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Polymers 2021, 13, 4197 were obtained using a 20-eV pass energy (resolution approximately 0.4 eV). eter was calibrated using the C1s peak of graphite. Peak fitting was perfo Origin 9 pro software (OriginLab Corp., Northampton, MA, USA), using (Voigt) line shapes and Shirley backgrounds. 4 of 13 CO2 adsorption isotherms were measured at 20 °C by using a TriStar I cromeritics Instrument Corporation, Norcross, GA, USA) after outgassing were obtained using a 20-eV pass energy (resolution approximately 0.4 eV). The spectrome- 150 °C under vacuum. Thermogravimetric analysis (TGA) performed on a ter was calibrated using the C1s peak of graphite. Peak fitting was performed by using 209 F1 Libra was used to assess the selectivity for CO2 adsorption by the el Origin 9 pro software (OriginLab Corp., Northampton, MA, USA), using mixed Gaussian (Voigt) line shapes and Shirley backgrounds. in a simulated post-combustion flue gas mixture (20/80 v/v, CO2/N2) [38]. CO2 adsorption isotherms were measured at 20 ◦C by using a TriStar II analyzer sorption step (8 mL min−1 of CO2 in a total flow of 40 mL min−1) was carri (Micromeritics Instrument Corporation, Norcross, GA, USA) after outgassing the samples and ambient laboratory pressure (~1 bar). The samples were activated b at 150 ◦C under vacuum. Thermogravimetric analysis (TGA) performed on a NETZSCH TG209F1LibrawasusedtoassesstheselectivityforCO adsorptionbytheelectrospun under vacuum at 120 °C for 30 min in order to2 remove previously adsorbed mats in a simulated post-combustion flue gas mixture (20/80 v/v, CO2/N2) [38]. The CO2/N2 adsorption step (8 mL min−1 of CO2 in a total flow of 40 mL min−1) was carried 3. Resu◦lts and Discussion out at 30 C and ambient laboratory pressure (~1 bar). The samples were activated before each test under vacuum at 120 ◦C for 30 min in order to remove previously adsorbed gases 3.1. Stabilization and Carbonization or water. Carbon fibers are well known as suitable materials to reinforce com 3. Results and Discussion this end, commercial nanofibers are very often produced by thermal trea 3.1. Stabilization and Carbonization PAN is a robust, high melting polymer that, when used as a precursor, giv Carbon fibers are well known as suitable materials to reinforce composites, and to this ewndit,hcomamheirgchiael nrapnoefirbfoerrsmaraenvecrey,osfternenprgotdhucaedndbysthtiefrfmnaelstsreactommenpt oafrPeAdNt.oPApNiticsh, ray a robust, high melting polymer that, when used as a precursor, gives carbon fibers with deed, the electrospun fibers showed exceptional mechanical stability tha a higher performance, strength and stiffness compared to pitch, rayon etc. [32]. Indeed, handling. The morphological characteristics of the mats were evaluated b the electrospun fibers showed exceptional mechanical stability that allowed easy handling. 2). The morphological characteristics of the mats were evaluated by SEM (Figure 2). Figure 2. SEM images of (i,ii) as-spun carbon nanofibers at different magnifications; (iii) carbonized Figure 2. SEM images of (i,ii) as-spun carbon nanofibers at different magnifications fibers with analysis of diameter; (iv) cross section of the mat. fibers with analysis of diameter; (iv) cross section of the mat. The samples appeared as a non-woven mat of fibers with an estimated average diameter of about 320 nm. After the spinning, the second step was the stabilization of the The samples appeared as a non-woven mat of fibers with an estimat fibers. The resulting chain structure guarantees an improved stability during carbonization ameter of about 320 nm. After the spinning, the second step was the stab and the final CNFs were more flexible. The carbonization process took place as soon as fibers. The resulting chain structure guarantees an improved stability dur the stabilization ended to avoid moisture absorption. The set temperature was 900 C and the carbonization took about 2 h to be completed. The morphology of the fibers (see tion and the final CNFs were more flexible. The carbonization process too Figure 2iii) was not affected after stabilization and carbonization, and the diameter was not as the stabilization ended to avoid moisture absorption. The set temperat significantly altered since an average value of 341 (47) nm was determined. The average diameter was reduced to 173 (14) nm after the carbonization step which is 45% of the and the carbonization took about 2 h to be completed. The morphology of pre-carbonization value. Weight loss of about 50% was also observed after carbonization. Figure 2iii) was not affected after stabilization and carbonization, and th not significantly altered since an average value of 341 (47) nm was determ age diameter was reduced to 173 (14) nm after the carbonization step whic pre-carbonization value. Weight loss of about 50% was also observed after ◦ r m I e T e e g p t e o t ; i k u e iPDF Image | Effect of Thermal Stabilization on PAN-Derived Electrospun Carbon Nanofibers
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