微波辅助法制备氢氧化镍-石墨烯纳米复合结构及在葡萄糖检测中的应用

doi:10.7503/cjcu20150593

高等学校化学学报 ›› 2016, Vol. 37 ›› Issue (3): 468.doi: 10.7503/cjcu20150593

微波辅助法制备氢氧化镍-石墨烯纳米复合结构及在葡萄糖检测中的应用

胡耀娟(), 黄梦丹, 陈昌云, 张长丽

南京晓庄学院环境科学学院, 南京 211171

收稿日期:2015-07-29 出版日期:2016-03-10 发布日期:2015-12-26
基金资助:
国家自然科学青年基金(批准号: 21401106)、江苏省自然科学青年基金(批准号: BK20140090)、江苏省新型动力电池重点实验室开放课题(批准号: Power-2013-1)、江苏省大学生实践创新训练计划项目(批准号: 201411460046X)和南京晓庄学院重点项目(批准号: 2015NXY02)资助

Microwave-assisted Fabrication of Nickel Hydroxide-Graphene Nanostructures and Their Application in Electrochemical Detection of Glucose^†

HU Yaojuan^*(), HUANG Mengdan, CHEN Changyun, ZHANG Changli

School of Environmental Science, Nanjing Xiaozhuang University, Nanjing 211171, China

Received:2015-07-29 Online:2016-03-10 Published:2015-12-26
Contact: HU Yaojuan E-mail:huyaojuan@njxzc.edu.cn
Supported by:
† Supported by the National Natural Science Foundation of China(No.21401106), the Natural Science Foundation of Jiangsu Province, China(No.BK20140090), the Open Project of Jiangsu Key Laboratory of New Power Batteries, China(No.Power-2013-1), the Jiangsu Provincial Undergraduate Innovation Training Programs, China(No.201411460046X) and the Key Research Project of Nanjing Xiaozhuang University, China(No.2015NXY02)

摘要/Abstract

摘要：

采用微波辅助合成法制备了氢氧化镍-石墨烯[Ni(OH)₂-graphene]纳米复合结构, 利用扫描电子显微镜(SEM)、 X射线光电子能谱(XPS)、电子能谱(EDS)、 X射线衍射(XRD)及电化学阻抗谱(EIS)对其结构和性质进行了表征. 电化学实验结果表明, 与单独的Ni(OH)₂相比, Ni(OH)₂-graphene纳米复合结构对葡萄糖氧化反应表现出更高的电催化活性; 同时, 据此构建的无酶葡萄糖传感器具有良好的性能, 检测线性范围为10 μmol/L~7.5 mmol/L, 灵敏度为174.7 μA·cm^-2·mmol·L^-1, 检出限为2.0 μmol/L(S/N=3), 且该传感器具有良好的稳定性和选择性, 可用于实际样品检测.

关键词: 氢氧化镍-石墨烯复合结构, 微波辅助法, 无酶葡萄糖传感器

Abstract:

The nickel hydroxide-graphene[Ni(OH)₂-graphene] nanostructures were fabricated by facile microwave method, and the structure and electrocatalytic activities of the synthesized nanostructures were characterized via scanning electron microscopy(SEM), X-ray photoelectron spectroscopy(XPS), X-ray powder diffraction(XRD), energy-dispersive spectroscopy(EDS), electrochemical impedance spectroscopy(EIS) and cyclic voltammetry. The results indicated that the Ni(OH)₂-graphene nanotructures exhibited a higher electrocatalytic activity than the Ni(OH)₂ nanoparticles. A glucose nonenzyme sensor was developed based on the Ni(OH)₂-graphene nanotructures. The sensor exhibited a low detection limit of 2 μmol/L, a wide linear range from 0.01 to 7.5 mmol/L, and a high sensitivity of 174.7 μA·cm^-2·mmol·L^-1. In addition, the sensor exhibited excellent stability and selectivity for the glucose detection, and it could be used to analyze real samples.

Key words: Nickel hydroxide-graphene nanostructure, Microware-assisted method, Nonenzyme glucose sensor

中图分类号:

O657

TrendMD:

胡耀娟, 黄梦丹, 陈昌云, 张长丽. 微波辅助法制备氢氧化镍-石墨烯纳米复合结构及在葡萄糖检测中的应用. 高等学校化学学报, 2016, 37(3): 468.

HU Yaojuan, HUANG Mengdan, CHEN Changyun, ZHANG Changli. Microwave-assisted Fabrication of Nickel Hydroxide-Graphene Nanostructures and Their Application in Electrochemical Detection of Glucose^†. Chem. J. Chinese Universities, 2016, 37(3): 468.

图/表 10

Fig.1 SEM images of Ni(OH)2(A, B) and Ni(OH)2-graphene nanostructures(C, D)

Fig.2 Typical XRD patterns of Ni(OH)2(a) and Ni(OH)2-graphene nanostructures(b)

Fig.3 EIS of Ni(OH)2/GCE(a) and Ni(OH)2-graphene/GCE(b) in 0.1 mol/L KCl electrolyte solution containing 5.0 mmol/L K3Fe(CN)6/K4Fe(CN)6

Fig.4 CVs of the bare GCE(a), Ni(OH)2/GCE(b) and Ni(OH)2-graphene/GCE(c) in 0.1 mol/L NaOH solution at scan rate of 50 mV/s(A) and CVs of Ni(OH)2-graphene/GCE in 0.1 mol/L NaOH solution at different scan rates(B)(B) Scan rate/(mV·s-1), a—h: 25, 50, 75, 100, 125, 150, 175, 200. Inset of (B) is plot of the peak current vs. the square root of scan rate.

Fig.5 CVs of Ni(OH)2/GCE(A) and Ni(OH)2-graphene/GCE(B) in 0.1 mol/L NaOH without(a) and with(b) 10 mmol/L glucose The scan rate is 50 mV/s.

Fig.6 Dependence of the response of electrocatalytic oxidation of 1 mmol/L glucose at Ni(OH)2-graphene/GCE on the detection potential

Fig.7 Amperometric response of Ni(OH)2-graphene/GCE to successive addition of glucose in NaOH at the applied potential of 0.50 V(A) and calibration curve for glucose obtained at the electrode(B)

Table 1 Analytical parameters obtained at different glucose sensors

Electrode material	Sensitivity/ (μA·cm^-2·mmol·L^-1)	Detect limit/ (μmol·L^-1)	Linear range/(mmol·L^-1)	Reference
Ni(OH)₂-graphene	174.70	2.0	0.01—7.5	This work
Ni(OH)₂	29.93	10	0.5—7.0	This work
RGO-Ni(OH)₂	11.43	0.6	0.002—3.1	[20]
CuO/TiO₂	79.79	1.0	To 2.0	[23]
Cu/graphene		0.5	To 4.5	[24]
Cu@Cu₂O/rGO	145.20	0.5	0.005—7.0	[25]
NiO-Pt NFs	180.80	0.313	To 3.67	[26]
CuFe₂O₄-MWCNTs		0.2	0.0005—1.4	[17]

Fig.8 Amperometric responses of the Ni(OH)2-graphene/GCE to 1 mmol/L glucose, 0.1 mmol/L AA and 0.1 mmol/L DA at an applied potential of 0.50 V

Table 2 Determination of glucose concentration in the blood sample by Ni(OH)2-graphene/GCE(n=5)

Sample	Ni(OH)₂-graphene/GCE		Blood glucose monitor
Sample	Test result/(mmol·L^-1)	RSD(%)	Test result/(mmol·L^-1)	RSD(%)
1	3.36	2.16	3.32	2.32
2	4.25	2.52	4.22	2.15
3	5.32	3.27	5.35	2.28
4	5.67	3.53	5.70	2.04
5	6.89	3.25	6.84	2.57

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微波辅助法制备氢氧化镍-石墨烯纳米复合结构及在葡萄糖检测中的应用

Microwave-assisted Fabrication of Nickel Hydroxide-Graphene Nanostructures and Their Application in Electrochemical Detection of Glucose^†

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微波辅助法制备氢氧化镍-石墨烯纳米复合结构及在葡萄糖检测中的应用

Microwave-assisted Fabrication of Nickel Hydroxide-Graphene Nanostructures and Their Application in Electrochemical Detection of Glucose†

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Microwave-assisted Fabrication of Nickel Hydroxide-Graphene Nanostructures and Their Application in Electrochemical Detection of Glucose^†