Qms 403 c

TGA/DTA-MS-FTIR measurements were performed on an STA 449C Jupiter (TGA/DTA) and an Aeolos QMS 403 C (MS) from Netzsch, Germany, and a Bruker Tensor 27 (Billerica, MA, USA) with a gas chamber (FTIR). Lyophilized 3HFWC and fullerenol dried under vacuum (10 mbar/30 °C) were weighed in Al₂O₃ crucibles. During the measurements, the samples were heated from 30 to 900 °C with a constant heating rate of 10 K/min under a synthetic air atmosphere.

The phase purity and crystallinity were characterized by XRD (Bruker D8 Advance DaVinci, Karlsruhe, Germany), powders in Bragg-Brentano setup with a variable slit size, and films using grazing incidence setup with 2° incidence angle. All samples were measured with equal scan conditions, and no data manipulations other than vertical offset were applied. Rietveld refinements were carried out in Bruker AXS Topas version 5. Fundamental parameters peak shape was employed, with starting point in R3c reference unit cell parameters [30 (link)]. Background signal was refined for the most crystalline samples, and fixed to the same value for the remaining samples, where only unit cell parameters and crystallite size were refined. Powder samples were refined by the 2θ range 20°–75°, and films by 21°–49°.
Thermogravimetric analysis combined with mass spectroscopy (TGA-MS, Netzsch STA 449 C and Netzsch QMS 403 C, Selb, Germany) was conducted in synthetic air (20% ${\mathrm{O}}_2$ , 80% ${\mathrm{N}}_2$ ) and argon on dried sols, heating and cooling at 10 °C/min. Scanning electron images were captured on a field emission gun SEM (Zeiss Ultra 55, Limited Edition, Oberkochen, Germany). Fourier transform infrared spectroscopy (FTIR) was done in vacuum by the attenuated total reflectance (ATR) method (Bruker Vertex 80v) on the ground calcined powders.

The physical or chemical reaction occurring in the sample during heating can be analyzed using the mass- and heat-change data. Therefore, a combined thermogravimetric–differential scanning calorimetric (TG-DSC) system was used to test the static thermal decomposition process of the ternary reactive materials. The physical and chemical changes in the material during the impact process can be reasonably inferred from the fixed thermal decomposition laws. The test apparatus was a differential scanning calorimeter (NETZSCH-STA449F3, Shanghai, China) and a thermogravimetric analyzer (NETZSCH-QMS403C, Shanghai, China).
Since the ratio of the mixture of the formulations has a negligible effect on the thermal reaction properties of the materials [21 ], we performed only two sets of experiments with 1#PA and 4#PAB. The two composites were heated linearly at 10 °C/min from 25 °C to 930 °C. The experiments were carried out under a high-purity argon atmosphere to avoid the effect of oxygen in the air, with an argon purge rate of 60 mL/min.

A quadrupole mass spectrometer (NETZSCH QMS 403 C) with a leak inlet was applied to measure the gas evolution of the total water electrolysis process at a constant applied current of 200 mA. The electrolysis process was performed using a Solarton Instrument Model 1287 electrochemical interface. As shown in Supplementary Fig. 15, the mass spectrometer is connected to the new-type alkaline water electrolysis cell with two tubes as the purge/carrier gas inlet and outlet. A pure Ar gas stream was used as the purge gas before electrolysis and the carrier gas during the electrolysis process. The gas flows were typically 10 ml min⁻¹. Before the online gas analysis, the system was purged with a pure Ar stream for 1 h. The system was further purged with a pure Ar stream for another 1 h before Step 1 began. The duration time of Step 1 was 30 min. After the end of Step 1, a rest step of 130 min was performed with a pure Ar stream to eliminate remnant H₂ in the system. Then, Step 2 was started and continued until the cell voltage sharply increased. The experiment completed when all remaining O₂ in the electrolysis cell was removed.