High quality YbxY1-xAG (0≤x≤1) single crystals were grown by using the Czochralski method. The structural properties of YbxY1-xAG (0≤x≤1) single crystals were also investigated using the EXAFS method. Additionally, for the first time, EXAFS results were compared with XRD results. Moreover, without essential lattice structure transformation, YbxY1-xAG crystals can be found due to the varying of doping concentration in XRD measurements. However, EXAFS measurements indicated that the local fine structural variation around the Yb3+ ion depends on the Yb3+ concentration. This work also studies the two-photon luminescence spectra of a Yb3+ doped YAG crystals. To study the spectral performance of Yb:YAG crystal, intense green light (centered at about 544nm) was generated by the crystal upon excitation using a 973nm InGaAs LD pump source. The luminescence spectra were obtained for various Yb concentrations and the emission intensity were plotted versus Yb3+ concentration. The green emission light attributed to Yb3+ two-photon transition.