CN115029751B - 一种Pt/MoS2纳米片的电镀制备方法 - Google Patents

一种Pt/MoS2纳米片的电镀制备方法 Download PDF

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CN115029751B
CN115029751B CN202210486979.2A CN202210486979A CN115029751B CN 115029751 B CN115029751 B CN 115029751B CN 202210486979 A CN202210486979 A CN 202210486979A CN 115029751 B CN115029751 B CN 115029751B
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王江丽
汤文
张光振
段宇晨
谢宇
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Abstract

本发明提供一种Pt/MoS2纳米片的电镀制备方法。该制备方法的主要步骤包括：将四硫代钼酸铵和少量的氯铂酸溶解到DMF与水的混合溶液中，并以此溶液为电解质溶液。采用三电极体系：铂丝为对电极，Ag/AgCl电极为参比电极，ITO导电玻璃为工作电极，在恒压条件下（‑0.2V）电镀2分钟，便可以在ITO表面形成一层Pt/MoS2纳米薄片。本发明采用一步电镀法生成Pt/MoS2纳米片,在MoS2纳米片的表面负载痕量的Pt纳米颗粒，该方法具有条件温和,制备简单,重复性好,可操作性强等优点。且本发明制备的MoS2纳米片，比表面积较大，极大提高了Pt的电催化性能。

Description

一种Pt/MoS2纳米片的电镀制备方法
技术领域
本发明属于无机纳米材料领域,具体是一种Pt/MoS2纳米片的制备方法。
背景介绍
MoS2做为一种类似石墨烯的具有带隙结构的二维材料，具有1T、2H、3R三种晶体结构,其层内的原子以强的化合键键合,层间以弱的范德华力结合。MoS2因其独特的三明治状的层状结构和优异的物理化学性能，在光电、润滑、储氢、催化、锂离子电池、加氢脱硫方面有广泛的用途。此外，作为催化剂的载体材料，MoS2可以提高催化剂的比表面积进而提高其催化活性。贵金属铂被广泛用作小分子醇类物质的电催化剂，但因其价格昂贵，而具有一定的局限性。目前研究的热点主要集中在降低成本和提高催化活性两个方面，选择合适的催化剂载体材料便是有效的措施之一。常用的载体材料有碳材料、MoS2等。目前，Pt/MoS2的合成方法有水热法、微机械剥离法、锂离子插层法、热分解法及CVD法等，但一步电镀法合成Pt/MoS2纳米片却鲜有报道。现有技术的缺陷包括:微机械剥离法虽然工艺简单，但产量较低和重复性差。锂离子插层法制备过程复杂,成本高。水热法的影响因素较多，很难调控和重复操作。CVD法的工艺还不成熟。本发明的目的在于针对现有技术的不足，提供一种简便、快速、低成本的Pt/MoS2纳米片的制备方法。
发明内容
本发明的目的在于提供一种简便、快速、低成本的Pt/MoS2纳米片的制备方法。
本发明的技术方案：
一种Pt/MoS2纳米片的电镀制备方法，包括如下步骤：
（1）将DMF与水混合，得到DMF水溶液；
（2）将四硫代钼酸铵和氯铂酸溶解到DMF水溶液中，得到电解质溶液；
（3）在电解质溶液中，采用三电极体系电镀得到Pt/MoS2纳米片。
优选的，所述DMF与水的体积比为2:1.0-1.1。
优选的，所述四硫代钼酸铵与DMF的摩尔比为1:8-12。
优选的，所述氯铂酸与DMF的摩尔比为1:95-110。
优选的，三电极体系中铂丝为对电极，Ag/AgCl电极为参比电极，ITO导电玻璃为工作电极。
优选的，三电极体系电解中在恒压条件下电镀2分钟，在ITO表面形成一层Pt/MoS2纳米薄片。
优选的，所述恒压条件为-0.2V。
优选的，所述DMF与水的体积比为2:1，所述四硫代钼酸铵与DMF的摩尔比为1:10，所述氯铂酸与DMF的摩尔比为1:100。
本发明的有益效果：
本发明采用一步电镀法生成Pt/MoS2纳米片,在MoS2纳米片的表面负载痕量的Pt纳米颗粒，该方法具有条件温和，制备简单，重复性好，可操作性强等优点。且本发明制备的MoS2纳米片，比表面积较大，极大提高了Pt的电催化性能。
附图说明
图1为本发明实施例1的Pt/MoS2纳米片的XRD谱图；
图2(a)为本发明实施例1的Pt/MoS2纳米片的扫描电镜图；
图2(b)为本发明实施例1的Pt/MoS2纳米片的透射电镜图；
图2(c)为本发明实施例1的Pt/MoS2纳米片的高分辨透射电镜图；
图3(a)为商用Pt/C和本申请实施例1 Pt/MoS2纳米片在硫酸溶液中的循环伏安曲线图；
图3(b)为商用Pt/C和本申请实施例1 Pt/MoS2纳米片在乙醇溶液中的循环伏安曲线图。
具体实施方式
实施例1
如图1和图2（a）、图2（b）、图2（c）、图3（a）和图3（b）所示，一种Pt/MoS2纳米片的电镀制备方法，包括以下步骤：将0.2摩尔四硫代钼酸铵和0.02摩尔氯铂酸溶解到DMF与水（DMF 154.08mL，H2O 77.04mL）的混合溶液中，并以此溶液为电解质溶液。采用三电极体系：铂丝为对电极，Ag/AgCl电极为参比电极，ITO导电玻璃为工作电极，在恒压条件下（-0.2V）电镀2分钟，便可以在ITO表面形成一层Pt/MoS2纳米薄片。
实施例2
将0.2摩尔四硫代钼酸铵和0.02摩尔氯铂酸溶解到77.04mL水中，并以此溶液为电解质溶液。采用三电极体系：铂丝为对电极，Ag/AgCl电极为参比电极，ITO导电玻璃为工作电极，在恒压条件下（-0.2V）电镀2分钟，无法在ITO表面形成一层Pt/MoS2纳米薄片。
实施例3
将0.2摩尔四硫代钼酸铵和0.02摩尔氯铂酸溶解到154.08mL DMF中，并以此溶液为电解质溶液。采用三电极体系：铂丝为对电极，Ag/AgCl电极为参比电极，ITO导电玻璃为工作电极，在恒压条件下（-0.2V）电镀2分钟，无法在ITO表面形成一层Pt/MoS2纳米薄片。
实施例4
将0.2摩尔四硫代钼酸铵和0.02摩尔氯铂酸溶解到DMF与水（DMF 154.08mL，H2O77.04mL）的混合溶液中，并以此溶液为电解质溶液。采用三电极体系：铂丝为对电极，Ag/AgCl电极为参比电极，ITO导电玻璃为工作电极，在恒压条件下（-0.1V,-0.3V,0.1V,）电镀2分钟，均无法在ITO表面形成一层Pt/MoS2纳米薄片。
实施例5
将0.2摩尔四硫代钼酸铵和0.02摩尔氯铂酸溶解到DMF与水（DMF 154.08mL，H2O77.04mL）的混合溶液中，搅拌均匀，置于高压反应釜中，在200℃水热12h，可以在ITO表面形成一层Pt/MoS2纳米花，无纳米薄片生成。
实施例6
将0.2摩尔四硫代钼酸铵和0.02摩尔氯铂酸溶解到DMF与水（DMF 115.56mL，H2O115.56mL）的混合溶液中，并以此溶液为电解质溶液。采用三电极体系：铂丝为对电极，Ag/AgCl电极为参比电极，ITO导电玻璃为工作电极，在恒压条件下（-0.2V）电镀2分钟，无法在ITO表面形成一层Pt/MoS2纳米薄片。
从实施例2-6说明：改变反应条件，包括电解质的配比，电镀电压以及改变合成方法都无法获得性能良好的Pt/MoS2纳米薄片。
实施例7
将0.16摩尔四硫代钼酸铵和0.019摩尔氯铂酸溶解到DMF与水（DMF 154.08mL，H2O84.74mL）的混合溶液中，并以此溶液为电解质溶液。采用三电极体系：铂丝为对电极，Ag/AgCl电极为参比电极，ITO导电玻璃为工作电极，在恒压条件下（-0.2V）电镀2分钟，便可以在ITO表面形成一层Pt/MoS2纳米薄片。
实施例8
将0.24摩尔四硫代钼酸铵和0.022摩尔氯铂酸溶解到DMF与水（DMF 154.08mL，H2O77.04mL）的混合溶液中，并以此溶液为电解质溶液。采用三电极体系：铂丝为对电极，Ag/AgCl电极为参比电极，ITO导电玻璃为工作电极，在恒压条件下（-0.2V）电镀2分钟，便可以在ITO表面形成一层Pt/MoS2纳米薄片。
实施例9
将0.22摩尔四硫代钼酸铵和0.021摩尔氯铂酸溶解到DMF与水（DMF 154.08mL，H2O80.00mL）的混合溶液中，并以此溶液为电解质溶液。采用三电极体系：铂丝为对电极，Ag/AgCl电极为参比电极，ITO导电玻璃为工作电极，在恒压条件下（-0.2V）电镀2分钟，便可以在ITO表面形成一层Pt/MoS2纳米薄片。

Claims (2)

1.一种Pt/MoS2纳米片的电镀制备方法，其特征在于，包括如下步骤：
（1）将DMF与水混合，得到DMF水溶液；
（2）将四硫代钼酸铵和氯铂酸溶解到DMF水溶液中，得到电解质溶液；
（3）在电解质溶液中，采用三电极体系电镀得到Pt/MoS2纳米片；
所述DMF与水的体积比为2:1.0-1.1；
所述四硫代钼酸铵与DMF的摩尔比为1:8-12；
所述氯铂酸与DMF的摩尔比为1:95-110；
三电极体系中铂丝为对电极，Ag/AgCl电极为参比电极，ITO导电玻璃为工作电极；
三电极体系电镀中在恒压条件下电镀2分钟，在ITO表面形成一层Pt/MoS2纳米薄片；
所述恒压条件为-0.2V。
2.根据权利要求1所述的一种Pt/MoS2纳米片的电镀制备方法，其特征在于，所述DMF与水的体积比为2:1，所述四硫代钼酸铵与DMF的摩尔比为1:10，所述氯铂酸与DMF的摩尔比为1:100。
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CN112864404B (zh) * 2019-11-28 2023-06-02 大连大学 一种三维花状金镍铂修饰的纳米复合电极
CN114373942A (zh) * 2021-12-01 2022-04-19 天津大学 一种用于高效电催化的Pt半空心球的制备方法

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