journal article·2018-08

Microstructure characterization of mullite foam by image analysis, mercury porosimetry and X-ray computed microtomography

Eva Gregorová, Tereza Uhlířová, Willi Pabst, Petra Diblíková, Ivona Sedlářová

Ceramics International· Volume 44· Issue 11
Publisher page

Abstract

Abstract It is well known that the effective properties of porous ceramics and ceramic foams depend strongly on the microstructure. That means, the prediction of effective properties of real materials generally requires quantitative values of well-defined microstructural descriptors as input parameters. The present contribution shows that ceramic foams with hierarchical microstructure require a complex microstructural characterization procedure based on a combination of different complementary techniques. Taking a light-weight mullite foam – an important and versatile ceramic material (e.g. for furnace linings, kiln furniture and high-temperature filters) – as a paradigmatic example, a systematic methodology is proposed for extracting relevant microstructural information. The microstructure of mullite foam with hierarchical microstructure has been characterized by stereology-based image analysis, mercury porosimetry and computed microtomography (X-ray µCT). Three metric descriptors (porosity, surface density, mean curvature integral density) and a topological descriptor (Euler characteristic density) have been determined, the latter being 192.4 ± 17.7·10−9 µm−3. SEM micrographs taken at different magnification allow to distinguish the porosity attributable to pore cavities (62.3–63.0%) and matrix (47.8–49.5%). Mean chord lengths and Jeffries sizes of the pores are 159–164 µm and 164–180 µm, respectively, for the pore cavities and 4.6–5.1 µm and 4.9–5.1 µm, respectively, for the matrix pores. Different types of pore size distributions have been determined, and it is found that in this specific case the size distribution of pore cavity sizes obeys a Rayleigh distribution. Mercury porosimetry covers small and medium-sized pore throats (median 76 µm), whereas image analysis captures pore cavities (median 234–247 µm) and X-ray µCT combines information on both pore throats and cavities, resulting in an intermediate median of 206 µm. The procedure proposed is very general and systematic and can be applied to porous materials with a wide range of microstructures.
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Research context

OpenAlex topics: Rock Mechanics and Modeling · Recycling and utilization of industrial and municipal waste in materials production · Advanced ceramic materials synthesis

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References (62)

Show source-provided references
1. 2005 · 20
2. Heat capacity of mullite – new data and evidence for a high-temperature phase transformation10.1111/j.1551-2916.2004.00227.x ↗
3. Thermal expansion of mullite
4. Thermal conductivity of ceramics – from monolithic to multiphase, from dense to porous, from micro to nano
5. Elastic properties of mullite and mullite-containing ceramics – Part I: theoretical aspects and review of monocrystal data
6. Theoretical and experimental analyses of thermal properties of dense polycrystalline mullite10.1016/j.ceramint.2017.05.076 ↗
7. Theoretical and experimental analyses of thermal properties of porous polycrystalline mullite10.1016/j.ceramint.2017.05.009 ↗
8. Thermal behavior of mullite between 4 K and 1320 K10.1111/jace.15028 ↗
9. Porous mullite templated from hard mullite beads10.1016/j.jeurceramsoc.2011.02.004 ↗
10. Thermal conductivity of highly porous mullite material10.1016/j.actamat.2005.03.040 ↗
11. Fabrication and characterization of highly porous mullite ceramics10.1016/S0254-0584(03)00080-4 ↗
12. Two alternative routes for starch consolidation of mullite green bodies10.1016/j.jeurceramsoc.2010.06.001 ↗
13. Processing of porous mullite ceramics using novel routes by starch consolidation casting10.1016/j.jeurceramsoc.2014.10.011 ↗
14. Porous mullite ceramics formed by direct consolidation using native and granular cold-water-soluble starches10.1111/jace.12852 ↗
15. Macroporous mullite materials prepared by novel shaping strategies based on starch thermogelation for thermal insulation10.1111/ijac.12673 ↗
16. Preparation and characterization of porous mullite ceramics via foam-gelcasting10.1016/j.ceramint.2015.03.237 ↗
17. Processing, microstructure and elastic properties of mullite-based ceramic foams prepared by direct foaming with wheat flour10.1016/j.jeurceramsoc.2015.09.028 ↗
18. Porous mullite thermal insulators from coal gangue fabricated by a starch-based foam gel-casting method10.1007/s41779-017-0035-9 ↗
19. Influence of pore characteristics on the properties of porous mullite ceramics10.1007/s41779-017-0094-y ↗
20. Foam-gelcasting preparation of high-strength self-reinforced porous mullite ceramics10.1016/j.jeurceramsoc.2017.05.009 ↗
21. Highly porous mullite ceramics from engineered alkali activated suspensions10.1111/jace.15327 ↗
22. Characterization of hierarchical pore structures in ceramics using multiscale tomography10.1016/j.actamat.2010.12.012 ↗
23. Hierarchically structured titanium foams for tissue scaffold applications10.1016/j.actbio.2010.06.027 ↗
24. Multi-scale multi-dimensional microstructure imaging of oil shale pyrolysis using X-ray micro-tomography, automated ultra-high resolution SEM, MAPS Mineralogy and FIB-SEM10.1016/j.apenergy.2017.05.039 ↗
25. Novel 3D centimetre- to nano-scale quantification of an organic-rich mudstone10.1016/j.marpetgeo.2016.02.008 ↗
26. Processing, microstructure, properties, applications and curvature-based classification schemes of porous ceramics
27. Shear and bulk moduli of isotropic porous and cellular alumina ceramics predicted from thermal conductivity via cross-property relations10.1016/j.ceramint.2018.01.254 ↗
28. Young‘s modulus and thermal conductivity of closed-cell, open-cell and inverse ceramic foams – model-based predictions, cross-property predictions and numerical calculations10.1016/j.jeurceramsoc.2018.01.019 ↗
29. W. Pabst, E. Gregorová, T. Uhlířová, Numerical modeling of elastic modulus and conductivity of porous alumina – effects of pore shape, pore size distribution and pore distance, in: D. Singh, M. Fukushima, Y.-W. Kim, K. Shimamura, N. Imanaka, T. Ohji, J. Amoroso, M. Lanagan (eds.), Proceedings of the 12th Pacific Rim Conference on Ceramic and Glass Technology (Ceramic Transactions, Vol. 264), The American Ceramic Society/John Wiley & Sons, Inc., Hoboken/NJ, USA, 2018, pp. 65–76.10.1002/9781119494096.ch7 ↗
30. Minkowski · 1911 · 103
31. Ohser · 2000 · 25
32. Additivity, convexity, and beyond: applications of Minkowski functionals
33. Stoyan · 1995 · 11
34. Liquid intrusion and alternative methods for the characaterization of macroporous materials (IUPAC technical report)10.1351/PAC-REP-10-11-19 ↗
35. The PZT system – specific features of recrystallization sintering and microstructures of solid solutions (Part 1)10.1016/j.ceramint.2012.06.088 ↗
36. Fractal approach to BaTiO3-ceramics micro-impedances10.1016/j.ceramint.2015.01.102 ↗
37. Heterogeneity of surfaces and materials, as reflected in multifractal analysis10.1002/(SICI)1234-985X(199609)3:3<269::AID-HCR63>3.0.CO;2-L ↗
38. Multifractal properties of pore-size distribution in apple tissue using X-ray imaging10.1016/j.jfoodeng.2010.02.021 ↗
39. The elastic moduli of heterogeneous materials
40. Micromechanics of heterogeneous media
41. A variational approach to the theory of the effective magnetic permeability of multiphase materials10.1063/1.1728579 ↗
42. A variational approach to the theory of the elastic behavior of multiphase materials10.1016/0022-5096(63)90060-7 ↗
43. Critical assessment 18: elastic and thermal properties of porous materials – rigorous bounds and cross-property relations10.1080/02670836.2015.1114697 ↗
44. Microstructure characterization via stereological relations – a shortcut for beginners10.1016/j.matchar.2015.04.013 ↗
45. Preparation of cellular alumina ceramics via biological foaming with yeast and its microstructural characterization via stereological relations10.1016/j.jeurceramsoc.2014.08.020 ↗
46. A generalized class of transformation matrices for the reconstruction of sphere size distributions from section circle size distributions10.13168/cs.2017.0010 ↗
47. Russ · 2000 · 1
48. Hadwiger · 1957
49. The unbiased estimation of numbers and sizes of arbitrary particles using the disector10.1111/j.1365-2818.1984.tb02501.x ↗
50. Use of the disector to estimate the Euler characteristic of three-dimensional microstructures
51. The estimation of the Euler-Poincaré characteristic from observations on parallel sections10.1111/j.1365-2818.1996.tb00006.x ↗
52. Gregg · 1982 · 173
53. The corpuscle problem – a mathematical study of a biometric problem
54. Saltykov · 1974
55. Particle size-shape distributions: the general spheroid problem – I. Mathematical model10.1111/j.1365-2818.1976.tb02446.x ↗
56. Particle size-shape distributions: the general spheroid problem – II. Stochastic model and practical guide10.1111/j.1365-2818.1978.tb01162.x ↗
57. Higginson · 2003
58. A new method for the model-independent assessment of thickness in three-dimensional images10.1046/j.1365-2818.1997.1340694.x ↗
59. Porous alumina ceramics prepared with wheat flour10.1016/j.jeurceramsoc.2010.03.020 ↗
60. A model for the body formation in starch consolidation casting10.1023/A:1016558516677 ↗
61. Starch consolidation casting of alumina ceramics – body formation and microstructural characterization
62. T. Uhlířová, E. Gregorová, V. Nečina, M. Veselý, W. Pabst, Influence of ethanol addition on the microstructure of ceramic foams prepared by yeast-mediated biological foaming of alumina suspensions, in: R. Řápková, J. Čopíková, E. Šárka (eds.), Proceedings of the 10th International Conference on Polysaccharides – Glycoscience, Czech Chemical Society, Prague, 2014, pp. 48–53.