Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

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Journal of the European Ceramic Society

journal homepage: www.elsevier.com/locate/jeurceramsoc

Original article

A multi-scale material model for the estimation of the transversely isotropic

thermal conductivity tensor of fired clay bricks
Thomas Kiefera,*, Josef Füssla, Hawraa Kariema, Johannes Konnerthb, Wolfgang Gagglc,
Christian Hellmicha
a
Institute for Mechanics of Materials and Structures, TU Wien - Vienna University of Technology, Karlsplatz 13, A-1040 Vienna, Austria
b
Institute of Wood Technology and Renewable Materials, University of Natural Resources and Life Sciences, Konrad Lorenz-Str. 24, A-3430 Tulln an der Donau, Austria
c
Wienerberger AG, Clay Building Materials Europe, Hauptstrasse 4, A-2332 Hennersdorf bei Wien, Austria

ARTICLE INFO ABSTRACT

Keywords: Fired clay bricks are employed in increasingly demanding application domains, such as multi-storey buildings
Thermal conductivity and façades allowing only minimal heat loss. The latter requirement is often met by the use of pore forming
Fired clay bricks agents. Then, pore size and morphology, as well as the thermal conductivity of the solid constituents of fired
Multiscale material model clay, govern the material's overall thermal conductivity tensor. We here quantify corresponding structure–-
Sensitivity analysis
property relations in the framework of random homogenization theory, introducing ellipsoidal shape and or-
Homogenization
ientation distributions of material phases (including pores) at three different organizational levels. The model is
validated by experimental techniques, such as scanning thermal microscopy, micro-computed tomography, and
scanning electron microscopy. A final sensitivity analysis reveals that four design parameters heavily contribute
to the overall thermal conductivity of fired clay bricks; namely the thermal conductivity of the fired clay matrix
as well as the porosity of each of the three organizational levels.

1. Introduction microstructural characteristics of fired clay. In this way, a deeper un-

Fired clay brick, a traditional building material which combines
mechanical performance, flexibility, and sustainability in a unique way,
has gained popularity in recent years. This is mainly due to continuous
product development, allowing this material to be used in multi-storey
constructions as well as in façade systems, making conventional
thermal insulation obsolete. Key for such developments is the im-
provement of the thermal resistance of fired clay bricks by simulta-
neously maintaining their required stiffness and strength. An im-
provement of the thermal resistance can either be reached by
optimizing the geometry of vertically perforated clay bricks or by
changing the (micro)structure of the fired clay mixture itself. Thereby,
the pore structure introduced by pore-forming agents represents one of
the main influencing parameters. This is not only because the pores
change the effective bulk density [7,19,24,57]; it is also important that
the pore size distribution, the pore morphology, and the thermal con-
ductivities of the key substances making up fired clay, along with the
firing temperature, affect the overall thermal conductivity of fired clay
bricks [6,13,25,30].
This fact suggests the development of a multiscale material model,
able to predict effective thermal conductivities as a function of the
derstanding of this kind of materials could be gained and a basis for
new concepts in product development would be laid. It is the focus of
the present paper to propose such a model for the prediction of trans-
versely isotropic thermal conductivities. The model is built in a way
which allows its application to fired clay characterized by different pore
forming agents, firing temperatures, and chemical compositions. In this
context, we put a particular emphasis on careful experimental valida-
tion, through different measurement techniques revealing various ma-
terial properties at different length scales. In order to establish such a
model, the (micro)structure of fired clay is divided into meaningful
scales of observation. At each scale of observation, the constituent
material phases as well as their thermal and geometrical properties
were identified. To accomplish that, the comprehensive work of
Krakowiak et al. [46], focusing on the microstructure of fired clay,
provided a base line for developing the proposed scientific concepts.
The gained morphological information serves as input for a multiscale
model for fired clay, allowing the prediction of effective thermal con-
ductivities via an efficient analytical approach. For this purpose, a
multiscale homogenization scheme successfully applied for the predic-
tion of the thermal conductivity of partly saturated sedimentary rock
(see, e.g. [32,33,37]) is adapted. Setting up this multiscale model

⁎
Corresponding author.
E-mail address: thomas.kiefer@tuwien.ac.at (T. Kiefer).

https://doi.org/10.1016/j.jeurceramsoc.2020.05.018
Received 15 November 2019; Received in revised form 3 March 2020; Accepted 8 May 2020
0955-2219/ © 2020 Elsevier Ltd. All rights reserved.

Please cite this article as: Thomas Kiefer, et al., Journal of the European Ceramic Society, https://doi.org/10.1016/j.jeurceramsoc.2020.05.018
T. Kiefer, et al.
requires the determination of four key quantities characterizing each
material constituent: (i) the thermal conductivity, (ii) the volume
fraction, (iii) the aspect ratios of spheropidal inclusions mimicking the
actual micromorphology, and (iv) the spatial orientations of the
aforementioned inclusions. Measurements of the thermal conductivity
at microscopic scales have been performed successfully by various au-
thors (see, e.g. [27,28,35,53,55,60]) by means of scanning thermal
microscopy (SThM), which suggested the utilization of this technique
for our purpose. Concerning the volume fraction, aspect ratio, and
phase orientation, various techniques (scanning electron microscopy
with energy dispersive X-ray analysis, µ -CT, and mercury intrusion
porosimetry) have been used for their determination on different length
scales.
Based on that motivation, the main objectives of this work can be
summarized as follows:
1. Identification of the thermal conductivity and morphology of all
constituent material phases in selected fired clay samples.
2. Development of a multiscale material model able to accurately
predict the effective thermal conductivity of brick ceramic bodies by
taking their complex microstructural system into account.
3. Validation of this multiscale material model by means of macro-
scopic measurements on brick ceramic bodies.
4. Identification of the most significant variables affecting the macro-
scopic thermal conductivity by performing a sensitivity analysis.
These objectives are dealt with in appropriate detail in the re-
mainder of this paper, along the following flow of development: Section
2 introduces a hierarchical random homogenization scheme for heat
transport in fired clay. This starts, in Section 2.1, with introducing the
representative volume element (RVE) concept, comprising the pre-
scription of homogeneous temperature gradients at the boundary of the
RVEs, and the derivation of corresponding consequences: namely, the
validity of a heat flux averaging rule for thermodynamical systems, the
steady state of which is governed by the temperature only. Thereafter,
the matter within the RVEs is equipped with thermal conductivity
properties, which, in combination with the homogeneous boundary
conditions, leads to a localization or scale transition problem described
in Section 2.2. A short description of the investigated samples and their
preperation is given in Section 3. Results from the identification ex-
periments on the fired clay porosity and morphology on different scales
of observation are described in Section 4, followed by the identification
experiments on the thermal conductivity of the distinguished material
phases as well as the macroscopic measurements on solid brick bodies
for the purpose of verification in Section 5. Section 6 comprises the
description of the proposed multiscale material model and its hier-
archical organization. In order to identify those input variables of the
proposed model, which have the biggest effect on the derived thermal
conductivity tensor, and in order to quantify their impact, a sensitivity
analysis is performed on the fired clay samples, as described in Section
7. Finally, results from the multiscale material model are presented in
Section 8 and compared to experimental data from macroscopic testing.
Concluding remarks are given in Section 9. Complementing information
on RVE-specific formulation of the laws of thermodynamics, on the
concentration or downscaling tensors, and on the Hill or morphology
tensors are given in the Appendices A to C.
2. Hierarchical random homogenization scheme for heat
transport in fired clay
2.1. Introduction of representative volume elements (RVEs) – laws of
thermodynamics – heat flux averaging
We consider fired clay as being composed of a sequence of three
representative volume elements (RVEs, see Fig. 12), with the following
characteristics: The largest RVE has to fulfill the separation-of-scale
2
Journal of the European Ceramic Society xxx (xxxx) xxx–xxx
requirement. That means that its characteristic length lRVE has to be
considerably larger than the size dRVE of the inhomogeneities within the
(largest) RVE, and significantly smaller than the structural length .
The latter is given by the macroscopic temperature field through [2]:
|T (X)|
(X) = ,
GRAD T (X) (1)
where X is the macroscopic location vector (resolved up to length scale
lRVE ), and GRAD (·) = (·)/ X is the macroscopic gradient. Accordingly,
the aforementioned separation-of-scales requirement reads as [63]:
dRVE lRVE . (2)
It is known from the field of linear elasticity, which is in mathematical
analogy to the linear heat conduction problem tackled further below,
that the left “ ”-sign in (2) refers to a factor of only 1.5–3 [22,54],
while the “ ”-sign on the right-hand side of (2) relates to a factor of
5–10 [45].
The two smaller RVEs in Fig. 12 have to be accommodated within
the phases of the respectively larger RVEs, so that they fulfill the
modified separability conditions [29]:
dRVE,II lRVE,II dRVE
dRVE,III lRVE,III dRVE,II (3)
Within each RVE, we introduce a field of “microscopic” heat flux vec-
tors q (x) , the “microscopic” location vector x being resolved down to a
resolution of dRVE (or of dRVE,II and dRVE,III , respectively, depending on
the scale we focus on). For such a thermodynamics-associated RVE, a
power averaging rule for heat flux problems can be established, linking
the “microscopic” heat flux vectors q (x) and the local temperature
gradient grad T (x) to a “macroscopic” heat flux vector Q and the cor-
responding global temperature gradient GRAD T in the form (for a
detailed derivation the reader is referred to Appendix A):
1
grad T (x)·q (x) dV = GRAD T · Q ,
VRVE VRVE (4)
which is analogous to the so-called Hill's lemma in continuum me-
chanics [39]. The average rule presented in Eq. (4) is now applied to the
three different RVEs representing the hierarchical organization of fired
clay, see Fig. 12: (i) the RVE of porous glass (“microscale”); (ii) the RVE
of glass-embedded crystal platelets (“mesoscale”); (iii) the RVE of a
porous geomaterial with cracks (“macroscale”). As the microstructure
within the RVE is typically so complex that it cannot be described in
complete detail, it is common in the field of continuum micromechanics
or random homogenization theory to introduce material phases, i.e.
quasi-homogeneous subdomains within the RVE, over which additional
spatial averages (here of the heat flux and of the temperature gradient)
are introduced. Accordingly, all the three RVEs introduced in the con-
text of fired clay modeling, consist of one matrix phase and of Ninc fa-
milies of spheroidal inclusion phases with family-specific orientation
distribution functions Wi ( ) , with being the latitudinal Euler angle.
When introducing heat flux and temperature gradient averages over
these phases, i.e. qm , as well as qi ( , ) and (grad T )i ( , ) , with as
the longitudinal Euler angle, then the average rules for heat flux and for
the temperature gradient, (38) and (35), can be re-written to:
Ninc
sin
Q = fm qm + fi Wi ( ) qi ( , ) d d ,
4 (5)
i
as well as
Ninc
sin
GRAD T = fm (grad T )m + fi Wi ( )(grad T )i ( , ) d d .
i
4
(6)
In the sequel, we will adopt the orientation distribution function pro-
posed by Ulm et al. [59], reading as:
T. Kiefer, et al.
Fig. 1. Local coordinate system defining transveral isotropy directions (x , y , z ), with the x – y -plane being the isotropic plane, while z marks the axis of symmetry.
The local system coincides with the global coordinate system x , y, z when samples are cut from the specimen's center.
i·cosh( cos( ))
Wi ( ) = .
sinh( i )
Thereby, the preferred alignment of clay particles with respect to axis z ,
described by Bourret et al. [6] and Viani et al. [61], can be fully taken
into account by the determination of the solid angle and its dis-
tribution, being defined via the distribution parameter (Eq. (7)). As
we consider all inclusions being of spheroidal shape, uniformly dis-
tributed in the x y plane (see Fig. 5a), the orientation distribution
function is solely dependent on the angle .
2.2. Scale transition problem – upscaling of thermal conductivity
The description of the “microscopic” system (4) needs to be com-
pleted by evolution equations linking the thermodynamic force grad T
to its effect, the heat flux q . This is achieved by the introduction of the
classical Fourier's heat conduction law, reading as:
q (x) = (x)· grad T (x),
with the second-order heat conductivity tensor . In line of the material
phases introduced with Fig. 12, Eqs. (5) and (6), the version of (8)
specified for the matrix phase reads as:
qm = m·(grad T )m
and the version of (8) for the , -oriented inclusion phase of the i-th
family reads as:
qi ( , ) = i. (grad T )i ( , ).
The conductivity relations (9) and (10), together with the boundary
conditions (34) and the steady-state conditions (30) define the so-called
concentration, localization, or scale-transition problem of thermal
conductivity homogenization, inducing the existence of so-called con-
centration, localization, or down-scaling tensors Am and Ai , relating, in
a multilinear fashion analogous to the linear elastic case [39,62], the
macroscopic temperature gradient to its microscopic counterparts, ac-
cording to [37]:
(grad T )m = Am·GRAD T ,
and, respectively
(grad T )i ( , ) = Ai ( , )·GRAD T for i = 1, 2, …, Ninc.
Finally, insertion of down-scaling relations (11) and (12) into Eqs.
(9) and (10) and subsequent use in the heat flux averaging rule (5)
Journal of the European Ceramic Society xxx (xxxx) xxx–xxx
yields a macroscopic heat conduction law in the form:
(7)
Q= · GRAD T (13)
with the macroscopic (homogenized) heat conduction tensor reading
as:
Ninc
sin
= fm m· A m + fi Wi ( ) i·Ai ( , ) d d .
i
4 (14)
3. Investigated samples and material characterization
Two different clay mixtures (subsequently referred to as ‘HD’ and
‘KV’), conventually used for brick production, were investigated. Both
clays were fired at a temperature of 880 °C and 1100 °C, respectively,
representing standard firing temperatures in backing brick and tile
production. Additionally, different pore-forming additives in different
concentrations were added to clay HD880 in order to investigate the
(8)
correspondingly induced additional porous space; namely expanded
polystyrene (‘EPS’) in mass fractions of 10% and 20%, paper sludge
(‘PS’) in mass fractions of 10%, 20% and 40%, as well as saw dust (‘SD’)
in mass fractions of 10%, 20% and 40%.
Two different measurement methods have been applied to gain vi-
(9)
sual information of the material on different length scales: (i) scanning
electron microscopy (SEM) with energy dispersive X-ray spectroscopy
(EDX) for the determination of of the chemical characteristics of the
material phases (along with a preliminary powder diffraction analysis),
(10)
their volume fraction, aspect ratio, and phase orientation at a micron
length scale [42] and (ii) micro-computed tomography to identify the
volume fraction, aspect ratio, and phase orientation of pores at a scale
of some tens of micrometers to some millimeters [41]. Additionally,
mercury intrusion porosimetry measurements were conducted for the
determination of the porosity not identifiable with the aforementioned
visual measurement methods.
3.1. Sample preparation
(11)
Ceramic specimens of dimensions mm30 × 15 × 125 mm3 as well as
60 × 15 × 100 mm3 were extruded and fired at 880 °C and 1100 °C, re-
spectively. From these specimens, cuboids of dimensions
(12)
6 × 5 × 15 mm3 were cut with a distilled water cooled diamond saw
(Isomet, Buehler, USA), with the longest edge of 15 mm of the cuboid as
the thickness of the extruded specimen (see Fig. 1a). Later on, these
3
T. Kiefer, et al.
Fig. 2. Micro-, meso-, and macroporosity of all 12 investigated fired clay
samples. The macroporosity is obtained from µ -CT measurements, while dis-
tinction between meso- and microporosity is made via the relative pore size
distribution gained by the SEM micrographs, cross-checked with results from
Mercury intrusion porosimetry (MIP) measurements. While EPS and saw dust
(SD) mainly form macropores, paper sludge (PS) increases the meso- and mi-
croporosity.
samples were investigated by micro-computed tomography, allowing
for a detailed description of larger pores (and cracks) within the sam-
ples (see Fig. 4).
To investigate the morphology of the material at the micron length
scale, three samples each were cut from the extracted cuboids (see
Fig. 1), embedded in a low viscocity resin and oriented in such a way
that each surface is perpendicular to the three orthogonal directions.
Subsequently, the embedded samples are subjected to an extensive
Fig. 3. Phase distribution on SEM-EDX images. Offprint from [40].
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Journal of the European Ceramic Society xxx (xxxx) xxx–xxx
polishing protocol [41], in order to obtain the smoothest possible sur-
face [40]. This is not only to guarantee reliable results when executing
the scanning thermal microscope measurements, which require a sur-
face roughness of ∼10 nm, but also to achieve high quality images with
the SEM-EDX.
3.2. Characterization of the porous space
The overall porosity of the investigated samples was analyzed by
means of µ -CT measurements (thoroughly described in [41]), cross-
checking results with weighing tests and mercury intrusion porosimetry
analysis. Furthermore, the results of the µ -CT measurements allow for a
first assignment of the porous space to different length scales by iden-
tifying pores at a scale of some tens of micrometers up to millimeters,
enclosed by a macroscopically homogeneous clay matrix with an in-
herent microporosity, the latter being accessible by an intravoxel ana-
lysis. This inherent microporosity was further resolved based on results
from SEM images (see Fig. 3), revealing a clay matrix embedding
crystal platelets and pores ranging from half a micrometer to some tens
of micrometers. On this observation scale, pores could be detected by
converting the backscattered electron micrograph into a binary image
using Otsu's threshold. Pores smaller than half a micrometer were as-
signed as being included in the clay matrix detected in the SEM images.
The volume fraction of pores as obtained from the µ -CT intravoxel
analysis is then substracted by the volume fraction of pores detected in
the backscattered electron micrograph, thereby yielding the fraction of
pores smaller than half a micrometer.
3.3. Characterization of the phase morphology
In order to identify different material phases, scanning electron
microscopy (SEM) images using backscattered electrons in low vacuum
(Quanta 200 FEG, FEI, USA) were coupled with the information from an
energy-dispersive X-ray spectroscope (EDX) (Pegasus XM4, EDAX,
USA), as illustrated in Fig. 8a and b. More precisely, material phases
could be identified by using a conventional EDX elemental mapping on
the polished fired clay samples, resulting in distribution maps of the
commonly occurring elements, as are: aluminum, silicon, calcium,
magnesium, potassium, sodium, iron and titanium. The sample HD,
T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

fired at a temperature of 880 °C, consists of quartz, feldspar, phyllosi-

licates (where those containing iron and magnesium were segregated),
de-carbonized dolomite and a surrounding glassy matrix (see Fig. 3a).
At the higher maximum firing temperature of 1100 °C, sample HD so-
lely shows quartz, feldspar, phyllosilicates containing iron and mag-
nesium, some remaining rings of the de-carbonized dolomite and a
glassy matrix, being now much denser than before (see Fig. 3b). The
sample KV, fired at a temperature of 880 °C, contains quartz, feldspar,
phyllosilicates and a glassy matrix (see Fig. 3c). At the maximum firing
temperatures of 1100 °C the phyllosilicates dissolve (see Fig. 3d). Again,
the glassy matrix seems much denser at a higher firing temperature.
With a scanned area of ≈300 × 215 μm2 and a resolution of 512 × 400
pixel, we were able to resolve structures down to half a micrometer.
Using ImageJ [56], structures observed in the SEM could be differ-
entiated by means of the information from the EDX and assigned to a
specific material phase.

4. Microscopic characterization of RVE morphology

Regarding the hierarchical organization of fired clay, we could

identify three clearly distinguishable scales of observation, which can
be represented at three different length scales (thereby following sug-
gestions from [4,15,18,34,46], omitting the lowest scale of observation,
where single clay particles/aggregates form the clay matrix).
Fig. 4. Two representative 3D images generated from the µ -CT measurements,
4.1. Macroscale
for fired clay material with (a) 20% EPS and (b) 20% SD. Even (micro)cracks,
evolving from the macropores introduced by EPS, can be detected. Offprint
As highest scale of observation, named macroscale, a quasi-homo- from Kariem et al. [41] (CC BY 4.0).
geneous fired clay matrix with embedded macropores has been iden-
tified, where pores visible to the naked eye with a radius up to 1 mm are
morphology of clay platelets and pores embedded in a clay matrix. The
defined as macropores. Two different investigated pore-forming agents
experimental program, the evaluation, and detailed results of these
introduced such macropores, namely expanded polystyrene (EPS) and
measurements have been described and thoroughly discussed in [42].
sawdust (SD). The exact morphology could be identified using micro-
The observed inclusions were further approximated with ellipsoids,
computed tomography, by scanning a sample with dimensions of
defined by their aspect ratio as well as two solid angles. Since the
6 × 5 × 15 mm3 . The resolution of the used µ -CT was restricted to
material can be considered as transversely isotropic, only the solid
6 × 6 × 6 µm3 (1 voxel). To reduce noise, only connected pores larger
angle , as given in Fig. 5a, will be of relevance for the micromechanical
than 50 voxels were taken into consideration. Pores with a diameter
model presented in the following. As shown in Fig. 1b and c, and
larger than 30 µm (assuming an aspect ratio of the ellipsoid of 4, see
schematically illustrated in Fig. 5a, the orientation of clay platelets
Table 1) were therefore considered as macropores. Using the non-
varies around the xy -plane, which is also reported in [6,46,61]). The
commercial software ImageJ [56], ellipsoids were fitted into the pores,
preferential orientation of each type of subdomain (quartz, feldspar,
thereby yielding the solid angle (defined in Fig. 5a) as well as the
phyllosilicates, decarbonized dolomite, pores) can be taken into ac-
aspect ratio of each pore. Two representative 3D images generated from
count by calculating the distribution factor , as given in Eq. (7).
the µ -CT measurements, for fired clay material with 20% EPS and 20%
Thereby, the alignment distribution of the inclusions can be approxi-
SD, are shown in Fig. 4.
mated, as shown in Fig. 5b. Next, each aspect ratio as well as solid angle
were weighted by the volume of the associated inclusion, yielding a
4.2. Mesoscale
weighted normal distribution for both parameters and for each identi-
fied material phase. All mean values and standard deviations of these
The quasi-homogeneous clay matrix at the macroscale is then re-
distributions are given in Table 2, together with the volume fraction fr
solved at the next lower scale of observation, named mesoscale. At this
of each identified material phase.
scale, results from the scattered electron micrographs, coupled with the
elemental mapping from the EDX, give access to volume fraction and
4.3. Microscale
Table 1
Aspect ratios ar / az of identified macropores (with ar being the average value of
the two longer axes of the identified ellipsoids in the local x – y plane, see Based on high resolution SEM images, as exemplary shown in Fig. 6
Fig. 5a), weighted standard deviation of the solid angle (defined in Fig. 5a) for two different pore-forming agents, the observed glassy matrix at the
defining the orientation distribution, and the volume fraction fr of the macro- mesoscale is further resolved in a matrix embedding micropores, re-
scale porosity, obtained from µ -CT measurements. presenting the lowest scale of observation, named microscale. Since at
this scale of observation it was not possible to quantitatively evaluate
EPS 10% EPS 20% SD 10% SD 20% SD 40%
the shape and orientation of the pores, the morphological parameters
ar /a z 4.074 3.056 5.674 4.797 4.030 for the pores at the mesoscale were adopted, whereas the volume
36.11 32.81 42.81 38.84 38.39 fraction of these micropores was deduced from mercury intrusion
fr 0.0387 0.0628 0.0465 0.1067 0.1728 porosimetry measurements.

5
T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

Fig. 5. Definition of solid angle and distribution of orientation around the axis of symmetry.

Table 2 5. Identification of invariant thermal conductivities of basic

Morphological information derived from SEM-EDX measurements: Mean values building blocks
and standard deviations of aspect ratios a1/ a3 , weighted standard deviations
of the solid angles , and the volume fraction fr of the identified material phases 5.1. Derivation of phase thermal conductivity by means of scanning thermal
at the mesoscale for the four investigated fired clay samples without pore- microscopy
forming agents.
HD880 HD1100 KV880 KV1100 As outlined in [23], the determination of the thermal conductivity
of each material phase at a scale of a few micrometers is quite a chal-
Quartz a1/a3 1.722 1.867 1.769(±0.260) 1.783
lenging task. Additionally, given values in literature for the constituent
(±0.161) (±0.055) (±0.031)
35.71° 37.80° 42.26° 36.38°
phases in clay show a wide range, depending on the chemical compo-
fr 0.15765 0.15479 0.15985 0.28896 sition and purity of each and every constituent. It is therefore inevitable
Feldspar a1/a3 2.199 2.786 1.726 (±0.152) 2.816 to determine the thermal conductivities of the constituents of the in-
(±0.390) (±0.014) (±0.315) vestigated clay experimentally. A promising, and in our case the only
26.98° 30.58° 39.13° 37.37° possible, method to determine absolute values of thermal conductivities
fr 0.08563 0.04595 0.02278 0.05249
on a sub-micron length scale is the scanning thermal microscopy
Mesopores a1/a3 2.668 2.350 3.881 (±0.344) 3.671
(±0.452) (±0.383) (±0.373)
(SThM). Some authors have already shown encouraging results re-
31.02° 35.84° 39.08° 38.23° garding the determination of thermal conductivities using the SThM
fr 0.25586 0.26223 0.07834 0.09435 (see, e.g. [5,10,27,28,35,44,55]), especially for low thermal con-
Dec. dolomite a1/a3 1.664 – – – ductivities [49] (in a range of 0.1–20 W/mK [28]). The basic procedure
(±0.149) is to heat a small tip moving over a flat surface and measuring the
29.80° – – –
energy needed to keep the tip at a constant temperature, which can be
fr 0.07479 – – –
determined via the electric resistance of the wire.
Phyllosilica a1/a3 6.414 – – –
(±1.508)
For the derivation of absolute values of the thermal conductivity of
23.96° – – – the investigated material it is necessary to define a calibration standard,
fr 0.06984 – – – as the heat flux between the heated tip and the sample is affected by
Fe–Mg-phyllosilica a1/a3 7.137 7.771 5.078 (±0.819) - various parameters, such as contact radius, heat transfer to the sur-
(±1.887) (±0.152) rounding air by convection [27], near-field radiation, and liquid con-
16.58° 26.57° 34.91° –
duction [49]. To determine the thermal conductivity, we apply the
fr 0.01688 0.01502 0.03601 -
relation proposed by Fischer [28], reading:
matrix fr 0.33935 0.52201 0.70302 0.56420

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T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

Fig. 6. SEM images of two different fired clay samples, giving access to the structure of the microscale, which is further represented by a continuous matrix with
embedded ellipsoidal pores. The matrix of the sample with 40% SD shows less micropores than the one with 40% PS.

Table 3 Bruker Dimension Icon AFM, coming along with a Anasys Instruments
Calibration materials for SThM measurements and their thermal nano-TA SThM, equipped with Bruker VITA-DM-GLA-1 probes with a
conductivities. tip radius < 100 nm, operating in DC mode. Recalibration of the in-
Material Thermal conductivity [W/mK] strument is needed in brief intervals, as the control signal Vs Vr (the
resistance in the sample probe is determined by comparison with a
PMMA 0.19 variable resistor) shows some baseline signal after a certain testing
SiO 2 (fused) 2.00
time. This baseline skip in the controlling current is recorded and the
Al 2 O 3 30.0
Cu 300 acquired data is adjusted accordingly. A calibration curve corrected by
the baseline signal, which in case of recalibration is near to zero, is
shown in Fig. 7.
A g All samples as well as the calibration materials were embedded in
Q= ,
B+ g (15) an epoxy resin and polished according to the same protocol, resulting in
surface roughnesses (RMS) between 2 and 20 nm , determined via AFM
where Q denotes the heat flux from the probe, g is the generalized in contact mode [40]. According to Fischer [28], very stable results for
thermal conductivity given by 1/ g = 1/ s + 1/ p (where s denotes the samples with a low thermal conductivity can be estimated for a
thermal conductivity of the sample, and p is the thermal conductivity roughness of less than 10 nm . As the SThM probe measures the mor-
of the probe), and A and B denote calibration parameters. The two phology of the surface simultaneously, regions with a higher roughness
parameters A and B were determined based on measurements of four than required could be identified and excluded.
different calibration materials with well-known thermal conductivity, When the phase composition on a surface area is known, we can
listed in Table 3. The used device for the SThM-measurements was a scan this specific area (strictly speaking: snippets of this area) with the

Fig. 7. Calibration curve (heat flux Q as a function of the thermal conductivity ) for SThM measurements, determined by means of the four calibration materials
(x) given in Table 3. Coefficient of determination R2 = 0.99953.

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T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

Fig. 8. (a) Exemplary SEM image of sample HD1100 at a firing temperature of 1100 °C, (b) identified material phases by means of the information from EDX, along
with an SThM picture gained for a small area within the sample (c). (d–f) Exemplary results for the voltage needed to keep the SThM tip at a constant temperature,
showing inclusions of different material phases embedded in the matrix phase.

Table 4
SThM results: mean values and associated standard deviations of thermal conductivities for the different material phases identified in the investigated fired clay
samples.
HD880 HD1100 KV880 KV1100
[W/mK] [W/mK] [W/mK] [W/mK]

Quartz 1.085 (41.01%) 0.958 (26.0%) 1.048 (43.2%) 1.351 (29.9%)

Feldspar 0.820 (31.6%) 0.788 (39.0%) 0.825 (14.1%) 1.008 (39.5%)
Matrix 0.730 (22.8%) 1.368 (8.5%) 0.657 (18.9%) 0.909 (19.0%)
Dec. dolomite 0.845 (16.2%) – – –
Phyllosilica 0.780 (28.9%) 0.933 (32.0%) 0.712 (16.3%) –
Fe–Mg-phyllosilica 0.788 (21.6%) – – –

SThM. Scanning larger areas proved to be difficult, as a combination of
a large area and a high resolution resulted in long measurement per-
iods, which makes it impossible to check for the occurring baseline shift
in the control signal Vs Vr . Therefore, mostly smaller areas with a size
of 8 × 8 µm2 were measured, allowing for a check every two minutes.
SThM results on quartz and feldspar are shown in Fig. 8c, while
Fig. 8d–f show results for different inclusions embedded in the matrix.
The mean values and associated standard deviations for the determined
thermal conductivity of each material phase are given in Table 4.
Considering the volume affected by the heat of the SThM tip, respec-
tively the penetration depth of the heat load governing the signal re-
ceived by the SThM probe, we arrive at a critical length of at least
15–30 μm (see Section 5.2) in order to ensure the result being measured
to be predominantly governed by the thermal conductivity of the tar-
geted inclusion. This requirement holds for the larger quartz, feldspar
and decarbonated dolomite grains, but could be violated especially in
case of the phyllosilica, where the result could be affected by nearby
pores or the surrounding matrix. Plus, the depth of each targeted in-
clusion is unknown, so results still could be affected by surrounding
phases, even if the requirement of a minimum size is fulfilled. In case of
the quartz grains, the identified thermal conductivities show com-
paratively low values with respect to values found in literature (ranging
from 2 W/mK [28] up to 7 W/mK [14]), which can be explained by
microcracks and corresponding imperfect interfaces within the quartz
grains, a result of the thermal expansion mismatch between quartz and
matrix during the transition of the quartz’ crystal system in the firing
process at 573 °C [1,43] (see also Fig. 3d). Now, if the cracks in the
quartz grains are small enough to meet the requirement dRVE lRVE ,
then the measured value obtained by the SThM probe would be the
homogenized thermal conductivity of a quartz grain with a network of
microcracks. Taking into account the requirement of the seperation of
scales, dRVE lRVE , with lRVE = 15 30 µm d quartz (the

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T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

Fig. 9. Calculated heat penetration depth of the SThM tip.

requirement dRVE lRVE being fulfilled for a ratio of

lRVE/dRVE = 1.5 3), we can assume that the measured values actually
can be considered as the “effective” thermal conductivity of the mate-
rial phase. Thereby, no imperfect interphases have to be considered in
Fig. 10. Plot of the temperature over its partial derivative T / grad T in the
the multiscale material model for the quartz grains, nor are such in-
plane perpendicular to the movement of the SThM tip, exemplary on sample
cluded for the other material phases, as images obtained by the SEM do HD880.
not indicate a debonding between grains and surrounding matrix.

a= ,
5.2. Back-calculation of the thermal conductivity of the fired clay matrix c (18)

where the thermal conductivity of the sample can be derived from the
Regarding the identification of the thermal conductivity of the
SThM measurements. Plotting the obtained temperature distribution
matrix at this scale, we had to consider that the penetration depth (load
over its partial derivative yields the characteristic length of the loading
of structure, see Fig. 9) of the SThM is, according to [60], within the
of the structure (see Eq. (1)), resulting in the distribution shown in
range of tens of micrometers. The measured results with the SThM are
Fig. 10 in the xy -plane around a tip located at the center.
therefore affected by embedded pores. For this reason, the following
As apparent in Fig. 10, the characteristic length of the loading of the
approach was chosen: In a first step, we calculated the penetration
structure is not constant in throughout the sample. However, its mean
depth of the SThM, determining the characteristic length of the load of
value for the exemplary sample HD880 can be estimated to be around
the structure . From this characteristic length we could derive the
150 µm . Considering the separation of scales principle, d l ,
volume fraction of pores affecting the SThM measurements of the ma-
[22,54] as well as [45] give some quantitative estimates for a minimum
trix phase. Then, the Mori–Tanaka scheme was used to back-calculate
RVE size. For the ratio of the characteristic length of the loading
the thermal conductivity of the matrix at the microscale, with the
compared to the size of the RVE, /lRVE , a factor of at least 5 10 [45]
homogenized thermal conductivity Khom given by the SThM results.
is reported, whilst the ratio of the size of the RVE to the characteristic
For the estimation of the heat penetration depth, the following so-
length of an inhomogeneity, lRVE/dRVE should be greater than 1.5 3
lution for the temperature distribution T (x , y , z , t1) under a moving heat
[22,54]. With a characteristic length of the loading of 150 µm , we
point source, given by Carslaw and Jaeger [11] (adjusted to the semi-
therefore arrive at the length scale of the RVE at the microscale (see
infinite solid), was used:
Section 4.1, Fig. 12). Therefore, the thermal conductivity gained
[{x v·(t )}2 + y 2 + z 2]/[4a (t )] through SThM measurements can be considered as the homogenized
q t e
T (x , y, z, t1) = · d , thermal conductivity of our RVE on the smallest scale of observation.
4 c( a)3/2 0 (t )3/2
Based on these assumptions, the actual thermal conductivity of the
(16) matrix at the microscale can now be back-calculated by means of a
Mori–Tanaka homogenization scheme, (47):
where q denotes the release of heat per unit time by the SThM probe, v
the movement speed, the density, c the heat capacity and a the
={fm m
thermal diffusivity of the sample. In our case, q = 4 mW and
1 sin
v = 7.5 µm/s , while the density has to be determined in an iterative + fpore Wpore ( ) pore [1 + Ppore ( )·( pore m)]
4
d
.
process, because the heat penetration depth determines the amount of d }
pore space which needs to be taken into account, itself affecting the
× {fm + fpore Wpore ( )[1 + Ppore ( )·( 1 sin 1
density of the sample. For the bulk density the effective parameters are m)] d d }
(19)
pore
4
given by:
The volume fractions are determined as follows: the micropores are
composite = fmatrix · matrix + fpores · pores , (17) embedded in the clay matrix, therefore the value for the microporosity
given in Fig. 2 has to be referred to the volume fraction of the matrix,
with matrix = 2.7 kg/dm3 as the density of the fired clay matrix [41]. with f micro
pores,rel.
as the volume fraction of pores on the microscale and
The heat capacity of the glassy clay matrix, with a high amount of f meso as the volume fraction of the matrix phase on the mesoscale:
matrix
Al 2 O 3 and SiO 2 [42], is assumed to be mainly driven by these two
constituent phases, which themselves have a heat capacity of pores
pores,rel.
f micro
f micro = .
c Al2O3 = 775 J/kg K [58] and cSiO2 = 740 J/kg K [12], respectively. We matrix
f meso (20)
therefore estimate the heat capacity of the glassy clay matrix to be
approximately cm = 750 J/kg K . The thermal diffusivity in Eq. (16) reads Results for the investigated fired clay samples without pore-forming
as: agents are given in Table 5.

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T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

Table 5 RVE on different length scales. The identification of these parameters

Back-calculated isotropic thermal conductivities of the matrix at the microscale has been described in the previous sections. The thereon based multi-
for four different fired clay mixtures without pore-forming agents. scale model for fired clay (illustrated in Fig. 12) is described in the
HD 880 HD1100 KV 880 KV 1100 following, starting with the lowest scale of observation, referred to as
microscale.
Thermal conductivity matrix [W/m K] 1.41 1.51 1.03 1.11

5.3. Verification experiments to determine the effective thermal conductivity
of the investigated fired clays
The effective thermal conductivities of the investigated fired clay
samples were measured using a guarded heat flow meter apparatus,
which is a steady-state measurement device operating with the two-
thickness method, thereby able to exclude the thermal contact re-
sistance from the total thermal resistance. The design of the measure-
ment device follows the ASTM E1530-06 “Standard Test Method for
evaluating the resistance to thermal transmission of materials by the
guarded heat flow meter technique”. Its high resolution regarding
temperature measurement ( 0.01 K ), sample thickness determination
( 0.025 mm ), and temperature stability of the heating plates ( 0.02 K )
allows for a precise determination of the thermal conductivity.
According to the manufacturer, the maximum error is limited to 3% .
The thermal contact resistance R can be derived from multiple thick-
ness measurements via:
R=
(U2·d2 U1·d1 ) T
, minimum size of 20 µm , so we expect the measured thermal con-
U1·U2· Scal (d2 d1 )
where U denotes the voltage measured in the thermocouple, d the
thickness of the sample, and T the temperature difference between the
heating and the cooling plate. Scal [W m 2 µV 1] is a calibration factor
linking the measured Voltage U in the thermocouple with the actual
heat flow q . The measured values (MV), the number of samples (nu.) as
well as the standard deviation (SD) for the thermal conductivity mea-
sured in the anisotropy direction z are given for each sample in
Table 6. Regarding the thermal conductivity in the isotropy plane, only
two measurements were conducted due to a difficult sample prepara-
tion: as the diameter of the disks to be tested in the guarded hot plate
apparatus exceeds the thickness of the extruded specimens by a factor
of 3, three disk specimens had to be glued together (see Fig. 11b).
From these blocks, disks with a circular shape were cut (see Figure
11a). In order to determine the effect of the bond seam, four HD880
samples were measured, cut, glued together and measured again. From
these tests, an error of to the thermal conductivity of 5% could be
estimated, which is subsequently used to correct the results for samples
HD880 and SD20, for which the thermal conductivities in the isotropic
plane were determined. The corrected results are displayed in Fig. 15.
6. Multiscale material model
6.1. Microscale
The microscale is represented by an RVE with a characteristic length
of ∼10 μm, composed of a matrix embedding micropores, proposing
the Mori–Tanaka scheme as an appropriate homogenization method. As
no detailed information about the morphology of the micropores could
be deduced from SEM images (see, e.g. Fig. 6), we assume them to be of
the same shape as the pores at the mesoscale.
6.2. Mesoscale
At the next higher scale of observation, the mesoscale, the homo-
genized material described at the microscale is now forming a new RVE
with a size of l meso 300 µm , with the other constituent phases listed in
Table 2 embedded, showing characteristic lengths of d 0.5 20 µm .
Again, a contiguous matrix embedding constituent phases allows for the
use of a Mori–Tanaka homogenization scheme.. Besides the matrix, all
inclusions for which SThM measurements were conducted had a
(21) ductivities not being seriously affected by the surrounding material
and, thus, they can be assigned to the inclusion material exclusively. As
the volume fraction of the mesoporosity depends on the pore-forming
agent, the volume fractions of the solid constituents (given in Table 2)
are scaled in a way that the control volume stays constant.
6.3. Macroscale
The highest scale of observation, the macroscale, is build up by a
continuous matrix represented by the material described at the me-
soscale. The embedded macropores are formed by EPS and SD and
exhibit a characteristic length of d 20 µm 1 mm . The defined RVE
with a size of l 10 mm , thus, again allows for the use of a Mori-Tanaka
homogenization scheme, taking into account the ellipsoidal macropores
along with their orientation distribution according to the P-tensor de-
fined in Eq. (41). Additionally, EPS spherules as pore-forming agents
induce macrocracks into the material. Those cracks are taken into ac-
count as flat penny-shaped ellipsoids with an aspect ratio = c /r , as
perceptible from Fig. 4. Based on the μ-CT images, the radius r and
thickness c of the macrocracks is identified, allowing for the determi-
nation of the P-tensor as well as the crack volume fraction, given in
[8,9,21] to:

4 2 4
Setting up the multiscale model requires the determination of the fcr = rc= d,
3 3 (22)
following parameters for each material constituent: (i) the thermal
conductivity, (ii) the volume fraction, (iii) the aspect ratio, and (iv) the where is the amount of cracks in a unit volume, and d = r 3 denotes
orientation distribution of non-spherical inclusions for each and every the crack density.

Table 6
Mean values, standard deviations, and the number of different thickness measurements taken into account by the macroscopic measurements of the thermal
conductivity in the anisotropy direction z by the Guarded hot plate apparatus. Most results are based on at least four different thicknesses and show only little
deviations. Mean values and standard deviations are given in [W/mK].
HD880 EPS Paper sludge (PS) Saw dust (SD) HD KV KV

10% 20% 10% 20% 40% 10% 20% 40% 1100 880 1100

MV 0.475 0.430 0.346 0.460 0.374 0.282 0.461 0.385 0.271 0.771 0.438 1.042
SD 0.006 0.002 0.003 0.006 0.000 0.005 0.001 0.003 0.003 0.012 0.019 –
nu. 5 4 3 4 4 4 4 4 4 5 5 2

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T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

Fig. 11. Preperation of specimens for measurements of the thermal conductivity in the isotropy plane.

7. Sensitivity analysis uses metamodels to approximate the model response, based on poly-
nomial regression analysis. As the most important result, the so-called
The proposed multiscale material model is finally coupled with a coefficient of prognosis (CoP) [51], a model independent measure able
probabilistic scheme to identify the model variables with the highest to determine the quality of the metamodel of optimal prognosis, is
influence on the model response, the effective thermal conductivity of obtained, given by:
the investigated fired clay samples. Therefore, sensitivity analysis tools
implemented into the commercial software optiSLang™ were used. To SSPrediction
E
CoP = 1 ,
apply these tools, the design space, build up by all input parameters of SST (23)
the developed multiscale material model, needs to be scanned, and by a
where SSPrediction denotes the sum of the squares of the prediction errors
Latin Hypercube Sampling scheme, which is recommended in [52] for E
with regard to the model response for the probabilistic design set of
high-dimensional design spaces, an appropriate set of discrete realiza-
input parameters, and SST denotes the total variation of the model re-
tions is generated. Using this kind of sampling normally allows to not
sponse, both determined via cross validation.
only obtain reliable results for a relatively small number of discrete
Using the CoP, the single input parameters contribution Xi to the
realizations, but also undesired correlations between input parameters
model response can be calculated as:
tend to be avoided. The sensitivity/importance of each input parameter
with respect to a certain result of the multiscale material model (e.g. the CoP(Xi ) = CoP· STMOP (Xi ), (24)
effective thermal conductivity) is then computed by optiSLang, which
with STMOP (Xi ) as the total effect sensitivity index.

Fig. 12. Multiscale material model.

11
T. Kiefer, et al.
Fig. 13. Comparison of experimentally-obtained effective thermal con-
ductivities (crosses) to results from the proposed multiscale material model
(circles), for 12 different fired clay samples. Additionally, the mean values and
standard deviations of the effective thermal conductivities, computed on the
basis of a 200 realizations large input parameter set for each sample, are given.
Thereby, the design space of input parameters is constrained by the estimated
measurement inaccuracies of the identification experiments.
8. Model validation
In the following, results from the multiscale material model are
compared to the experimental values from macroscopic measurements.
The homogenized thermal conductivity is given in the anisotropy di-
rection for all 12 samples, values for the isotropic plane are available
for two samples only (see Fig. 15), due to the difficult sample pre-
peration and uncertainties in the consideration of the bond seam.
However, values for the ratio of the perpendicular directions show si-
milar results compared to measurements conducted by Erker [25].
Macroscopic measurements of the effective thermal conductivity were
conducted on twelve different specimens (see Table 6), and for each
specimen different thicknesses were investigated to determine the
thermal contact resistance. The experimentally-obtained effective
thermal conductivities are compared with predictions of the multiscale
model in Fig. 13. Additionally, mean values and the standard deviations
for the effective thermal conductivities are given, obtained by the
performed sensitivity analysis by varying the input parameters of the
multiscale model in the range of possible measuring inaccuracies. The
Fig. 14. Cross Section of KV880, showing a strongly differing body structure over thickness. Multiple thickness measurements show a decreasing thermal con-
ductivity at the edge.
12
Journal of the European Ceramic Society xxx (xxxx) xxx–xxx
agreement between experimental values and model predictions is very
satisfying, especially when considering that no calibration of the mul-
tiscale model with respect to these experimental results has taken place.
Only the thermal conductivity of sample KV880 is significantly
overestimated by the model. This could be traced back to a strongly
varying body structure over its thickness, and measurements conducted
on samples with varying thickness indicate that the core of the sample
has a considerably higher thermal conductivity than the edge (see
Fig. 14). As the samples for the scanning thermal microscopy were cut
out from the core of the extruded body, this might be an explanation for
the unsatisfactory results of this specific sample.
8.1. Influence of different pore spaces and transversal isotropy
With the validated model, the driving question about the perfor-
mance of different pore-forming additives may be answered by in-
vestigating the response of the model due to additional pores arising on
different levels of observation (with PS forming micro- and mesopores,
SD forming meso- and macropores, and EPS forming macropores so-
lely). Therefore, porosities at all three scales of observation were in-
creased separately, based on the morphology of the HD880 sample
without pore-forming agents at a firing temperature of 880° . The ob-
tained results are shown in Fig. 15 and compared to experimental re-
sults for PS and SD (EPS is not considered because of the arising mac-
rocracks, which would introduce an additional degree of freedom). The
trends depicted in Fig. 15 were additionally compared to analytical two
phase mixture models, namely a modified Maxwell–Eucken model [48]
and the Landauer relation [47,57]. Both models estimate the thermal
conductivity when incorporating porosity in an isotropic, homogeneous
material. While the Maxwell–Eucken model assumes the pores being
dispersed uniformly in the material, representing closed porosity, the
Landauer relation based on the effective medium percolation theory
assumes connectivity of the pores. Comparing results from the multi-
scale model to those from the simplified approaches reveals the benefits
of a multiscale model, taking the complex morphology into account,
thereby not only being able to predict transversal isotropic thermal
conductivities, but furthermore matching results from measurements
accurately by a homogenization scheme over several scales of ob-
servation.
Regarding the obtained results shown in Fig. 15, we can state that
micro- and mesopores have a significantly higher effect on the reduc-
tion of the thermal conductivity, compared with macropores.
8.2. Sensitivity analysis
A sensitivity analysis for the multiscale material model has been
performed to determine the parameters with the highest impact on the
thermal conductivity, and to identify with the given standard devia-
tions of measured values those parameters introducing the major un-
certainties into the model. The latter results are based on 200 discrete
T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

Fig. 15. Transversely isotropic thermal conductivities versus pore volume fraction. Measurements on paper sludge samples (inducing micro- and mesopores) almost
perfectly match the values predicted by the multiscale material model, while measurements on samples with saw dust as pore-forming agent (inducing meso- and
macropores) indicate that with rising pore volume fraction the effect of additional mesopores becomes more dominant. The upper and lower bounds as predicted by
the modified Maxwell–Eucken and the Landauer relation, assuming an isotropic, homogeneous medium, fail to predict the thermal conductivities with higher
porosity accurately, not taking into account the pore distribution over several scales of observation and the effect of oriented inclusions.

realizations, covering the design space using an advanced hypercube Table 7

sampling scheme. To estimate the upper and lower bounds of the
multiscale material model with regards to the measurement errors (see
Table 2 and 4), their range is defined within optiSLang, allowing for a
determination of a standard deviation of the model response, see
Fig. 13.
However, the determination of the effect of each and every input
parameter on the overall model response is based on a design space
generated by a standard deviation of 10% on all input parameters, so
the effect of all parameters, independent from their measurement de-
rivation, can be assessed. Exemplary, the Metamodel of Optimal
Prognosis (MOP), the Coefficient of Prognosis (CoP) and the corre-
spondent deviations from the actual response of the multiscale material
model with regards to the MOP are discussed for sample HD880.
Taking the 10 most significant input parameters into account (from
initially 27), the CoP for the MOP, approximating the model response,
shows a very promising result of 97.72%. This does not only clearly
indicate that the model response can be dedicated to a restricted set of
input parameters, but also that the approximating model is capable to
yield highly reliable results in the given range of the input parameters,
therefore being a suitable tool allowing for case studies within rea-
sonable computing time. Deviations from the predicted values com-
pared to the model response from the multiscale model are depicted in
Statistical data for the metamodel of optimal prognosis,
refer to Figure 16
Statistical data
Maximum error 0.01264
Mean error 0.00327
Root mean square error 0.00407
Fig. 16, along with the correspondent statistical data in Table 7.
Finally, values for the CoP of every input parameter for every
sample are given in Table 8, showing the good approximation of the
multiscale model response by the MOP. Additionally, those input
parameters having the most significant effect on the model response can
be identified clearly.
9. Conclusion
Within this work, a multiscale material model for the prediction of
the transversely thermal conductivity tensor of brick ceramic bodies
with complex pore structures at different scales of observation has been
presented. The model has been validated by means of two different
fired clay mixtures fired at two different maximum temperatures and

Fig. 16. Deviations of the actual model response compared to predicted values from the Metamodel of optimal prognosis.

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T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

Table 8
Coefficients of Prognosis in [%] in ascending order for all investigated samples, summed up to the model CoP taking the 10 most significant para-
meters into account (last line). It applies to all samples that only 3–4 parameters are heavily contributing to the effective thermal conductivity, which
are the volume fraction of micro- and mesopores as well as the thermal conductivity of the matrix. In contrast, the macroporosity seems to have only
little effect on the effective thermal conductivity, keeping in mind the volume fraction of 17.28 % (see Table 1) of sample SD40.

for eight different mixtures containing three different pore-forming
agents. Based on the results presented, the following main conclusions
can be drawn:
1. The measurement of thermal conductivities of the constituent
phases with a Scanning Thermal Microscope has been performed on
brick ceramic bodies for the first time, yielding reproducible results
within acceptable deviations. Along with the results from mea-
surements for the determination of the complex microstructure on
different length scales an extensive data set is available, whereupon
the proposed multiscale model could be developed.
2. The multiscale material model has been validated by means of
macroscopic measurements of the thermal conductivity for a set of
12 different brick ceramic bodies. For all these 12 different samples,
the predicted effective thermal conductivity is in good agreement
with macroscopic measurements, without introducing any empiri-
cally-determined calibration parameter.
3. The validated model allows to link certain (micro)structural char-
acteristics to the effective thermal conductivity of brick ceramic
bodies, and in this way gaining a physically-based understanding of
how this kind of material could be optimized. E.g. introducing
micro- and mesopore structures seems to be much more effective to
improve the effective thermal conductivity than introducing mac-
ropores.
4. By identifying the most influential parameters on the effective
thermal conductivity by using sensitivity analysis, valuable in-
formation could be generated based on the developed multiscale
model, which will be directly applicable by the industry within
product development and optimization strategies.
Conflict of interest
None declared.
Acknowledgments
The authors gratefully acknowledge the financial support of the
Austrian Research Promotion Agency (FFG, project number 843897)
and the industry partner Wienerberger for funding the research work
within the project “Innovative Brick”. We would also like to thank Mr.
Coriand, Leoni AG, and Mr. Giester, University of Vienna, for supplying
calibration materials. Jerome Colson and Laurin Andorfer from the
University of Natural Resources and Life Sciences is thanked for their
guidance on the Scanning Thermal Microscope.

Appendix A. Laws of thermodynamics - Heat flux averaging

In the absence of local volumetric heat source terms and of remarkable work done by mechanical forces, the “microscopic” heat flux vectors fulfill
the local form of the first law of thermodynamics [16,36,38]:
e = div q, (25)
with the “microscopic” internal energy density e , being standardly decomposed into the free (Helmholtz) energy and the product of entropy
density s times (absolute) temperature T :
e= + T s. (26)
The physical quantities appearing on the right-hand side of (26) enter the Clausius–Duhem inequality, stating that the (microscopic) dissipation
needs to be non-negative,

14
T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

q
= sT · grad T 0.
T (27)
Expression (27) needs to be fulfilled for any temperature evolution T or grad T ; with grad (·) = (·)/ x being the microscopic gradient and x
referring to the microscopic position vector labeling points within the RVE. Considering the free energy to be (remarkably) dependent only on the
temperature (and not on deformation, chemical reactions and other phenomena which are typically associated with “material behavior”), i.e.
= (T ) , the requirement (27) immediately implies the standard state equation for the entropy, reading as:

s= .
T (28)
Subsequent insertion of (26) into (25), while considering (28), yields:
sT = div q, (29)
so that for steady state conditions, with vanishing temporal derivatives, in particular T = 0 , we arrive at:
div q = 0. (30)
Adopting the strategy outlined in the context of the method of virtual power introduced by Germain [31] and in analogy to the procedure outlined in
[17] for mass flux problems, we multiply the “equilibrium condition” (30) by a “virtual”, i.e. arbitrary, continuous temperature field T (x) , and
integrate over the volume of the RVE, VRVE ,

x VRVE: T (x)[div q (x)]dV = 0.

VRVE (31)
The term on the left-hand side of Eq. (31) is then considered as one of the terms associated with the application of the chain rule to the term
div [T (x) q (x)], yielding:

div[T (x) q (x)]dV = T (x)[div q (x)]dV + grad T (x)· q (x) dV .

VRVE VRVE VRVE (32)
Specification of (32) for (30) and applying the divergence theorem to the left-hand side of Eq. (32) finally yields:

[T (x) q (x)· n (x)]dS = grad T (x)· q (x) dV ,

VRVE VRVE (33)
with VRVE as the boundary of the RVE. In analogy to contributions targeting mass flux problems [17,20] a homogeneous macroscopic temperature
gradient GRAD T is prescribed at the boundary of the RVE, in the form of a microscopically resolved temperature field reading as [32]:
x VRVE: T (x) = GRAD T · x. (34)
Expression (34), together with the divergence theorem applied the scalar temperature field, induces a temperature gradient averaging rule in the
form:
1 1
VRVE grad T (x) dV = T (x)· n dS
VRVE VRVE VRVE

1
= GRAD T · (x n) dS
VRVE VRVE

1
= GRAD T · 1 dS = GRAD T .
VRVE VRVE (35)
Furthermore, insertion of (34) into the left-hand side of (33) yields:

grad T (x)· q (x) dV = (GRAD T ·x)[q (x)·n (x)]dS

VRVE VRVE

=GRAD T · [x q (x)] n (x) dS

VRVE

=GRAD T · q (x) dV .
VRVE (36)
Defining a macroscopic heat flux vector as the quantity which performs power on the macroscopic temperature gradient, we have:

VRVE GRAD T · Q = grad T (x)·q (x) dV ,

VRVE (37)
which leads to an averaging rule for the heat flux reading as:
1
Q= q (x) dV .
VRVE VRVE (38)
Use of this average rule in relation (36) yields a power averaging rule for heat flux problems in the form:
1
grad T (x)·q (x) dV = GRAD T · Q .
VRVE VRVE (39)

Appendix B. Derivation of the concentration tensor

The concentration or down-scaling tensors Am and Ai ( , ) are now estimated from the so-called matrix-inhomogeneity problem (pioneered for
the linear elastic case by Eshelby [26]), which relates the (homogeneous) temperature gradient in a spheroidal inclusion with thermal conductivity
IH embedded in an infinitely extended (transversely isotropic) matrix with thermal conductivity m , according to:

15
T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

(grad T ) IH = [1 + PIH ( )·( IH m)]

1: GRAD T , (40)
whereby measures the angle between the axis of transverse isotropy of the matrix and the rotational symmetry axis of the spheroid, and 1 as the
2nd order identity tensor. The form of the interaction tensor PIH was determined in [32], and reads as:
2
PIH ( ) = p ( , , ) sin( ) d d .
=0 =0 (41)
For the numerical determination of this integral, we refer to the C.
The temperature gradients in the inclusion phases are now approximated by those associated with inhomogenenities of the same shape, ac-
cording to
(grad T )i ( , ) = [1 + Pi ( )·( i m)]
1: GRAD T , (42)
and similar reasoning for the matrix phase leads to the choice
(grad T )m = GRAD T . (43)
Use of (42) and (43) in the temperature average rule (6) yields a relation between the macroscopic temperature gradient subjected to the RVE,
GRAD T , and the auxiliary temperature gradient (GRAD T ) associated with the infinitely remote boundary of the inhomogeneity problem, reading
as:
Ninc
GRAD T = fm + fi Wi ( )[1 + PIH ( )·( 1 sin
i m)] d d : GRAD T ,
i
4 (44)
Insertion of (44) into (42) and (43) yields the concentration tensors of the so-called Mori-Tanaka scheme [3,50] in the form:
Ai ( , ) =[1 + PIH ( )·( i m)]
1

Ninc
×[fm + fi Wi ( )[1 + PIH ( )·( 1 sin 1
i m)] d d ]
i
4 (45)

Ninc 1

Am = 1 · fm + fi Wi ( )[1 + PIH ( )·( 1 sin

i m)] d d
i
4 (46)
and use of (45) and (46) within the expression for the homogenized thermal conductivity (14) yields the sought explicity expression for the latter,
reading as:
Ninc
={fm + fi Wi ( ) 1 sin
m i [1 + PIH ( )·( i m)] d d }
i
4
Ninc
× {fm + fi Wi ( )[1 + PIH ( )·( 1 sin 1
i m)] d d }
i
4 (47)

Appendix C. Detail on the derivation of the P-tensor

The derivation of the Hill tensor P for the effective thermal conductivity of transversely isotropic media with oriented ellipsoïdal inclusions has
been done by Giraud et al. [32], and is given here in a short form for the sake of completeness. The Hill tensor is given to (see Eq. (41)):
Pij 1 2
= W ( ) Pkl Q ki Q lj
4 =0 =0

× sin d d
i, j , k , l [1, 2, 3]. (48)
Pkl denotes the oriented P-tensor, and Qki , resp. Qlj denote the rotation matrix, which reads:

cos( ) sin( ) 0
Qki = Qlj = cos( )sin( ) cos( )cos( ) sin( ) .
sin( )sin( ) sin( )cos( ) cos( ) (49)
Pkl is the Hill tensor dependent on the angle . It is given to:
2
Pkl ( ) = pkl ( , , )·sin( ) d d ,
=0 =0 (50)
and can be numerically integrated by:
NG NG

Pkl ( ) = wiG wGj pkl ( , G

i ,
G G
j )·sin( j ),
i=1 j =1 (51)
where wiG , i ,
G
wGj and j are the Gauss–Legendre
G
weights and coordinates on the interval [0, ]( ) and [0, ]( ) , for N G
resp. N G
points. The
interaction tensor pkl ( , i , j ) is given to:
G G

16
T. Kiefer, et al. Journal of the European Ceramic Society xxx (xxxx) xxx–xxx

f gi ( )
pkl = d
zj g (52)
with
z1 1 + z2 2 z3 3
f = + ,
a2 a2 2 (53)
where z1, z2 and z 3 denote the coordinates of an ellipsoid in a Cartesian coordinate system, with a being the semi-length in plane z1 z2 , and z 3 being
the symmetry axis, = a3/ a representing the aspect ratio of the ellipsoid. The unit vector and solid angle d are defined in spherical coordinates:

1 = sin cos
2 = sin sin
3 = cos (54)

d = sin d d , [0, ], [0, 2 ] (55)

The components of f / z j therefore become:

i
fi = a2 , i [ 1, 2]
f3
= 23 2
a (56)
The components gi ( ) and g are given to:
i
gi ( ) = , i [1, 2]
4 2
0( 1 + 2
2 + 2 2 )3/2
3 (57)

3
= ,
g3 ( ) 4 2
0( 1 + 2
2 + 2 2)3/2
3
g 1 + 2 3
= + ,
a2 a2 2
(58)
where denotes the ratio of transversal orthotropic thermal conductivities in the surrounding medium, =
2
i/ 0 , i [1, 2], and 0 being the
thermal conductivity along the symmetry axis. For a more detailed description of the derivation of the interaction tensor, see [32].

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