The application discloses a
sample preparation and characterization method of a
crystal interface with a rotation angle, which is suitable for a sample with
dislocation at the interface of two crystals and comprises
sample preparation and relative rotation angle θ measurement of the two crystals; the
sample preparation is performed in a
cutting direction with a certain angle with the interface to prepare the sample, the thin slice is taken out, and three thin areas of the thin slice are obtained, namely, a top material A
crystal, a top material A / bottom material B
crystal mixed area and a bottom material B crystal; the rotation angle θ measurement is performed by parallelizing the
electron beam direction with the top
sample rotation axis, and the rotation angle θ is directly measured by analyzing crystallographic information of the three thin areas. The method can accurately measure the rotation angle of the top crystal relative to the bottom crystal by
TEM analysis of the three thin areas, and improves the
fault tolerance of TEM sample preparation and analysis experiments. In addition, the sample preparation technology can be used for monitoring changes in physical properties of the sample, such as
mechanics, heat,
optics and
electricity, with the size of the sample decreasing from microns to nanometers.