A new mixed laser crystal, Yb0.005Y0.848Lu0.147VO4, has been successfully grown using the Czochralski method. An ICP‐OES was used to measure the concentrations of elements (Yb, Y, Lu, V) in the crystal, and the chemical formula was determined. X‐ray powder diffraction analysis shows that the crystal has ZrSiO4 structure. A pair of edge dislocations with certain orientation was observed by the HREM, and the orientation was confirmed by the calibration of the diffraction spots. The formation mechanism of this type dislocation was given by analysis on structure and thermal expansion of crystal. The suggestion to avoid these dislocations was also given.