The invention discloses a Fe3 + selective microelectrode capable of being used for nondestructive micrometry, and a preparation method and application thereof, and relates to the field of microelectrodes. Comprises a glass microelectrode tube, The front part of the glass micro-electrode tube comprises a sharp end formed by hot drawing, the glass micro-electrode tube is filled with a filling solution, the sharp end is filled with a liquid ion exchanger, and the glass micro-electrode tube is also provided with an Ag/AgCl wire which extends into the filling solution from the rear end of the glass micro-electrode tube and is immersed in the filling solution, and the Ag/AgCl wire is sealed and fixed through epoxy resin. The method can realize real-time, dynamic and nondestructive detection of information such as Fe3 + concentration, flow velocity and movement direction of the microscopic area, and provides a new method for researching the microscopic process and mechanism of Fe3 + on the surfaces of biological and abiotic materials.
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