The invention discloses a preparation method of a TEM sample of a nickel metal silicide. The method includes steps of: 1) providing a chip, wherein the nickel metal silicide is formed in selected zones in a device layer and a semiconductor substrate interface of the chip; 2) forming a metal protective layer so as to completely cover a target zone that requires TEM analysis; 3) cutting the TEM sample used for TEM analysis by means of ion beam; 4) turning the chip to a certain degree, and performing ion bombarding to the semiconductor substrate layer of the chip by means of the ion beam to completely amorphize the semiconductor substrate layer. The method can improve the TEM contract imaging difference between the semiconductor substrate layer and the TEM sample, and can form the TEM samplewhich allows clear imaging of the nickel metal silicide in a TEM mode, thereby reducing TEM observation time and reducing observation cost of the sample.