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Polymers 2021, 13, 4197 10 of 13 Table 2. Adsorption performances at different conditions, preparation steps, and nitrogen content of literature samples compared to this work. Preparation REF. • Electrospinning • Stabilization • Carbonization • Electrospinning • Stabilization • Carbonization • Addition of pore forming agent (PVP d) • Cross-linking by HH e • Electrospinning • Stabilization • Carbonization • Addition of pore forming agent (PVP d) • Electrospinning • Carbonization • Electrospinning • Stabilization • Carbonization • CO2 activation • Electrospinning • Stabilization • Carbonization • KOH activation • Urea doping • Electrospinning • Carbonization • CO2 activation • Melamine doping • Electrospinning • Stabilization • CO2 activation Samples REF. CNF_230 this work CNF_260 this work PCF-H5 [32] PCNF-2-1000 [45] AFH2 [46] PAN-PK [30] N-AnF(1:5) [43] MACNF-7 [47] MACNF-10 [47] N Content % 7.1 a 6.6 a 16.48 b 9.08 a 9.0 a 8.13 b m.i. c m.i. c CO2 Capacity mmol·g−1 0.53 (CO2 :N2 = 20:80) 2.75 (100% CO2 ) (CO2 :N2 = 20:80) 4.16 (100% CO2) 0.73 (CO2:N2 = 10:90) 2.29 (100% CO2 ) 3.11 (100% CO2) 3.17 (100% CO2 ) 4.4 (100% CO2 ) 2.98 (100% CO2 ) 1.22 (CO2 :N2 = 15:85) 3.15 (100% CO2 ) T b◦C P cbar T d◦C ads ads act 35 20 35 20 25 25 25 25 25 m.i. c 25 0 1 1 1 1 1 1 1 1 1 m.i. c 1 1 150 150 110 200 105 350 150 m.i. c 120 m.i. c a determined by XPS (at.%); b determined by elemental analysis (wt.%); c m.i. denotes missing information; d PVP: polyvinylpyrrolidone; e HH: hydrazine hydrate. According to the mechanism reported in Figure 3, during the cyclization process, the nitrile residues condensate into aromatic structures rich in pyridine moieties that can be rearranged in NQ groups as confirmed by our FT-IR results. Therefore, a more suitable precursor for the production of carbon rich in nitrogen basic sites was obtained, that interacted more efficiently with CO2 [42,48]. 4. Conclusions Among various sorbent materials, electrospun CNFs can be an excellent solution for carbon dioxide adsorption due to the easy, fast, and low-cost fabrication method. In this work, robust PAN nanofibers mats were produced at two different stabilization temper- atures, namely 230 ◦C and 260 ◦C, while the carbonization step was set at 900 ◦C. The CNFs-based membranes were tested for CO2 adsorption in pure CO2 and in a N2/CO2 mixture for gas separation applications, and the favorable effect of a higher stabilization temperature was proven. The improvement of the adsorption efficiency is ascribed to the formation of a stabilized precursor rich in nitrogen containing condensed carbon structures that could be turned into N6 and NQ rich carbon materials. The massive presence of nitrogen basic sites is the key to the best performances showed by CNF_260 compared to CNF_230. The combination of a facile production technique such as the electrospinning coupled with the temperature tunable properties of carbonized PAN opens the way to fur-PDF Image | Effect of Thermal Stabilization on PAN-Derived Electrospun Carbon Nanofibers
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