1：Experimental Design and Method Selection:

A one-pot synthesis method involving simultaneous hydrolysis and reduction of (3-aminopropyl)triethoxysilane (APTES) with sodium ascorbate to form colloidal silicon nanoparticles, followed by slow evaporation and freezing to create a gel glass matrix.

2：Sample Selection and Data Sources:

APTES (99%) and sodium ascorbate were used as reagents; deionized water (Millipore,

3：2 MΩ cm?1) was the solvent. List of Experimental Equipment and Materials:

Magnetic stirrer, water bath, household refrigerator, Zeiss Sigma field emission scanning electron microscope, JEOL JEM 2200FS high-resolution transmission electron microscope, Bruker D8 advanced X-ray diffractometer, Omicron Multiprobe spectrometer for XPS, TGA/SDTA851e for thermogravimetric analysis, Netzsch DSC-200 PC for differential scanning calorimetry, CSM Instruments nanoindentation system, JASCO V-750 UV–vis spectrophotometer, Horiba Jobin Yvon Fluorolog-3 spectrofluorometer.

4：Experimental Procedures and Operational Workflow:

Mix APTES with water, add sodium ascorbate, stir to form colloidal Si NPs, heat at 50-60°C for slow evaporation, freeze at 4°C for 2-3 days to form gel glass. Characterize using SEM, TEM, XRD, XPS, TGA, DSC, nanoindentation, UV-vis, and PL spectroscopy.

5：Data Analysis Methods:

Use Oliver–Pharr model for nanoindentation data, Gaussian deconvolution for XPS spectra, standard methods for PL quantum yield calculation.