石墨烯负载纳米银的制备及其对H2O2的电化学检测

doi:10.16085/j.issn.1000-6613.2018-2464

化工进展 ›› 2019, Vol. 38 ›› Issue (9): 4191-4196.DOI: 10.16085/j.issn.1000-6613.2018-2464

石墨烯负载纳米银的制备及其对H₂O₂的电化学检测

马园园¹(),寇伟¹,丁国生¹,徐联宾^1,²()

1. 北京化工大学教育部超重力工程研究中心，北京 100029
2. 北京化工大学有机无机复合材料国家重点实验室，北京 100029

收稿日期:2018-12-25 出版日期:2019-09-05 发布日期:2019-09-05
通讯作者: 徐联宾
作者简介:马园园（1992—），女，硕士研究生，研究方向为电催化。E-mail：myy199211@163.com。
基金资助:
国家自然科学基金(21676018)

Preparation of graphene-supported nano-silver and its electrochemical detection of H₂O₂

Yuanyuan MA¹(),Wei KOU¹,Guosheng DING¹,Lianbin XU^1,²()

1. Research Center of the Ministry of Education for High Gravity Engineering and Technology, Beijing University of Chemical Technology, Beijing 100029, China
2. State Key Laboratory of Organic-Inorganic Composites, Beijing University of Chemical Technology, Beijing 100029, China

Received:2018-12-25 Online:2019-09-05 Published:2019-09-05
Contact: Lianbin XU

摘要/Abstract

摘要：

采用改进的Hummers法制备了氧化石墨烯（GO），然后以水合肼作为还原剂，并控制反应的pH=10来制备还原氧化石墨烯（RGO）。采用化学还原法，以石墨烯为载体，以乙酰丙酮银为前体，以硼氢化锂四氢呋喃溶液为还原剂将银离子还原，制备了石墨烯负载纳米银复合材料。通过X 射线粉末衍射（XRD）、傅里叶变换红外光谱（FTIR）和透射电子显微镜（TEM）等表征方法证明了石墨烯上负载的银纳米颗粒结晶良好、尺寸均一、分布均匀，其中银纳米颗粒直径约为8nm。通过循环伏安和计时电流技术对石墨烯负载纳米银复合材料进行电化学测试，结果表明，石墨烯负载纳米银复合材料对过氧化氢的还原具有良好的电催化活性。以此复合纳米结构构建的过氧化氢传感器测试过氧化氢浓度的线性范围为0.1～62.3mmol/L（R=0.990），检出限为0.017mmol/L（S/N=3），响应时间小于2s。

关键词: 石墨烯, 纳米粒子, 电化学检测, 催化剂, 过氧化氢

Abstract:

Graphene oxide (GO) was prepared by the modified Hummers method. The reduced oxidized graphene (RGO) was prepared by using hydrazine hydrate as a reducing agent and controlling the pH of the reaction to 10. The graphene-loaded nano-silver composites were prepared by hydrothermal synthesis using graphene as the support, silver acetylacetonate as the precursor and lithium borohydride tetrahydrofuran as the reducing agent. X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and other characterization methods demonstrated that the silver nanoparticles supported on graphene had good crystallinity, uniform size and even distribution. The average diameter of the silver nanoparticles was about 8nm. Electrochemical tests of the graphene-loaded nano-silver composites by cyclic voltammetry and chronoamperometry showed that the graphene-loaded nano-silver composites had good electrocatalytic activity for the reduction of hydrogen peroxide. The linear range of hydrogen peroxide concentration measured by the hydrogen peroxide sensor constructed from the composite nanostructure was 0.1—62.3mmol/L (R=0.990) with the detection limit of 0.017mmol/L (S/N=3) and the response time of less than 2s.

Key words: graphene, nanoparticles, electrochemical detection, catalyst, hydrogen peroxide

中图分类号:

TQ035

马园园,寇伟,丁国生,徐联宾. 石墨烯负载纳米银的制备及其对H₂O₂的电化学检测[J]. 化工进展, 2019, 38(9): 4191-4196.

Yuanyuan MA,Wei KOU,Guosheng DING,Lianbin XU. Preparation of graphene-supported nano-silver and its electrochemical detection of H₂O₂[J]. Chemical Industry and Engineering Progress, 2019, 38(9): 4191-4196.

图/表 8

图1 氧化石墨烯、还原氧化石墨烯红外光谱图

图 2 GO和RGO的XPS全谱图及C 1s分峰图

图3 GO、RGO和Ag/RGO复合材料的XRD图

图4 GO、RGO和Ag/RGO的TEM图及Ag粒径分布图

图5 不同电极在PBS溶液中(pH=6.5)检测H2O2的循环伏安图

图6 Ag/RGO在PBS溶液中（pH=6.5）检测不同浓度H2O2的循环伏安图

图7 Ag/RGO在PBS溶液中（pH=6.5）不同扫描速率下的循环伏安图

图8 Ag/RGO电催化还原过氧化氢的计时电流曲线

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石墨烯负载纳米银的制备及其对H₂O₂的电化学检测

Preparation of graphene-supported nano-silver and its electrochemical detection of H₂O₂

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