢复速度以及优异的气体选择性。
Description
技术领域
本发明涉及材料制备技术领域,具体涉及一种二维氧掺杂GaSe纳米片的制备方法及应用。
背景技术
二维材料的氧掺杂是改变和增强二维材料器件性能的重要策略之一。二维材料经氧掺杂后能获得性能的提升,包括器件的化学稳定性、宽带隙、高开/关比、高迁移率和透明性等。各种二维材料共混的掺杂,在器件最大化电子迁移率和光电异质结构方面有着巨大的前景和潜力。随着二维材料器件的发展,各种特殊需要不断提出。
现有的二维氧掺杂技术如CN106898691A公开了一种氧掺杂二硫化钼热电材料的制备方法,氧掺杂二硫化钼热电材料的制备方法包括以下步骤:首先称取一定质量的MoS2粉末,平铺于刚玉舟中,然后放到水平管式炉的石英管中,升到一定的温度,在空气气氛下恒温一定时间,得到氧掺杂二硫化钼粉末。这种方法制备过程复杂,不适合进行工业化生产。
发明内容
本发明针对现有技术存在的问题提供一种二维氧掺杂GaSe纳米片的制备方法及应用。
本发明采用的技术方案是:
一种二维氧掺杂GaSe纳米片的制备方法,包括以下步骤:
步骤1:将GaSe粉末置于溶剂中,超声处理;
步骤2:在步骤1得到的溶液中滴加H2O2水溶液;其中GaSe粉末和H2O2的质量比为4:1;
步骤3:滴加完成后超声处理,离心得到二维氧掺杂GaSe纳米片。
进一步的,所述步骤1中GaSe粉末首先进行研磨,研磨时间为30 min。
进一步的,所述步骤1中溶剂为异丙醇。
进一步的,所述步骤1中超声功率为100 W,超声时间为2 h。
进一步的,所述步骤2中H2O2水溶液滴加时间为30 min。
进一步的,所述步骤3中离心转速为4000 rpm,离心时间为30 min,得到离心后上清液,然后以10000 rpm的高速离心收集上清液中的材料。
二维氧掺杂GaSe纳米片的应用,二维氧掺杂GaSe纳米片用于制备气体传感器。
进一步的,所述气体传感器的制备过程如下:将含有二维氧掺杂GaSe纳米片分散液滴注在插值电极上即可得到气体传感器。
本发明的有益效果是:
(1)本发明通过简单的制备方法实现二维材料的剥离和氧的掺杂,得到玻璃的二维GaSe纳米片,其平均厚度为3.7 nm;
(2)本发明得到的氧掺杂GaSe纳米片制备得到的气敏传感器件,在UV光激发条件下实现了室温下的可逆传感,其具有较低的NO2检测极限,较快的气敏响应和恢复速度以及优异的气体选择性。
附图说明
图1为本发明实施例1得到的二维氧掺杂GaSe纳米片的测试结果,a为原子力显微镜图,b、c、d为X射线光子谱分析曲线,b为Ga3D的XPS,c为Se3d的XPS图,d为O1s的XPS图,e为紫外-可见光吸收光谱,f为能带隙计算的Tauc plot图。
图2为采用本发明实施例1得到的二维氧掺杂GaSe纳米片制备得到的气敏传感器测试结果,a为实物图,b为GaSe和二维氧掺杂GaSe纳米片对NO2气敏响应对比图,c为传感器对不同气体的选择性,d为气体传感器的动态气敏响应图,e为传感器对不同NO2的响应时间和恢复时间,f为传感器在UV光激发条件下对10 ppm NO2气敏传感的重复性。
具体实施方式
下面结合附图和具体实施例对本发明做进一步说明。
一种二维氧掺杂GaSe纳米片的制备方法,包括以下步骤:
步骤1:将GaSe粉末置于溶剂中,超声处理;其中GaSe首先置于研钵中研磨30 min,以获得更小尺寸的体相GaSe从而提高材料的制备效率。将研磨后的GaSe倒入烧杯中加入40mL的异丙醇作为剥离溶剂。将烧杯放入超声破碎仪中以100 W的超声功率处理2 h。
步骤2:在步骤1得到的溶液中滴加H2O2水溶液;其中GaSe粉末和H2O2的质量比为4:1;其中H2O2浓度为1 %,滴加时间为30 min。
步骤3:滴加完成后超声处理,离心得到含二维氧掺杂GaSe纳米片的上清液;超声处理后,将烧杯中的分散液离心处理30 min,离心转速为4000 rpm,以除去分散液中的未被完全剥离的体相GaSe,取4000 rpm离心的上清液,对其进行10000 rpm的高速离心收集上清液中的材料。
实施例1
一种二维氧掺杂GaSe纳米片的制备方法,包括以下步骤:
步骤1:将40 mg GaSe粉末置于溶剂中,超声处理;其中GaSe首先置于研钵中研磨30 min,以获得更小尺寸的体相GaSe从而提高材料的制备效率。将研磨后的GaSe倒入烧杯中加入40 mL的异丙醇作为剥离溶剂。将烧杯放入超声破碎仪中以100 W的超声功率处理2h。
步骤2:在步骤1得到的溶液逐滴加入10 mL 0.1 % H2O2;滴加时间为30 min。
步骤3:滴加完成后超声处理,离心得到含二维氧掺杂GaSe纳米片的上清液;超声处理后,将烧杯中的分散液离心处理30 min,离心转速为4000 rpm,以除去分散液中的未被完全剥离的体相GaSe,取4000 rpm离心的上清液,对其进行10000 rpm的高速离心收集上清液中的材料。
将该实施例得到的二维氧掺杂GaSe纳米片进行表征,其原子力显微镜如图1a所示,剥离得到了材料厚度为3.7 nm的薄片,表面成功剥离得到了少层的二维材料。随后对剥离得到的少层二维材料进行X射线光电子谱分析,结果如图b、c和d所示。二维材料中同时存在Ga、Se、O元素,表面GaSe剥离的同时发生了氧掺杂。二维氧掺杂GaSe的紫外-可见光吸收光谱如图e所示,其对700 nm范围内的光内有较强的吸收,通过Tauc plot法计算的直接能带间隙为1.8 eV如图f所示。
将本实施例得到的二维氧掺杂GaSe纳米片制备得到气体传感器,方法如下:将含有氧掺杂GaSe纳米片的分散液滴注在间距为10 μm的插值电极上获得,如图2a所示。其气体传感测试在室温、365 nmUV光光照射下进行,传感器的电阻通过Tektronix DMM 4040数字万用表进行测量。进入气敏腔室的总气体流速保持在200标准立方厘米/分钟(sccm),由高精度质量流量控制器控制。气敏响应定义为(R0-Rg)/Rg×100%,其中R0和Rg分别代表器件在N2平衡气体和分析气体中的电阻。
如图2b所示,氧掺杂后的GaSe对比纯GaSe对10 ppm NO2的气敏响应值提升了接近两倍。此外,基于氧掺杂GaSe的气敏器件对NO2展现出优异的选择性如图2c所示。其对10ppm NO2的响应值为500 ppm CO、1% CH4、1% H2、50 ppm H2S、50 ppm SO2、300 ppm NH3的6.65倍,这源于NO2分子对氧掺杂GaSe纳米片较强的亲和力。其在室温条件下该传感器对10ppm NO2的响应值达到了82.1%,且其实际测试极限对0.05 ppm NO2的响应值为12.6%,如图2d所示。该传感器对不同浓度的NO2的响应时间和恢复时间分析如图2e所示,随着NO2浓度的增加,其响应时间逐渐降低(6 min、3 min、3 min、3 min、2 min、1 min),但其恢复时间基本为6 min。UV光激发下的室温条件下,该传感器对10 ppm NO2气敏传感的可重复性如图2f所示,实验可以观察到经过六个连续测试循环后响应幅度几乎没有变化。
通过在超声玻璃GaSe的过程中加入特殊的氧化剂H2O2,同时实现了二维材料的剥离与氧掺杂,从而获得了二维氧掺杂GaSe。通过滴注法获得了二维氧掺杂GaSe的气敏传感器件,其相关气敏测试表面,该气敏传感器在UV光激发条件下实现了室温下的可逆传感,具有较低的NO2检测极限(0.05 ppm),较快的气敏响应和恢复速度以及优异的气体选择性。
本发明制备方法简单,实现了二维材料的剥离与氧掺杂,得到二维氧掺杂GaSe。通过滴注法获得了二维氧掺杂GaSe气敏传感器件,其气敏测试表面,该气敏传感器在UV光激发条件下实现了室温下的可逆传感,其具有较低的NO2检测极限(0.05 ppm),较快的气敏响应和恢复速度以及优异的气体选择性。
Claims (8)
1.一种二维氧掺杂GaSe纳米片的制备方法,其特征在于,包括以下步骤:
步骤1:将GaSe粉末置于溶剂中,超声处理;
步骤2:在步骤1得到的溶液中滴加H2O2水溶液;其中GaSe粉末和H2O2的质量比为4:1;
步骤3:滴加完成后超声处理,离心后得到二维氧掺杂GaSe纳米片。
2.根据权利要求1所述的一种二维氧掺杂GaSe纳米片的制备方法,其特征在于,所述步骤1中GaSe粉末首先进行研磨,研磨时间为30 min。
3.根据权利要求1所述的一种二维氧掺杂GaSe纳米片的制备方法,其特征在于,所述步骤1中溶剂为异丙醇。
4.根据权利要求1所述的一种二维氧掺杂GaSe纳米片的制备方法,其特征在于,所述步骤1中超声功率为100 W,超声时间为2 h。
5.根据权利要求1所述的一种二维氧掺杂GaSe纳米片的制备方法,其特征在于,所述步骤2中H2O2水溶液滴加时间为30 min。
6.根据权利要求1所述的一种二维氧掺杂GaSe纳米片的制备方法,其特征在于,所述步骤3中离心转速为4000 rpm,离心时间为30 min,得到离心后上清液,然后以10000 rpm的高速离心收集上清液中的材料。
7.如权利要求1~6任一项所述二维氧掺杂GaSe纳米片的制备方法得到的二维氧掺杂GaSe纳米片的应用,其特征在于,二维氧掺杂GaSe纳米片用于制备气体传感器。
8.根据权利要求7所述的一种二维氧掺杂GaSe纳米片的应用,其特征在于,所述气体传感器的制备过程如下:将含有二维氧掺杂GaSe纳米片分散液滴注在插值电极上即可得到气体传感器。
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