Lambda 365 spectrometer

¹H NMR and ¹³C NMR spectra were recorded on a 400 MHz Bruker Biospin Avance III spectrometer or a 400 MHz JEOL JNM-ECZ400S spectrometer. The chemical shifts (δ) for ¹H NMR spectra, given in ppm, are referenced to the residual proton signal of the deuterated solvent. Crystallographic data was collected on a Mercury single crystal diffractometer at room temperature. The structures were solved with direct methods by using OlexSys or SHELXS-97 and refined with the full-matrix least-squares technique based on F2. The UV-vis spectra were measured on a PerkinElmer Lambda 365 spectrometer. All other reagents were obtained from commercial sources and were used without further purification, unless indicated otherwise.

UV–vis spectra were
recorded on a PerkinElmer Lambda 365 spectrometer. Fluorescence measurements
were recorded on an Edinburgh Instruments FLS980 spectrometer equipped
with a PMT 400 detector. Photoluminescence quantum yields were measured
in accordance with IUPAC methodology^{25 (link)} against
a coumarin 102 dye solution in ethanol (purity >99.8%) at an excitation
wavelength of 387 nm (OD at 387 nm for all samples ∼0.1). Integrated
emission intensities were corrected using a detector calibration curve.
Measuring the coumarin 102 quantum yield in an integrating sphere
in the same setup gave a value of 99%, but to calculate the quantum
yield, the literature value of 95% was considered for the quantum
yield of coumarin 102.^{26 (link)} Additionally,
a typical in situ HF + ZnCl₂ treated InP sample was measured
in an integrating sphere in the same instrument to have a PLQY of
84% (Figure S19), confirming the values
obtained in the dye measurements. PL decay traces were collected on
a Edinburgh Instruments Lifespec TCSPC setup with a 400 nm pulsed
laser. The emission was measured at 540 nm. TRPL traces were fitted
with a biexponential fitting curve, after which intensity-weighted
average lifetimes were calculated by the following equation: τ_ave = (A₁τ₁² + A₂τ₂²)/(A₁τ₁ + A₂τ₂), where A_n and τ_n are the nth amplitude and lifetime parameters
obtained from the biexponential fit.^{27 (link)}

¹H NMR spectra of samples were performed on a 400 MHz NMR instrument (AVANCE III HD 400 MHz, Swiss Bruker, Brooke, Switzerland) and tetramethylsilane was used as an internal standard in deuterated chloroform (CDCl₃). The ultraviolet-visible (UV-vis) spectra were recorded on a PerkinElmer Lambda 365 spectrometer (PerkinElmer, Waltham, MA, USA). The molecular weight and molecular weight distribution were conducted on an Agilent 1260 HPLC system (Agilent Technologies Inc., Santa Clara, CA, USA), tetrahydrofuran (THF) was used as eluent at 20 °C at a flow rate of 0.5 mL/min while using a refractive index (RI) detector and polystyrene calibration. The photo-liquefied photos were acquired by the microscope (XP-300C) (Shanghai Caikon Optical Instrument Co., Ltd. Shanghai, China). The ultraviolet light source is provided by Mightex (Mightex, Toronto, Ont., Canada).

¹H NMR and ¹³C NMR spectra were recorded on a 400 MHz Bruker Biospin avance III spectrometer. Deuterated reagents for characterization and in situ reactions were purchased from Sigma-Aldrich Chemical Co. and Cambridge Isotope Laboratories, Inc. (purity ≥99.9%). All other reagents were obtained from commercial sources and were used without further purification, unless indicated otherwise. The chemical shifts (δ) for ¹H NMR spectra, given in ppm, are referenced to the residual proton signal of the deuterated solvent. Mass spectra were recorded on a Bruker IMPACT-II or ThermoScientific LCQ Fleet spectrometer. Crystallographic data was collected on a Mercury single crystal diffractometer at room temperature. The structures were solved with direct methods by using OlexSys or SHELXS-97 and refined with the full-matrix least-squares technique based on F2 by using the OlexSys or SHELXL-97. The UV-Vis spectra were recorded on a Perkin-Elmer Lambda 365 spectrometer. TEM images were obtained on a Tecnai F20 Field Emission transmission electron microscope. SEM images were obtained on a SU-8010 Field Emission scanning electron microscope. The UV and visible light irradiation experiments were carried out on a CEL − HXF 300 xenon lamp with bandpass filters at 313 ± 10 nm (2.6 W) and 650 ± 10 nm (16.6 W), respectively.

The changes in crystallographic
behavior result from variations in substrate temperature affecting
the spatial lattice of TiO₂ deposited through both spraying
and sputtering techniques. These changes were explored using (XRD)
X-ray diffraction, employing a Bruker D8 Discover X-ray diffractometer
with a copper source (40 kV, 40 mA) and a 1D detector in Bragg–Brentano
geometry. For an investigation into surface morphologies, field emission
scanning electron microscopy (FESEM) was employed. Specifically, a
JEOL 7800F FEGSEM equipped with an Oxford Instrument X-MaxN energy
dispersion spectra (EDS) detector featuring a 50 mm² window
was utilized. The chemical composition of the thin films was analyzed
through X-ray photoelectron spectroscopy, employing the Kratos Axis
Supra instrument with a monochromatic Al K X-ray source operating
at 225 W (15 mA emission current). This analysis was conducted to
identify the presence of elements and their oxidation states. To determine
the thickness of the produced thin films, an Ambios XP2 surface profiler
was employed. The optical absorption characteristics of the photoactive
layers WO₃, BiVO₄, with passivation layers were
assessed using a PerkinElmer Lambda 365 spectrometer.

All of the EPR measurements were performed
at X-band using a Bruker EMXmicro-6/1/S/L spectrometer equipped with
a Bruker E4119001 super high sensitivity cavity. X-band EPR spectra
were obtained with a microwave power of 0.6456–0.6348 mW, frequency
at 9.41 GHz, conversion time of 66.68 ms, receiver gain of 30, and
modulation amplitude of 10.0 G at 100 kHz. UV–vis spectra were
recorded on a PerkinElmer Lambda 365 spectrometer. Fourier transform
infrared (FT-IR) spectra were recorded using a sealed solution cell
(0.1 mm, CaF₂ windows). Reactions of dinuclear DNIC–COOH/DNIC–COOMe with O₂ in the presence of DTBP were characterized using
Trace 1300 Gas Chromatograph in combination with a mass spectrometer
with a 5MS column. The confocal microscopic images were recorded using
ZEISS LSM 780 or Leica TCS–SP5-X AOBS confocal microscope systems.
The absorbance of the assay was recorded using a microplate reader
SpectraMax iD3, Molecular Devices, San Jose, CA.

FT-IR spectra were recorded on a PerkinElmer Spectrum Two ATR spectrometer. UV-vis spectra were recorded on a PerkinElmer Lambda 365 spectrometer. Scanning Electron Microscopy (SEM) was performed using a JEOL JSM-7000F instrument. To see the surface morphology, the cycled Si electrodes were washed with dimethyl carbonate before being imaged. For evaluating the mechanical properties of the electrodes with various polymer binders, the prepared electrodes were each cut into rectangular shapes (1.2 cm × 3.0 cm) and attached to 12-mm-wide 3 M tape. The peel strength of each tested electrode specimen was then recorded with a universal testing machine (UTM, Shimadzu EZ-L) by pulling the tape at a constant displacement rate of 30 mm min⁻¹.