Focussed ion beam nanotomography reveals the 3D morphology of different solid phases in hardened cement pastes

Due to the development of integrated low‐keV back‐scattered electron detectors, it has become possible in focussed ion beam nanotomography to segment not only solid matter and porosity of hardened cement paste, but also to distinguish different phases within the solid matter. This paper illustrates a method that combines two different approaches for improving the contrast between different phases in the solid matrix of a cement paste. The first approach is based on the application of a specially developed 3D diffusion filter. The second approach is based on a modified data‐acquisition procedure during focussed ion beam nanotomography. A pair of electron images is acquired for each slice in the focussed ion beam nanotomography dataset. The first image is captured immediately after ion beam milling; the second image is taken after a prolonged exposure to electron beam scanning. The acquisition of complementary focussed ion beam nanotomography datasets and processing the images with a 3D anisotropic diffusion filter allows distinguishing different phases within the hydration products.

[1]  F. Mücklich,et al.  Interaction of cracks with precipitates and grain boundaries: Understanding crack growth mechanisms through focused ion beam tomography , 2007 .

[2]  Jitendra Malik,et al.  Scale-Space and Edge Detection Using Anisotropic Diffusion , 1990, IEEE Trans. Pattern Anal. Mach. Intell..

[3]  E. Wachsman,et al.  Three-Dimensional Reconstruction of Porous LSCF Cathodes , 2007 .

[4]  Robert J. Flatt,et al.  FIB-Nanotomography of Particulate Systems—Part I: Particle Shape and Topology of Interfaces , 2006 .

[5]  H. Jinnai,et al.  Three‐dimensional structural analysis of a block copolymer by scanning electron microscopy combined with a focused ion beam , 2007 .

[6]  U. Sennhauser,et al.  Preparative methods for nanoanalysis of materials with focused ion beam instruments , 2006 .

[7]  Robert J. Flatt,et al.  FIB-Nanotomography of Particulate Systems—Part II: Particle Recognition and Effect of Boundary Truncation , 2006 .

[8]  Robert Hull,et al.  Reconstruction of three-dimensional chemistry and geometry using focused ion beam microscopy , 1999 .

[9]  B. Münch,et al.  A critical examination of statistical nanoindentation on model materials and hardened cement pastes based on virtual experiments , 2009 .

[10]  R. Wepf,et al.  Cryo‐FIB‐nanotomography for quantitative analysis of particle structures in cement suspensions , 2007, Journal of microscopy.

[11]  B. Ripley,et al.  Pattern Recognition , 1968, Nature.

[12]  Michael Angelo B. Promentilla,et al.  Quantification of Tortuosity in Hardened Cement Pastes using Synchrotron-based X-ray Computed Microtomography , 2009 .

[13]  B Münch,et al.  Three‐dimensional analysis of porous BaTiO3 ceramics using FIB nanotomography , 2004, Journal of microscopy.

[14]  J. Wagner,et al.  Automated three-dimensional X-ray analysis using a dual-beam FIB. , 2007, Ultramicroscopy.

[15]  Paul Munroe,et al.  Three-Dimensional Microstructural Characterization Using Focused Ion Beam Tomography , 2007 .

[16]  F. Steiniger,et al.  Limited‐Dose Electron Microscopy Reveals the Crystallinity of Fibrous C–S–H Phases , 2006 .

[17]  R. L. Berger.  Calcium Hydroxide: Its Role in the Fracture of Tricalcium Silicate Paste , 1972, Science.

[18]  F. Mücklich,et al.  Quantitative 3D characterisation of graphite morphology in cast iron – correlation between processing, microstructure and properties , 2009 .

[19]  Rachid Deriche,et al.  Vector-valued image regularization with PDE's: a common framework for different applications , 2003, 2003 IEEE Computer Society Conference on Computer Vision and Pattern Recognition, 2003. Proceedings..

[20]  I. Richardson,et al.  Microstructure and microanalysis of hardened ordinary Portland cement pastes , 1993 .

[21]  B. Münch,et al.  Stripe and ring artifact removal with combined wavelet--Fourier filtering. , 2009, Optics express.

[22]  M. N. Lebbink,et al.  Tomography of insulating biological and geological materials using focused ion beam (FIB) sectioning and low‐kV BSE imaging , 2009, Journal of microscopy.

[23]  H. Siegrist,et al.  Influence of water hardness on concrete surface deterioration caused by nitrifying biofilms in wastewater treatment plants , 2010 .

[24]  G. Saoût,et al.  Influence of limestone on the hydration of Portland cements , 2008 .

[25]  B. Inkson,et al.  Subsurface nanoindentation deformation of Cu–Al multilayers mapped in 3D by focused ion beam microscopy , 2001, Journal of microscopy.

[26]  P. Gasser,et al.  QUANTIFICATION OF CAPILLARY PORES AND HADLEY GRAINS IN CEMENT PASTE USING FIB-NANOTOMOGRAPHY , 2006 .

[27]  Rachid Deriche,et al.  Vector-valued image regularization with PDEs: a common framework for different applications , 2005, IEEE Transactions on Pattern Analysis and Machine Intelligence.

[28]  Surendra P. Shah,et al.  Early age microstructure of the paste-aggregate interface and its evolution , 1998 .

[29]  Lorenz Holzer,et al.  Contradicting Geometrical Concepts in Pore Size Analysis Attained with Electron Microscopy and Mercury Intrusion , 2008 .