Abstract: An apparatus and a method for preparing glow discharge sputtering samples for materials microscopic characterization are provided. The apparatus includes a glow discharge sputtering unit, a glow discharge power supply, a gas circuit automatic control unit, a spectrometer, and a computer. The structure of the glow discharge sputtering unit is optimized to be more suitable for sample preparation by simulation. By adding a magnetic field to the glow discharge plasma, uniform sample sputtering is realized within a large size range of the sample surface. The spectrometer monitors multi-element signal in a depth direction of the sample sputtering, so that precise preparation of different layer microstructures is realized. In conjunction with the acquisition of the sample position marks and the precise spatial coordinates (x, y, z) information, the correspondence between the surface space coordinates and the microstructure of the sample is conveniently realized.