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Journal of the European Ceramic Society xxx (2014) xxxxxx

Investigation of the impact of micro-cracks on fracture behavior of magnesia

products using wedge splitting test and digital image correlation
Y. Belrhiti a, , O. Pop b , A. Germaneau c , P. Doumalin c , J.C. Dupr c ,
H. Harmuth d , M. Huger a, , T. Chotard a,e,
a

Science des Procds Cramiques et Traitements de Surface (SPCTS UMR CNRS 7315), CEC, 12 rue Atlantis, 87068 Limoges Cedex, France
b Groupe dEtude des Matriaux Htrognes (GEMH), Universit de Limoges, 12 rue Atlantis, 87068 Limoges Cedex, France
c Institut Pprime, CNRS, Universit de Poitiers, 11 Boulevard Marie et Pierre Curie, 86962 Futuroscope Chasseneuil Cedex, France
d Montanuniversitt Leoben, Department of Ceramics, Peter-Tunner-Strasse 5, A-8700 Leoben, Austria
e Institut Universitaire Technologique du limousin, Dpartement GMP, 2 Alle Andr Maurois, 87065 Limoges Cedex, France
Received 6 December 2013; received in revised form 1 September 2014; accepted 2 September 2014

Abstract
For refractory materials, a large strain behavior before failure is desired to improve their thermal shock resistance during their service life in
industry. Their microstructure (micro-cracked) induces a non-linear mechanical behavior.
The present paper aims at applying digital image correlation (DIC) during wedge splitting test on magnesia spinel sample and comparing it to
pure magnesia sample so as to study the influence of spinel addition on fracture behavior. From strain measurements based on DIC, the initiation
and the propagation of the macro-crack are investigated and the development of micro-cracks network in the case of magnesia spinel which is
behind crack branching phenomenon is analyzed. The evolution of the fracture energy required in crack propagation is studied for each material.
The experimental results highlight also their mechanical properties dependent on their microstructure.
2014 Elsevier Ltd. All rights reserved.
Keywords: Fracture; MgO; Spinels; Refractories; Digital image correlation

1. Introduction
In refractory industry, the ability to sustain severe thermal
shocks is of prime importance in order to increase the length
of the refractory material life and to avoid their failure. These
characteristics are generally obtained by the development
of specific microstructure patterns on well-chosen refractory
materials. Among the materials used in refractory industry
magnesia refractories are to be good candidates due to their
thermo-mechanical properties at room and elevated temperature. Due to their properties, pure magnesia and magnesia

Corresponding authors. Tel.: +33 5 87 50 25 60.

Corresponding author at: Science des Procds Cramiques et Traitements
de Surface (SPCTS UMR CNRS 7315), CEC, 12 rue Atlantis, 87068 Limoges
Cedex, France. Tel.: +33 5 87 50 25 60.
E-mail addresses: younes.belrhiti@etu.unilim.fr (Y. Belrhiti),
marc.huger@unilim.fr (M. Huger), thierry.chotard@unilim.fr (T. Chotard).

spinel materials showed a great interest for commercials

and researchers.1,2 Pure magnesia bricks are known by their
resistance to corrosion and their relatively low thermal shock
resistance. Besides, the incorporation of spinel improves the
thermal shock resistance and can extend to three times longer
service life of cement rotary kiln3 compared to conventional
magnesia chrome bricks. Indeed, spinel addition, leads to a better adaptability of the material to severe solicitations generated
during high and quick temperature variations. Magnesia spinel
refractories still preferable to magnesia chromite ones which
are not recommended because of their toxicity due to chromite
contain. These two types of refractory have nearly the same
properties such as a high thermal shock resistance.
Even if their process of processing can affect the economy,
but they still preferable to magnesia chromite refractories which
have nearly the same properties such as their high resistance
against thermal shock damage, erosion and corrosion but are not
recommended due to the toxicity of waste refractories containing
chrome.

http://dx.doi.org/10.1016/j.jeurceramsoc.2014.09.001
0955-2219/ 2014 Elsevier Ltd. All rights reserved.

Please cite this article in press as: Belrhiti Y, et al. Investigation of the impact of micro-cracks on fracture behavior of magnesia products using
wedge splitting test and digital image correlation. J Eur Ceram Soc (2014), http://dx.doi.org/10.1016/j.jeurceramsoc.2014.09.001

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The behavior of magnesia spinel is related to their microstructure and especially to the difference between the thermal
expansion of magnesia and spinel which is behind the development of micro-cracks around the spinel grains and can
prevent crack propagation generated by thermal shock.47
Moreover, their microstructure induces a significant non-linear
stressstrain mechanical behavior allowing a high strain to
rupture, high fracture energy and as a consequence improves
their thermal shock resistance. It has been reported that microcracking caused by the addition of spinel reduces both strength
and stiffness, and affect the fracture behavior.68 Both the
knowledge of the mechanisms initiating such behavior and the
possibility to characterize those in the best accurate way are
essential.
From these considerations, this study is a part of a work aiming to understand the relationship between microstructure and
the non-linear mechanical behavior of magnesia-spinel materials and compared to pure magnesia materials.
The fracture characterization is conducted through wedge
splitting test (WST) results. This test is well known for its ability to produce reliable data on stable crack propagation.915
This means that material characterization quality depends on
test evaluation.
To assess to strain measurements based on DIC on material
surface, digital image correlation technique has been chosen.
This full-fields practical and effective tool for quantitative displacement and strain measurement of a planar sample surface is
now widely accepted and commonly used in the field of experimental mechanics. This non-contact optical method compares
digital images of the sample surface obtained before and during
deformation.1626 It allows highlighting the crack branching
phenomenon. It is a complex process of heterogeneous materials
in which crack propagation induces the coalescence of existing
branches that correspond to existing micro-cracks. Such phenomenon occurs due to the particularity of the microstructure of
magnesia spinel materials.

2. Materials and methods

2.1. Materials
Pure magnesia and magnesia 15%-spinel (MSp) used in
this study were processed from different grain distribution
of industrial magnesia with low iron content (fines < 0.1 mm;
01 mm; 13 mm; 35 mm) and additional sub-stoichiometric

Magnesia matrix

Microcracks
Spinel inclusion

Fig. 1. Microstructure of magnesia-spinel material.

spinel (13 mm) in the case of MSp. Spinel grains replaced the
same content of magnesia aggregates having the same amount.
Their processing was done using a maximum pressure of
140 MPa and a maximum firing temperature of 1600 C.
Information concerning these materials such as granulometry, density and porosity are given in Table 1.
Due to the thermal expansion mismatch existing between
the magnesia matrix (the whole material except spinel inclusions) and the spinel inclusions (MgO = 13.3 106 K1 and
MgAl2 O4 = 8.9 106 K1 ), it appears that there are some
micro-cracks around the spinel inclusions (Fig. 1). These microcracks appear during the cooling stage of the process conferring
the material a thermally damaged character.
From each type of material, two cubic-shaped specimens with
cross-section of 100 100 100 mm3 were tested, although, in
this paper only one will be presented since the results are quite
similar.
2.2. Wedge splitting test
A more recent and widely accepted test, which has been
used frequently for materials with coarse microstructures, is
the method patented by Tschegg under the name wedge splitting test.10 This technique is being used by a numerous
research centers and universities, as well as by manufacturers
of refractories.27,28
As shown in Fig. 2b the WST consists of opening a crack
using a wedge. The principle of this test is to apply a vertical
force FV received from the device which is transformed in a
much higher horizontal force FH causing a symmetrical opening
mode of the crack. Samples were equipped with a groove in order
to apply the splitting load and a starter notch.
Since the thermal shock resistance of these materials has to be
improved, the brittleness of these materials has to be reduced and

Table 1
Granulometry and properties of MgO-15% spinel samples compared to pure magnesia samples.

Granulometry

Properties

Spinel 13 mm (%)
MgO 35 mm (%)
MgO 13 mm (%)
MgO 01 mm (%)
MgO fines (<0.1 mm) (%)
Bulk density (g cm3 )
Total porosity (%)

Pure MgO

MgO-15% spinel

0
13.5
34.0
24.0
28.5
2.98
17.5

15
13.5
19.0
24.0
28.5
2.95
15.3

Please cite this article in press as: Belrhiti Y, et al. Investigation of the impact of micro-cracks on fracture behavior of magnesia products using
wedge splitting test and digital image correlation. J Eur Ceram Soc (2014), http://dx.doi.org/10.1016/j.jeurceramsoc.2014.09.001

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Fig. 2. Principle of wedge splitting test with samples geometry (a) and image acquisition setup (b).

the deformation before cracking has to be higher by modifying

the microstructure of the refractory.
Then, from the experimental data in terms of loaddisplacement, the surface fracture energy GF (N m1 ) is defined
as the mean work per unit of projected fracture area required
to propagate a crack, and represented by the sum of distinct
energies consumed during the crack propagation process (elastic energy and dissipated one) due to the crack bridging, the
spinel interlocking, shear in zigzag fracture planes and other
mechanisms. GF is calculated using Eq. (1).

max
1
GF =
FH dH
(1)
A
0

where A is the area of the crack surface projection, FH is the

horizontal force and H is the horizontal deformation. This surface fracture energy is calculated for values from zero up to
the displacement max corresponding to 10% of the maximum
load.
The horizontal force FH is calculated from the vertical force
FV neglecting any friction effects using the Eq. (2).
FH =

FV
2 tan(/2)

(2)

where is the wedge angle. The fact that FH is much higher than
FV reduces the load applied on the machines frame and storing
less elastic energy in it and helping stable crack propagation.
Another mechanical property of material estimated from the
WST is the nominal notch tensile strength NT . It represents

the stress at the point of beginning of rupture when the stress

concentration at the notch tip is neglected, is calculated by the
Eq. (3).
NT =

6 y FH,max
FH,max
+
2
bh
bh

(3)

Where b (mm), h (mm) are samples dimensions and y (mm)

is the distance between FH,max and the middle of h as shown in
Fig. 2a.
In addition to the experimental setup, a 8-bits CMOS camera
(1600 1900 pixels2 ) used to record images is placed in front of
the speckled surface in order to perform optical measurements
thanks to digital image correlation (Fig. 2b). This allows studying crack growth during mechanical tests and the strain state
around the crack tip. The acquisition frequency was 1 image/s.
2.3. Digital image correlation technique
The damage level neighborhood to the crack tip and the
crack advancement are estimated from the strain cartographies
obtained by DIC. This full fields optical method is based on
the analysis of successive digital images of a same sample during a mechanical test. The displacement fields are obtained by
measuring the degree of similarity of series of subsets between
the image corresponding to an unloaded state and the deformed
image recorded during the test. The zone of interest (ZOI), on
which the calculation is done, is represented in Fig. 2a. Each
pixel of these images stores a gray level value due to a pattern
at the surface. To avoid ambiguities in the similarity process a

Please cite this article in press as: Belrhiti Y, et al. Investigation of the impact of micro-cracks on fracture behavior of magnesia products using
wedge splitting test and digital image correlation. J Eur Ceram Soc (2014), http://dx.doi.org/10.1016/j.jeurceramsoc.2014.09.001

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random distribution of gray levels can be used called speckle

pattern. This pattern can be the natural texture of the specimen surface or artificially made by spraying black and/or white
paints. As an example for samples surface preparation, a black
opaque paint layer is deposited on the surface of sample then
dried. After that, white speckles will be carefully projected on
using spray paint.
The used DIC process consists in calculating displacements
on specific points of several subsets which constitute a grid.
From these displacements, strains will be calculated. The principle of this technique is represented in Fig. 3 and equations used
for the calculation of displacements are detailed in the previous
study.29
3. Results and discussion
3.1. Mechanical properties
Fig. 4 represents the characteristic horizontal load vs.
displacement curves of pure magnesia and magnesia spinel
materials obtained by wedge splitting test.
Horizontal load vs. displacement curve of MSp presents a
non-linear mechanical behavior up to the peak with a significant
post-peak region and residual strain when unloading. Moreover,
the increase of spinel content seems mainly to lower the maximum load and to enhance the pre-peak non-linearity of the
mechanical behavior. This material has a higher strain and a
low mechanical resistance in comparison with pure magnesia;
this can be explained by the higher volume of micro-cracks in the
case of MSp developed during cooling and toughening mechanisms occurring around the crack, especially in the following
wake region, which may increase the resistance to crack propagation. As explained before, the higher volume of micro-cracks
in the case of magnesia spinel is due to the difference between
the thermal expansion coefficient of magnesia and spinel which
leads to the apparition of micro-cracks around the grain of spinel.
In addition to that, pure magnesia affords a lower strain at
the peak, and a thinner peak due to a smaller post-peak region
in comparison with MSp.
In the two cases, the mechanical behavior of these materials is
characterized by three phases. One corresponding to the elastic
behavior, a second one characterized by the elastic behavior
coupled with damage increased by the addition of spinel and
this phase is usually referred as localization of macro-crack,
and the last one corresponding to the crack growth.
Only the main macro-crack can be easily observed, but the
early apparition of the macro-crack, as well as all the stressed
micro-cracks pre-existing around the middle plane, is not really
visible. That is why; strain fields calculated from displacement
fields were chosen so as to analyze the crack propagation and
the presence of damage process.
Thanks to digital image correlation, the evolution of the
strains along X-axis has been represented for different instants
corresponding to different loading states (Fig. 4). These maps
correspond to the zone of interest ZOI defined in Fig. 2a. According to DIC principle, this area is subdivided using subsets of
32 32 pixels2 with a gap of 8 8 pixels2 and a scale factor of

Table 2
Nominal notched tensile strength and surface fracture energy values.

Pure MgO
MgO-15%
spinel

NT (MPa)

GF (N m1 )

GF / NT (mm) 103

14.36
14.38
6.65
6.75

206.50
182.00
361.00
396.00

14.39
12.66
54.25
58.63

0.067 mm/pixels. Four maps were represented in Fig. 4a and b.

Crack presence and its opening correspond to the local higher
strain values (Fig. 4). To underline these latter, a specific strain
color scale has been chosen. The choice of colors was done
first in order to identify the evolution of local higher strains
(from gray to red) and to eliminate measurement disturbance
(black color). A presence of a crack corresponds to a threshold
higher than 0.001 (gray color) taking into account the accuracy
of measurement.
For the two materials, the initiation and the propagation of the
crack take place after reaching critical load (FH,max ). Besides,
before reaching this critical load, there is a development of damage zone in the neighborhood of the crack tip in the case of MSp.
This zone gets larger and moves with the increase of the applied
load and the propagation of the crack unlike the case of pure
magnesia in which there is a lack of damage associated to the
coalescence of the micro-cracks.
Nominal notch tensile strength and surface fracture energy
for each sample have been calculated thanks to the Eqs. (1) and
(3) and represented in Table 2.
These fracture parameters introduced in Table 2 show that
the mechanical resistance decreases and the fracture resistance
increases with the increase of the spinel rate. The ratio GF / NT
is a parameter of the brittleness of the material: the more brittle
material is, the lower value of the ratio is.
Fig. 4a and b represent also the evolution of the total energy
during the test. The total energies are deduced from the total
area under horizontal load vs. displacement curves obtained by
wedge splitting test divided by final crack surface and represent
the sum of the elastic energy and dissipated one. The curves
confirm that during the test, the total energy is higher in the case
of MSp than pure magnesia. The high dissipated energy in the
case of MSp is due to the dense network of micro-cracks created
during the crack initiation and propagation.
3.2. Crack branching phenomenon
To underline the presence of damage process, this study
focused also on the strains along X and Y axis created by the
propagation of the crack during wedge splitting test. Indeed,
crack growth in heterogeneous materials is often a very complex process, featuring many different physical mechanisms. In
brittle materials, the damage is quite absent or confined in a
small area. To underline its presence, different maps of strains
along X and Y axis were obtained using digital image correlation
at different loads (Figs. 5 and 6).
Unlike pure magnesia, in addition to X-axis strains which
have the same direction as the crack opening, we notice the

Please cite this article in press as: Belrhiti Y, et al. Investigation of the impact of micro-cracks on fracture behavior of magnesia products using
wedge splitting test and digital image correlation. J Eur Ceram Soc (2014), http://dx.doi.org/10.1016/j.jeurceramsoc.2014.09.001

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Fig. 3. Principle of digital image correlation method.

presence of strains along Y-axis perpendicular to the crack opening direction. However, their intensity stills lower than X-axis
strains. Y-axis strains are related to the creation of micro-cracks
around grains of spinel during mechanical test. This is due to
the difference of the expansion coefficient of MgO and spinel.
In the case of MSp, thanks to xx strains obtained by digital
image correlation results, we notice the complexity of crack
growth in heterogeneous materials which feature many physical
mechanisms such as crack branching phenomenon. It results of

many interacting micro-cracks or micro-branches (coalescence

of micro-cracks). Besides, the branches evolve from the microcracks which are initially parallel to the main crack, but deviate
smoothly from the original crack orientation.
As perspectives, it is worth mentioning that experimental
results obtained by digital image correlation can be coupled
with numerical results by finite element simulation in order
to have access to nonlinear stressstrain laws. Besides, fracture parameters could be determined also using digital image

Fig. 4. Horizontal load vs. displacement and energy curves of pure magnesia (a) and magnesia-15% spinel (b) obtained thanks to WST.

Please cite this article in press as: Belrhiti Y, et al. Investigation of the impact of micro-cracks on fracture behavior of magnesia products using
wedge splitting test and digital image correlation. J Eur Ceram Soc (2014), http://dx.doi.org/10.1016/j.jeurceramsoc.2014.09.001

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Fig. 5. Maps of longitudinal strains along X axis (a) and Y axis (b) for pure magnesia sample.

Fig. 6. Maps of longitudinal strains along X axis (a) and Y axis (b) for magnesia spinel sample.

Please cite this article in press as: Belrhiti Y, et al. Investigation of the impact of micro-cracks on fracture behavior of magnesia products using
wedge splitting test and digital image correlation. J Eur Ceram Soc (2014), http://dx.doi.org/10.1016/j.jeurceramsoc.2014.09.001

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correlation using energetic methods such as the integral invariant

method.
8.

4. Conclusion
9.

This study was dedicated for a better understanding of the

relationship between mechanical behavior of products and their
microstructure. To do so, magnesia spinel materials have been
investigated and compared to pure magnesia materials. The difference between the mechanical behaviors of these materials
is due to the development of the network of micro-cracks in
the case of magnesia-spinel materials. This is a consequence of
the thermal expansion mismatch between magnesia and spinel
grains. To study the mechanisms of micro-cracking and the
influence of damage on the non-linearity, wedge splitting test
has been associated (instrumented) to digital image correlation.
Indeed, by the calculation of mechanical properties such as nominal notch tensile strength and fracture energy in addition to
the measurement of strain fields, the influence of the addition
of spinel is clarified. In fact, it was confirmed that the addition of spinel influences clearly mechanical properties and the
non-linearity of the mechanical behavior due to the presence of
high level of damage induced by micro-cracks as shown thanks
to digital image correlation. This microstructure optimization
allows an increase of strain-to-rupture of refractories, which
is considered as a key parameter for improving thermal shock
resistance.

10.

11.

12.

13.

14.

15.
16.

17.
18.

19.

Acknowledgements
20.

This work is a part of a global research program engaged

through collaboration between the University of Leoben
(Austria) and ENSCI (Limoges, France) thanks to the F.I.R.E
network. The authors are thankful to RHI AG for providing the
materials.

21.

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Please cite this article in press as: Belrhiti Y, et al. Investigation of the impact of micro-cracks on fracture behavior of magnesia products using
wedge splitting test and digital image correlation. J Eur Ceram Soc (2014), http://dx.doi.org/10.1016/j.jeurceramsoc.2014.09.001