International Journal of Thermal Sciences 185 (2023) 108063

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International Journal of Thermal Sciences

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

Combined transient 3D simulation and experimental methods to assess a

slow heat-up curve used to dry a refractory concrete
J. Juárez Trujillo a, b, *, J.A. Castro b, M.D.M. Innocentini c, F. Vernilli a
a
Universidade de São Paulo, EEL/DEMAR, Lorena, 12600-970, Brazil
b
Universidade Federal Fluminense, EEIMVR/PPGEM, Volta Redonda, 27255-125, Brazil
c
Universidade de Ribeirão Preto, CCET, Ribeirânia, 14096900, Brazil

A R T I C L E I N F O A B S T R A C T

Keywords: Explosive spalling is a major concern when drying refractory concretes. For safety, empirically defined over­
Refractory drying estimated slow heat-up curves are used in industry. Polypropylene fibres reduce spalling; however, they are
Heat-up curve inconvenient for certain castables due to properties deterioration, such as slag penetration. There is neither a
Moisture migration
generally accepted methodology to define monolithic refractories dry-out schedules nor agreement about a
Pore pressure
Permeability
mathematical model to predict spalling phenomena. This paper presents original numerical and experimental
results of castable drying investigation using slow heating. Modifications in experimental methods were made to
reproduce refractory lining boundary conditions. A conservative fully implicit finite volume method in three-
dimensions was developed to predict pressure and moisture migration. The influence of the methods used to
characterize the properties needed for the mathematical model was discussed. The combined analyses suggest
that the first holding time used was not productive for drying; however, its effect on curing must be reviewed.

1. Introduction
In industrial installations, large refractory monoliths are used to
produce and convey hot fluids while protecting an external steel shell
that holds them. These complex, large scale structures must be moulded,
cured, and dried within an ample range of temperatures, usually above
550 ◦ C [1]. Drying out new refractory linings is a time-consuming pro­
cess that uses heat to remove the mass of free and chemically combined
water remained in the concrete after moulding and curing. It is intended
to optimize the drying operation to reduce downtime, energy con­
sumption and pollution. The problem is that concrete heating presents
the risk of cracks or explosive spalling. Therefore, the thermal stresses
must be controlled while providing time for the water vapour to escape
without raising the internal pressures above the tensile strength of re­
fractory concrete [2]. In heated high-performance concrete (HPC), the
addition of polypropylene fibres has shown to be efficient to mitigate
spalling [3,4]; nonetheless, in the case of some refractory concretes, fi­
bres have shown to be detrimental for important properties like corro­
sion resistance, mechanical strength, flowability and slag penetration
[5–7]. Currently, the heat-up curves are defined by refractory manu­
facturers from empirical experience [2,8,9]. Any change is subject to
hesitation as it involves safety, quality, and costs because drying should
be fast but cautiously due to the risk of cracks that would become hot
spots, source of leaks and reduced life span, or explosions with over­
whelming losses. Consequently, experimental, and computational re­
sources are needed to predict concrete’s hydro thermomechanical
behaviour and define efficient dry-out schedules.
Research on HPC has the objective of preventing structural failure in
case of accidental fire. Hence, the investigations usually apply fast heat-
up curves, like ISO-834 [10,11]. However, the cementitious systems
used in industrial applications are exposed to different thermal condi­
tions; therefore, they require to be studied from additional approaches.
Refractory linings are normally dried with progressive heat by one
surface, having the opposite side in contact with an impermeable steel
shell exposed to environmental conditions. Recent works have contrib­
uted with different experimental setups and improvements in the in­
struments used to measure pore pressures [2,4,10–19]; however, there is
neither standard methods nor commercial devices nor gauges to mea­
sure vapour pore pressure and evaluate the hydro thermomechanical
behaviour in heated concrete [20]. Sophisticated experiments have been
proposed by means of nuclear magnetic resonance, neutron radiography
and tomography for detailed visualization of the moisture migration and
its obstruction, representing valuable resources to understand the in­
ternal mechanisms during heating [21–24]. The image experiments

* Corresponding author. UFF/EEIMVR, Av. dos Trabalhadores 420, 27255-125, V. R., RJ, Brazil.
E-mail address: jorgejuareztrujillo@id.uff.br (J. Juárez Trujillo).

https://doi.org/10.1016/j.ijthermalsci.2022.108063
Received 9 March 2022; Received in revised form 12 October 2022; Accepted 24 November 2022
1290-0729/© 2022 Elsevier Masson SAS. All rights reserved.
J. Juárez Trujillo et al.
have been useful to shown how gauges inside concrete influence the
measurements [25]; although limitations arise in the image analyses due
to the reduced size of the sample, and the high cost. Other experimental
arrangements have presented reproduction difficulties, even to replicate
the explosive condition that has been considered a complex and not
well-interpreted phenomenon [15,26,27]. Therefore, solutions to these
problems are needed, as internal pressure is pointed out to explain the
explosive spalling and quantitative data is relevant to validate numerical
models. To date, there is no consensus for the industrial use of neither
experimental methodologies nor mathematical models. But the most
important is that few works in the literature provide details of the
problems and errors to prevent their repetition [2,16].
The mathematical models proposed in the literature are complex.
Strongly non-linear parameters are involved, such as desorption iso­
therms, permeability, and thermal conductivity. Those parameters are
function of several variables and require specific methods to charac­
terize the properties involved. The models are also controversial, either
considering one or several phases with distinction between liquid water,
vapour, and air, balancing those species separately or together, with
arguments over the capillary pressure effect and pores supersaturation
[2,28–31]. Moreira et al. performed a direct comparison of different
theoretical approaches, concluding that the single-phase model is a
convenient election to model refractory drying in practical applications
[32]. The election of the most convenient numerical method for the
solution is also a matter of discussion. The finite element method (FEM)
has been traditionally adopted to investigate the behaviour of structural
concrete under thermal stress [8,28,33,34]. Dal Pont et al. pioneered the
use of the finite volume method (FVM) for this kind of problem
obtaining a qualitative description of the complex phenomena [18].
Meftah et al. proposed a FVM-FEM comparison with two algorithms
obtaining similar numerical results, with one algorithm slightly faster
[35]. In contrast, Fey et al. used the finite difference method (FDM) in an
extensive investigation of refractory concrete drying for optimized
pressure-driven heat-up curves [2,12,36]. The increased effort needed to
solve models with added dimensions is also a matter of discussion. To
investigate the drying behaviour of a furnace’s two walls edge, Fey et al.
evolved from a 1D to a 2D model [2,36]. Yet, for more complex geom­
etries, such as three walls’ corners, a 3D model would be more suitable.
Meftah et al. [37] emphasized the need for 3D modelling to treat con­
crete heterogeneity, obtaining a proper description of the spatial fluc­
tuations in the solution fields. Dauti et al. [27] developed 3D simulations
and compared with neutron tomography images, showing how useful
those tools are to better understand the behaviour of HPC under thermal
stress. Nevertheless, in the case of castables drying, a model and its
numerical solution will be satisfactory only when it is finally able to
effectively define the time in which a certain geometry of a specific type
of concrete has lost its free and bound water and predict the time and
spatial position in which a crack or explosive spalling would occur or
not, as a result of a peculiar heat-up curve. Important insights have been
obtained, but more investigation is still needed.
Moreover, HPC and refractory concretes have different binders and
hydration products that influence their final properties and spalling
behaviour, besides their differences in particle size distribution. In the
case of HPC the most important binder is Portland cement, whose main
hydration phases affecting the hydro thermomechanical behaviour are
cement calcium silicate hydrate (CSH) and calcium hydroxide (CH). In
the case of refractory castables, the main binder is calcium aluminate
cement (CAC) whose hydration reactions produce CAH10, C2AHx, C3AH6
and variated amounts of AH3 depending on the Ca/Al ratio of clinker.
The effect of temperature during hydration of CAC has been broadly
studied, reporting that different Ca–Al phases can be formed, depending
on temperature during hydration [38,39]. Notwithstanding, the effect of
phase composition after hydration and during the first heat-up has
limited investigation. It may be expected that the different phases pro­
duced after hydration can result in different behaviour during heating.
For castables dying, Hips and Brown considered the dehydration
2
International Journal of Thermal Sciences 185 (2023) 108063
reactions of CAC to propose holding times at 150◦ , 300◦ and 565 ◦ C with
the use of internal pressure measurements to define the duration of each
one [40].
In this research, a phenomenological model was implemented using
the FVM in 3D to analyse transient moisture migration during the drying
of a conventional, hydraulic bonding high-alumina castable. As simu­
lated results of temperature, pressure, and mass loss must be validated,
an experimental setup was developed to dry a castable slab reproducing
the specific conditions of refractory lining, heating by one face and with
the opposite face joined to an impermeable surface. The objective is to
explore strategies to identify the most convenient practices that lead to
the prediction of the drying behaviour of complex geometries to eval­
uate heat-up curves. As the phenomenon is considerably intricate, and as
previous investigations have shown the distinguishable influence of
bound water on the drying rate curve [41], the proposed idea is to
perform the analyses by steps, isolating the drying stages [42] to
distinguish the effect of heating on the different types of water in a
prismatic specimen. For that, this research was focused on the complete
removal of only the free water. Therefore, we evaluated transient and
stationary states of a slow heat-up curve used in some industries to dry a
specific refractory castable with a holding time at 110 ◦ C and a
maximum temperature of 300 ◦ C.
2. Materials and experimental methods
2.1. Experimental setup
A device was developed to dry calcium aluminate concrete slabs 300
× 300 × 120 mm through controlled upper face radiating heat, based on
Kalifa’s et al. experimental setup [10,11]. Modifications were made to
reproduce the boundary conditions of a refractory lining by coupling the
bottom face with a steel shell 4 mm thick which also served as a support
to hold measuring probes in vertical position, Fig. 1 (a). As previous tests
made with smaller samples confirmed, in agreement with Jansson et al.
[16], that the size of the specimen influences the results; thus, the
specimen height of this setup was selected to match the thickness of a
blast furnace blow pipe refractory lining.
To reduce the loose of thermal energy by the lateral faces, 100 mm
thick alumina silicate insulating refractory bricks were used, with high
porosity (50–60%), low density (800 kg/m3) and low thermal conduc­
tivity (0.29 W/mK). Additional 150 mm fiberglass insulation above the
5000 W radiating elements and by the sides of the furnace proved to be
important to achieve the temperatures and heating rates required. Two
upper chimneys for natural air and vapour circulation were made with
cuts in some bricks of the lateral insulation, so that the heating chamber
can be sealed or opened for exchange with the environment; likewise,
any condensation from the specimen may come out freely, Fig. 1 (b). A
proportional integral derivative controller was fitted to program heat-up
curves for drying experiments, it was connected to an alumina-coated K-
type thermocouple placed between the radiating elements and the
specimen.
2.2. Pressure – temperature probes
Six simultaneous temperature-pressure probes were manufactured
using a seamless A269 stainless steel tube (outer diameter 9.53 mm,
inner diameter 6.53 mm). To prevent the entrance of concrete into the
probes during casting, sintered steel tablet filters of ballistic shape with
diameter 7.2 mm, height 4.0 mm, and 50 μm pore size were inserted at
one end of the tubes. At the other end, a “T” connection was linked to a
high sensitivity piezoresistive pressure transducer MPX5999D (capacity
from 0 to 1.0 MPa) and to a K-type thermocouple inserted into the tube
in contact with the filter to obtain temperature and pressure measure­
ments in the same coordinates, Fig. 2 (a) and (b). As the thermocouples
have a diameter of 3 mm, once inserted into the tubes they left an air
volume gap of 10 ml. To reduce air negative effect on vapour pressure
J. Juárez Trujillo et al. International Journal of Thermal Sciences 185 (2023) 108063

Fig. 1. (a) Device scheme showing internal components, depths of pressure-

temperature measuring points and the bottom steel shell. (b) Furnace with
upper radiating heat, controlling thermocouple, insulation, and chimney.

measurement, a paraffinic oil with boiling point above 200 ◦ C was used
to serve as a pressure transfer medium to the transducers; it was left a
free volume for oil expansion, as proposed by Li et al. [17], and probes
were hold in vertical position to prevent oil drain off. The calibration of
instruments was confirmed before and after experiments. The detach­
able mould used to prepare the specimen was a tight assembly of
stainless-steel plates 4 mm thick with exact measurements to obtain the
prismatic specimen size. The plates were covered with mineral grease to
facilitate unmoulding after curing. To obtain unilateral thermal flow in
the probes, they were mounted at the bottom of the mould within a 100
mm2 central area of the steel plate with depths of 20, 30, 40, 50, 70 and
100 mm in relation to heated surface, Fig. 2 (c).
One of the main problems detected for pressure measuring was the
vapour leakage along the interface between the concrete and the steel of
the probes because the lack of adhesion which result in surrounding
cracks or air bubbles, as observed in Ref. [25]; the following modifica­
Fig. 2. Probes for simultaneous pressure-temperature measurement. (a) Inter­
tions were performed: nal arrangement. (b) Probes with knurled surface and fastening O-rings; (c)
Mould assembled and sealed with probes located in a central squared area. (d)
1. The tube surface was knurled to improve the adhesion between steel Concrete moulding covered with PVC for hydration. (e) Specimen unmoulded
and concrete Fig. 2 (b); with sensors and wires connections underneath.
2. Steel O-rings were welded to the probes to prevent movements that
break the adhesion. A twisted one was located 20 mm below the top 2.3. Specimen preparation
of the tube to prevent rotational movements and a flat one at the
bottom, upheld by the steel plate, to prevent vertical movements Table 1 shows the composition, aggregate size, and water/binder
Fig. 2 (a, b); ratios of the high-alumina castable. For the specimen preparation, the
3. All joints were sealed with high-temperature resistant silicone Fig. 2 mass of anhydrous castable was 24.2 kg and the water added to the mix
(c). was 2.8 kg (10.3 wt %). It was not possible to vibrate the specimen due
to false contact problems that vibration was causing in the electronic
sensors. The specimen was weighted before and after curing and heating

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J. Juárez Trujillo et al. International Journal of Thermal Sciences 185 (2023) 108063

Table 1 released by dehydration; J is the mass flux (kg/m2s) proportional to the

High alumina castable composition. vapour pressure gradient ∇P (Pa/m); g is the gravitational acceleration; t
Compound wt % is time, and a = a(h,T) is the concrete relative permeability to humidity,
Al2O3 73.0 dependent on temperature and the water properties as liquid or vapour.
SiO2 13.0 See appendix A and B for nomenclature, values, units, and parametric
Fe2O3 1.3
equations.
CaO 9.3
Binder wt % Equation (3) is the energy balance, which considers the main en­
CAC (60% Al2O3; 40% CaO) 23 thalpies of the system. Equation (4) is the Fourier’s law for heat con­
Aggregate maximum size mm duction generated by the temperature gradient. The heat convection
Mullite 10.0 results from the mass of vapour transported through the porous medium.
Ratios
Water/Solid 11.6 ∂T ∂W
Water/Binder 50.3 ρC − Ca = − ∇ • q + Cw J • ∇T (3)
∂t ∂t

to register the total mass loss, Fig. 2 (e).
2.3.1. Concrete curing
The specimen was covered with polyvinyl chloride (PVC) film during
48 h for hydration at room conditions, 29 ◦ C and 56% RH; see Fig. 2 (d).
Afterwards, the cover and the mould lateral plates were removed,
leaving the concrete in contact with the bottom steel shell that was also
holding the probes. More samples were prepared with the same condi­
tions to characterize physical properties of recently cured concrete, i.e.,
in “green” condition.
2.4. Heat-up curve (HUC)
The aim of the experiment was to analyse the drying behaviour to
remove only the free water. Therefore, it was used a slow heat-up curve
currently used in industry to avoid cracks and risks of explosive spalling.
It was programmed a first heating rate of 20 ◦ C/h to reach 110 ◦ C at the
specimen’s upper face with a holding time of 10 h. Thereafter, a heating
rate of 30 ◦ C/h to reach the final temperature of 300 ◦ C at the specimen’s
upper face. The final temperature was held until reaching thermal and
hydraulic stationary state. Thereafter, the specimen was kept inside the
furnace for natural cooling. The thick red line in Fig. 5 shows the heat-up
curve (HUC).
q = − λ∇T (4)
where ρ is concrete solid matrix density, C is its isobaric heat capacity,
Ca = Ca(T) is the free water latent heat of vaporization, Cw is water
isobaric heat capacity, q is the heat flux (J/m2s) proportional to the
temperature gradient ∇T (K/m), λ is the concrete thermal conductivity;
see appendix A and B. This simplified model considers concrete as a
porous medium partially filled with humidity, without considering the
air mass neither the latent heat of dehydration.
By coupling the mass and energy balance equations, a system of two
parabolic PDE with four state variables (Wd, W, T, P) is obtained. Wd, is
calculated at each node and iteration according to equation B.10 in
appendix B. As W is a thermodynamic function of temperature T and
pressure P, its variation over time, ∂W/∂t, can be substituted in both
PDEs using its variation over pressure, ∂W/∂P, and its variation over
temperature, ∂W/∂T, whose values can be calculated by central differ­
ences approximation. Therefore, two unknown state variables, temper­
ature T and pressure P, remain to be calculated with two PDEs. Details
about the method for conditioning equations (1) and (3) for the numeric
solution, according to Refs. [8,28,43,44,46], can be found in Appendix
C.
3.2. Discretization method

3. Mathematical model and numerical methods The domain was divided in non-overlapping regular control volumes
with a representative node at the centre, as shown in Fig. 3. The in­
The mathematical model is based on a system of two coupled para­ terfaces of the control volumes were placed midway between adjacent
bolic partial differential equations (PDE) proposed by Bazant [28], re­ nodes in a cartesian 3D stencil forming a rectangular grid point cluster
ported as a practical option for technological applications [43,44]. It
considers the flow of energy and a simplified one-fluid flow of mass, i.e.,
moisture (liquid water and vapour) in a porous medium. The perme­
ability is a function of humidity and temperature for the microstructural
evolution that follows the dehydration reactions. A fully implicit FVM
was implemented to convert the PDEs into systems of linear equations
solved by iterative procedures [45]. The solution were the scalar fields
of temperature T, pore vapour pressure P, and moisture content W over
time in a 3D domain standing for the concrete specimen.

3.1. Conservation equations

Equation (1) is the mass balance, which includes a mass source term
for the release of chemically bound water, triggered by heat during
dehydration. Equation (2) is the Darcy’s law for the transport of mois­
ture generated by the pressure gradient inside the concrete pores.
∂W ∂Wd
= − ∇•J+ (1)
∂t ∂t
a
J= − ∇P (2)
g
Fig. 3. Control volume rectangular stencil for coordinates (x, y, z), showing the
where W = W(h,T) is the free water content dependent on the pores’ node P, with consecutive nodes W, E, T, B, N, S and the interfaces w, e, t, b, n, s.
relative humidity h, and temperature; Wd = Wd (T) is the bound water Here, the distance between nodes is the same for all directions δx = δy = δz.

4
J. Juárez Trujillo et al. International Journal of Thermal Sciences 185 (2023) 108063

for the relationships between volumes at top, bottom, west, east, north,
and south. The upper case and lower case in Fig. 3 are used to differ­
entiate the consecutive nodes from the control volume interfaces in the
mesh, respectively. The central node in the stencil may stand for pres­
sure, temperature, or moisture content. To obtain the solution fields,
equations (1) and (3) were integrated over the control volume and over
time interval from t to Δt considering the principles of mass and energy
conservation within the boundary conditions shown in Fig. 4.
For the spatial discretization, the two conditioned PDEs (see Eq. (C7)
and C11 in appendix C) were integrated on each control volume shown
in Fig. 3. A piecewise-linear profile was assumed with linear interpola­
tion functions for the state variables P and T between the nodes in the
grid to calculate the fluxes at the control volume interfaces. For the time
discretization it was adopted a fully implicit scheme to define the vari­
able behaviour on each time step according [45]. With this strategy, two Fig. 5. Heat-up curve (HUC) programmed in the electric furnace and behaviour
systems of discretized linear algebraic equations were developed for the of measured internal temperatures over time at different depths in the pris­
nodal values of temperature and pressure. The systems of equations matic specimen.
were solved alternately with a staggered procedure, calculating first the
temperatures field, then that result was used to calculate the pressures 3.3. Boundary conditions
field; thereafter, a time step advanced to compute a next iteration. A
line-by-line procedure was used combining the Gauss-Seidel with the 3.3.1. Mass transport boundary conditions
Thomas algorithms with relaxation through inertia in a top-to-bottom The boundary conditions reproduced the experimental setup, as
sweep direction to transmit the temperatures of the experiment shown in Fig. 4. Concrete surfaces were assumed as permeable bound­
heat-up curve into the domain at each iteration. The solution implies aries, except the lower surface which is joint to the steel shell forming an
that for this highly nonlinear problem, the conservation of mass and impermeable boundary where moisture flux disappears with a Neumann
energy magnitudes are satisfied in every control volume at every time type boundary condition [43], according to Eq. (5):
step. That is the advantage of the FVM, featured for ensuring exact mass
J • n=0 (5)
balance [18,28,35]. Implementations of this method to obtain the dis­
cretized equations for 1D and 2D porous thermo-hydral models can be where n is the orthogonal normal unit vector of the surface.
found in Refs. [18,35,47,48]. For more details about this development in The upper surface was in contact with the atmosphere, the lateral
3D, the reader is referred to Refs. [46,49,50]. surfaces were in contact with the insulating refractory bricks of high
porosity, where vapour was considered to flow freely. Thus, in all those
surfaces P equals the environmental pressure Penv. The vapour exchange
between the surfaces and the environment is not instantaneous, it was

Fig. 4. Discretized mesh with the boundary conditions scheme for a concrete slab heated by the upper face with lateral thermal insulation, and impermeable surface
at the bottom. A control volume is highlighted in the centre denoting its consecutive nodes.

5
J. Juárez Trujillo et al.
adopted that the normal flow is proportional to the pressure difference,
according to Eq. (6):
J • n = Bw (P − Penv ) (6)
where, Bw is the surface vapour transfer coefficient that depends on air
movement or the partial insulation in contact with lateral faces [28]. See
table A3 in appendix A for values and units.
3.3.2. Heat transport boundary conditions
The radiation condition is described by Stefan-Boltzmann’s law in
Eq. (7).
( )
qr • n = εc σSB T 4 − THUC
4
(7)
where n is the normal unit vector of the boundary surface, qr is the heat
flux by radiation, THUC is the radiating elements’ temperature according
to the heat-up curve, T is the concrete temperature, σSB is the Stefan-
Boltzmann constant, and εc is the heat emissivity of the concrete sur­
face [28]; see table A3.
The lateral surfaces of the specimen were considered thermally
insulated because of the low thermal conductivity of the insulating re­
fractory bricks, with a Neumann type boundary condition [43], ac­
cording to Eq. (8):
q • n=0 (8)
The slab’s bottom face was in contact with a 4 mm thick steel plate
with a considerable thermal conductivity λs (see table A3 for value) and
subsequently with environmental air using the Newton’s law of cooling,
Eq. (9):
qc • n = BT (T − Tenv ) (9)
where T is the slab’s surface temperature. It was considered a surface
free convection and BT is the heat transfer coefficient [28]; see table A3.
Since the specimen is in the absence of a vacuum, radiation and heat
conduction occur simultaneously, so the total heat flux at the heated
face is obtained by adding Eq. (7) and Eq. (9) with Tenv = THUC, i.e.,
following the heat-up curve used in the experiment.
3.4. Initial values and parameters
A set of concrete and fluid properties were necessary as input pa­
rameters. Appendix A summarizes the values of the parameters used and
appendix B the parametric equations to obtain them. The intrinsic
permeability, κ, was measured from cured concrete samples at room
temperature using the method proposed by Innocentini et al. [51]. The
initial relative permeability a0, its evolution a(h,T), the desorption iso­
therms W(h,T) and the water latent heat of vaporization Ca(T) were
calculated according to Refs. [28,43]. The function for bound water
dehydration Wd was obtained by thermogravimetric analysis (TGA)
from “green” concrete samples. The thermal conductivity λ, was initially
assumed as constant [43], using the value reported by manufacturer.
The isobaric heat capacity of concrete C was assumed constant, as re­
ported by Ref. [8]. Apparent density and porosity were measured from
dried concrete samples. Environmental temperature Tenv and pressure
Penv were measured from local conditions. It was supposed an initial pore
relative humidity h0 = 90%, and a uniform initial field of temperatures
in equilibrium T0 = Tenv; therefore, according to Eq. B.1, the initial pore
pressure in all nodes was P0 = 3595 Pa. The mass of anhydrous cement
Wc and the initial water content W0 were the same as the experiment.
Concrete physical properties for heat and mass fluxes were assumed
isotropic. Water properties were taken from steam tables.
6
International Journal of Thermal Sciences 185 (2023) 108063
4. Experimental results analysis
4.1. Measured temperatures
Fig. 5 shows the heat-up curve and temperatures at different depths
over time. T20 is the thermocouple at 20 mm, T30 is at 30 mm and so on.
The first 10-h holding time at 110 ◦ C in the upper face was not efficient
for drying, i.e., that time did not promote the elimination of free water.
That is because the temperatures inside the specimen stayed below the
boiling point, at around 70 ◦ C. These internal temperatures were
beneficial only for the hydration reactions of concrete curing [38]. Had
it been kept for a longer period, temperatures would have stabilized in
this range, remaining free water. On the other hand, if this holding time
is to be reduced or eliminated, the influence of total real curing time on
concrete properties should be evaluated.
In the second and last holding time, the time needed to reach steady-
state temperatures in all depths was investigated. The heat-up curve was
programmed to reach 300 ◦ C at 21 h and kept stable. About 8 h after that
were necessary for all internal temperatures to become stable, at around
t = 30 h; with T20 = T30 = 220 ◦ C; T40 = T50 = 200 ◦ C; T70 = 175 ◦ C,
and T100 = 160 ◦ C. Those internal temperatures were indeed efficient to
dry, i.e., to boil the free water and trigger the transport mechanisms to
remove the steam from the pores. In the transient trajectory of the
curves, a deflection can be observed at around 20 h, better noticed in
T100; when temperatures are reaching boiling point. This deviation is
explained by the higher energy demand of the latent heat of vapor­
ization. This agrees with the findings reported by Refs. [2,10,13,14,52].
In this experiment, the frequency of the data gathering permitted to
distinguish those small temperature variations. In the steady-state, T20
and T30 remained 80 ◦ C below the heat-up curve; however, they
reached the oil’s boiling temperature. This could result in false pressure
measurements. This condition brings a restriction for this type of
experimental arrangement. The thermocouple in the deepest position is
an important reference for concrete drying research. Mainly in this
investigation in which, unlike other projects in the literature, the spec­
imen bottom was considered as a composed impermeable boundary
condition because the 4 mm thick steel plate. A natural cooling stage
begun at 40 h with the specimen kept inside the furnace until all ther­
mocouples reached room temperature, which took about 24 more hours.
4.2. Measured pore pressure
Obtaining reproducible pore pressure measurements is a challenging
task [2,16,28,53], they are laborious and time-consuming experiments;
however, they are crucial for validating numerical simulations. To
capture the pressure variations reported here, it was necessary to
perform several, repetitive previous unsuccessful tests, many adjust­
ments with state-of-the-art piezoresistive pressure sensors and frequent
readings in time intervals of 2 min during a 40-h lasting experiment.
Fig. 6 shows the experimental pressures over time; P20 is the probe
at 20 mm depth and so on. All sensors, except P70, began to sense
pressures when t ≈ 15 h, and detected a pressure peak at t ≈ 18 h. The
maximum pressure value registered was 17.2 × 10− 3 MPa in P20, which
is a pressure peak significantly lower than those reported in the litera­
ture and below the saturation pressure, despite the slow heating rate
used. The peaks momentum coincides with water boiling point and the
deflection observed in the temperature curves shown in Fig. 5. The
curves of the other pressure sensors also showed a bell-shape behaviour,
which is a characteristic found in literature [10,15,19,53]. Another
distinctive feature to notice is the second peak detected by all sensors at
t ≈ 21 h, except failed P70. Other authors have noticed this second peak
behaviour [2,8,19]; it is assumed that the cause of this second peak is
related to the chemically bound water release.
Before concrete casting, all sensors were calibrated and tested. The
possible reason for P70 fail could had been a not detected leakage or a
faulty electronic connection between the sensor, the wires, and the
J. Juárez Trujillo et al.
Fig. 6. Measured pressures over time at different depths in the specimen. Ps(T)
is the vapour saturation pressure corresponding to the temperature of
measuring point T20 along the time.
capturing data hardware, since the beginning of the drying. Because no
pressure was sensed in only this probe, in any moment of this experi­
ment. Then, this sensor’s data should not be considered, but it is shown
here as an example of the possible errors that may occur. The highest-
pressure peaks were sensed in the experiment only when boiling point
was reached internally; albeit low values, the behaviour was consistent
in all the sensors working properly. This was confirmed by repeating the
experiment and observing the same behaviour. It is assumed that slow
heating is best suited to attain higher pressures since fast heating in­
duces thermal damage. However, this assumption may not be general­
ized, as results depend on several conditions, since sample preparation.
The curing time and conditions used in this research contrast to previous
experiments, e.g., Kalifa et al. [10] kept the specimens for 6 months in a
sealed bag, Bangi et al. [4] and Choe et al. [14] cured in water bath at
20 ◦ C for 28 days. Thus, the differences regarding the initial pore relative
humidity and desorption isotherms could be markedly different.
The total amount of time that sensors detected positive pressures was
considerable. The bell-shaped curve in P20 lasted about 10 h, the
pressure rose from 0 to 17.2 kPa in 3 h and then drop to zero in 7 h,
including the second peak. The other sensors were detecting pressures
for about 6 h in total, including the second peak. This means that there
was not a sudden drop of pressure caused by any crack or leak in the
system and the length of the bell-shaped curves was the time vapour
needed to exit the concrete. It is important to notice here that during the
10-h holding time at 110 ◦ C in the upper face, there was not detected any
pressure that may cause structural risk to the concrete. Therefore, ac­
cording to the result of this experiment, for this concrete composition,
thickness, and preparation method, the holding time of 10 h at a tem­
perature of 110 ◦ C on the heated face can be inferred as an unproductive
time for the drying operation. Simultaneous peaks at different depths for
one face heated specimen coincide with some results reported in the
literature [11,19]. However, this contrasts some others in which sensors
with different depths detected peaks at considerably different times [4,
10,52,53]. Although it is not determinant to make direct comparisons
between experiments in literature, peaks intensity and timing differ­
ences are due to several factors. The different heating speeds and dis­
tance between probes affect timing. Differences in concrete
composition, preparation, and cure greatly influence the hydraulic
properties of concrete as a porous media. For example, on the one hand,
permeability is affected by vibration, on the other hand, thermal con­
ductivity, and desorption isotherms are influenced by initial humidity.
All of them are critical for this kind of problem and should be measured
and reported. Besides that, the boundary conditions used in this study
which have important influence in the fluids mechanics are also
different. Therefore, to this point, it is not possible to define the degree
of accuracy of the pore pressure measurements obtained; future analyses
with more repeated experiments are needed. In this study, the consistent
record of a pressure peak and the similar behaviour in five out of six
7
International Journal of Thermal Sciences 185 (2023) 108063
sensors was remarkable.
Regarding the measuring instruments, the use of oil as a transfer
medium has a limitation that may become a source of error. Specialized
silicone oils typically boil at around 300 ◦ C, but depending on supplier,
some react at lower temperatures. Some works in the literature report its
use without mentioning its boiling/firing point or thermal expansion. In
this research, although some probes attained the oil’s boiling point, it
was not when the pressure peaks were detected; therefore, measure­
ments were not influenced by oil expansion. The importance of sealing
the system was confirmed. A high temperature silicone sealant was used
in the area where probes exit the concrete; however, it was not enough
to prevent vapour leaks. The negative influence of inserted instruments
to accumulate air bubbles or cracks along them, since moulding and
curing, is aggravated by the lack of adhesion between the concrete and
the polished stainless steel tube surface. This condition is even worse if
the surface is unintentionally polluted with oil. Any minor movement
causes the materials to detach, opening a route for vapour to escape or
air to enter. The solution to improve adhesion was by modifying the tube
surface texture with knurling, after that modification, pressure readings
were possible. The welded O-rings also helped to avoid circular or lon­
gitudinal movements that could break the adhesion; nevertheless, the O-
ring located 20 mm below the top of the tube could be substituted by a
fastener at the bottom to also avoid discontinuity and air bubbles in the
mass of concrete around the measuring point. As probes extremely
invasive introduce errors in the system, reduction in tubes diameter is
suggested. Moreover, these modifications must still be tested at faster
heating rates and higher temperatures for future work, highlighting the
importance of including explosion-proof protection, as proposed by
Auvray et al. [54].
4.3. Measured mass loss
During curing there was no water loss, this was confirmed by
measuring the total mass of the specimen before and after curing. The
total mass was measured just before heating and after cooling. The
specimen mass that entered the furnace was 27.0 kg. The specimen mass
that came out of the furnace was 25.1 kg, so that it lost 1.9 kg. Therefore,
inside the specimen, 0.9 kg of water remained (3.7 wt %), as shown in
Fig. 7.
As T100 reached a stationary state at 160 ◦ C and kept stable for more
than 10 h, it is believed that all the free water came out and probably
some bound water also. The remaining water is assumed to be exclu­
sively bound water that would need higher temperatures to get out of
the specimen; for this reason, the concrete cannot yet be considered
totally dried.
4.4. Concrete physical behaviour analysis
When furnace temperature reached 300 ◦ C, water dripping was seen.
It is assumed that it was the moisture transported from the inside out
that condensed on the surface and slipped down through the sides of the
specimen. Similar behaviour was reported by Refs. [11,27]. Specimen
dimensions were measured before and after drying, finding neither
dimensional changes nor trace of spalling, cracking nor any other
damage by naked eye. Therefore, pressure leaks due to cracks were
discarded. Irregular zones in the external shape of the specimen were
perceived, Fig. 2 (e), which are due to the lack of vibration. After
removing the specimen from the furnace, samples were taken by cutting
sections from different regions of the volume to characterize physical
properties of dried concrete; no internal cracks were found.
5. Numerical results and discussion
In this section, the numerical solutions are compared with experi­
mental measurements at the corresponding coordinates and times. A
Fortran 90 code was developed to solve the discretized linear equations.
J. Juárez Trujillo et al. International Journal of Thermal Sciences 185 (2023) 108063

Fig. 7. Reduction of water content sowing the remaining bound water in the specimen dried with a slow one face heating up to 300 ◦ C, as shown in Fig. 5.

The control volumes were refined to form 37.5 × 37.5 × 5.0 mm prisms
for a total of 2025 nodes placed at the centre of each control volume in
the slab’s domain.
To validate the computational code, comparisons were made with
the experimental measurements reported by Fey et al. [2] to dry a
similar refractory concrete with the same specimen size and a heat-up
curve with an analogous holding time. A simulation was made repro­
ducing their boundary conditions with a first heating rate of 75 ◦ C/h to
reach 200 ◦ C at the specimen’s upper face. Subsequently, a slow heating
rate of 5 ◦ C/h during approximately 6 h. Thereafter, a heating rate of
75 ◦ C/h to the final temperature of 700 ◦ C. Fig. 8 (a) and (b) point out
the experimental results obtained by Fey et al. and the curves obtained
with the numerical implementation of this study, showing a reasonable
agreement along the time. It must be noticed that the permeability and
thermal conductivity were adjusted to find the best match with the
experimental measurements.
5.1. Simulated temperatures
For the next simulations, the initial and boundary conditions of the
experimental setup of Fig. 1 were used, they are resumed in Table 2. The
parameters needed are listed in Appendix A.
Fig. 9 (a) shows the simulated temperatures; T20sim is the node at
20 mm, T30sim is at 30 mm and so on; these profiles can be compared
with Fig. 5. A direct comparison between the simulated and measured
temperatures for the nearest and farthest thermocouple in relation to the
heated surface is in Fig. 9 (b) and (c) respectively. Measured and pre­
dicted temperatures show similar behaviour during the transient state
(seen in Fig. 5, from 0 < t < 30 h). Some sections presented better
proximity, e.g., T20sim with T20exp from 0 < t < 14 h in Fig. 9 (b).
In the second heating ramp, starting at t = 14 h, the predicted tem­
peratures show a faster response, if compared to the gradual increment
of the temperatures measured in the experiment. This difference is due
to the real thermal conductivity variations with temperature. From t >
30 h, the simulated temperatures did not reach a steady state but a
tendency to equalize the plateau at 300 ◦ C; different from the experi­
mental temperatures whose stability started at t = 30 h. This is explained
by the fact that the model reproduced the energy conservation assuming
zero loss in the lateral surfaces and a small loss at the bottom, as shown
in the boundary conditions in Fig. 4; by contrast, the experimental re­
sults showed that there was a larger energy loss. Part of the unconsid­
ered energy loss in the system was due to the air circulation promoted by
the chimneys and a millimetric air gap between the specimen and the
lateral insulating bricks. That gap was there because the specimen was
inserted and removed from below the furnace. Fibreglass was added to
cover the gap and avoid air circulation; however, the energy loss was

Table 2
3D model initial and boundary conditions.
Space and time discretization
Slab dimensions 300 × 300 × 120 mm
Calculated time 40 h
Space step δx = δy = 37.5; δz = 5.0
mm
Time step Δt = 0.25 s
Initial conditions
T (x, y, z, t = 0) T0 = 302.15 K
P (x, y, z, t = 0) P0 = 3595 Pa
W (x, y, z, t = 0) W0 = 258.98 kg/m3
Boundary conditions
T (x, y, z = 120, t) Rad. + Conv.: q • n = εc σSB (T4 − THUC
4
)+
BT (T − THUC )
T(x|x=300
y=300 Adiabatic: q • n = 0;
x=0 , y|y=0 ,
z, t)
T (x, y, z = 0, t) Convection: q • n = BT (T − Tenv );
P (x, y, z = 120, t) Permeable: J • n = Bw (P − Penv )
P(x|x=300
y=300 Permeable: J • n = Bw (P − Penv );
Fig. 8. Comparison of measured (Exp) and simulated (Sim) results of (a) x=0 ,y|y=0 ,z,
t)
Temperatures and (b) Pressures. The marked points were obtained from the
P (x, y, z = 0, t) Impermeable: J • n = 0;
experimental results originally measured by Fey et al. [2].

8
J. Juárez Trujillo et al.
Fig. 9. (a) Simulated temperatures over time in nodes at the same coordinates
of thermocouples. (b) Comparison of simulated and experimental temperature
profiles at 20 mm depth from heated surface. (c) Comparison at 100 mm depth.
higher than assumed. This is evidence of the strong influence of
boundary conditions. Further experiments with adjusted experimental
and numerical boundary conditions are required. To avoid lateral losses,
an option is to use aluminium foils glued with epoxy resin in the lateral
surfaces, as reported by Refs. [13,21,22], although its influence was
found minimal in small samples [25], more tests are needed in larger
specimens.
The model was not sensitive to the deflection in the temperature
curves caused by water vaporization, as seen in the experiment at t = 20
h, better noticed in T100 exp, Fig. 9 (c). Although it was used a
formulation for the water latent heat of vaporization as a function of
temperature (see equation B.12 in appendix B), it did not reproduce the
deflection observed close to the boiling temperature. One reason for the
difference is that concrete and water isobaric heat capacities were
assumed as constants.
5.1.1. Temperature field
Fig. 10 illustrates the simulated temperatures distribution in the
concrete domain at t = 25 h; this is a moment before the physical
experiment reached the thermal steady-state. The radiant heating is
evident at the upper surface with no thermal loos in the sides because of
the thermal insulation condition in the lateral surfaces. A uniform
temperature gradient with a uniform pattern towards the colder lower
9
International Journal of Thermal Sciences 185 (2023) 108063
Fig. 10. Temperature field in the specimen at t = 25 h. The coloured scale
reports the intensity of simulated temperature (◦ C) for the rectangular control
volumes in the domain.
surface in contact with the steel plate is perceived, as a result of a ver­
tical unidirectional thermal flow. At the bottom, the thermal flow
continued unidirectional through the steel shell that has a thermal
conductivity considerably larger than the specimen’s thermal conduc­
tivity (see tables A.1 and A.3 in appendix A).
5.2. Simulated pore pressures
Fig. 11 (a) shows the simulated pressures in the nodes at the same
coordinates of the probes. The predicted maximum pressure was 2.6
MPa with the highest value in the bottom node P100 at t = 36 h. It is
important to notice that these numerical results are first-hand with no
adjustments in any parameter to match the experimental results. To be
aware of the effect caused by parameter adjustments, another simulation
was performed modifying only one parameter. Instead of using a con­
stant concrete thermal conductivity, a function of temperature obtained
from a similar concrete was used (equation B.11 in appendix B). Fig. 11
(b) shows that in this other simulation the predicted pressure peak was
less than the half of the previous one. It reached 1.1 MPa, 6 h before, at
time t = 30 h, with a narrower bell shape and it presented a small second
peak of 0.75 MPa in the descending part of the curve, at t = 32 h. The
thermal conductivity as a function of temperature resulted in values five
times higher, modifying the speed of the thermal processes.
Theoretically, the pressure starts to rise when the evaporation front
passes through the respective finite volume. Fig. 11 (a) and (b) show
how the pressure started to rise at t = 15 h. If Fig. 9 is reviewed, this
happens when T20sim = 100 ◦ C. In the experimental measurements, the
pressure started to rise at the same time, but with different intensity, as
seen in Fig. 11 (c), where the numerical results of the second simulation
are compared with the experimental results in P20 and P100. The
experimental peak reached a maximum 17.2 × 10− 3 MPa in the node
P20, which is closer to heated face, at t = 18 h. A detailed analysis in
Fig. 11 (a) reveals that P20 > P100 when t < 23 h; but when t > 23 h they
invert, remaining P100 > P20, a similar behaviour can be perceived in
Fig. 11 (b). This contrasts with the experimental results in Fig. 11 (c),
where P20 remained higher along the time. Samples may present
explosive spalling close to heated face, or, when they accumulate energy
in the core, a catastrophic explosion occurs [56,57]. In this study, any
pore pressure attained excessive values, e.g., the saturation pressure was
not reached at any time. If there are not high pressures, that is because
the pressured steam flowed away, and the pressure dropped. This may
happen during a long period of time, as needed for the steam to find the
way out through the pores, or in a fast pressure drop originated by a
sudden crack in the structure that lets the steam escape.
J. Juárez Trujillo et al.
Fig. 11. Predicted pressures at different depths inside the domain over time.
(a) Profile with constant thermal conductivity λ = 1.34 W/mK; (b) Profile with
variable thermal conductivity λ = λ(T), see Eq. B.11 in appendix B. The vapour
saturation pressure curve, Ps(T), was calculated with Eq. B.2 using the simu­
lated temperature T20 along the time; (c) Comparison of experimentally
measured and numerically simulated pressures.
In this study, the only similitude between numerical and experi­
mental results is the bell-shaped behaviour which is observed repeatedly
in the literature. However, by comparing the numerical results of Fig. 11
(a) and (b) with the numerical and/or experimental results of previous
authors [2,4,9–11,14,53,55], where similar pressure magnitudes are
reported, it can be inferred that the experimental pressure measure­
ments of this study are not convincing. Nevertheless, it is important to
consider that the mathematical model implemented to obtain the nu­
merical results conveys important simplifications, and, although inter­
esting results are shown, they cannot be considered definitive. The lack
of exact reproduction of the boundary conditions, that brought a larger
energy loss than assumed, contributed to the indecisive match between
the experimental and the numerical results in this study. Therefore, for
the prediction of pressures and eventual explosions, accurate replication
of the boundary conditions and satisfactory comparisons of numeric
results with a large set of reproducible experiments are necessary.
5.2.1. Pressure field
The sequence of 3D images in Fig. 12 shows the simulated pore
pressure evolution over space and time for different sections of the
domain. In Fig. 12 (a), the upper representative volumes were reaching
the boiling temperature, and as expected, the higher vapour pressures
were predicted to be close to the heating source with a gradient in
10
International Journal of Thermal Sciences 185 (2023) 108063
Fig. 12. Pore pressure evolution over space and time. The coloured scale re­
ports the intensity of simulated pressure (Pa) in the rectangular control volumes
of the domain. (a) pressure field in a 25% section of the domain at t = 15 h. (b)
pressure field in a 50% section at t = 25 h. (c) pressure field in a 25% section at
t = 30 h.
direction to the lower volumes.
In Fig. 12(b), the temperature in all the volumes had surpassed the
boiling point and the predicted higher pressures moved to the centre;
therefore, the simulation reproduced the pressure migration as theo­
retically expected. Fig. 11 (c) shows the advance of pressure to the lower
and lateral volumes unveiling a low-pressure area at the bottom centre
due to a higher water saturation resulting from the impermeable
boundary condition. It is also seen an increase in the lateral moisture
transfer as the lateral sides would be the natural way to release pressure.
Reaching the boiling temperature in the system does not guarantee
that all the free water has been removed. A transitory period is necessary
for the steam to flow, triggered by pore pressures, and leave the porous
medium. Free liquid water can be considered to cease being present in
J. Juárez Trujillo et al.
the domain when all the nodes reach thermal equilibrium above 100 ◦ C
without subsequent mass-loss. Furthermore, drying can be considered
complete only when both, physically adsorbed and chemically bound
water, are totally released, and that can occur when temperatures reach
around 550 ◦ C [28].
5.3. Simulated moisture content
Fig. 13 shows the simulated water content profile. All the finite
volumes were integrated to analyse the total water mass-loss starting
from W0 used to prepare the concrete mix. The graph shows a slow mass
variation from 0 < t < 15 h; if collated with Fig. 9, a steep mass-loss is
predicted only after internal temperatures exceed 100 ◦ C, when t > 15 h.
Conversely, if Fig. 13 is collated with Fig. 11 (a), the highest pore
pressure is reached at t = 36 h. That is, the highest pressure was attained
when free water amount was reaching a minimum. A reason for that is
found in Fig. 14, where a pronounced increase of bound water release is
predicted around that time. Therefore, the model predicted a significant
effect on pressures caused by the release and evaporation of bound
water. This result comes from the combination of the desorption iso­
therms and the TGA interpolated function that predicted the release of
bound water at a temperature above boiling point, i.e., a violent
expansion of water that suddenly appeared. Figure B1 in appendix B
presents the TGA results showing that the steepest mass-loss takes place
when the temperature exceeds 225 ◦ C; if Fig. 9 is reviewed, this internal
temperature is predicted at t = 35 h. However, in the experiment the
specimen did not reach that temperature, as seen in Fig. 5.
In this research, the mass of the experimental specimen was
measured only before and after heating, Fey et al. [2] did not measure
the mass considering that a 1D model is unsuitable for mass loss com­
parisons. Nonetheless, to define the precise time in which all the free
water was removed, and for better numerical validation, the most
convenient practice would have been to measure the mass variation
continuously and perform transient comparisons in 3D.
5.3.1. Moisture content field
Fig. 15 shows the simulated evolution of moisture distribution over
space and time for different sections of the domain. The results predict
how, although the thermal flow perceived in Fig. 10 was unidirectional,
due to the boundary conditions, the moisture has multidirectional
migration to the upper and lateral surfaces to gradually exit the domain.
This can be perceived thanks to the analysis in 3D. Initially, in the upper
region, the drying front advances parallel to the heated surface, Fig. 15
(a). The subsequent drying front by the sides results from the lateral
boundary condition that permeates moisture through the porous bricks,
Fig. 15 (b). This is not the case for the lower coldest region and the
central volumes, as delayed moisture loss is observed due to the
impermeable surface, Fig. 15 (c). In the finite volumes at the bottom, the
Fig. 13. Prediction of water mass-loss in the domain over time.
11
International Journal of Thermal Sciences 185 (2023) 108063
Fig. 14. Prediction of chemically bound water release in the domain over time.
direction of the vapour flow begins a multidirectional trajectory that
will subsequently affect the finite volumes of other areas in the domain.
The impermeable bottom surface forces the vapour to flow to the sides,
but, as it is a porous media which also restricts the flow, part of it ac­
cumulates in the centre. The transient patterns of the sections shown in
Figs. 12 and 15 appear because of the vapour accumulation and vapour
turbulence in different directions. This complex pattern is only possible
to unveil with a transient 3D model. The drying mechanism starts with
the evaporation of free water, increasing the vapour content in the finite
volumes, later by the vapour pressure resulting from the restriction of
the porous media. Pressure increment forces the vapour to flow. Part of
the vapour exits the domain and part flows toward the colder internal
volumes. Finally, a font of moisture appears in every finite volume due
to the bound water release, repeating the cycle of flow forced by
pressure.
The model reproduced the blocking exerted by the impermeable
surface in the xy-plane on the vertical moisture flow, forcing it to
permeate horizontally along the steel shell in a transversal direction to
the slab’s lateral surfaces, see Fig. 14 (b). The effect of water saturation
on pore pressure development becomes clear if Figs. 14 (c) and Fig 11 (c)
are collated to notice that the large liquid saturation in the lower central
finite volumes creates a barrier of condensed moisture so that the vol­
umes with higher pore pressure are located outside that zone. The
saturated areas become a thermal barrier since moisture consumes a
large amount of thermal energy to evaporate, reducing the flow of heat
and delaying the development of pressure.
From a qualitative point of view, the 3D simulation replicated the
moisture content behaviour. The advance of the drying front within the
domain is in accordance with reality. These images can be compared
with state-of-the-art experimental procedures, where neutron radiog­
raphy or neutron tomography have been used, like those performed by
Refs. [21,22]. As dehydration decomposes concrete, the model coupled
the mechanisms of heat and moisture flow with the simulation of the
microstructure evolution performed through the increase of perme­
ability as a function of temperature and humidity, according to Eq. B.4
in Appendix B.
Collating Fig. 12 with Fig. 15 permits to notice that in Fig. 12 (b) and
(c), the maximum pressure is no longer in the upper volumes, the
pressure distribution was inverted since at t = 15 h the water content in
the upper volumes is minimal, as they are already dried, Fig. 15 (b) and
(c). As the drying front advances, the pressure is transported to a lower
central region.
Behind the drying front, a fraction of the evaporated water condenses
when it finds lower temperatures. That condensation increases the
saturation again and decreases the permeability to a critical point until it
blocks the pores and prevents the scape of subsequent steam. This is
known as the “moisture clog”. If temperatures and pressures continue
increasing faster than the vapour release, the probability of explosive
J. Juárez Trujillo et al.
Fig. 15. Moisture content evolution over space and time. The coloured scale
reports the intensity of simulated water concentration (kg/m3) in the rectan­
gular control volumes of the domain. (a) moisture content field in a 40% section
of the domain at t = 15 h. (b) moisture content in a 15% section at t = 25 h. (c)
moisture content in a 20% section at t = 30 h.
spalling increases.
During heating up to 300 ◦ C, the experimentally measured, and the
numerically calculated pore pressures were low. Those pressures in the
pores do not represent any risk to create a stress that could overpass the
tensile strength σT reported by manufacturer for this specific concrete
(see table A1). After heating, no traces of cracks were found. The heat-up
curve started to be effective to dry only after 20 h of heating. For this
specific concrete, the empirical practice of holding time at 100 ◦ C in the
heating face represents an important waste of time and energy.
Notwithstanding, further research is needed to apply modifications in
the industry for the effect of this holding time in curing and because the
presented model is not yet considering the utterly mechanical aspects
and the addition of stresses resulting from the next drying step, which is
12
International Journal of Thermal Sciences 185 (2023) 108063
the removal of the chemically bound water at higher temperatures.
5.4. Influence of the methods used to characterize properties
The methods to define the necessary parameters may bring signifi­
cant variations in the simulations. In sensitivity analyses Fey et al. [2]
and Moreira et al. [44] concluded that permeability, thermal conduc­
tivity, and desorption isotherms, in that order, had the biggest impact on
results. However, it is necessary to consider the effect of other param­
eters because of the differences in composition, preparation, cure, age,
geometry, and boundary conditions.
In this research, the measured initial intrinsic permeability had a
significant standard deviation among samples and the resulting value
can be considered high for this type of concrete. That is the result of a
non-vibrated specimen, which highlights the importance of controlled
vibration to prepare the samples. The relative permeability as a function
of temperature and humidity determined by an empirical formula for
generic concretes [28] gave pressure values comparable to those found
in the literature; albeit, different to the measured pressures. Initial
intrinsic permeability can be measured using a Cembureau per­
meameter; however, measuring the evolution of intrinsic permeability
in recently cured CAC concrete while it is being heated, and modelling it,
becomes a complex endeavour [58]. Several models are proposed in the
literature to describe permeability as a function of temperature, hu­
midity, pressure, damage, tortuosity, and the consideration of the
Klinkenberg and inertial effects [9,33]. A convenient practice would be
to characterize this parameter with the method at high temperatures
proposed by Innocentini et al. [59], from “green” concrete.
Thermal conductivity variation was initially assumed slight and
disregarded, as originally supposed by Gong and Mujumdar [60];
however, the simulations shown in Fig. 11 (b) proved a keen effect,
alerting that a function of temperature is more representative. Accord­
ing to Bazant and Jirásek [28] the thermal conductivity varies consid­
erably as a function of temperature and humidity and can be expressed
as proposed by Gawin et al. [61]. Fey et al. [2] obtained this
double-dependent parameter from “green” concrete, resulting four times
higher than the value reported by the manufacturer. Further simulations
and comparisons are necessary using functions of temperature and hu­
midity obtained by characterizing “green” samples of the specific cast­
able with the hot-wire method.
It was confirmed that one of the most challenging model components
are the desorption isotherms. The generic formulation for temperatures
above 100 ◦ C adopted from Ref. [28] provided moisture content results
qualitatively in accordance with reality. Fey et al. [2] used a sorption
isotherm obtained at 20 ◦ C with the aid of dynamic vapour sorption
(DVS) and reported a big effect on maximum pressure curve.
Baroghel-Bounny [62] made available a useful isotherms database and
Davie et al. [63] proposed an alternative formulation. Notwithstanding,
the difficulties arise from the need for a formulation for the specific
concrete at high temperatures. The use of neutron image analyses [25,
64] is a promising alternative to improve the numerical results. As a
consensus, this parameter represents an opportunity for higher research.
The simulation was performed assuming the initial value of pore
relative humidity h0 = 90%, as originally supposed by Gong and
Mujumdar to model refractory concrete drying [8,43,60]. Nonetheless,
this value must be evaluated to accurately represent the specific “green”
castable. The overestimation of this parameter may lead to pressure
results higher than reality. Refractory concretes curing condition and
initial pore saturation contrasts with the case of aged HPC in environ­
mental conditions, or the case of specimens in water bath or longer
curing times. Chemical balance analysis of hydration and dehydration
reactions at different temperatures would be useful to estimate the
initial pore relative humidity and bound water amount that would be
expected to stay or leave at different stages of curing and drying.
Scanning electron microscopy of “green” microstructure and neutron
tomography could be helpful resources.
J. Juárez Trujillo et al.
The effect of bound water release was perceived in the simulation
performed in this research, although its resulting effect on pressures is
debatable. The prediction of a fast increment of pressure when bound
water is released was also perceived by Fey et al. [2], considering it an
accuracy fail. According to Mindeguia et al. [11] a small amount of
bound water does not amplify the build-up of pressure neither repre­
sents a risk of explosion, and Fey et al. [2] affirms that bound water
mostly affects the drying time and disregarding it will not modify
maximum pressures unless released at temperatures close to saturation
temperature. Hence, it is convenient to obtain this parameter from the
specific castable with the appropriate methodology. It must be consid­
ered that the characterization of bound water release is performed using
considerably small samples in an equilibrium state; when heating a
larger volume in different conditions the equilibrium is attained in
different times and places for the reactions that release bound water.
Besides that, the desorption isotherm determines the ultimate behaviour
of the bound water recently released. This confirms the need for more
research regarding the effect of chemical reactions during drying and the
determination of more accurate specific models of desorption isotherms.
Therefore, for bound water release input data, the most convenient
practice is to perform representative TGA from concrete samples
without free water, i.e., previously dried at 100 ◦ C, and not from “green”
samples. It is also convenient to ensure the presence of aggregates and
matrix in the samples. The late is applicable to characterize the concrete
latent heat of dehydration through differential scanning calorimetry
(DSC). Conversely, for concrete heat capacity as function of temperature
and humidity, to obtain representative DSC analysis, they should be
performed with “green” samples. Appropriate TGA characterization
together with thermal conductivity are also necessary for the confir­
mation of the second pressure peak that was detected in the experiment
and predicted in the model.
In this research, the amount of air and its effect was assumed
negligible. That might be expected from a “green” castable, especially if
the mix has been vibrated and the air bubbles removed. Fey et al. [2,12,
36] implemented an advanced model considering the air mass in the
balance equations, resulting in a minimal contribution to the pore
pressures. Nevertheless, some experimental works in the literature re­
ported pressure measurements higher than vapour saturation and
explained that the reason was the air mass expansion [10,11]. In this
work such effect was not perceived, as pressures remained below vapour
saturation. To confirm the effect of air on the drying of refractory con­
crete linings, a future step is to apply multiphase models existing in the
literature, like [2,29,31,34,37,65,66], and perform analyses in 3D with
the specific boundary conditions at higher temperatures.
Regarding the use of a specific numeric method to solve the PDEs,
there are arguments about the convenience of using one or another. For
example, there are questions about the use of FVM because the non-
linearity of the problem is stronger than the non-conservativity of
FEM. It must be considered that the two methods handle strong non-
linearities in a similar form, with approximations using the tangents of
the interpolation functions for the state variables at each node. How­
ever, the FVM, besides handling non-linearities, adds a treatment for
mass conservation in the grid, which is important if an abrupt moving
interface between oversaturated and dried concrete occurs. In those
cases, the local mass conservation is guaranteed by using FVM. For
example, in the accidental cases of fire with rapid heating of a structural
column, or an abrupt thermal load due to cooling failure in a refractory
wall. FVM is recommended for complex geometries, and for interfacing
coatings with layers of different castables and properties, as frequently
found in refractory linings. For example, to analyse the drying of the
blast furnace running channels, as intended for future research. The FEM
and FDM can also provide reliable results in those cases, but with special
care, additional derivations, using the lowest-order finite elements and
implicit time integration.
13
International Journal of Thermal Sciences 185 (2023) 108063
6. Conclusions
1) The definition of safe and efficient dry-out schedules to install
monolithic refractories is a scientific and technological challenge.
This research tested combined experimental and numerical meth­
odologies aimed to evaluate a heat-up curve currently used to dry a
high-alumina castable through the analysis of pore pressures, inter­
nal temperatures, and mass loss behaviour. Details of some diffi­
culties and sources of error are presented as well as suggestions to
overcome them.
2) For the castable prepared in this research, the 10-h holding time at
110 ◦ C on the heated surface was inefficient to remove the free water,
therefore it misspends time and energy. However, as the internal
temperatures reached are beneficial for hydration reactions (around
70 ◦ C), further evaluations of the real total curing time and final
properties of the concrete should be performed, before suggesting
any change. The second ramp and the plateau at 300 ◦ C on the heated
surface shows to be effective to remove the free water. After 10 h
with T100 at 160 ◦ C, only one-third of the water originally used in
the mix remained, which is believed to be exclusively chemically
bound water. Nevertheless, for the sake of energy efficiency, a
unique heating rate of 30 ◦ C/h with only one holding time at 250 ◦ C
would have been enough to remove the free water from the 120 mm
thick slab of this specific concrete.
3) From a quantitative point of view, the experimental method to
measure temperatures is the most reliable result, followed by mass
variation measurement. The numerical validations can be reliably
performed using those two variables initially to predict the heat and
mass loss behaviour. In laboratory practice, reaching the boiling
point in the thermocouple close to the cold side, along with stability
in mass variation, can help to define the time in which free water
removal is complete.
4) It was possible to sense pore pressures with the use of oil and knurled
probes; however, measured pressures resulted considerably lower in
comparison to simulated pressures. Although the sensors were cali­
brated before the experiment, and the numeric methodology is mass-
conservative, the pressure data obtained in this investigation is
neither enough to draw definitive inferences nor suitable to control
drying in a technological application.
5) The numerical results in 3D of this research are a valuable resource to
visualize the transport phenomena, although they can still only be
used as a rough guide. Yet, this experience showed that by combining
the experimental and numerical methodologies, more comprehen­
sive and useful insights can be obtained to evaluate the current heat-
up curves used in industry.
Funding sources
This study was financed in part by the Conselho Nacional de
Desenvolvimento Científico e Tecnológico – CNPq (grant number:
140142/2017–7), by Fundação de Apoio à Ciência, Tecnologia e Edu­
cação - FACTE and by the Coordenação de Aperfeiçoamento de Pessoal
de Nível Superior - Brasil (CAPES) - Finance Code 001. No one of the
funding sources was involved in the study design, collection, analysis,
and interpretation of data, neither in the writing report nor the decision
to submit the article for publication.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
J. Juárez Trujillo et al. International Journal of Thermal Sciences 185 (2023) 108063

Acknowledgement development of the experimental device, and to Gabriel Antonio Mar­

sola, Leonardo Augusto Damasceno and Isli Samara Flauzino from
The authors wish to thank Bento Ferreira and Leandro Kellermann de Universidade de Ribeirão Preto for their valuable support to measure
Oliveira from EEL-USP for their valuable contributions in the concrete permeability.

Appendix A. Parameters needed for the simulations

Table A.1
Parameters from concrete physical properties.

Description Nomenclature Value Units

Initial pore relative humidity h0 90 %
Pore relative humidity evolution h(T,P) Eq. B.1 %
Intrinsic permeability κ 1.45 x 10-15 m2
Initial relative permeability a0 Eq. B.3 m/s
Relative permeability evolution a(h,T) Eq. B.4 m/s
Free water content W(h,T) Eq. B.8 kg/m3
Chemically bound water released Wd (T) Eq. B.10 kg/m3
Mass of anhydrous CAC (23 wt %) Wc 504.23 kg/m3
Thermal conductivity as a constant λ 1.34 W/m K
Thermal conductivity as a variable λ(T) Eq. B.11 W/m K
Isobaric heat capacity C 1100 J/kg K
Apparent solid matrix density ρ 2380 kg/m3
Apparent porosity n 23.17 %
Tensile strength σT 11.5 MPa

Table A.2
Parameters from fluid properties (water liquid or vapour).

Description Nomenclature Value Units

Vapour saturation pressure Ps(T) Eq. B.2 Pa
Isobaric heat capacity Cw 4182 J/kg K
Latent heat of vaporization Ca(T) Eq. B.12 J/kg
Density, at 25 ◦ C ρa 997.05 kg/m3
Viscosity, at 25 ◦ C ηa 890 × 10− 6 N s/m2
6
Vapour viscosity, at 99,6 ◦ C ηv 282.7 × 10− N s/m2

Table A.3
Parameters for boundary conditions.

Description Nomenclature Value Units

Environmental temperature Tenv 302.15 K
Environmental relative humidity (RH) henv 56 %
Environmental pressure Penv 101,325 Pa
Gravitational acceleration g 9.81 m/s2
Convection vapour transference Bw 1 × 10− 6 s/m
Surface convection heat transference BT 1 W/m2K
8
Stefan-Boltzmann constant σSB 5.67 × 10− W/m2K4
Concrete surface heat emissivity εc 0.9 –
Steel plate thermal conductivity λs 50.2 W/m K

Appendix B. Parametric equations

Pore relative humidity [28,44,60]

P
h(T, P) = × 100% (B.1)
Ps (T)

where, P is pore vapour pressure (Pa), and Ps(T) is the saturation vapour pressure (Pa) dependent of absolute temperature T (K) according to Antoine’s
function:

14
J. Juárez Trujillo et al. International Journal of Thermal Sciences 185 (2023) 108063

⎧ ( )
⎪
⎪ 11.9515(T− 373.15 )

⎪
⎨ Penv e
T− 39.724
(T < 373.15 K);
Ps (T) = . (B.2)
⎪
⎪ ( )
⎪
⎩ 12.1074(T− 373.15 )
T− 28.665
Penv e ( T ≥ 373.15 K);

Initial Relative permeability [60]

ρa g
a0 = κ (B.3)
ηa

Variable Relative permeability [8,28]

{
a0 f1 (h, T) f2 (T)(T ≤ Ttr );
a(h, T) = (B.4)
a0 f2 (Ttr ) f3 (T)(T > Ttr );

where,
⎧
⎪
⎪ 1.2893 − 0.01357 (T − 273)
⎪
⎪ + 0.01357(T − 273) − 0.2893(h < 1);
⎪
⎪
⎨ 1 + [4(1 − h)]4
.
f1 (h, T) = (B.5)
⎪
⎪
⎪
⎪ .
⎪
⎪
⎩
1; (h ≥ 1)
[ ( )]
2700 1 1
T0 − T
f2 (T) = exp (B.6)
[ ]
T− Ttr

(B.7)
0.881+0.214(T− Ttr )
f3 (T) = exp

with T and T0 = Tenv (K), and the transition temperature for high permeability Ttr = 368.15 K.

Free water content [8,28]

⎧ )1/ (
⎪
⎪ W0 m(T)
⎪
⎪ h Wc
(h ≤ 0.96);
⎪
⎪ Wc
⎪
⎪
⎪
⎪ .
⎪
⎪
⎨ W2 − W1
W(h, T) = W1 + (h − 0.96)
1.04 − 0.96
(0.96 < h < 1.04); (B.8)
⎪
⎪
⎪
⎪ .
⎪
⎪
⎪
⎪ [ ( )]
⎪
⎪ (T − 273)2
⎪
⎪ W 0.037(h − 1.04) + 0.3335 1 − (h ≥ 1.04);
⎩ c
3.6 ∗ 105

Where, W1 and W2 are the water content calculated at a given temperature when h = 0.96 and h = 1.04, respectively; and m(T) is a temperature-
dependent empirical coefficient:
1
m(T) = 0.04 + / (B.9)
1 + (T − 263)2 27370

where T is absolute temperature.

Chemically bound water released

⎧
⎪
⎪ 0.0017 ∗ T̂ − 0.0171(0 < T
̂ < 200 ◦ C)
⎪
⎪
⎨ .
Wd (T) = 0.0407 ∗ T̂ − 7.5143(200 ≤ T̂ < 400◦ C) (B.10)
⎪
⎪
⎪
⎪ .
⎩ ̂ + 6.5253(400 ≤ T̂ ≥ 800◦ C)
0.0025 ∗ T

15
J. Juárez Trujillo et al. International Journal of Thermal Sciences 185 (2023) 108063

Where T
̂ is temperature in ◦ C.

Fig. B.1. TGA (green) and DSC (brown) curves from cured concrete samples.

Variable thermal conductivity

λ(T) = 11.5 − 0.029 T + 3.88x10− 5 T 2 − 1.89x10− 8 T 3 (B.11)

With T in K; obtained using the parallel hot-wire method ISO 8894–2 from a similar high-alumina castable.

Water latent heat of evaporation [61]

{
2.672x105 (Tcr − T)0.38 (T ≤ Tcr )
Ca (T) = (B.12)
0(T > Tcr )
With T in K, and the critical water temperature Tcr = 647.15 K.

Appendix C. Partial Differential Equations conditioning

Mass conservation equation [8,28]

Substituting equation (2) in equation (1),

( )
∂W a ∂Wd
= ∇ • ∇P + (C.1)
∂t g ∂t
As W is a thermodynamic function of T and P, that is, W = W(P,T), it can be written
∂W ∂W ∂P ∂W ∂T
= + (C.2)
∂t ∂P ∂t ∂T ∂t
Using
from equation (C.2) in equation (C.1),
∂W
∂t
( )
∂W ∂P ∂W ∂T a ∂Wd
+ = ∇ • ∇P + (C.3)
∂P ∂t ∂T ∂t g ∂t
For practicality, coefficients A1 and A3 are defined as
⃒ ⃒
∂W ⃒⃒ ∂W ⃒⃒
A1 = ; A = (C.4)
∂P ⃒T ∂T ⃒P
3

∂W
∂Pand ∂∂W
T
can be calculated by central difference approximation to obtain step n+1, by
( )
∂W(P, T) W(P + ΔP, T) − W(P − ΔP, T)
≅ (C.5)
∂P T 2ΔP
( )
∂W(P, T) W(P, T + ΔT) − W(P, T − ΔT)
≅ (C.6)
∂T P 2ΔT

Employing (C.4) in equation (C.3) and rearranging, the pressure transient term is isolated as
⎛ ⎞
∂P a/g
⎜ ⎟ 1 ∂Wd A3 ∂T
=∇ • ⎝ ∇P⎠ + − (C.7)
∂t A1 A1 ∂t A1 ∂ t

16
J. Juárez Trujillo et al. International Journal of Thermal Sciences 185 (2023) 108063

Energy conservation equation [8,28]

Substituting equation (4) in equation (3),

( )
∂T ∂W a
ρC − Ca = ∇ • (λ∇T) − Cw ∇P • ∇T (C.8)
∂t ∂t g

Using from equation (C.2) in equation (C.8) and rearranging,

∂W
∂t
( ) ( )
∂W ∂P ∂W ∂T a
− Ca + ρC − C a = ∇ • (λ∇T) − Cw ∇P • ∇T (C.9)
∂P ∂t ∂T ∂t g
For practicality, coefficients A2 and A4 are defined as
⃒ ⃒
∂W ⃒ ∂W ⃒
A2 = − Ca ⃒⃒ ; A4 = ρC − Ca ⃒⃒ (C.10)
∂P T ∂T P
Using (C.5) and (C.6), substituting (C.10) in (C.9) and rearranging, the temperature transient term is isolated as
( ) ( )
∂T λ Cw a A2 ∂P
=∇ • ∇T − ∇P • ∇T − (C.11)
∂t A4 A4 g A4 ∂ t

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