CN110801851B - 黑磷纳米片/硫化镉光催化固氮催化剂的制备方法和应用 - Google Patents
黑磷纳米片/硫化镉光催化固氮催化剂的制备方法和应用 Download PDFInfo
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Abstract
本发明公开一种黑磷纳米片/硫化镉光催化固氮催化剂的制备方法和应用。黑磷纳米片/硫化镉光催化固氮催化剂首先通过电化学膨胀辅和超声分散方法制备得到黑磷纳米片,然后在黑磷纳米片表面生长硫化镉纳米粒子获得黑磷纳米片/硫化镉光催化剂。所制备的黑磷纳米片/硫化镉光催化剂在可见光光照下可以将氮气还原为氨气,实现了光催化人工固氮。本发明的黑磷纳米片/硫化镉光催化剂具有低成本,稳定、制备快和工艺简单等优点。
Description
技术领域
本发明属于环境友好材料领域,尤其是涉及一种黑磷纳米片/硫化镉光催 化固氮催化剂的制备方法和应用。
背景技术
黑磷是一种在近几年受到广泛关注的二维材料。黑磷是磷元素的三种 同素异形体之一,并且是其中最稳定的存在形式。黑磷有着很多独特且出 色的性能特点,比如高载流子迁移率,高开关比,强面内各向异性,以及 可调的能带结构,随着层数的减少禁带宽度变大。基于上述优点,黑磷已 经广泛应用于场效应晶体管,电池,光催化产氢,生物医学等领域。但是 如何以较快的速度制备黑磷纳米片依然是限制其广泛应用的一个重要因 素。目前使用最广泛的方法有机械剥离和液相剥离,但这两者的剥离速度 较慢,所得纳米片的尺寸较小,并且在制备过程中会产生一定的噪音。因 此,发明一种制备工艺简单,产量大,绿色的方法将极大地推动黑磷的应 用。
氨是一种在工业和农业上都必不可少的重要材料。在工业上,目前普 遍使用哈伯合成法来制备氨。但这是一个高能耗的过程,其年消耗能源量 占全球能源总消耗量的2%左右。因此,开发一种绿色的合成方法是众多研 究的重点。而光催化固氮是其中比较理想和有前景的方式,在这过程中, 直接利用太阳能将水和空气中的氮气直接转化为氨。目前所使用的光催化 固氮材料可分成金属材料,非金属材料,金属硫化物等。但这些材料都受活性低,产量低等缺点的限制,阻碍了其广泛应用。因此,设计制备高活 性,制备简单的光催化剂具有重要的研究意义。
基于此,本发明提出一种黑磷纳米片/硫化镉光催化固氮催化剂制备方 法和应用。本发明的黑磷纳米片/硫化镉光催化剂制备方法,具有快速、高 效和低成本的特点,可制备高质量黑磷纳米片/硫化镉,并应用于光催化固 氮领域。
发明内容
本发明的第一个目的是针对现有光催化固氮催化剂活性低、成本高、 制备工艺复杂等不足,提出一种新型黑磷纳米片/硫化镉光催化剂的制备方 法。该催化剂具有典型的0D-2D结构,黑磷尺寸最大可以达到2μm,硫化 镉尺寸在50nm。
本发明黑磷纳米片/硫化镉光催化剂的制备方法,包括以下步骤:
步骤一、黑磷纳米片的制备
以二甲基亚砜为溶剂,以四丁基四氟硼酸铵为溶质所组成的溶液作为 电解液;以铂电极为阳极,以黑磷晶体为阴极,施加电压4.6-5.2V,进行 电化学剥离黑磷1-6小时;最后辅以超声5-10分钟从而使其均匀分散在溶 液中,通过离心即得所需的黑磷纳米片。
电解液中四丁基四氟硼酸铵的浓度为0.01mol/L。
根据本发明,制备全程需要保护气体保护,包括但不限于氮气,氩气 等单一或混合气体。
上述黑磷纳米片光,具有二维结构,尺寸最大可以达到2μm,厚度不 超过8nm。
步骤二、黑磷纳米片/硫化镉光催化剂的制备
在乙二醇溶液中,将步骤一电化学剥离得到黑磷纳米片与乙酸镉、硫 脲混合,在氮气气氛下于120-180℃反应12-18h,制备得到黑磷纳米片/ 硫化镉光催化剂。
黑磷纳米片/硫化镉光催化剂,为黑磷纳米片表面生长硫化镉纳米粒 子,其中黑磷纳米片的质量含量为0.5-2.5wt%。
本发明的另一个目的是涉及上述黑磷纳米片/硫化镉光催化剂在光催 化固氮上的应用。
将本发明的黑磷纳米片/硫化镉分散在含5vol%甲醇的水溶液中,可见 光照射下可将氮气和水转化成氨。
本发明的黑磷纳米片/硫化镉是一种稳定、制备快速、工艺简单以及光 催化固氮性能优异的光催化剂。在这种复合光催化剂助,硫化镉吸收光并 被激发形成光生电子空穴对,光生电子转移到黑磷纳米片上将N2还原为NH3。因此,在这种黑磷纳米片/硫化镉催化剂中,黑磷纳米片是助催化剂, 硫化镉是主催化剂,只有两者协同作用才能实现固氮反应,两者缺一不可。
附图说明
图1为使用本发明剥离后的黑磷纳米片的扫描电镜图。
图2(a)、(b)分别为使用本发明剥离后的黑磷纳米片扫描电镜图和原 子力显微镜图。
图3为0.5%BP/CdS光催化剂的透射电镜图。
图4(a)、(b)分别为不同黑磷含量的BP/CdS催化剂的光催化固氮性能 和6h平均光催化固氮性能。
具体实施方式
以下将通过具体实施例对本发明进行详细描述,但本领域技术人员了 解,下述实施例不是对本发明保护范围的限制,任何在本发明基础上做出 的改进和变化都在本发明的保护范围之内。
实施例1-1:
在80ml的二甲基亚砜溶液中加入0.2634g四丁基四氟硼酸铵,搅拌均 匀,在溶液中通氮气20min。将黑磷晶体夹在电极夹上作为阴极,以铂丝 电极为阳极,施加电压4.6-5.2V,在液面之上通氮气。剥离结束后,对溶 液超声30min。在2000rpm/min转速下离心去除未剥离的黑磷,所得溶液 以10000rpm/min转速离心得到黑磷纳米片。黑磷纳米片的尺寸最大在2μm 左右,如图1所示,厚度在6nm左右,如图2所示。
实施例1-2:
将实施例1-1制备得到的黑磷纳米片用乙醇清洗并干燥。取4mg黑磷 纳米片,1.194g醋酸镉和1.194g硫脲于100ml乙二醇中,使其分散均匀。 在150℃下加热16小时,并通以氮气保护。反应结束后以7000rpm/min的 转速离心3min,得到BP/CdS光催化剂,其中黑磷的质量分数含量为0.5%, 记为0.5%BP/CdS。所得硫化镉颗粒的大小在50nm左右,如图3所示。
实施例1-3至1-7如表1所示对实施例1-2中黑磷纳米片的加入量,醋酸镉 的加入量,硫脲的加入量做更改的基础上制备得到不同黑磷含量的BP/CdS 催化剂。
表1
实施例2-1:
以实施例1-2制备得到BP/CdS为光催化剂,在容量为500ml的玻璃 反应器中倒入12.5ml甲醇,237.5ml去离子水,60mg光催化剂,在溶液中 通氮气30min,从溶液中取样1ml。以300W的氙灯为光源,在可见照射 下(λ>420nm)测试光催化剂的固氮性能。每隔1h将体系中的溶液取出 (1ml),离心去除沉淀,通过纳氏试剂分光光度法测量溶液中的氮含量,如图4所示。测试6h,平均固氮速率为47.73μmol L-1h-1,如图4所示。
实施例2-2至2-6如表2所示对实施例2-1使用的光催化做更改的基础上, 即使用不同黑磷含量的BP/CdS催化剂为光催化剂,光催化固氮性能如表2 所示。
表2
催化剂 | 平均固氮速率(μmol L<sup>-1</sup>h<sup>-1</sup>) | |
实施例2-2 | 1.0%BP/CdS | 72.88 |
实施例2-3 | 1.5%BP/CdS | 123.26 |
实施例2-4 | 2.0%BP/CdS | 104.86 |
实施例2-5 | 2.5%BP/CdS | 66.49 |
实施例2-6 | CdS | 33.85 |
Claims (8)
1.黑磷纳米片/硫化镉光催化固氮催化剂在光催化固氮上的应用,其特征在于所述黑磷纳米片/硫化镉光催化固氮催化剂采用以下方法制备得到:
步骤一、黑磷纳米片的制备
以二甲基亚砜为溶剂,以四丁基四氟硼酸铵为溶质所组成的溶液作为电解液;以铂电极为阳极,以黑磷晶体为阴极,施加一定电压进行电化学剥离黑磷;最后辅以超声从而使其均匀分散在溶液中,通过离心即得所需的黑磷纳米片;
步骤二、黑磷纳米片/硫化镉光催化剂的制备
在乙二醇溶液中,将步骤一电化学剥离得到黑磷纳米片与乙酸镉、硫脲混合,在氮气气氛下于120-180 oC反应12-18 h,制备得到黑磷纳米片/硫化镉光催化剂;
上述黑磷纳米片/硫化镉光催化剂,为黑磷纳米片表面生长硫化镉纳米粒子,其中黑磷纳米片的质量含量为0.5-2.5wt%。
2.如权利要求1所述的应用,其特征在于步骤一电解液中四丁基四氟硼酸铵的浓度为0.01mol/L。
3.如权利要求1或2所述的应用,其特征在于步骤一黑磷纳米片的制备过程中保护气体包括氮气、氩气中一种或两种混合气体。
4.如权利要求1或2所述的应用,其特征在于步骤一黑磷纳米片光具有二维结构,尺寸小于等于2μm,厚度小于等于8nm。
5.如权利要求1或2所述的应用,其特征在于步骤一电剥离电压为4.6-5.2V。
6.如权利要求5所述的应用,其特征在于步骤一电剥离时间为1-6小时。
7.如权利要求1所述的应用,其特征在于步骤一超声时间为5-10分钟。
8.如权利要求1所述的应用,其特征在于黑磷纳米片/硫化镉在可见光光照下将氮气和水转化成氨。
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