Single crystal fibers of 30% Er3+-doped compound of Y3(ScxGa1−x)5O12 have been grown by using the micro-pulling down (μ-PD) technique successfully. Our main purpose is to tune the fluorescence properties by adjusting the ratios of Sc3+ and Ga3+ ions inside the matrix crystals. The crystal structures of the series compounds were measured and analyzed through X-ray diffraction (XRD) measurements. The components and doping elements distributions were measured by the X-ray Fluorescence spectrometry and electron-probe microanalyzer. The absorption and mid-infrared fluorescence spectra, including the fluorescent lifetime of Er3+:4I13/2 and 4I11/2 levels were measured and compared systematically at room temperature. Spectral analysis indicated that the fluorescent lifetime of Er3+:4I13/2 tended to shorten and the emission spectra began to show a red shift when the proportion of YSG increased in the compound. Furthermore, the Raman spectra were measured to reveal the variations of lattice vibration and phonon energy.
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