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.
Tga 50 system
Manufactured by Shimadzu
The TGA-50 system is a thermogravimetric analyzer manufactured by Shimadzu. It is designed to measure the changes in the mass of a sample as a function of temperature or time, under a controlled atmosphere. The core function of the TGA-50 is to provide accurate and reliable thermal analysis data to researchers and scientists.
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Lab products found in correlation
Integrating sphere, by PerkinElmer (1 mentions)
Cm200 microscope, by Philips (1 mentions)
Su 70 electron microscope, by Hitachi (1 mentions)
K950x turbo evaporator, by Emitech (1 mentions)
Lambda 950 uv vis nir spectrophotometer, by PerkinElmer (1 mentions)
Bx41 microscope, by Olympus (1 mentions)
Su 1510 sem, by Horiba (1 mentions)
Emax energy e 250 edx system, by Horiba (1 mentions)
Nexion 350d, by PerkinElmer (1 mentions)
Jsm 7001f field, by JEOL (1 mentions)
Avance 3 hd 300 spectrometer, by Bruker (1 mentions)
Ultima 4, by Rigaku (1 mentions)
Su 70 microscope, by Hitachi (1 mentions)
K950 carbon evaporator, by Emitech (1 mentions)
Avance 400 spectrometer, by Bruker (1 mentions)
4 protocols using tga 50 system
1
Thermogravimetric Analysis of Samples
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 inSupplementary Scheme 1 .
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
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.
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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