以葡萄糖、六水合氯化镍和尿素为原料,通过水热反应一步制备前驱体Ni(OH)2/C,在高纯度氮气中煅烧获得NiO/Ni/C微球三元复合材料.采用扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、X射线光谱(EDS)和拉曼(Raman)等手段,分析NiO/Ni/C微球三元复合材料的形貌结构以及物相组成.结果表明:NiO/Ni/C微球为珊瑚花状结构,直径约1.7μm,Ni、NiO呈立方相.通过循环伏安法和计时电流法研究了NiO/Ni/C微球三元复合材料的电化学行为及葡萄糖传感性能.当Ni/NiO摩尔比为0.19时,形成的NiO/Ni/C三元复合微球具有优异的葡萄糖传感性能,其灵敏度为241.09μA·mmol/(L·cm2),线性响应范围为10μmol/L~5.05 mmol/L,最低检测限位10μmol/L.该传感器具有灵敏度高、抗干扰能力强以及稳定性好等特点.
Ternary NiO/Ni/C microspheres was obtained by calcination of the precursor Ni(OH)2/C in pure nitrogen. The precursor was preparedvia an one-pot hydrothermal synthesis technology using glucose, nickel chloride and urea. Scanning electron microscope (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray en-ergy dispersive (EDS), and Raman were used to characterize the morphology and structure of the sample. Results show that the NiO/Ni/C microspheres have a coral-like structure with diameter of about 1.7μm, and the crystalline phase of Ni and NiO are cubic. Electrochemical behavior and sensing property of ternary NiO/Ni/C microspheres composites were studiedvia cyclic voltammetry and amperometric method. When the Ni/NiO molar ratio is 0.19, the ternary NiO/Ni/C microspheres have excellent glucose sensor performance with a sensitivity of 241.09μA·mmol/(L·cm2) in a range of 10–5.05 mmol/L, and a detecting limit of 10μmol/L. Furthermore, the sensor has good stability and anti-interference ability.
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