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Drying Technology: An International Journal

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Modeling and Experimental Identification of Cracks in

Porous Materials During Drying
a a
Stefan J. Kowalski & Jacek Banaszak
a
Poznan University of Technology, Institute of Technology and Chemical Engineering ,
Poznan , Poland
Published online: 26 Aug 2013.

To cite this article: Stefan J. Kowalski & Jacek Banaszak (2013) Modeling and Experimental Identification of Cracks in Porous
Materials During Drying, Drying Technology: An International Journal, 31:12, 1388-1399, DOI: 10.1080/07373937.2013.796484

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 Drying Technology, 31: 1388–1399, 2013
Copyright # 2013 Taylor & Francis Group, LLC
ISSN: 0737-3937 print=1532-2300 online
DOI: 10.1080/07373937.2013.796484

Modeling and Experimental Identification

of Cracks in Porous Materials During Drying
Stefan J. Kowalski and Jacek Banaszak
Poznan University of Technology, Institute of Technology and Chemical Engineering,
Poznan, Poland

responsible for material damage.[2] During the last two

The main aim of this paper is to mathematically describe and
experimentally determine the self-fracturing of fluid-saturated
porous materials during drying processes. The thermo-hydro-
mechanical model of drying that is suitable for a mathematical
Downloaded by [Aston University] at 03:47 09 January 2014
decades, the basic principles of damage mechanics were
formulated and some special problems were solved. Exten-
sive reviews of papers dealing with the above-mentioned
mechanical aspects of drying were presented in Hasatani

description of these phenomena as well as the acoustic emission

(AE) technique for their experimental detection are presented.
Numerical solutions based on the thermo-hydro-mechanical drying
model are used to analyze stress development and to formulate
the crack criterion in dried material. The studies concern the con-
vective drying of kaolin-clay material. Bar-shaped samples with
a rectangular cross-section were used for the mechanical tests and
cylindrically shaped samples of kaolin-clay were used for the drying
tests. Good agreement of the theoretical predictions to the
experimental data is shown.
Keywords Acoustic emission; Cracking; Drying; Experimental;
Kaolin-clay; Modeling
INTRODUCTION
Engineering materials subjected to drying processes may
sustain structural changes and reduction of mechanical
strength. Studies on mechanical phenomena which occur
in drying materials and, in particular, the examination of
drying-induced stresses and strains become relevant when
the quality of the dried products is of prime importance.
A detailed description of these phenomena is necessary to
control the process and to prevent permanent deformations
(warping, collapse) or fracture of these products.
The danger of material damage during drying can be
predicted on the basis of a thermo-hydro-mechanical
model of drying based on the mechanics of continua.[1]
The experimental validation of the theoretical predictions
of material damage is possible to carry out by utilizing
the one-, two-, or three-point acoustic emission (AE)
technique. This paper examines the mechanical aspects of
drying capillary-porous materials, such as kaolin-clay, with
special emphasis on the drying-induced stresses that are
Correspondence: Stefan J. Kowalski, Poznan University of
Technology, Institute of Technology and Chemical Engineering,
pl. Marii Skłodowskiej Curie 2, 60-965 Poznan, Poland; E-mail:
stefan.j.kowalski@put.poznan.pl
and Itaya[3] and Katekawa and Silva[4]. The problem of
mechanical deformations and drying-induced stresses was
discussed in a broader context in the author’s book.[1] Dif-
ferent aspects of mechanical phenomena arising during
drying were also discussed in a number of works.[5–10]
A series of articles on ‘‘Damage of Materials by Drying:
Modeling, Numerical Simulations, Experimental Studies’’
was published in a special edition of Drying Technology.[11]
A method of damage control by drying was discussed in
Kowalski,[12] where the one-point acoustic emission tech-
nique was used as an effective tool for monitoring on-line
drying processes. The damage analysis of microwave-dried
materials is presented in Kowalski et al.[13]
The present study concerns mathematical modeling and
numerical simulations of spots where possible damage may
occur. The one-point AE technique, which has been used
by the authors up until now, provided a unique tool for
early detection and monitoring of sub-critical crack growth
and for recognizing the time at which the crack could be
formed. In this paper, on the other hand, the two-point
AE method is employed to localize both the time and the
place of crack occurrence in cylindrical kaolin samples sub-
jected to convective drying. Thus, the AE technique is
becoming important as a diagnostic and measuring tool.
It is very useful for the monitoring of material damage
and can be used to alert the operator on potential material
fracture so that he can change the drying conditions in
advance in order to prevent material destruction.
The mathematical model presented in this paper is used
for determination and calculations of drying-induced stres-
ses. In numerical analysis, the place of possible material
damage during drying is identified by the strength criterion
formulated by using the effective and admissible stresses.
The formulation of the strength criterion, which depends
on the moisture content, constitutes a new element in the
mechanical analysis of drying processes. Examples of

1388
 IDENTIFICATION OF CRACKS IN POROUS MATERIALS
damage in kaolin-clay samples subjected to convective
drying at different drying conditions are presented. The AE
technique is used to validate the theoretical predictions of
numerically determined spots of possible damage estimated
on the basis of the thermo-hydro-mechanical drying model.
MATERIALS AND METHODS
Experimental Set-Up
Figure 1 presents the scheme of the experimental equip-
ment used for the tests of convective drying.
The kaolin samples, cylindrical in shape (7), were dried
convectively in the laboratory dryer chamber (Zalmed
SML 42=250=M) (1). The temperature and relative
humidity of the air in the dryer chamber were measured
every 30 seconds with a Pt 100 temperature probe and a
humidity sensor DO 9861T Delta OHM (3), which was
located close to the drying sample (7). The digital indicator
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showed the air temperature with an accuracy of 0.1
C,
while the air humidity was measured with an accuracy of
0.01%. The holder with the sample was suspended on an
electronic balance (Radwag WPS2100=C) (8), which
recorded the sample mass with an accuracy of 0.01 g. The
band-width (5 kHz to 1 MHz) of the AE sensors (2), which
were attached both to the bottom and the upper surfaces of
the sample, registered the AE signals and transferred them
into electric ones, and as such they were strengthened by
the preamplifier (Vallen AEP3) (4). Next, the acquisition
system (Vallen AMSY5) (5) filtered these signals, amplified
them, converted them from voltage impulses to current
impulses, and finally, sent them to a personal computer
(6). Furthermore, the analysis of the AE signal parameters
was done with the help of Visual AE software delivered by
the Vallen Company.
The yield stress and failure strength of kaolin-clay with
various moisture contents were examined in the tensile tests
FIG. 1. Experimental set-up: 1 – dryer; 2 – AE sensors; 3 – temperature
and humidity probe; 4 – AE preamplifiers; 5 – acquisition system; 6 – com-
puter; 7 – sample; 8 – electronic balance (color figure available online).
1389
at constant force increments of 1 N=s on a universal
strength-measuring instrument Cometech QC-508A1.[8]
Material
The experimental tests were carried out on cylindrical
samples made of KOC kaolin-clay produced by the
Surmin-Kaolin S.A. Co., Nowogrodziec, Poland. The
chemical composition and physical properties of KOC
kaolin are presented in Fig. 2 and given in Table 1.
The kaolin-clay was delivered in a dry state and before
the experiments it was wetted with a prescribed amount
of water and mixed to achieve a greasy paste of initial
moisture content (MC) approximately equal to X ¼ 0.45
[kg water=kg dry kaolin]. (X denotes the ratio of water
mass inside the body to the body’s dry mass, and is
expressed as both dimensionless or in a percentage.) The
greasy paste was stored and homogenized in a closed box
for 48 h to level the moisture distribution in the whole
material. The kaolin-clay plastic mass obtained in this
way was used to manufacture both the bar-shaped samples
with a rectangular cross-section (dimensions 10  14 mm
(b  h) and 80 mm long), which were used for the mechan-
ical tests, and the cylindrical samples (R ¼ 0.03 m,
H ¼ 0.06 m), which were subjected to the drying tests.
Because of the wide range of MC, ca. 0%  45%, the rec-
tangular samples were tested in three different modes.
Firstly, the samples with an MC above 30% were tested just
after molding to avoid material creeping. In the next mode,
a number of samples were molded at MC ca. 30%, then
partially dried to different MCs between 3% and 30%,
and stored for 24 h to unify the distribution of moisture.
Thus-prepared portions of samples with different MCs
were then used for the mechanical tests. In the third mode,
the samples were molded at 30% MC, then dried in the
open air and, finally, dried in the laboratory oven to obtain
an MC below 3%, and as such stored for 24 h before being
used for mechanical tests.
To determine the actual MC of the tested samples, each
one was weighed just after the tension test and then dried in
the drying scales until its mass did not change.
Acoustic Emission (AE)
The non-destructive acoustic emission (AE) method is
becoming a very popular measurement and diagnostic
FIG. 2. Micro- and macrostructure of KOC kaolin (color figure avail-
able online).
 1390 KOWALSKI AND BANASZAK
TABLE 1
Chemical and mineralogical composition of KOC kaolin
Chemical composition [%]
SiO2 Al2O3 Na2O TiO2 Fe2O3
51.5 34.5 0.63 0.54 0.54
Mineralogical composition [%]
Kaolinite Illite
80 9 9
technique in material engineering. The AE arises in stressed
materials when the elastic energy accumulated in these
materials is released. The released energy is then trans-
ported throughout the material in the form of elastic waves
propagating in various directions. It can be measured by an
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AE sensor installed at the material surface and registered
by a variety of AE descriptors; e.g., AE energy per time
period (e.g., 30 s), total AE energy, total number of AE
signals, etc. Knowing these descriptors, one can assess
the quality of dried samples because they measure the
intensity and number of micro- and macro-cracks. These
descriptors constitute solely the source of information on
the dried material quality.[14–17]
In our studies, the one- and two-point acoustic emission
(AE) technique was used to monitor the effect of crack
formation in the kaolin-clay samples during drying. The
advantage of the AE method is that it enables monitoring
on line time and place of material damage.
MATERIAL BEHAVIOR BY DRYING
Cohesion Forces
Kaolin-clay after wetting has the consistency of a dis-
persed system, which after dehydration to a moisture con-
tent (MC) that is approximately equal to 45% becomes a
greasy paste. The particles of the suspension have the tend-
ency to agglomerate due to the liquid bridges between
them. The negative capillary pressures in these bridges
involve compressive forces that favor particle aggregation.
The value of this pressure determine Laplace’s formula[18]


1 1
Fk ¼ c  ð1Þ
R1 R2
where c denotes the liquid surface tension, and R1 and R2
are the main radii of curvature of the concave surface of
the bridge (Fig. 3).
The necessary condition for negative pressure is that
R2 < R1. For water surface tension c ¼ 7.2  102 N=m and
particle dimension 106 to 108, the magnitude of capillary
force Fk is of the order 2  107 N to 109 N. These values
are comparable with those for disperse forces at atomic
MgO CaO K 2O roasting loss
0.12 0.08 0.01 12.08
Quartz Others
2
contacts. Thus, the capillary forces may bring the particles
to atomic contacts at the final stages of the drying process.
During drying and calcination, the material becomes
porous with a relatively high mechanical strength. A charac-
teristic feature of the dispersed systems is the large value of
the interfacial surfaces. This means that such a system
contains a large amount of surface energy. As a consequence
of this, the particles (crystalline grains) tend to join each
other and create a porous material of a disordered structure.
The solid skeleton is created so that the surface energy
is decreased, but the particle bonds become thermo-
dynamically stable. Two kinds of interactions between
particles exist: electrostatic forces (repulsive) resulting
from the existence of monomial charges on the particle
surfaces, and London’s disperse forces (attractive) caused
by an instantaneous asymmetry of charge distribution as
a result of electron fluctuation. The dispersed forces are of
a long range and create the main force that attracts the
particles to each other.
According to London-Heitler’s theory, the energy of
attraction of two spherical particles of radius r at a distance
L from each other reads[19]
r
U ¼ A ð2Þ
12L
where A (1020 J) is the Hamaker constant of interaction
between particles.
FIG. 3. Forces acting on the solid particles due to surface tension in the
liquid bridge (color figure available online).
 IDENTIFICATION OF CRACKS IN POROUS MATERIALS
The cohesion force between particles is determined by
the derivative of the above-mentioned energy with respect
to distance
@U r then the stress r is approximately equal to F =L20 , and the
Fk ¼ ¼A ð3Þ
@L 12L2
The relations above are valid when the distance between
particles is less than 100 nm. For greater distances, the rela-
tions ought to take into account the phase retardation of
the vibrating dipoles.[19]
Material Strength
Let us consider the strength of material in the form of
paste in which particles are in atomic contact. The structure
of such a material has a stable character; i.e., it can be
damaged only due to an action of de-cohesion forces.
The potential energy of particle interactions U results
from attraction and repulsion effects between atoms
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A B
U ¼ þ ð4Þ
Ln Lm
where A and B are the proportionality constants referring
to attraction and repulsion, respectively, and m and n are
the exponents of the current inter-particle distance.
The alteration of potential energy for the interaction of
particles subjected to tension or compression is illustrated
in Fig. 4.
The minimum potential energy corresponds to the inter-
particle distance L0 at which the interaction force is equal
to zero (equilibrium state). If the inter-particle distance is
changed (L ¼ 6 L0), a force F arises and tends to bring the
system to the equilibrium. It will be a repulsion force if
L < L0, or an attraction force if L > L0. This force is equal
to the alteration of potential energy with respect to distance
@U A B
F¼ ¼ n nþ1  m mþ1 ð5Þ
@L L L
The minus sign results from the fact that the potential
energy increases and the force decreases or vice versa, when
the particle goes away from the equilibrium position.
FIG. 4. Interaction between material particles during drying: (a)
compression or tension; (b) stress vs. inter-particle distance.
1391
Let us imagine two particles adjoining each other but
placed on opposite sides of a cross-section in a tensed bar
(Fig. 4a). If the force interacting between two atoms is F,
strain e ¼ (L – L0)=L0. For stretching the two adjoining
particles by dL, the stress increases as (Fig. 4b)



1 @F 1 @F
dr ¼ 2 dL ¼ de ¼ EðX Þde ð6Þ
L0 @L L¼L0 L0 @L L¼L0
where EðX Þ ¼ ð@F =@LÞL¼L0 =L0 denotes the modulus of
elasticity, which is a function of the moisture content
(MC).
Figure 5 presents Young’s modulus for kaolin-clay
determined experimentally as a function of the moisture
content.
One can state that each drying process is accompanied
by drying-induced stresses that counteract shrinkage.
When a wet material dries, the drier surface attempts to
shrink but is restrained by the wet core. The surface
is stressed in tension and the core in compression. The
tension stresses can cause damage of the surface structure.
The tension of a dried sample until damage takes place can
be performed similarly to the curve presented in Fig. 4b.
This curve has a shape which can be approximated with
a sinus function[19]
2pu
r ¼ rm sin ð7Þ
k
where rm denotes the theoretical (maximal) strength of the
material, u ¼ L  L0 is the displacement equivalent to the
applied stress, and k denotes the period of sinus function
that is dependent on the moisture content.
One determines the magnitude of rm from the work that
ought to be applied to the material to displace the particles
at a distance k=2, (i.e., at which their separation takes
place). This work is expressed by the following integral
FIG. 5. Young’s modulus as a function of the moisture content (color
figure available online).
 1392 KOWALSKI AND BANASZAK

Z k=2 Z k=2 concentrated at the flaw tip of length c having radius r at

2pu krm
U¼ rdu ¼ rm sin du ¼ ð8Þ the tip[19,21]
0 0 k p

rffiffiffi
By calculating the derivative of the stress function (7) c
rc ¼ r 1 þ 2 ð12Þ
with respect to displacement u and taking the limit con- r
ditions (i.e., the tangent to the tension curve at the equili-
brium state), we get The fracture occurs when stress rc is greater than the
yield strength rm, that is
dr  2p E sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
rffiffiffi
u¼0 ¼ rm ¼ ð9Þ
du k L EðX Þ c
c <r 1þ2 ð13Þ
LðX Þ r
The limit condition in Eq. (9) was compared with Eq. (6)
substituting de ¼ du=L. Calculating k from Eq. (9) and The fracture criterion formulated in macroscopic
substituting it into (8), we get stresses reads
2LðX Þ r > rcr ð14Þ
U¼ ½rm ðX Þ2 ð10Þ
EðX Þ
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where
When the drying proceeds further, the surface of sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi

kaolin-clay becomes more and more rigid and stressed, rffiffiffi1
EðX Þ c
and in the critical stress state the particle bonds on the rcr ¼ c  1þ2 ð15Þ
LðX Þ r
surface can be broken off. The rupture of the particle
bonds involves an increase in the free surfaces and thus
The above fracture criterion is suitable for drying
also in some amount of surface energy. If we can consider
material, whose boundary surface is in tension. Then the
the energy lost for plastic deformations and reconstruction
fracture takes place on the surface.
of a crystal lattice during the fracture as negligible, then the
Let us consider an elastic layer in the form of a thin plate
newly created surface energy is, according to Griffith’s
having a flaw (pore) of dimension 2c in the middle. Let us
theory, equal to the work U.[20] Denoting the surface
imagine first a similar layer without a flaw but being sub-
energy as c, then U ¼ 2c, hence two new surfaces arise by
jected to a tensional state of stress generating elastic energy
the fracture. This statement allows us to express the
U0 ¼ const in this sample. A similar layer but with a flaw
maximum strength from Eq. (10) as
in the middle and subjected to the same loading as before
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi contains elastic energy expressed by
EðX Þ
rm ðX Þ ¼ c ð11Þ
LðX Þ pr2 c2
U ¼ U0  þ 2cð2cÞ ð16Þ
E
where L(X) ¼ L0[1 þ jX(X – X0)] is the inter-particle dis-
tance in the drying material at moisture content X, and The second term expresses the released energy of the
jX is the coefficient of linear shrinkage. material because of the flaw, and the third one the
Equation (11) expresses the theoretical strength of dried additional surface energy on the flaw. The slit will increase
material. It informs us that the strength of the dried its size spontaneously only when a decrease of energy takes
material increases due to an increase in Young’s modulus place during the drying process,[20] that is
and decreases in the distance between the particles.
@U
0 ð17Þ
Fracture @c
Any suitable theory of cracking during drying should Differentiating (16), one can find the critical length of
account for the common observations that cracking is the slit ccr, by which the crack formation may begin to arise
more likely if the body is thick or the drying rate is high.[5] for a given stress
This is because these circumstances involve great hetero-
geneity in moisture distribution and induce great stresses. 2cE
Generally, cracks appear at the tips of flaws or pores, ccr ¼ ð18Þ
pr2
where the stress concentration takes place.
The stress that causes the fracture is not the macroscopic The fracture will proceed spontaneously at a given stress
stress r that acts on the network, but rather the stress rc r for all slits with c > ccr.
 IDENTIFICATION OF CRACKS IN POROUS MATERIALS 1393

MODELING Shear modulus M and bulk modulus A can be expressed

Assumptions
The drying model used for the numerical analysis of
drying-induced stresses was developed on the basis of
mechanics of continua, incorporating the following
assumptions[1,12,22]:
The drying material is an unsaturated porous
medium consisting of a solid skeleton, liquid,
and gas in the pores;
The skeleton of the drying material is elastic and
its strains are infinitesimal;
The considerations exclude thermal shocks, so the
dynamic terms (accelerations, inertia forces,
kinetic energy, etc.) are neglected in the momen-
tum and energy balance equations;
The stress in the moisture is simply pressure Pa; i.e.,
deviatory (shear) stress is neglected and considered
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by Young’s modulus E and Poisson’s ratio n as follows
E En
M¼ ; A¼ ; 3K ¼ 2M þ 3A
2ð1 þ nÞ ð1  2nÞð1 þ nÞ
Poisson’s ratio is assumed to be constant and equal to
n ¼ 0.4.
Numerical calculations were carried out for the cylindri-
cal sample placed on a moisture-impermeable plate at the
bottom (Fig. 6).
Substituting the physical relation (20) into the force
equilibrium condition (19) (with gi ¼ 0) and assuming
axial (cylindrical) symmetry leads to two coupled equations
for the radial and longitudinal displacements (ur and uz),
in cylindrical polar coordinates (r, u, z) with no depen-
dence on u

as much smaller than that in the solid skeleton;

The temperatures of the drying body constituents
@ h i

ur
are equal to one another in a given place. The Mr2 ur þ ðM þ AÞe  cðTÞ W  cðX Þ h ¼ M 2 ; ð21aÞ
@r r
numerical analysis presented in this paper is con-
fined to elastic samples in the form of cylinders.
@ h i
Mr2 uz þ ðM þ AÞe  cðTÞ W  cðX Þ h ¼ 0; ð21bÞ
@z
Drying-Induced Stresses
The mechanical state of a drying body is described by where r2 denotes the axially symmetric Laplace operator.
the coupled system of differential equations composed of The mechanical boundary conditions assume zero radial
the equilibrium of internal forces and the constitutive equa- rrr and longitudinal rzz stresses on the external surfaces,
tions relating the stresses with thermo-hydro-mechanical and zero radial ur and longitudinal uz displacements on
strains. the cylinder axis and at the bottom of the cylinder, that
The equation of the mechanical internal equilibrium is is (see Fig. 6)

rij;j þ qgi
0; ð19Þ

where rij denotes the stress tensor, q is the mass density of

the dried body, and gi is the gravity acceleration. The
gravity term is insignificant and neglected in further
considerations.
The physical relation for deformable (elastic) material
takes the form[1]

rij ¼ 2Meij þ ½Ae  cðTÞ W  cðX Þ hdij with

1 
eij ¼ ui;j þ uj;i ; ð20Þ
2

where eij is the infinitesimal strain tensor, e ¼ eii is the

infinitesimal volumetric strain, ui denotes the displacement
in the i-th direction, W ¼ T – Tr and h ¼ X – Xr are the
increments of temperature and moisture content,
c(T) ¼ (2M þ 3A)j(T), c(X) ¼ (2M þ 3A)j(X), and j(T) and
j(X) are the respective coefficients of linear thermal expan-
sion and hydro-expansion, M and A denote the elastic FIG. 6. Cylindrical sample placed on a moisture-impermeable plate
shear and bulk modules. (color figure available online).
 1394 KOWALSKI AND BANASZAK

rrr jr¼R ¼ 0 and rzz jz¼H ¼ 0; ð22aÞ rate equations for the heat and mass transfer. The
distribution and time evolution of the moisture content
ur jr¼0 ¼ 0 and uz jz¼0 ¼ 0: ð22bÞ and temperature in the cylinder can be determined from
the following system of equations[22,23]
The state of stress in the cylinder is fully described by
four components of the stress tensor; namely, rrr, ruu, qs h_ ¼ Kl r2 ðcT W þ cX hÞ  vðcT W þ cX hÞ: ð25aÞ
rzz, and rrz. The relation between radial rrr, longitudinal
rzz, circumferential ruu, shear rrz stresses and the displace-
qs cv W_ ¼ KT r2 W  lvðcT W þ cX hÞ; ð25bÞ
ments, temperature and moisture content are given by the
constitutive relations
where Kl and KT are the coefficients of moisture mass and
heat transfer, cT and cX are the thermo-diffusion and dif-
@ur
rrr ¼ 2M þ Ae  cðTÞ W  cðX Þ h; ð23aÞ fusion coefficients, cv
csv þ clv h is the total specific heat
@r of the drying body, l is the latent heat of evaporation,
@uz and v is the coefficient that affects the rate of phase tran-
rzz ¼ 2M þ Ae  cðTÞ W  cðX Þ h; ð23bÞ sition of liquid into vapor. The influence of body defor-
@r
mation on the distribution of temperature and moisture
ur content is neglected in Eqs. (25a, b) since strains are
ruu ¼ 2M þ Ae  cðTÞ W  cðX Þ h; ð23cÞ
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r assumed to be infinitesimal.

 The boundary and initial conditions for mass and heat
@ur @uz transfer are as follows (Fig. 6):
rrz ¼ M þ : ð23dÞ
@z @r
j j@B ¼ Kl gradðcT W þ cX hÞj@B  n ¼ am ðlj@B  la Þ; ð26aÞ
One of the main problems arising through the drying of
saturated porous materials is the cracking initiated by the
qj@B ¼ KT grad Wj@B  n ¼ aT ðWa  Wj@B Þ  lam ðlj@B  la Þ;
drying-induced stresses. Cracks arise when the strength of
the material is exceeded. The energetic strength hypothesis ð26bÞ
is based on the mechanical energy accumulated in the
stressed material and is formulated in terms of an overall cX grad hjz¼0 ¼ cT grad Wjz¼0 ; ð26cÞ
effective stress given by an invariant of the stress tensor
components expressed as follows qjz¼0 ¼ KT grad Wjz¼0  n ¼ aT ðWa  Wjz¼0 Þ; ð26dÞ

qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi hðr; u; z; tÞjt¼0 ¼ h0 ; Wðr; u; z; tÞjt¼0 ¼ W0 ; ð26eÞ

1
reff ¼ ðrrr  rzz Þ2 þ ðrrr  ruu Þ2 þ ðruu  rzz Þ2 þ 6r2rz :
2
Fracture of the material arises at a given point and time
when this effective stress exceeds the admissible stress
(material strength) in the drying material at a given moist-
ure content h
radm ¼ ah2 þ bh þ c
where a ¼ 3.665 [MPa], b ¼ 1.445 [MPa], c ¼ 0.028 [MPa].
Once cracking occurs, the above system of equations is
no longer valid.
As seen from Eqs. (23a, b, c), the stresses are tempera-
ture- and moisture-content-dependent. Thus, in order to
determine the state of stress, the distributions of moisture
content and temperature have to be determined first.
Drying Kinetics
Drying kinetics expresses the hydro-thermal state, which
is described by the coupled system of differential equations
composed of equations of balance of mass and energy and
where @B denotes the upper and lateral surfaces of the cyl-
ð24Þ
inder, lj@B and la denote the chemical potential of vapor at
the boundary surface and in the ambient air, am and aT are
the coefficients of the convective vapor and heat exchange
between the dried body and the ambient air, and h0 and W0
are the initial moisture content and temperature.
Condition (26a) expresses convective moisture transfer
ð25Þ and (26b) convective heat transfer between the cylindrical
sample and the ambient air. Condition (26c) expresses
hydro-insulation of the cylinder at the bottom due to the
support on the metal plate. Condition (26d) expresses con-
vective heat exchange between the cylinder and the ambient
air at the bottom through the metal plate. Condition (26c)
states the uniform distribution of moisture content and
temperature at the beginning of the process.
The driving force for vapor transfer from the body to
the surroundings is assumed to be dependent on the differ-
ence between the chemical potentials of vapor at the
boundary surface lj@B and in the surroundings la. The
chemical potentials expressed by the air temperature and
the vapor mole fraction in the air read[25]
 IDENTIFICATION OF CRACKS IN POROUS MATERIALS 1395

to include or exclude the term of phase transition, the

coefficient of phase transitions v(W,h) (Eq. (25a, b))
is postulated to be of the following binary function:
(
v 0 for h  hcr
 2
¼ hhA ð28Þ
v0 1 hcr hA for hA  h  hcr

where v0(W) is the temperature-dependent phase transition

efficiency, hcr denotes the critical moisture content, and
hA is the moisture content at the final stage of drying, being
in equilibrium with the ambient air. In the CDRP (h  hcr),
the phase transition inside the body is neglected as a very
small one in comparison to that at the body surface.
The moisture transport inside the body is dependent on
both the liquid physical properties and the body structure,
that is
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rðWÞ
Kl ðW; hÞ ¼ f ðhÞ; ð29Þ
gðWÞ

where r(W) ¼ 75(1  0.002W) and g(W) ¼ 183  105 

FIG. 7. Drying curve and the conditions inside the dryer (color figure (1 þ 0.053W)1 denote the surface tension and liquid
available online).
viscosity as functions of temperature, and f(h) is the
moisture transport parameter distinguished in the two
lj@B  la ¼ 0:462Ta lnðxj@B =xa Þ stages of drying as follows[23]
ð27Þ (
 ð7:36  0:462 ln xj@B ÞðT j@B  Ta Þ; 1 for h  hcr
f ðhÞ  2
¼ hhA ð30Þ
f0 hcr hA for hA  h  hcr
where Tj@B and Ta are the temperatures and xj@B and xa
the mole fractions of vapor at the cylinder surface and
in the surroundings. where f0 is the parameter dependent on the body structure
In order to consider moisture transfer mechanisms determined numerically and experimentally from drying
suitable for the constant drying rate period (CDRP) and curves.
the falling drying rate period (FDRP), and in particular The coefficient of heat conduction is considered to be an
average of heat conduction through skeleton KsT and
moisture KlT [24]

KT ¼ ð1  /ÞKsT þ /hKlT ; ð31Þ

where / denotes the porosity.

FIG. 8. Distribution of stresses at the bottom surface of the cylinder
(H ¼ 0) along radius r: (a) individual stresses rrr, rzz, ruu; (b) admissible
and effective stresses, radm, reff, (radm – reff). The places at which (radm –
reff) < 0 denote violation of the admissible strength (color figure available
online).
RESULTS
Numerical calculations were carried out for a cylindrical
sample placed on a moisture-impermeable plate (Fig. 6).
Calculations of the time evolution of temperature and
moisture content as well as the distribution of temperature,
moisture content, and stresses in the cylindrical sample
were performed for the data given in Table 2.
The thermal coefficients for water, water vapor, and
moist air are tabled in a range from 0 to 100
C with a step
of one degree in the textbooks.[26–28] The coefficients of
convective vapor transfer am and convective heat transfer
aT were estimated experimentally on the basis of drying
processes carried out in air temperature Wa ¼ 41.5
C.[22]
 1396 KOWALSKI AND BANASZAK
TABLE 2
Data for numerical calculations
KsT ¼ 1.78 W=m  K KlT ¼ 2.32 W=m  K
cT ¼ 0.52 J=kg  K cX ¼ 3.06 J=kg
am ¼ 8.64  105 kg  s=m4 aT ¼ 40 W= m2  K
Wa ¼ 70
C Wn ¼ 50
C
3
qs ¼ 2640 kg=m / ¼ 0.35
2 3
M ¼ 6.25  10 MPa A ¼ 10 MPa
Cr ¼ 29.653 h0 ¼ 40%
Some data for vapor pressure were taken from Molnar,[29]
and those referring to the moisture diffusivity from
Marinos-Kouris and Maroulis.[30]
Figure 7 presents the drying curve for given drying con-
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ditions; i.e., humidity and temperature of the drying
medium. The sample was dried at 120
C and the equivalent
humidity of hot air was registered for this temperature.
One can notice that the humidity slightly rises between
15–130 min of drying, which is caused by the evaporated
water from the sample. After 100–120 min, one can observe
the beginning of the falling drying rate period (FDRP).
Distributions of radial rrr, longitudinal rzz, and circum-
ferential ruu stresses along radius r at the bottom surface
of the cylinder (H ¼ 0) are presented in Fig. 8a (see
also [23]). Figure 8b presents the distribution of admissible
radm and effective reff stresses and their difference at the
surface mentioned above.
Figure 9a illustrates the evolution of the moisture
content at the bottom of the cylinder. A crack in the
convectively dried sample is predicted to occur at spots
of the cylinder where the stress (radm – reff) reaches
a maximum. Figure 9b presents the time evolution of the
difference between admissible and effective stresses.
As follows from Fig. 9b, the crack is most probable to
occur at the cylinder surface where (radm – reff) < 0.
Figure 10 presents the time evolution of the effective
stresses in different points of the cylinder.
FIG. 9. Time evolution of the drying effects: (a) distribution of moisture
content along radius r; (b) distribution of stress difference (radm – reff)
along radius r (color figure available online).
csv ¼ 728.5 J=kg  K clv ¼ 4186 J=kg  K
j(X) ¼ 2.4  103 j(T) ¼ 3  108 1=K
v0 ¼ 2.5  106 kg  s=m5 f0 ¼ 6  107 kg  s2=m4
xa ¼ 0.075 l ¼ 2300 kJ=kg
H ¼ 0.06 m R ¼ 0.03 m
r0 ¼ 142 858 Pa rX ¼ 1 688 320 Pa
hcr ¼ 15% hA ¼ 5%
The effective stress is zero at the beginning, then starts
to increase, attaining a maximum at some time, and finally
tends to zero. The maximum of the effective stresses is
reached at the top of the cylinder in the point (r ¼ 0,
z ¼ H). Figure 10 allows us to estimate the time at which
the crack formation may occur. This numerically predicted
moment of possible material damage was monitored
experimentally with the acoustic emission (AE) method.
In our experiments, a two-point AE technique was used
to monitor the development of fractures and, indirectly,
drying-induced stresses. Two AE sensors were fixed to
the sample, one at the upper and the other at the lower
sample surfaces, so that the AE signals were registered on
both surfaces (Fig. 6). The sample with the fixed AE sen-
sors was suspended to the balance to measure the reduction
of moisture mass in time and, simultaneously, the develop-
ment of cracks in the sample. The drying experiment was
performed in extremely harsh, dried conditions (high tem-
perature and low air humidity) to excite easier fracture
appearances in the sample and to obtain better AE activity.
Figure 11 presents the number of registered AE signals
per unit time during drying.
As is seen in Fig. 11, most of these signals were evi-
denced in the CDRP, which can be explained by the ten-
sional stresses that arise at the external layers of the
cylinder due to shrinkage. The surface of the body becomes
drier, while its core is still kept wet. The AE hits rate
descriptor is strictly connected with the development of
FIG. 10. Time evolution of the effective stresses reff in different points of
the cylinder (color figure available online).
 IDENTIFICATION OF CRACKS IN POROUS MATERIALS
FIG. 11. The number of AE signals per time period of 60 s for drying
temperature of 120
C (color figure available online).
the drying-induced stresses, so this descriptor offers a good
Downloaded by [Aston University] at 03:47 09 January 2014
tool for on-line prediction of approaching material destruc-
tion. So, one can state that the intensity of AE signals and
the time of their occurrence are both related to the
development of the drying-induced stresses.
Figure 12 illustrates the rise of mean acoustic energy
referred to as a single hit during the drying process.
Although most of the AE signals were evidenced in the
CDRP, they turned out to be of low energy in general.
These signals are referred to as stresses involving rather
inelastic shape deformations of still strongly wet material,
which caused dissipation of the accumulated energy inside
the material. In the FDRP fewer signals were observed, but
their mean energy per hit was much higher than those aris-
ing in the CDRP. This is because in the FDRP the surface
became dry, so the formed cracks released stronger elastic
energy propagating through the material.
Figure 13 presents the total energy of the AE signals.
Monitoring of the total AE energy of all AE signals makes
it possible to foresee the final quality of the dried samples.
FIG. 12. The mean acoustic energy of a single hit during drying.
1397
FIG. 13. Total energy of AE signals (color figure available online).
A highly fractured material is qualified as a bad-quality
one. The description of total energy released may serve as
an indicator as to whether the dried product is of good
or bad quality at the end-state. Strong cracks in the body
structure release high energetic EA signals. The high and
medium energetic signals are evidenced in Fig. 13 as the
straight, upright lines. In some cases the high energetic sig-
nals denote macro cracks or material splits that are visible
on the sample surface. Thus, from the analysis of the total
AE energy description one can deduce whether the dried
product is of good or bad quality.
The fractures of materials subjected to drying are more
likely to take place in fair-sized dried products and when the
drying conditions are severe (e.g., too high temperature or
too low drying medium humidity). An optimal drying process
should be able to eliminate or minimize the high or medium
energetic AE impulses by the drying. The majority of notified
AE signals ought to be low energetic (horizontal or almost
horizontal lines in Fig. 13). Such an AE energy descriptor
would mean a lack of destruction of the dried products.
The AE method can be applied not only to register the
time of the crack commences in the drying sample on-line,
but also to localize the cracks in the sample. Localization
of fractures by the AE method can be possible when
FIG. 14. Localization of fractures during drying: (a) AE source locations
(the energy of AE hits is represented by the circle sizes); (b) visible
fractures on a kaolin sample after drying (color figure available online).
 1398 KOWALSKI AND BANASZAK

responsible for this phenomenon the drying-induced

FIG. 15. Fractures in the dried cylinders (left) and their position (right)
as observed under a microscope (color figure available online).
using two or more acoustic sensors distributed around the
sample. Figure 14 presents the results of AE source locations
on the sample height as a function of the drying time for the
dried kaolin cylinder. Energetic enhancements of the AE hits
are represented by the circle sizes in Fig. 14. As was already
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stresses, which result from a non-uniform distribution of
the moisture content and thus a non-uniform shrinkage
of the body during drying. The gradient in the moisture
content distribution increases with the drying rate and
the size of the body, and is inversely related to the per-
meability of the porous structure. The cohesion force, on
the other hand, is proportional to the body particle size
and inversely proportional to the square of inter-particle
distance. The latter evidently depends on the moisture con-
tent, which causes the porous body to swell.
Based on the considerations presented in this paper, one
can conclude that a rigorous mechanistic drying model
enables a realistic simulation of the stresses induced in dry-
ing materials and determines where and when the spatial
and temporal maxima of the effective stress responsible
for crack formation occur.
The difference between the effective stress and the

shown on the total energy descriptor (Fig. 13), the AE

hits were generated during the whole drying process. Some admissible stress expressed as a function of the moisture
of them were generated at the initial stage of drying near content enables identification of the spots at the time of
the upper and bottom surfaces of the cylinder where the crack initiation in a dried body.
AE sensors were attached. Unfortunately, at the very begin- The acoustic emission (AE) technique enables early
ning of drying some AE signals come from the heating of detection of crack initiation in a drying body, and thus
the AE sensors. It was difficult to decide which AE signals the operator can be alerted early enough to change the dry-
at this stage of drying originated from the deformed sample ing conditions to prevent the development of the fracture
and which came from other sources. phenomenon.
We observed a greater concentration of AE hits near the Among the several AE descriptors, the most informative
bottom of the sample in the first 60 min of drying, but are the total number and the total energy of AE signals.
these hits were of low AE energy. The reason for the gene- The rapid increase of the total AE energy indicates the
ration of these hits is partly the free shrinkage of wet and occurrence of a macro-crack in the body.
still deformable kaolin material at the bottom that causes The multichannel AE system can provide on-line infor-
rubbing of its grains against the aluminum plate. Energeti- mation about acoustic source locations. These locations
cally higher AE hits were generated later and were mostly can indicate areas where the material suffers destruction
located at the top of the sample. In the FDRP (i.e., between (deformations, fractures). It is very useful, especially in
100 and 120 min of drying), the appearance of fractures was situations where there is no possibility of external obser-
observed near and along the upper cylinder surface (Fig. 14). vation of the sample.
The fractures were propagated along the circumference
of the cylinder (A, B, C). The system of cracks was finally
NOMENCLATURE
expanded in the direction of the bottom of the cylinder (D,
E, F) during the last hour of the drying process. This is
confirmed by the AE signals in the middle of the cylinder A elastic bulk modulus MPa
at 240 min of drying (Figs. 14a and 15). cv specific heat J=kg  K
Figure 15 illustrates the final damage of the kaolin cT coefficient of thermodiffusion J=kg  K
sample after convective drying in hot air at a tem- cX coefficient of diffusion J=kg
perature of 120
C. This photograph confirms both the eij strain deviator 1
theoretical prediction based on the mechanistic drying f(h) moisture transport parameter kg  s2=m4
model and the experimental monitoring done with gi gravity acceleration m=s2
the AE method. H cylinder height m
j moisture flux kg=m2  s
l latent heat of evaporation J=kg
CONCLUSIONS K elastic volumetric modulus MPa
There is no generally accepted explanation for the crack- M elastic shear modulus MPa
ing phenomenon of solid materials during drying. Some m total mass of dried sample g
statements resulting from experimental observations render p pressure Pa
 IDENTIFICATION OF CRACKS IN POROUS MATERIALS 1399

R cylinder radius m 7. Couture, F.; Bernada, P.; Roques, M.A. Continuous thermome-
chanical models using volume-averaging theory. In Modern Drying
r radial coordinate m Technology, Vol. 1; Tsotsas, E., Mujumdar, A., Eds.; Wiley-VCH
< individual gas constant J=kg  K Verlag GmbH & Co. KgaH: Weinheim, Germany, 2007; 103–154.
sij stress deviator Pa 8. Kowalski, S.J.; Banaszak, J.; Rybicki, A. Plasticity of materials
t time s exposed to drying. Chemical Engineering Science 2010, 65,
tR relaxation time s 5105–5116.
9. Perre, P.; Remond, R.; Turner, I.W. Comprehensive drying models
T temperature K based on volume averaging: Background, application and perspective.
ur, uz displacements m In Modern Drying Technology, Vol. 1; Tsotsas, E., Mujumdar, A.,
xa, xn mole fractions of vapor in air 1 Eds.; Wiley-VCH Verlag GmbH & Co. KgaH: Weinheim, Germany,
X moisture content (dry basis) 1 2007; 1–55.
Xcr critical moisture content 1 10. Mihoubi, D.; Bellagi, A. Two-dimensional heat and mass transfer dur-
ing drying of deformable media. Applied Mathematical Modelling
XA final moisture content 1 2008, 32, 303–314.
z longitudinal coordinate m 11. Kowalski, S.J.; Perre, P., Guest Eds. Special issue: Damage of
Greek letters materials by drying: Modeling, numerical simulations, experimental
am vapor transfer coefficient kg  s=m4 studies. Drying Technology: An International Journal 2009, 27(78).
aT heat transfer coefficient W=m2  K 12. Kowalski, S.J. Control of mechanical processes in drying: Theory and
experiment. Chemical Engineering Science 2010, 65, 890–899.
jv viscous bulk modulus Pa  s 13. Kowalski, S.J.; Banaszak, J.; Rybicki, A. Damage analysis of microwave-
j(T) coefficient of thermal expansion 1=K
Downloaded by [Aston University] at 03:47 09 January 2014

dried materials. AIChE Journal 2012, 58(7), 2097–2104.

j(X) coefficient of humid expansion 1 14. Rajewska, K.; Kowalski, S.J. Acoustic emission as a method of
eij strain tensor 1 monitoring of fracture phenomena in dried materials. Diagnostics
e volumetric strain 1 2002, 27, 95–101 (in Polish).
15. Kowalski, S.J.; Banaszak, J.; Rajewska, K. Acoustic emission in dried
/ porosity 1 materials. Chemical Engineering and Apparatus 2003, 4, 3–8 (in Polish).
rij stress tensor Pa 16. Ranachowski, J., Ed. Problems and Methods of Modern Acoustics;
radm admissible stress Pa National Scientific Publisher (PWN): Warsaw, 1989 (in Polish).
rred reduced stress Pa 17. Banaszak, J.; Kowalski, S.J. Theoretical and experimental analysis of
r0, rX components of admissible stress Pa stresses and fractures in clay like materials during drying. Chemical
Engineering and Processing 2005, 44(4), 497–503.
r spherical stress, surface tension Pa, N=m 18. Cho, G.C.; Santamarina, J.C. Unsaturated particulate materials:
q mass density kg=m3 Particle-level studies. Studies of Geotechnical and Geoenvironmental
l chemical potential J=kg Engineering 2001, 1, 84–96.
g viscosity Pa  s 19. Pampuch, R. Ceramic Materials; National Scientific Publisher
v rate of phase transition kg  s=m5 (PWN): Warsaw, 1989 (in Polish).

20. Griffith, A.A. The phenomena of rupture and flow in solids.
W ¼ T – Tr increment of temperature C Philosophical Transactions of the Royal Society of London 1920, Series
h ¼ X – Xr increment of moisture content 1 A (221), 163–198.
Kl moisture transport coefficient kg  s=m3 21. Siedov, L.I. Macroscopic Theories of Matter and Fields: A Thermodynamic
KT thermal conductivity W=m  K Approach; Mir Publisher: Moscow, 1983.
22. Kowalski, S.J.; Rybicki, A. The vapour-liquid interface and stres-
ses in dried bodies. Transport in Porous Media 2007, 66(1–2),
ACKNOWLEDGMENT 43–58.
This work was carried out as part of the research project 23. Kowalski, S.J.; Rybicki, A. Cohesive strength of materials during
drying processes. Drying Technology 2009, 27(7), 863–869.
N N209 104337 sponsored by the Ministry of Science and
24. Musielak, G. Modelling of the heat and mass transport phenomena in
Higher Education. kaolin during the first and the second periods of drying. Chemical and
Process Engineering 2004, 25, 393–409.
REFERENCES 25. Szarawara, J. Chemical Thermodynamics; Scientific-Technical
1. Kowalski, S.J. Thermomechanics of Drying Processes; Springer Verlag: Publisher (WNT): Warsaw, 1985 (in Polish).
Heidelberg, 2003. 26. Pikoń, J.; Hehlmann, J.; Sa˛siadek, B.; Janowicz, R. Chemical Apparatus;
2. Kachanov, L.M. Introduction to Continuum Damage Mechanics; M. Silesian Technical University Publisher: Gliwice, 1974 (in Polish).
Nijhoff: Boston, 1986. 27. Strumiłło, C. Foundations of Theory and Technology of Drying;
3. Hasatani, M.; Itaya, Y. Drying induced strain and stress: A review. Scientific-Technical Publisher (WNT): Warszawa, 1983 (in Polish).
Drying Technology 1996, 14(5), 1011–1040. 28. Wiśniewski, S.; Wiśniewski, T.S. Heat Exchange; Scientific-Technical
4. Katekawa, M.E.; Silva, M.A. A review of drying models including Publisher (WNT): Warsaw, 1997 (in Polish).
shrinkage effects. Drying Technology 2006, 26(1), 5–21. 29. Molnar, K. Experimental techniques in drying. In Handbook of Industrial
5. Scherer, G.W. Theory of drying. Journal of American Ceramic Society Drying; Mujumdar, A.S., Ed.; Taylor & Francis: New York, 2007.
1990, 73(1), 1–14. 30. Marinos-Kouris, D.; Maroulis, Z.B. 2007. Transport properties in the
6. Chemkhi, S.; Zagrouba, F.; Bellagi, A. Mathematical model for drying drying of solids. In Handbook of Industrial Drying; Mujumdar, A.S.,
of highly shrinkable media. Drying Technology 2004, 22(5), 1023–1039. Ed.; Taylor & Francis: New York, 2007.