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Toward Reproducible Three-Dimensional Microstructure Analysis of Granular Materials and Complex Suspensions

Published online by Cambridge University Press:  16 March 2009

Lorenz Holzer  and
Beat Münch
Lorenz Holzer*
Affiliation:
Empa Materials Science and Technology, 8600 Dübendorf, Switzerland
Beat Münch
Affiliation:
Empa Materials Science and Technology, 8600 Dübendorf, Switzerland
*
Corresponding author. E-mail: lorenz.holzer@empa.ch
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Abstract

Focused ion beam nanotomography (FIB-nt) is a novel method for high resolution three-dimensional (3D) imaging. In this investigation we assess the methodological parameters related to image acquisition and data processing that are critical for obtaining reproducible microstructural results from granular materials and from complex suspensions. For this purpose three case studies are performed: (1) The precision of FIB-nt is evaluated by analyzing a reference sample with nanospheres. Due to the implementation of an automated correction procedure, drift phenomena can be removed largely from the FIB data. However, at high magnifications remaining drift components can induce problems for 3D-shape reconstructions. (2) Correct object recognition from densely packed microstructures requires specific algorithms for splitting of agglomerated particles. To establish quantitative criteria for the correct degree of splitting, a parametric study with dry portland cement is performed. It is shown that splitting with a k-value of 0.6 leads to accurate results. (3) Finally, the reproducibility of the entire cryo-FIB analysis is investigated for high pressure frozen cement suspensions. Reproducible analyses can be obtained if the magnification is adapted to the particle size. At low magnifications the small particles and their surface area are underestimated. At high magnifications representativity is questioned because local inhomogeneities can become dominant.

Keywords

focused ion beam (FIB)nanotomographyimage analysisparticle size distributionnanoparticlesagglomerationordinary portland cementcryomicroscopy
Type
Image Formation and Analysis
Information
Microscopy and Microanalysis , Volume 15 , Issue 2 , April 2009 , pp. 130 - 146
Copyright
Copyright © Microscopy Society of America 2009

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References

REFERENCES

Bachmann, L. & Mayer, E. (1987). Physics of water and ice: Implications for cryofixation. In Cryotechniques in Biological Electron Microscopy, Steinbrecht, R.A. & Zierold, K. (Eds.), pp. 3–34. Berlin: Springer Press.CrossRefGoogle Scholar
Flatt, R. & Bowen, P. (2006). Yodel: A yield stress model for suspensions. J Am Ceram Soc 89, 1244–1256.CrossRefGoogle Scholar
Goodwin, J. (2004). Colloids and Interfaces with Surfactants and Polymers. Hoboken, NJ: Wiley Press.Google Scholar
Holzapfel, C., Schaef, W., Marx, M., Vehoff, H. & Muecklich, F. (2007). Interaction of cracks with precipitates and grain boundaries: Understanding crack growth mechanisms through focused ion beam tomography. Scripta Mater 56, 697–700.Google Scholar
Holzer, L., Gasser, P., Kaech, A., Wegmann, M., Zingg, A., Wepf, R. & Münch, B. (2007). Cryo-FIB-nanotomography for quantitative analysis of particle structures in cement suspensions. J Microsc 227, 216–228.CrossRefGoogle ScholarPubMed
Holzer, L., Indutnyi, F., Gasser, P., Münch, B. & Wegmann, M. (2004). 3D analysis of porous BaTiO3 ceramics using FIB nanotomography. J Microsc 216, 84–95.Google Scholar
Holzer, L., Münch, B., Wegmann, M., Gasser, P. & Flatt, R. (2006). FIB-nanotomography of particulate systems—Part I: Particle shape and topology of interfaces. J Am Ceram Soc 89, 2577–2585.CrossRefGoogle Scholar
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, 753–758.CrossRefGoogle Scholar
Jones, R.M. (2003). Particle size analysis by laser diffraction: ISO13320, standard operating procedures and Mie theory. Am Lab 35, 44–47.Google Scholar
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, 1369–1380.Google Scholar
McGrouther, D. & Munroe, P.R. (2007). Imaging and analysis of 3-D structure using dual beam FIB. Microsc Res Techn 70, 186–194.Google Scholar
Monaghan, P., Perushinghe, N. & Müller, M. (1998). High pressure freezing for immunocytochemistry. J Microsc 192, 248–258.Google Scholar
Moor, H. (1987). Theory and practice of high pressure freezing. In Cryotechniques in Biological Electron Microscopy, Steinbrecht, R.A. & Zierold, K. (Eds.), pp. 175–191. Berlin: Springer Press.CrossRefGoogle Scholar
Münch, B., Gasser, P., Flatt, R. & Holzer, L. (2006). FIB-nanotomography of particulate systems—Part II: Particle recognition and effect of boundary truncation. J Am Ceram Soc 89, 2586–2595.Google Scholar
Russel, W.B., Saville, D.A. & Schowater, W.R. (1989). Colloidal Dispersions. Cambridge, UK: Cambridge University Press.Google Scholar
Suzuki, M. & Oshima, T. (1983). Estimation of the coordination number in a multi-component mixture of spheres. Powder Technol 35, 159–166.Google Scholar
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. Scipta Mater 55, 23–28.Google Scholar
Uchic, M.D., Holzer, L., Inkson, B.J., Principe, E.L. & Munroe, P. (2007). 3D microstructural characterization using focused ion beam tomography. MRS Bull 32, 408–416.Google Scholar
Velichko, A., Holzapfel, C. & Mücklich, F. (2007). 3D characterization of graphite morphologies in cast iron. Adv Eng Mat 9, 39–45.CrossRefGoogle Scholar
Wilson, J.R., Kopsiriphat, W., Mendoza, R., Chen, H.Y., Hiller, J.M., 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, 541–544.Google Scholar
Zingg, A., Holzer, L., Kaech, A., Winnefeld, F., Pakusch, J., Becker, S. & Gauckler, L. (2008). The microstructure of dispersed and nondispersed fresh cement pastes—New insight by cryo-microscopy. Cem Concr Res 38, 522–529.Google Scholar