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A Direct and Quantitative Three-Dimensional Reconstruction of the Internal Structure of Disordered Mesoporous Carbon with Tailored Pore Size

  • Juan Balach (a1), Flavio Soldera (a2), Diego F. Acevedo (a1), Frank Mücklich (a2) and César A. Barbero (a1)...

A new technique that allows direct three-dimensional (3D) investigations of mesopores in carbon materials and quantitative characterization of their physical properties is reported. Focused ion beam nanotomography (FIB-nt) is performed by a serial sectioning procedure with a dual beam FIB-scanning electron microscopy instrument. Mesoporous carbons (MPCs) with tailored mesopore size are produced by carbonization of resorcinol-formaldehyde gels in the presence of a cationic surfactant as a pore stabilizer. A visual 3D morphology representation of disordered porous carbon is shown. Pore size distribution of MPCs is determined by the FIB-nt technique and nitrogen sorption isotherm methods to compare both results. The obtained MPCs exhibit pore sizes of 4.7, 7.2, and 18.3 nm, and a specific surface area of ca. 560 m2/g.

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Balach, J., Miguel, F., Soldera, F., Acevedo, D.F., Mücklich, F. & Barbero, C.A. (2012). A direct and quantitative image of the internal nanostructure of nonordered porous monolithic carbon using FIB nanotomography. J Microsc 246(3), 274278.
Brunauer, S., Emmett, P.H. & Teller, E. (1938). Adsorption of gases in multimolecular layers. J Am Chem Soc 60(2), 309319.
Bruno, M.M., Cotella, N.G., Miras, M.C. & Barbero, C.A. (2010). A novel way to maintain resorcinol-formaldehyde porosity during drying: Stabilization of the sol-gel nanostructure using a cationic polyelectrolyte. Colloid Surf A 362(1-3), 2832.
Frackowiak, E. & Béguin, F. (2001). Carbon materials for the electrochemical storage of energy in capacitors. Carbon 39(6), 937950.
Giannuzzi, L.A. & Stevie, F.A. (2005). Introduction to Focused Ion Beams: Instrumentation, Theory, Techniques and Practice. Berlin: Springer.
Gregg, S.J. & Sing, K.S.W. (1982). Adsorption, Surface Area and Porosity. London: Academic Press.
Holzer, L., Indutnyi, F., Gasser, P.H., Münch, B. & Wegmann, M. (2004). Three-dimensional analysis of porous BaTiO3 ceramics using FIB nanotomography. J Microsc 216(1), 8495.
Holzer, L., Muench, B., Wegmann, M., Gasser, P. & Flatt, R.J. (2006). FIB-nanotomography of particulate systems—Part I: Particle shape and topology of interfaces. J Am Ceram Soc 89(8), 25772585.
Inkson, B.J., Mulvihill, M. & Möbus, G. (2001). 3D determination of grain shape in a FeAl-based nanocomposite by 3D FIB tomography. Scripta Mater 45(7), 753758.
Konrad, J., Zaefferer, S. & Raabe, D. (2006). Investigation of orientation gradients around a hard Laves particle in a warm-rolled Fe3Al-based alloy using a 3D EBSD-FIB technique. Acta Mater 54(5), 13691380.
Lasagni, F., Lasagni, A., Engstler, M., Degischer, H.P. & Mücklich, F. (2008). Nano-characterization of cast structures by FIB-tomography. Adv Eng Mater 10(1-2), 6266.
Moreno-Castilla, C. & Maldonado-Hódar, F.J. (2005). Carbon aerogels for catalysis applications: An overview. Carbon 43(3), 455465.
Münch, B., Gasser, P., Holzer, L. & Flatt, R. (2006). FIB-nanotomography of particulate systems—Part II: Particle recognition and effect of boundary truncation. J Am Ceram Soc 89(8), 25862595.
Nagel, W., Ohser, J. & Pischang, K. (2000). An integral-geometric approach for the Euler–Poincaré characteristic of spatial images. J Microsc 198(1), 5462.
Ohser, J. & Mücklich, F. (2000). Statistical Analysis of Microstructures in Materials Science. New York: John Wiley.
Phaneuf, M.W. (1999). Applications of focused ion beam microscopy to materials science specimens. Micron 30(3), 277288.
Ravikovitch, P.I. & Neimark, A.V. (2001). Characterization of nanoporous materials from adsorption and desorption isotherms. Colloid Surf A 187188, 1121.
Russ, J.C. & Dehoff, R. (2000). Practical Stereology. New York: Kluwer Academic/Plenum Publishers.
Uchic, M.D., Groeber, M.A., Dimiduk, D.M. & Simmons, J.P. (2006). 3D microstructural characterization of nickel superalloys via serial-sectioning using a dual beam FIB-SEM. Scripta Mater 55(1), 2328.
Velichko, A., Holzapfel, C. & Mücklich, F. (2007). 3D Characterization of graphite morphologies in cast iron. Adv Eng Mat 9(1-2), 3945.
Wilson, J.R., Kobsiriphat, W., Mendoza, R., Chen, H.-Y., Hiller, J.M., Miller, D.J., Thornton, K., Voorhees, P.W., Adler, S.B. & Barnett, S.A. (2006). Three-dimensional reconstruction of a solid-oxide fuel-cell anode. Nat Mater 5(7), 541544.
Zhang, S., Klimentidis, R.E. & Barthelemy, P. (2011). Porosity and permeability analysis on nanoscale FIB-SEM 3D imaging of shale rock. In 25th International Symposium of the Society of Core Analysts, pp. 112. Austin, TX: Society of Core Analysts.
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Microscopy and Microanalysis
  • ISSN: 1431-9276
  • EISSN: 1435-8115
  • URL: /core/journals/microscopy-and-microanalysis
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