A300 spectrometer

The surface zeta potential data were obtained from a Zetasizer Nano ZS device (Malvern Instruments). X-ray diffraction (XRD) data were recorded using a Bruker Advanced D8 (Bruker Corp., Germany) instrument. Fourier transform infrared (FTIR) spectra were recorded by a Nicolet Nexus 470 instrument (Nicolet Instrument Corp., USA). X-ray photoelectron spectra (XPS) were analyzed by an ESCALAB 250 XPS instrument. Nitrogen (N₂) adsorption–desorption were determined by a Tristar 3000 analyzer. Transmission electron microscopy (TEM) images were taken using a JEM-2100F microscope (JEOL, Japan). UV-VIS-NIR absorption spectra were measured by a Cary 5000 spectrophotometer. Electrochemical impedance spectra (EIS) and photocurrent response curves were obtained through a CHI660C electrochemical workstation. Electron spin resonance (ESR) spectra were recorded by a Bruker model A300 spectrometer at room temperature. Phosphorescence spectra were tested on a Hitachi F-4600 spectrometer under an excitation wavelength of 808 nm.

The EPR spectra were obtained using a Bruker A300 spectrometer. EPR signal was obtained as soon as H₂O₂ (5 mM), FeSO₄ (2 mM, Sigma, >99%), DMPO (0.1 M, Dojindo, >99%) and PtsaN-C (5 µg/ml) or equal doses of PtnpN-C (5 µg/ml) were added to HAc/NaAc buffer (0.1 M, pH 4.5).

EPR spectra were obtained on a Bruker model A300 spectrometer (Berlin, Germany) at room temperature. The spectrometer parameters are shown as follows: sweep width, 100 G; center field, 3510.890 G; microwave bridge frequency, 9.839 GHz; power, 20.37 mW; modulation frequency, 100 kHz; modulation amplitude, 1 G; conversion time, 42.00 s; sweep time 42.00 s; receiver gain, 2.00 × 10⁴. The preparation of the liquid samples was similar to the photocatalyst reaction. The signal after irradiation was measured after 5 min of irradiation with a 50 W Xe lamp with stirring, and the mixture was transferred to 3 mm diameter glass tubes as soon as possible to record the signals. Furthermore, for solid samples, about 2 mg of target compound was put into a 3 mm diameter glass tube, and the signal after irradiation was also measured after 5 min of irradiation with a 50 W Xe lamp.

EPR spectra were recorded in PhCMe₃ on a Bruker A300 spectrometer (X band, 9.43 GHz, amplitude = 0.7 G) at room temperature. All analyses were carried out as follows: before acquiring the spectra, combinations of catalyst NC-800 with solvent, DMPO, and/or THQ were charged into the reaction vessel. The whole system was evacuated and then flushed with N₂ before warming up to 150°C for 2 hours. Then, the suspension cooled down to room temperature and tested for EPR.

The morphology of the prepared electrode was examined using a scanning electron microscope (SEM, Hitachi SU8000). XRD patterns of the electrode were recorded using a D8 advance X-ray diffractometer (Bruker) with Cu Kα radiation. XPS spectra were acquired on a Thermo ESCALAB250Xi spectrometer with a monochromated Al Kα X-ray source. ESR analysis was conducted using a Bruker A300 spectrometer. The pore size distribution was characterized using the mercury intrusion method (AutoPore IV 9500). The porosity of REMs was determined using Archimedes’ drainage method (Supplementary Table 3). All electrooxidation experiments were performed on a CHI660E electrochemical workstation (CH Instruments). All the electrochemical measurements were conducted on a Gamry Interface 1000 electrochemical workstation.

ENR concentrations were measured through a high-performance liquid chromatograph (HPLC, Agilent 1200, USA) with an Eclipse XDB-C18 column (5 μm particle, 150 × 4.5 mm), the concentrations were measured at λ = 278 nm using a mobile phase consisting of a mixture of acetonitrile and phosphoric acid (pH = 2.5) (v/v = 20 : 80) at a flow rate of 1.0 mL min⁻¹. The PMS concentrations were measured by the method of Waclawek et al.^{18 (link)} EPR analysis were performed on a Bruker A300 spectrometer (Germany) with DMPO as a spin-trapping agent. The parameters of EPR spectrometer were center field was 3360.67 G, sweep width was 100 G, static field was 3310.66 G, microwave frequency was 9.42 GHz, microwave power was 2.03 mW, modulation amplitude was 1.0 G and sweep time was 30.72 s.

The structures of as-synthesized materials were measured by X-ray diffraction (XRD, Cu Kα, λ = 1.54056 Å) with a Rigaku D/max-IIIA diffractometer at 293 K. The morphology and microstructure of the materials were characterized using a field-emission scanning electron microscope (FESEM, Quanta 200 FEG), and their detailed microstructure was further evaluated by transmission electron microscopy (TEM, Model JEM-2011, JEOL, Japan) with a Rontec EDX system. XPS spectra were obtained using a Thermo Fisher Scientific ESCALAB 250. All of the XPS spectra were calibrated with the C 1s peak at 284.8 eV as the binding energy reference. The electron paramagnetic resonance (EPR) spectra were obtained using a Bruker A300 spectrometer (microwave frequency = 9.74 GHz; modulation amplitude = 2 G; modulation frequency = 50 KHz; time constant = 10 ms; conversion time = 25 ms). The Fourier transform infrared spectroscopy (FTIR) spectra were collected using KBr as the reference sample on a Spectrum Two FTIR spectrophotometer (PerkinElmer, Waltham, USA). The TG spectra were measured using a Labsys evo TG-DTA/DSC (Setram, Lyon, France). The Raman spectra were obtained using a Raman spectrometer (Renishaw, London, UK). N₂ adsorption–desorption isotherms were performed on an A Micromeritics ASAP 2020 analyzer (Micromeritics, Georgia, USA) at liquid nitrogen temperature (77 K).