1：Experimental Design and Method Selection:

The 3DGA/Sb2WO6 hybrid photocatalyst was prepared by electrostatic self-assembly (ESSA) method using 3-aminopropyltriethoxysilane (APTES) as the surface modifier of Sb2WO6. The photocatalytic activity was evaluated by monitoring the degradation of methyl orange (MO) under UV- and visible-light irradiation.

2：The photocatalytic activity was evaluated by monitoring the degradation of methyl orange (MO) under UV- and visible-light irradiation. Sample Selection and Data Sources:

2. Sample Selection and Data Sources: Methyl orange (MO) was used as the model pollutant. The samples were characterized by FESEM, TEM, XRD, Raman, and UV–vis diffuse reflectance spectra.

3：List of Experimental Equipment and Materials:

Antimony trichloride (SbCl3), sodium tungstate dihydrate (Na2WO4·2H2O), ethylene glycol, ethylenediamine tetraacetic acid disodium salt (EDTA-2Na), 1,4-benzoquinone (BQ), isopropanol (IPA), 3-aminopropyltriethoxysilane (APTES), and natural graphite flakes were used. Equipment included a ZEN3600 zeta potential analyzer, Supra55 field-emission scanning electron microscope (FESEM), JEM 2100 transmission electron microscope (TEM), Rigaku D/max 2500PC X-ray diffractometer, DXR dispersive Raman spectrometer, UV-2700 UV–vis spectrophotometer, Cary Eclipse fluorescence spectrophotometer, and UV-160 A spectrophotometer.

4：Experimental Procedures and Operational Workflow:

Sb2WO6 was synthesized by solvothermal method. The 3DGA/Sb2WO6 hybrid was prepared by ESSA method. Photocatalytic degradation experiments were carried out under UV- and visible-light irradiation.

5：Data Analysis Methods:

The degradation efficiency of MO was calculated based on the change in concentration monitored by UV–vis spectrophotometry.