In this study, Yb:YAG-nanocrystal-doped silica glass with high transmission and excellent spectral properties was successfully prepared using a modified sol–gel method. The X-ray diffraction (XRD), micro-Raman spectroscopy, electron paramagnetic resonance (EPR), transmission electron microscopy (TEM), and high-resolution TEM (HR-TEM) analyses confirmed that the Yb:YAG nanocrystals, with their low content, homogeneous distribution, and small crystal size, directly crystallized into the silica glass network without annealing treatment. In contrast with conventional microcrystalline glass having large particles (>0.1 μm) and a large particle content, nanocrystalline glass with a homogeneous distribution and sizes of ~22 nm had higher optical transmittance and better spectral properties. Compared with Yb³⁺ doped silica glass without nanocrystals, the Yb:YAG-nanocrystal-doped silica glass had a 28% increase in absorption cross-section at 975 nm and a 172% enhanced emission cross-section at 1030 nm without any changes in the spectral pattern of the Yb³⁺ ions in the silica glass. Meanwhile, the Yb:YAG-doped silica glass with large size and high optical quality was easily prepared. Therefore, the Yb:YAG-nanocrystal-doped silica glass is expected to be a promising near-infrared laser material.

A high phosphorus Er³⁺/Yb³⁺ co-doped silica (EYPS) fiber core glass was prepared using the sol-gel method combined with high-temperature sintering. The absorption spectra, emission spectra, and fluorescence decay curves were measured and compared in temperatures ranging from 300 to 480 K. Compared to 915 and 97x nm, the absorption cross-section at ~940 nm (~0.173 pm²) demonstrates a weaker temperature dependence. Hence, the 940 nm pump mechanism is favorable for achieving a high-power laser output at 1.5 μm. Additionally, the double-exponential fluorescence decay of Yb³⁺ ions and the emission intensity ratio of I_1018nm/I_1534nm were measured to evaluate the energy transfer efficiency from Yb³⁺ ions to Er³⁺ ions. Through the external heating and active quantum defect heating methods, the emission intensity ratios of I_1018nm/I_1534nm increase by 30.6% and 709.1%, respectively, from ~300 to ~480 K. The results indicate that the temperature rises significantly reduce the efficiency of the energy transfer from the Yb³⁺ to the Er³⁺ ions.