1：Experimental Design and Method Selection:

The study employed a sol–gel method for synthesizing ZrO2–SiO2 nanoparticles and a photo-assisted deposition method for decorating them with copper at varying mass percentages (0.5, 1.0, 1.5, 2.0 wt%). The photocatalytic activity was evaluated by degrading thiophene under visible light irradiation.

2：5, 0, 5, 0 wt%). The photocatalytic activity was evaluated by degrading thiophene under visible light irradiation. Sample Selection and Data Sources:

2. Sample Selection and Data Sources: Samples included pure ZrO2–SiO2 and Cu-decorated ZrO2–SiO2 nanoparticles. Materials used were cupric acetate, zirconium nitrate, ethanol, nitric acid, tetraethylorthosilicate, and deionized water, all without further purification.

3：List of Experimental Equipment and Materials:

Equipment included a Nova 2000 set apparatus for BET surface area analysis, Bruker axis D8 apparatus for XRD, JEOL-JEM-1230 TEM for morphology, UV/Vis/NIR spectrophotometer for band gap measurement, Shimadzu RF-5301 fluorescence spectrophotometer for photoluminescence, Thermo Scientific K-ALPHA XPS for elemental state, Zahner Zennium electrochemical workstation for photocurrent, and a Pyrex cell with a 125 W mercury lamp and UV cut filter for photocatalytic experiments. GC-FPD (Agilent 7890) and GC–MS were used for product analysis.

4：Experimental Procedures and Operational Workflow:

Synthesis involved mixing TEOS with HNO3, C2H5OH, and H2O, adding zirconium nitrate, stirring, drying at 80°C, and calcining at 550°C. Copper decoration was done by exposing ZrO2–SiO2 and cupric acetate to UV light, drying at 100°C, and H2-reduction at 200°C. Characterization included BET, XRD, TEM, UV–Vis, PL, XPS, and photocurrent measurements. Photocatalytic tests involved dispersing nanoparticles in acetonitrile and thiophene, agitating in dark, irradiating with visible light, and analyzing degradation products.

5：Data Analysis Methods:

Band gap energies were calculated using Eg = 1239.8/λ, crystallite size from Scherer equation, and photocatalytic efficiency by measuring thiophene conversion over time using GC-FPD and GC–MS.