Effect of calcination temperature and chemical composition of pan-derived carbon microfibers on n2, co2, and ch4 adsorption

Reyna Ojeda-López, Guadalupe Ramos-Sánchez, Cinthia García-Mendoza, Diana C.S. Azevedo, Ariel Guzmán-Vargas, Carlos Felipe

Research output: Contribution to journalArticlepeer-review

9 Scopus citations

Abstract

This work investigates the interplay of carbonization temperature and the chemical composition of carbon microfibers (CMFs), and their impact on the equilibration time and adsorption of three molecules (N2, CO2, and CH4 ). PAN derived CMFs were synthesized by electrospinning and calcined at three distinct temperatures (600, 700 and 800C), which led to samples with different textural and chemical properties assessed by FTIR, TGA/DTA, XRD, Raman, TEM, XPS, and N2 adsorption. We examine why samples calcined at low/moderate temperatures (600 and 700C) show an open hysteresis loop in nitrogen adsorption/desorption isotherms at −196.15C. The equilibrium time in adsorption measurements is nearly the same for these samples, despite their distinct chemical compositions. Increasing the equilibrium time did not allow for the closure of the hysteresis loop, but by rising the analysis temperature this was achieved. By means of the isosteric enthalpy of adsorption measurements and ab initio calculations, adsorbent/adsorbate interactions for CO2, CH4 and N2 were found to be inversely proportional to the temperature of carbonization of the samples (CMF-600 > CMF-700 > CMF-800). The enhancement of adsorbent/adsorbate interaction at lower carbonization temperatures is directly related to the presence of nitrogen and oxygen functional groups on the surface of CMFs. Nonetheless, a higher concentration of heteroatoms also causes: (i) a reduction in the adsorption capacity of CO2 and CH4 and (ii) open hysteresis loops in N2 adsorption at cryogenic temperatures. Therefore, the calcination of PAN derived microfibers at temperatures above 800C is recommended, which results in materials with suitable micropore volume and a low content of surface heteroatoms, leading to high CO2 uptake while keeping acceptable selectivity with regards to CH4 and moderate adsorption enthalpies.

Original languageEnglish
Article number3914
JournalMaterials
Volume14
Issue number14
DOIs
StatePublished - 2 Jul 2021

Keywords

  • CO and CH adsorbed
  • Carbon microfibers (CMFs)
  • Electrospinning
  • Equilibration time
  • Open hysteresis loop

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