核壳结构氧化镍/碳微球的制备及葡萄糖传感性能

doi:10.15541/jim20140391

摘要/Abstract

摘要：

以碳球为模板, 六水合氯化镍和尿素为原料, 通过水热反应制备前驱体Ni(OH)₂/C, 在高纯氮气中煅烧获得核壳结构的NiO/C微球。采用扫描电镜(SEM)、X射线衍射(XRD)、X射线光谱(EDX)和热重分析(TGA)等技术手段, 分析NiO/C微球的形貌结构以及物相组成, 结果表明: NiO/C微球直径约1.4 μm, 由厚度为50 nm的纳米片包覆碳球形成花状核壳结构, NiO呈立方相。通过循环伏安法和计时电流法研究了NiO/C微球的电化学行为及葡萄糖传感能力。与单纯NiO相比, NiO/C具有优异的葡萄糖传感性能, 其灵敏度为31.37 mA/(mmol·L^-1·cm²)线性响应范围为2~1279 μmol/L, 最低检测限为2 μmol/L。该传感器具有灵敏度高、抗干扰能力强和稳定性好等特点。

关键词: 核壳结构, NiO/C花状微球, 葡萄糖, 电化学传感

Abstract:

By using carbon spheres as a template, precursor Ni(OH)₂/C were prepared by a hydrothermal synthesis technology with the reaction of hexahydrate nickel chloride and urea. And then the precursor was calcinated in pure nitrogen to obtain core-shelled NiO/C microspheres. Scanning electron microscope (SEM), X-ray diffraction (XRD), X-ray energy dispersive (EDX), and the thermo gravimetric analyzer (TGA) were used to characterize morphology and structure of the samples. Results show that the NiO/C microspheres have core-shell structure with diameter around 1.4 μm, carbon sphere as the core, and cubic NiO nanoplates with thickness of 50 nm as the shell. Electrochemical behavior and sensing property of core-shelled NiO/C microspheres were studied via cyclic voltammetry and amperometric method. The results displayed that glucose sensitivity of the NiO/C is 31.37 mA/(mmol·L^-1·cm²) better than that of NiO, among the linear range of 2-1279 μmol/L with detecting limit at 2 μmol/L. Furthermore, the core-shelled NiO/C microspheres exhibit good stability and anti-interference ability.

Key words: core-shelled structure, NiO/C flower-like microsphere, glucose, electrochemical sensor

中图分类号:

O614
O657

崔振珍, 殷好勇, 赵红挺, 聂秋林. 核壳结构氧化镍/碳微球的制备及葡萄糖传感性能[J]. 无机材料学报, 2015, 30(3): 305-310.

CUI Zhen-Zhen, YIN Hao-Yong, ZHAO Hong-Ting, NIE Qiu-Lin. Preparation and Glucose Sensing Property of Core-shelled Nikel
Oxide/Carbon Microspheres[J]. Journal of Inorganic Materials, 2015, 30(3): 305-310.

图/表 9

图1 前驱体Ni(OH)2/C(a)和Ni(OH)2 (b)热重分析曲线

Fig. 1 TGA curves of Ni(OH)2/C (a) and Ni(OH)2 (b)

图2 碳球(a)和不同放大倍数下NiO/C(b, c)的扫描电镜照片

Fig. 2 SEM images of carbon spheres(a) and NiO/C samples at different magnifications (b, c)

图3 NiO/C的XRD图谱

Fig. 3 XRD pattern of NiO/C

图4 NiO/C(a), 氯化镍和尿素用量减少一半时制得NiO/C(b)的EDX图谱

Fig. 4 EDX patterns of NiO/C (a), NiO/C obtained with half amount of NiCl2· 6H2O and urea (b)

图5 GCE、NiO/GCE和NiO/C/GCE在铁氰化钾溶液中的循环伏安曲线

Fig. 5 CV curves of GCE, NiO/GCE and NiO/C/GCE in potassium ferricyanide

图6 GCE(a)、NiO/GCE(b)和NiO/C/GCE(c)在5 mmol/L葡萄糖溶液中的循环伏安曲线

Fig. 6 CV curves of electrodes GCE (a), NiO/GCE (b) and NiO/C/GCE (c) in 5 mmol/L glucose

图7 NiO/C (a)和NiO (b)葡萄糖传感器的i-t响应曲线

Fig. 7 The i-t curves of NiO/C(a) and NiO (b) glucose sensors

图8 NiO/C传感器的不同葡萄糖浓度与其响应电流的关系

Fig. 8 Linear calibration of NiO/C sensor between current response and glucose concentration

图9 NiO/C葡萄糖传感器的干扰测试

Fig. 9 Interference tests of NiO/C glucose sensor

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