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4 protocols using tga 50 system

1

Thermogravimetric Analysis of Samples

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The thermogravimetric analysis (TG) was performed with a Shimadzu TGA-50 system under nitrogen atmosphere in an aluminum crucible. The analysis was performed with a heating rate of 10 °C min–1 and a nitrogen flow rate of 40 mL min–1 from room temperature to 600 °C.
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2

Comprehensive Thermal and Optical Characterization of Materials

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Thermogravimetric analysis (TGA) was performed using a Shimadzu TGA-50 system, in the temperature range from 25 to 800°C at a heating rate of 10°C min–1, under a static atmosphere of air. Polarized optical microscopy (POM) images were obtained with an Olympus BX41 microscope, using crossed polarizers. Scanning Electronic Microscopy (SEM) images were registered with a Hitachi SU-70 electron microscope. The samples were attached to aluminum stubs using double-sided carbon adhesive tape or carbon glue. Pictures were obtained from the surface and cross-section areas. All the samples were sputter-coated with carbon through an EMITECH K950X Turbo Evaporator, at a single pulse, on an outgassing time of 30 s and an evaporating time of 2 s. Transmission electron microscopy (TEM) images were obtained by a Philips CM200 microscope with an accelerating potential of 100 keV. TEM samples were prepared using a method described by Giasson et al. (1988) (link).
UV-Vis reflectance spectroscopy was carried out using a Perkin-Elmer Lambda 950 UV/Vis/NIR spectrophotometer and a Spectralon integrating sphere (Ø = 150 mm). The freestanding film surface was placed perpendicularly to the incident beam and the spectra were acquired as a function of the incident angle (15° < θ < 60°) with 5° steps, as illustrated in Supplementary Scheme 1.
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3

Characterization of Cobalt-based Catalyst

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All solvents and chemicals were purchased from commercial sources and used as received, unless otherwise stated. SEM images were captured using a JEOL JSM-7001F field-emission SEM (Yonsei Center for Research Facilities, Yonsei University). EDX spectra were acquired using a Hitachi SU 1510 SEM equipped with a Horiba EMAX Energy E-250 EDX system. PXRD patterns were obtained using a Rigaku Ultima IV equipped with a graphite monochromated Cu Kα radiation source (40 kV, 40 mA). The adsorption–desorption isotherms of N2 (77 K) were measured using a BELSORP Max volumetric adsorption instrument. All isotherms of samples were measured after soaking in methanol for 10 h and a pretreatment under a dynamic vacuum at 120 °C for 12 h. 1H NMR spectra were recorded on a Bruker Avance III HD 300 spectrometer (1H NMR, 300 MHz) with chemical shifts reported relative to residual deuterated solvent peaks. TGA curves were acquired using a Shimadzu TGA-50 system under a nitrogen atmosphere at a heating rate of 5 °C min−1. Inductively coupled plasma-mass spectrometer analysis was performed using a PerkinElmer NexION 350D instrument to quantify cobalt in the supernatant after catalytic reaction.
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4

Comprehensive Materials Characterization Protocol

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Elemental analysis for C, H, N and S was performed at the University of Aveiro with a Leco TruSpec 630-200-200 analyzer. PXRD patterns were recorded in transmission mode using a Philips Analytical Empyrean (θ/2θ) diffractometer equipped with a PIXcel1D detector, with automatic data acquisition (X'Pert Data Collector v4.2 software) and monochromatized Cu-Kα radiation (λ = 1.5406 Å). Each sample was mounted between two Mylar foils and then placed in the sample holder. The samples were step-scanned with 0.02º 2θ steps and a counting time of 50 s per step. Scanning electron microscopy (SEM) images were collected using a Hitachi SU-70 microscope operating at 15 kV. Samples were prepared by deposition on aluminium sample holders followed by carbon coating using an Emitech K 950 carbon evaporator. Thermogravimetric analysis (TGA) was performed using a Shimadzu TGA-50 system at a heating rate of 5 ºC min -1 under air. FT-IR spectra were obtained as KBr pellets using a FTIR Mattson-7000 spectrophotometer and recorded in transmission mode from 4000 to 300 cm -1 with a resolution of 4 cm -1 . Raman spectra were recorded on a Bruker RFS100/S FT instrument (Nd:YAG laser, 1064 nm excitation, InGaAs detector). Solid-state 13 C{ 1 H} cross-polarization (CP) magicangle spinning (MAS) NMR spectra were recorded at 100.62 MHz on a Bruker Avance 400 spectrometer using 3.5 µs 1 H 90º pulses, a 2 ms
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