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Characterization of Carbon Surface Chemistry by Combined Temperature Programmed Desorption with in Situ X-ray Photoelectron Spectrometry and Temperature Programmed Desorption with Mass Spectrometry Analysis

Brender, Patrice, Gadiou, Roger, Rietsch, Jean-Christophe, Fioux, Philippe, Dentzer, Joseph, Ponche, Arnaud, Vix-Guterl, Cathie
Analytical chemistry 2012 v.84 no.5 pp. 2147-2153
X-radiation, X-ray photoelectron spectroscopy, carbon, desorption, gases, heat, heat treatment, mass spectrometry, oxygen production, quantitative analysis, temperature
The analysis of the surface chemistry of carbon materials is of prime importance in numerous applications, but it is still a challenge to identify and quantify the surface functional groups which are present on a given carbon. Temperature programmed desorption with mass spectrometry analysis (TPD-MS) and X-ray photoelectron spectroscopy with an in situ heating device (TPD-XPS) were combined in order to improve the characterization of carbon surface chemistry. TPD-MS analysis allowed the quantitative analysis of the released gases as a function of temperature, while the use of a TPD device inside the XPS setup enabled the determination of the functional groups that remain on the surface at the same temperatures. TPD-MS results were then used to add constraints on the deconvolution of the O1s envelope of the XPS spectra. Furthermore, a better knowledge of the evolution of oxygen functional groups with temperature during a thermal treatment could be obtained. Hence, we show here that the combination of these two methods allows to increase the reliability of the analysis of the surface chemistry of carbon materials.