a multitechnique characterization and quantification of

1
ASESA A multitechnique characterization and quantification of the microstructures of bricks made of different clayey raw materials Thomas Buchner 1 , Thomas Kiefer 1 , Luis Zelaya-Lainez 1 , Wolfgang Gaggl 2 , Josef Füssl 1 Development and optimizations of clayey brick materials, e.g., regarding thermal insulation, stiffness, and strength properties, are still based on empirical knowledge gained by extensive laboratory test series. It is known that the thermal and mechanical properties of fired clay bricks strongly depend on their microstructures, whose properties are mainly defined by the mineralogical composition, the applied firing temperature and may be influenced by pore-forming additives. We present an extensive series of microstructural characterization tests, see [1] and [2], carried out on five mineralogically different fired brick clays representing a wide range of brick materials used in the European industry. The resulting knowledge enables the development of microstructure-based material models for physically-based predictions of macroscopic brick properties and, subsequently, will allow for innovative development and optimization of modern brick products. References: [1] T. Buchner, T. Kiefer, L. Zelaya-Lainez, W. Gaggl, T. Konegger, J. Füssl (2021). A multitechnique, quantitative characterization of the pore space of fired bricks made of five clayey raw materials used in European brick industry. Applied Clay Science 200: 105884. doi: 10.1016/j.clay.2020.105884 [2] T. Buchner, T. Kiefer, L. Zelaya-Lainez, W. Gaggl, J. Füssl (2021). Automated morphometrical characterization of material phases of fired clay bricks based on Scanning Electron Microscopy, Energy Dispersive X-ray Spectroscopy and Powder X-ray Diffraction. Construction and Building Materials 288: 122909. doi: 10.1016/j.conbuildmat.2021.122909 [3] T. Kiefer, J. Füssl, H. Kariem, J. Konnerth, W. Gaggl, C. Hellmich (2020). A multi-scale material model for the estimation of the transversely isotropic thermal conductivity tensor of fired clay bricks. J. Eur. Ceram. Soc. 40(15):6200-6217. doi: 10.1016/j.jeurceramsoc.2020.05.018 [4] T. Buchner, T. Kiefer, M. Königsberger, A. Jäger, J. Füssl (2021). Continuum micromechanics model for fired clay bricks: upscaling of experimentally identified microstructural features to macroscopic elastic stiffness and thermal conductivity. Submitted to Mater. Des. 37 th Danubia-Adria Symposium on Advances in Experimental Mechanics 21.-24. September 2021, Linz, Austria Poster ID: 18 1 Institute for Mechanics of Materials and Structures, TU Wien, e-Mail: [email protected] 2 Wienerberger AG pure clay clay + EPS clay + saw dust 1 cm Motivation Materials and Experimental Methods Five brick clays, showing very different mineralogical compositions and grain size distributions, were mined in Germany, Hungary and the Czech Republic. These clays were extruded to specimens measuring 125 x 30 x 15 mm and fired at 880 °C. B A C D E specimen cross sections show large variety of brick materials Materials Pore Space Analysis Micro-CT scan on volume V with voxel size of 1.2 μm Scanning Electron Microscopy (SEM) Micro-Computed Tomography (Micro-CT) DIA 3D illustration of pores with diameter down to a couple of micrometers Pore space extracted by thresholding procedure SEM image extruded and fired specimen (125 x 30 x 15 mm) mineralogical composition by XRD assigning single grains to certain minerals chemical composition of single grain Results and Outlook SEM on polished brick surfaces Pore space extracted by thresholding procedure Fitting ellipses into single pores Pore size distribution based on SEM and Micro-CT, compared with mercury intrusion porosimetry. Automated Identification of Mineral Material Phases binding matrix pores quartz K-feldspar Na-feldspar biotite muscovite rutile hematite 30 μm Scanning Electron Microscopy-Energy Dispersive X- ray Spectroscpy (SEM-EDX) Image analysis to extract grain structure (exemplary figures) Assignment of grains to minerals with EDX chemistry and XRD mineralogy Masonry wall Brick polished sample SEM image EDX: K-map grain structure phase image Acknowlegdements: This research work was funded by the Austrian Research Promotion Agency (FFG, project number 865067) and the industry partner Wienerberger AG through the project ‘Innovative Brick 2’. Low surface roughness 10 μm 100 μm Micro-CT image stack 10 -2 10 -1 10 0 10 1 10 2 10 3 pore diameter [μm] 0 2 4 6 8 porosity [%] resolution limit micro-CT resolution limit SEM SEM micro-CT mercury intrusion Pore size distributions based on real pore size, not affected by pore throat Mineral grain assemblage Geometry of mineral phases and pores Orientation distribution of mineral phases and pores Results Outlook Multiscale Material Model for thermal conductivity and elastic stiffness [3,4] = 3 µm = 300 µm ℒ = 15 mm ≤ 150 µm ≤ 1 µm brick matrix binding matrix foam matrix micropores mesopores feldspar Fe-Mg mica muscovite quartz Microscale Mesoscale Macroscale brick specimen Mori-Tanaka homogenization on each scale: Experimental model validation: [GPa] λ [W/(mK)] A B C D E 20 40 60 0.2 0.4 0.6 0.8 30 15 [mm] 15 4 V 6 0.5 80 peak shift!

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Page 1: A multitechnique characterization and quantification of

ASESA

A multitechnique characterization and quantification of the microstructures of bricks made of different clayey raw materialsThomas Buchner1, Thomas Kiefer1, Luis Zelaya-Lainez1, Wolfgang Gaggl2, Josef Füssl1

Development and optimizations of clayey brick materials, e.g., regarding thermalinsulation, stiffness, and strength properties, are still based on empirical knowledgegained by extensive laboratory test series. It is known that the thermal andmechanical properties of fired clay bricks strongly depend on their microstructures,whose properties are mainly defined by the mineralogical composition, the appliedfiring temperature and may be influenced by pore-forming additives. We present anextensive series of microstructural characterization tests, see [1] and [2], carried outon five mineralogically different fired brick clays representing a wide range of brickmaterials used in the European industry. The resulting knowledge enables thedevelopment of microstructure-based material models for physically-basedpredictions of macroscopic brick properties and, subsequently, will allow forinnovative development and optimization of modern brick products.

References:[1] T. Buchner, T. Kiefer, L. Zelaya-Lainez, W. Gaggl, T. Konegger, J. Füssl (2021). A multitechnique, quantitative characterization ofthe pore space of fired bricks made of five clayey raw materials used in European brick industry. Applied Clay Science 200: 105884.doi: 10.1016/j.clay.2020.105884[2] T. Buchner, T. Kiefer, L. Zelaya-Lainez, W. Gaggl, J. Füssl (2021). Automated morphometrical characterization of material phasesof fired clay bricks based on Scanning Electron Microscopy, Energy Dispersive X-ray Spectroscopy and Powder X-ray Diffraction.Construction and Building Materials 288: 122909. doi: 10.1016/j.conbuildmat.2021.122909[3] T. Kiefer, J. Füssl, H. Kariem, J. Konnerth, W. Gaggl, C. Hellmich (2020). A multi-scale material model for the estimation of the transversely isotropic thermal conductivity tensor of fired clay bricks. J. Eur. Ceram. Soc. 40(15):6200-6217. doi: 10.1016/j.jeurceramsoc.2020.05.018[4] T. Buchner, T. Kiefer, M. Königsberger, A. Jäger, J. Füssl (2021). Continuum micromechanics model for fired clay bricks: upscaling of experimentally identified microstructural features to macroscopic elastic stiffness and thermal conductivity. Submitted to Mater. Des.

37th Danubia-Adria Symposium on Advances in Experimental Mechanics 21.-24. September 2021, Linz, Austria

Poster ID: 18

1Institute for Mechanics of Materials and Structures, TU Wien, e-Mail: [email protected] AG

pure clay clay + EPSclay +

saw dust

1 cm

Motivation

Materials and Experimental Methods

Five brick clays, showing very different mineralogical compositions and grain size

distributions, were mined in Germany, Hungary and the Czech Republic. These

clays were extruded to specimens measuring 125 x 30 x 15 mm and fired at 880 °C.

BA C D E

specimen cross sections showlarge variety of brick materials

Materials Pore Space Analysis

Micro-CT scan on

volume V with voxel size

of 1.2 µm

Scanning Electron Microscopy (SEM) Micro-Computed Tomography (Micro-CT)

DIA

3D illustration of poreswith diameter down to a couple of micrometers

Pore space extracted bythresholding procedure

SEM image

extruded and fired specimen(125 x 30 x 15 mm)

mineralogicalcomposition by

XRD

assigning singlegrains

to certain minerals

chemicalcomposition

of single grain

Results and Outlook

SEM on polished brick

surfaces

Pore space extracted bythresholding procedure

Fitting ellipses intosingle pores

Pore size distribution basedon SEM and Micro-CT,compared with mercuryintrusion porosimetry.

Automated Identification of Mineral Material Phases

binding matrix

pores

quartz

K-feldspar

Na-feldspar

biotite

muscovite

rutile

hematite

30 µm

Scanning Electron Microscopy-Energy Dispersive X-

ray Spectroscpy (SEM-EDX)

Image analysis to extract grain structure (exemplary

figures)

Assignment of grains to minerals with EDX chemistry

and XRD mineralogy

Masonry wall Brick

polished sample SEM image EDX: K-map grain structure

phase image

Acknowlegdements:This research work was funded by the Austrian Research Promotion Agency (FFG, project number 865067) and the industry

partner Wienerberger AG through the project ‘Innovative Brick 2’.

Low surface roughness

10 µm 100 µm

Micro-CT image stack

10-2 10-1 100 101 102 103

pore diameter [µm]

0

2

4

6

8

po

rosi

ty[%

]

resolution limitmicro-CT

resolutionlimit SEM

SEMmicro-CT

mercury intrusion

• Pore size distributions based on real pore size, not affected by pore throat

• Mineral grain assemblage

• Geometry of mineral phases and pores

• Orientation distribution of mineral phases and pores

Results Outlook

Multiscale Material Model for thermal conductivity and elastic stiffness [3,4]

𝑙 𝑚𝑖𝑐𝑟𝑜=3µm

𝑙 𝑚𝑒𝑠𝑜

=300µm

ℒ=15mm

𝑥

𝑦𝑧

≤ 150 µm

≤ 1 µm

brick matrix

binding matrix

foam matrix

micropores

mesoporesfeldspar

Fe-Mg mica

muscovite

quartz

Microscale

Mesoscale

Macroscale

brick specimen

Mori-Tanaka homogenization on each scale:

Experimental model validation:

80

𝐶𝑥𝑥𝑥𝑥[GPa]

λ 𝑧[W

/(mK)]

A B C D E

20

40

60

0.2

0.4

0.6

0.8

30

15

[mm]

15

4

V

6

0.5

80

peak shift!