The invention relates to detection of calcium ions, in particular to preparation and application of an all-solid calcium ion selective electrode transduction layer electrode material. NiCo2S4 not only has the characteristics of semiconductors, but also has the properties of metals. Based on good conductivity and a controllable nanostructure, the NiCo2S4 is firstly applied to an ionic electron transduction layer of a potential type ion selective electrode, and the electrochemical performance of the ionic electron transduction layer is explored. According to the invention, NiCo2S4 with different nanostructures is prepared by adopting a one-step hydrothermal/solvothermal method through changing reaction solvents and is used as an ion/electron transduction layer to be modified on the surface of a glassy carbon electrode, and a sensitive film is attached on the surface of the glassy carbon electrode to construct a Ca2 + ion selective electrode (GC/NiCo2S4/Ca2 +/ISE) with NiCo2S4 as the transduction layer. According to the invention, NiCo2S4 has good conductivity and large specific capacitance, and can be used as a transduction layer to accelerate the conduction rate of ions and electrons and improve the stability of the electrode.
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