Nitrogen doped heat treated and activated hydrothermal carbon: NEXAFS examination of the carbon surface at different temperatures

Abstract

Hydrothermal carbons have been shown to have controllable surface functionalization through various post-treatment techniques, which indicates these materials may be tuned for specific applications. For this reason, Near Edge X-ray Absorption Fine Structure (NEXAFS) studies have been conducted on a series of nitrogen doped and non-doped heat treated and activated hydrothermal carbons to further understand the changes in surface functionality with treatment. The NEXAFS carbon K-edge spectrum of the non-doped samples displayed a loss of oxygen functionalities (CO and COH) as well as the furan ring structure with increasing temperature, while CC bonds from graphitic groups increased. This effect was amplified further upon the addition of phosphoric acid (H3PO4) during activation. The doped hydrothermal carbons displayed similar functionality to the non-doped, although the effect of both heat treatment and activation was diminished. The nitrogen K-edge displayed characteristic peaks for pyridine and imines/amides, with pyrroles located under the broad ionization step. This work represents the first time a series of heat treated and activated hydrothermal carbons have been examined via NEXAFS spectroscopy. Additionally, difference analysis has been applied to the NEXAFS spectra to obtain a deeper understanding in the changes in surface functionality, a previously unused technique for these materials.