Mira3 feg seminstrument

SEM images were taken with a Tescan MIRA3 FEG-SEM
instrument at an acceleration voltage of 5.0 kV. The electrodes were
not rinsed with solvent but mounted onto the SEM stage of the airtight
transfer module (Kammrath & Weiss, type CT0) and transferred into
the SEM chamber under an inert Ar atmosphere from the glovebox.

Solid-state UV–vis
spectra for the photocatalysts were recorded using a Varian Cary 50
UV–vis spectrophotometer equipped with a diffuse reflectance
accessory. FT-IR spectra of the samples were collected using a Thermo
Scientific Nicolet iS50 FTIR spectrometer (ATR mode). The PXRD measurements
were conducted using a PANalytical Empyrean Series 2 instrument using
Cu Kα irradiation. Transmission electron microscopy (TEM) images
were acquired using a Thermo Scientific (FEI) Talos F200X G2 TEM.
For the TEM measurements, the samples were dispersed in ethanol (∼4
μg mL^–1) and drop-casted on carbon-coated
Cu grids. The FESEM images were acquired using a TESCAN MIRA3 FEG-SEM
instrument. The ICP-OES measurements were performed by a Microanalysis
Service (Yusuf Hamied Department of Chemistry, University of Cambridge)
using a Thermo Scientific iCAP 700 spectrometer. XPS measurements
of the photocatalysts were performed at the Maxwell Centre, University
of Cambridge with a near ambient pressure (NAP) XPS system with a
SPECS XR 50 MF X-ray source, μ-FOCUS 600 X-ray monochromator
and a differentially pumped PHOIBOS 150 1D-DLD NAP analyzer. ¹H NMR spectra were recorded on a 400 MHz Bruker DPX spectrometer
and referenced against the residual solvent signal (H₂O:
δ = 4.79 ppm).

After electrochemical plating for 3 hours with a current density of 1 mA cm⁻², the coin cells were transferred into an Ar Glovebox and disassembled. The Li-metal electrode was mounted onto the SEM stage of the transfer module (Kammrath & Weiss, type CT0) and dried under vacuum for 1 hour. The electrodes were not rinsed with a solvent before the to avoid removal of loosely attached lithium microstuctures. The samples were transferred into the SEM chamber using the air-sensitive transfer module under an inert atmosphere (Ar), without being exposed to air. SEM images were acquired with a Tescan MIRA3 FEG-SEM instrument at an acceleration voltage of 5.0 kV.