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Springer Tracts in Civil Engineering

Marijana Serdar · Ivan Gabrijel ·

Dirk Schlicke · Stéphanie Staquet ·
Miguel Azenha Editors

Advanced
Techniques
for Testing
of Cement-Based
Materials
Springer Tracts in Civil Engineering

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Marijana Serdar Ivan Gabrijel
• •

Dirk Schlicke Stéphanie Staquet

• •

Miguel Azenha
Editors

Advanced Techniques
for Testing of Cement-Based
Materials

123
Editors
Marijana Serdar Ivan Gabrijel
Faculty of Civil Engineering Faculty of Civil Engineering
University of Zagreb University of Zagreb
Zagreb, Croatia Zagreb, Croatia

Dirk Schlicke Stéphanie Staquet

Institute of Structural Concrete BATir
Graz University of Technology Université Libre de Bruxelles
Graz, Austria Brussels, Belgium

Miguel Azenha
Department of Civil Engineering
University of Minho
Guimarães, Portugal

ISSN 2366-259X ISSN 2366-2603 (electronic)

Springer Tracts in Civil Engineering
ISBN 978-3-030-39737-1 ISBN 978-3-030-39738-8 (eBook)
https://doi.org/10.1007/978-3-030-39738-8
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Preface

The current book was conceived as one of the outputs of the EU-funded network
COST Action TU1404 “Towards the next generation of standards for service life of
cement-based materials and structures” (www.tu1404.eu), active between 2014 and
2018. This network intended to provide added value through collaborations across
the entire field of cement-based materials and structural concrete—ranging from
concrete technology, over simulation and structural design, production and build-
ing, up to operation, monitoring and maintenance.
Within the Working Group 1 of the Action, which was focussed on experi-
mentation, over 40 laboratories and institutes around the world participated in a
joint testing of cementitious materials using standardised and advanced techniques
within the extended round-robin programme, called RRT+. The idea behind the
book started to develop when it was realised by the editors that there are numerous
innovative concrete characterisation methods being developed across these labo-
ratories that deserve to be put in the forefront. The role of leaders of the WG1 was
to pinpoint these techniques and try to organise them into this book.
Advanced testing of cement-based materials gives rise to different associations.
Some may think of highly specialised techniques in research and development,
while others may perceive it as technical assistance towards the mindset shift from
applying concrete by its strength class towards establishing a performance-based
application of cement-based materials. This book focuses on both the research and
development as well as practical application, aiming to serve as idea generator and
reference work at the same time. Overall, this book contains seven targeted chapters
presenting highly specialised techniques for obtaining individual performance
characteristics of cement-based materials. The application fields of the presented
techniques range hereby from basic material properties up to structural behaviour as
well as from the beginning of mixing over hydration up to the performance during
service life.
In particular, Chap. 1 presents the characterisation of fresh cement-based
materials with acoustic emission measurements. In Chap. 2, up-to-date develop-
ments and achievements in the field of ultrasonic testing of the early-age
cement-based materials are presented. In Chap. 3, a novel method for the

v
vi Preface

continuous measurement of elastic modulus evolution during the hardening phase

of cement-based materials is presented. Chapters 4–6 are dealing also with the
characterisation of cement-based materials at early ages, particularly aiming at
viscoelastic properties by means of repeated minute-scale duration loadings (Chap.
4), the development of the autogenous strain and the coefficient of thermal
expansion (Chap. 5) and the consideration of the restraining condition in testing
concrete since setting time (Chap. 6). Besides these innovations, Chap. 7 presents
an experimental setting for the holistic investigation of crack width development in
reinforced concrete members under restrained conditions with the superposition of
hardening-induced stresses with restraint stresses during service life.
The presented experimental techniques were derived from profound develop-
ment and verification within the research of the presenting authors. Besides, they
were also applied, verified and/or advanced within the scientific work of the COST
Action TU1404. The application, verification and/or advancement of the presented
techniques refer hereby mainly to the RRT+. It also refers to the numerical
benchmark campaign in which the well-grounded database from the RRT+ was
further used for sophisticated modelling and simulation with multi-scale approaches
at time and spatial levels.
Beside pure technical aspects, the chapters in this book highlight that concrete—
a material perceived in the practice and everyday life as rather simple—is a
remarkable and complex material bringing constant challenges to scientist and
practitioners in grasping all aspects of its properties and behaviour.
The editors are grateful to all authors, who shared their knowledge and described
their methods in detail, allowing us to share this in the present book. The editors are
also greatly thankful to all participants in the COST Action TU1404, which took their
time to test, report, analyse and discuss results obtained during the Action, all on
purely volunteering bases. Finally, a remark shall be given regarding the wide
international support that was behind all the activities of the COST Action TU1404—
and hereby also behind the creation of this book. General support was appreciated
from COST, RILEM, fib, JCI and ACI as well as specific support of the RRT+ by the
Austrian Railway Association (ÖBB Infra), the Norwegian Road Administration
(Statens Vegvesen), Schleibinger Geräte GmbH from Germany, CEVA Logistics
and EDF.

Zagreb, Croatia Marijana Serdar

Zagreb, Croatia Ivan Gabrijel
Graz, Austria Dirk Schlicke
Brussels, Belgium Stéphanie Staquet
Guimarães, Portugal Miguel Azenha
Contents

1 Acoustic Emission Characterization of Fresh Cement-Based

Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
Dimitrios G. Aggelis, Christian U. Grosse and Tomoki Shiotani
2 Ultrasonic Techniques for Determination and Monitoring Various
Properties of Cementitious Materials at Early Ages . . . . . . . . . . . . . 23
Ivan Gabrijel, Stéphanie Staquet, Markus Krüger, Jérome Carette,
Christian U. Grosse and Gregor Trtnik
3 Elastic Modulus Measurement Through Ambient Response
Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
José Granja and Miguel Azenha
4 Monitoring the Viscoelastic Behaviour of Cement Based Materials
by Means of Repeated Minute-Scale-Duration Loadings . . . . . . . . . . 99
Brice Delsaute and Stéphanie Staquet
5 Monitoring of the Thermal and Autogenous Strain . . . . . . . . . . . . . 135
Brice Delsaute and Stéphanie Staquet
6 Testing Concrete Since Setting Time Under Free and Restrained
Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 177
Brice Delsaute and Stéphanie Staquet
7 Adjustable Restraining Frames for Systematic Investigation
of Cracking Risk and Crack Formation in Reinforced Concrete
Under Restrained Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 211
Dirk Schlicke, Katrin Hofer and Nguyen Viet Tue

vii
Chapter 1
Acoustic Emission Characterization
of Fresh Cement-Based Materials

Dimitrios G. Aggelis, Christian U. Grosse and Tomoki Shiotani

Abstract The increase of performance requirements for contemporary cement-

based media and structures calls for better control of the material processes. Acoustic
emission (AE) is one of the non-invasive techniques that can provide information
on the internal condition of the material. This includes the time of crack occurrence,
the location as well as the fracture mode. In addition, it can offer valuable insight
on the initial, crucial period of curing and hardening that has serious impact on the
performance and durability of concrete. The present chapter aims to review the back-
ground, offer the reader a basic overview of the application of the technique on fresh
cement-based material and at the same time give some new directions for testing of
concrete.

Keywords Curing · Monitoring · Sensor · Shrinkage · Settlement · Cracking ·

Source · Energy · Frequency · Fracture

1.1 Introduction

Acoustic emission is a technique offering specific benefits in the monitoring of

cement-based materials and structures. One of the most important AE features is
the high sensitivity to very low energy events, which practically means accurate
determination of the onset of micro-cracking or other processes occurring in fresh
or hardened cement. In addition, it can localize the sources in three dimensions even
though no visual contact is possible with the point of the source. Also, it helps to

D. G. Aggelis (B)
Department of Mechanics of Materials and Constructions, Vrije Universiteit Brussel, Pleinlaan 2,
Brussels 1050, Belgium
e-mail: [email protected]
C. U. Grosse
Non-Destructive Testing Lab, Center for Building Materials, Technische Universität München,
Franz-Langinger-Straße 10, 81245 Munich, Germany
T. Shiotani
Graduate School of Business & Graduate School of Engineering, Kyoto University, Kyoto
615-8540, Japan

© Springer Nature Switzerland AG 2020 1

M. Serdar et al. (eds.), Advanced Techniques for Testing of Cement-Based Materials,
Springer Tracts in Civil Engineering, https://doi.org/10.1007/978-3-030-39738-8_1
2 D. G. Aggelis et al.

characterize the fracture mode or in general the type of source based on the received
waveform shape and different methods of analysis. More specifically:
• The high sensitivity of the method allows monitoring the actual initiation of micro-
cracking or other processes in cement much earlier than other indications, either
macroscopic deflection measurements, stress-strain curves or even other monitor-
ing techniques can indicate. This capability also enables AE to monitor processes
like settlement of concrete, segregation, shrinkage or bubble formation. It is char-
acteristic that the absolute energy of the AE signals is measured in atto-Joules
(10−18 J). To realize the order of magnitude of such signal, it can be stated that one
single cement grain of diameter 10 µm, falling from a height of 15 cm possesses a
dynamic energy in the order of 10−14 J being already 4 orders of magnitude larger
than the sensitivity of the technique.
• Localization is another basic feature of AE. By applying at least four sensors in a
3D position pattern, the internal cracking system can be quite accurately visualized.
This is related to the delay of acquisition of a single acoustic event between the
different sensors. Knowing the propagation velocity of the medium (practically the
longitudinal wave velocity or pulse velocity) the exact location can be determined.
If certain conditions are met, the localization error is contained within maximum
15% of the gauge length (distance between the furthest sensors) even in cases
of severe damage where some linear wave paths are blocked. In that case higher
number of sensors (>4) would of course be recommended.
• Another advantage is the possibility to characterize the fracture mode or the source
type in general. The mode of the crack in a matrix or the type of process that
occurs is indicative of the deterioration process, thus providing information on the
remaining life of the component or structure. As an example, when a concrete beam
is under bending load, the initial cracks are from tension on the matrix. Later the
shear diagonal cracks are developed with the debonding between the reinforcement
and matrix while friction between the banks of the cracks is also included. On a
different material type, fibre composites (can also be textile reinforced cement) first
develop matrix crack, while later delaminations between layers occur, debonding
of fibres, pull-out and finally even fibre rupture. These distinct mechanisms do not
emit the same elastic waveform and therefore, detailed monitoring by AE gives the
possibility to characterize the phenomenon and know exactly what is happening in
the material. Such techniques are similar to seismology where the waves radiated
from an earthquake are analysed in respect to the rupture process in the earth
(Grosse and Ohtsu 2008).
In this chapter, after an initial overview of the technique, monitoring by AE is
discussed for the early age of cement-based material. In this case AE intends to
capture phenomena not only related to cracking as will be extensively mentioned.
In this stage, no external stress is applied, as the material is let to cure. However,
still thousands of AEs are recorded being related to intrinsic processes that take
place in fresh cement, mortar or paste. Possible sources that have been discussed
in literature are settlement of cement, segregation, cavitation, bubbles and water
migration, formation of hydrates as well as shrinkage cracking. A summary of the
1 Acoustic Emission Characterization of Fresh Cement … 3

basic literature in the field is given, recent advancements are highlighted and insights
on the possibility to enhance the understanding are proposed.

1.2 Overview of Acoustic Emission

The AE technique detects and records elastic waves that are radiated by irreversible
processes in the material. These processes include deteriorations in any form (mainly
cracking, delaminations, fiber pull-out etc.), development of corrosion and related
cracking in concrete or other specific irreversible processes, like the ones occurring in
fresh concrete. Usually piezoelectric transducers are applied, placed on the surface of
the material with suitable coupling (e.g. silicon grease). The piezoelectric elements of
these transducers transform transient pressure changes into electric waveforms. After
amplification, the signals are driven to the acquisition board where digitization takes
place, while the main waveform parameters are analysed (Grosse and Ohtsu 2008;
Mix 2005; Grosse et al. 2016). A representation of an AE setup is given in Fig. 1.1,
where two possibilities are demonstrated: monitoring of fracture of a concrete beam
on the left and monitoring of curing of fresh cement-based material on the right.
An AE waveform is depicted in Fig. 1.2. Following standards, like RILEM 2010,
one can extract parameters out of such a waveform that are representative for source
types or other influencing conditions like the media in which the wave propagates.
Sensor characteristics (frequency response functions) can have additional influences
on the waveform.
The waveform starts with a “threshold crossing”. The threshold is a predefined
voltage set by the user to define the onset of the wave. When background noise
allows the setting of a low threshold, then the measured onset is close to the real
one. The time between the first threshold crossing (count) of the signal and the
time of the maximum peak is called Rise time (RT). Similarly, duration (Dur) is
defined as the time between the first and last threshold crossings. Intensity related
parameters include Amplitude (A) which is the highest voltage of the waveform.
Additionally, energy (MARSE, measured area under the rectified signal envelope)
takes into account the content of the waveform between the 1st and last threshold
crossings. These parameters can be indicative of the mechanical energy released by

Fig. 1.1 Typical AE setups

4 D. G. Aggelis et al.

0.2
Duration

0.15 Rise Time

0.1

Amplitude
0.05
Voltage

Threshold
0
0 50 100 150 200 250 300
- 0.05

- 0.1

- 0.15
Time (μs)

Fig. 1.2 Typical AE and main parameters

the source. Based on the shape of the first part of the signal, the RA value (RT/A)
or the inverse of the rising angle has been introduced. The frequency content is also
important, and several parameters are used to exploit the frequency information. One
is the “average frequency” (AF) which is calculated in time domain as the ratio of
the total number of threshold crossings over the duration of the waveform in kHz.
Additionally, the peak frequency (PF) is defined as the frequency with the highest
magnitude in the FFT domain, while central frequency (CF) is the centroid of the
spectrum. Going back to the waveform shape, features like the RT, RA and Duration
occupy higher values for shear type of sources, while frequency ones are higher for
tension events (Shiotani 2008; Aggelis 2016).

1.3 Related Literature

In the literature related to elastic (or stress) waves, fresh cement-based material has
been extensively tested by ultrasound. Wave speed (or ultrasonic pulse velocity) and
other parameters show good sensitivity to the development of hydration process,
being able to examine the degree of curing. They also provide a reliable evidence of
stiffness at any given time of curing (Robeyst et al. 2009a, b; Carette and Staquet
2016; RILEM 2011). A comprehensive review can be found in Trtnik and Gams
(2014).
Similarly to other fields, application of AE followed ultrasound testing in fresh
cement-based material as well. The difficult point is to separate the AEs according to
their source mechanism, something complicated by the number of different processes
and their overlap in time. Still, the number of studies and research groups interested
in the application of AE for monitoring of the fresh state of the material has recently
started to increase as the results show that the processes occurring in the fresh material
emit elastic energy that can be monitored by AE sensors.
1 Acoustic Emission Characterization of Fresh Cement … 5

Different approaches have been used so far to first monitor experimentally and
then interpret the results. One of the main aims is the characterization of shrinkage
cracking. When fresh paste loses moisture to the environment it starts to shrink. This
shrinkage strain results in stresses due to movement restrains of the boundary con-
ditions, and finally to micro- or macro-cracking close to the surface of the material.
Since a part of the energy is released in the form of elastic waves, AE use is well moti-
vated as a tool to study shrinkage cracking (McLaskey et al. 2007) and specifically
where and when cracking takes place along with other characteristics. In this study
exactly this phenomenon of fresh concrete was targeted i.e. shrinkage cracking due
to aggregates restrain as well as from differential moisture loss at different depths.
This cracking may start from the shrinking paste, but it is likely to propagate through
the paste-aggregate interface which is the weakest zone of concrete. Two types of
specimen geometries were used, one cubic of 142 mm side and a larger wedge-
shaped (380 mm2 and 190 mm deep). The reason for applying the second type (see
Fig. 1.3a) was to avoid possible reflections that did not allow characterization of the
different wave modes in the smaller cube. Specimens were equipped with multiple
broadband sensors (8 for the cube and 16 for the wedge) and the monitoring lasted
at least four days for both specimens. Results were compatible with the drying (and
therefore, shrinkage) rate as AE started also with high rate being gradually decreased
after the first day of test. Cubic specimen exhibited about double the AE activity of
the wedge shape, something attributed to the smaller size and thus attenuation of the
material. As far as source localization is concerned, despite the inherent difficulties
(variations in propagation velocity, scattering, low signal-to-noise ratio) a standard
error of 5–8 mm was achieved as tested by artificial excitations of pencil lead breaks.
Most AE events appeared within a few centimetres from the surfaces of the cube and
many of them corresponded to visually observed surface cracks. A slight correlation
between the frequency content and the age was noted as high frequency emissions
were more densely recorded after the first two days (Fig. 1.3b). This was attributed
to the decrease of attenuation as the material cured. Examining the waveform shape
at the different sensor, the tensile surface crack model was confirmed, as sensor 1
at the surface felt large Rayleigh waves, while for the same events, sensors 2–4 felt
much stronger longitudinal waves and no sharply defined Rayleigh waves, Fig. 1.3a
(McLaskey et al. 2007).
Shiotani et al. (2003) monitored the shrinkage cracking of cement containing
glass spheres as aggregates, using AE sensors of frequency 200–800 kHz on the
surface of relatively fresh concrete after demoulding. The specimens were circular
with diameter of 235 mm and thickness of 42 mm. The results showed that more
activities were recorded from a concrete (paste with glass spheres) than a cement
paste, something attributed to shrinkage cracking that was more pronounced due
to the additional restrain of the stiff aggregates. Several AE events were localized
and validated with microscopy. The localized events for the composite continued for
more than 10 h compared to the plain paste. In addition, indices like the average
frequency and the Ib-value of the emissions indicated the moment when small scale
cracking gave its place to larger scale phenomena.
6 D. G. Aggelis et al.

Fig. 1.3 a Wedge type specimen with indicative positions of sensors (1–4) and exaggerated dis-
placement field after a tensile cracking event denoted by a star. b Peak frequency of AE events
versus time (McLaskey et al. 2007)

Still, in the same subject of detecting of early age cracking, another study uti-
lized concrete prisms of different water to cement ratio, strength class and curing
conditions (Bacharz et al. 2015). AE monitoring with two sensors at the band of
30–80 kHz started 10 days after mixing (allowing for the selected curing) continued
up to approximately 2 months and the authors investigated the possibility to charac-
terize different types of cracking (micro-cracks in paste, micro-cracks in aggregate
paste interface and cracks on the concrete surface). Although the background behind
the separation of classes is not thoroughly explained, it is reported that the surface
micro-cracks produce comparatively high AE energy, while the lowest energy is
produced by paste micro-cracking. According to the authors this allows to identify
1 Acoustic Emission Characterization of Fresh Cement … 7

classes and thus characterize these destructive processes in relatively young concrete
due to hardening, shrinkage, evaporation in the absence of external mechanical load.
Researchers have tried to acquire AE even earlier, while the material is still in
the liquid state in the mould. Most used waveguides inserted into the concrete to
transmit signals to the AE sensor, sometimes without details about the material of
the waveguide. For example, Van Den Abeele et al. (2009) used two sensors of
375 kHz resonance “attached on top of two protruding bars” to register the signals
from the microstructural activity of the cement mortar samples. For all specimens,
the main AE activity started after the temperature peaks. Specimens with lower w/c
ratio (0.33) exhibited higher amount of activity earlier being in accordance with the
speed of hydration compared to higher w/c (0.5). Self-compacting concrete which
showed higher temperature, implying more intensive chemical activity, exhibited also
more intense AE from the reference concrete of the same w/c at that stage but later
during the mechanical setting the activity was weaker. Results were also supported by
ultrasonic measurements (longitudinal and shear velocities and nonlinear indices).
Despite that AE activity showed good correlation to hydration and mix proportions, it
only emerged 15 h after mixing, showing no activity from other very early processes.
Another approach based on waveguide concerned the frequency band 100–
500 kHz (Skal’s’kyi et al. 2004). The waveguide had variable cross section and
was checked that its main resonant frequencies fell in the range of sensitivity of the
sensor. In this case AE started to be recorded earlier, between 10 to 20 min after
preparation of the 100 mm cubic concrete specimen. The accumulated AE was con-
nected to the development of the crystal structure and when it was mostly completed
(i.e. up to 6 h) the AE intensity noticeably decreased. It is stated that the formation
of the concrete microstructure and the increase of strength is correlated to the cumu-
lative AE numbers and therefore, AE monitoring can contribute to the optimization
of the mechanical characteristics of the final product.
In Chotard et al. (2001) despite that AE was not recorded for the first 3 h, it was
shown that the frequency content of emissions changed and specifically increased
with curing time by about 50 kHz, something mostly attributed to the change of the
medium illustrating the liquid-to-solid state shift. Here, again the main AE activity
started during the temperature peak. The authors used a small PMMA plate of 3 mm
thickness to couple the sensor to the fresh cement paste. The AE in this study was
attributed to the drying process, creation of porosity and formation of hydrates. The
sensors were sensitive between 50 and 300 kHz and the specimen had dimensions of
100 × 100 × 30 mm with the last being the height. Amplitude and frequency of AE
were proposed to characterize internal mechanisms like hydration, porosity onset,
micro-cracking.
Lura et al. (2009) recorded AE from 8 g samples of cement paste with varying
w/c ratio. They used a sensor of 375 kHz and received the maximum rate of AE after
8–10 h. Many mechanisms were considered as sources (dissolution of cement grains,
formation of hydration products, friction of the shrinking paste with the container
walls, shrinkage cracking) but it was concluded that nucleation of bubbles including
air and water vapour is the most dominant. As a preparation, the authors monitored
AE activity from carbonated liquids (soft drinks) which showed quite high activity
8 D. G. Aggelis et al.

for several minutes before losing carbon dioxide. The authors argued that possibly
the early age AE in cement could be attributed to formation of hydrates, but the
activity did not peak at the end of the dormant period, leading them to the conclusion
that possibly the settlement is responsible for the AE at this early stage. Slightly after
the setting time as measured by the Vicat needle, low w/c specimens (w/c = 0.3)
exhibited a peak of AE activity higher than samples with high w/c (0.4). However,
when the open top surface of the small samples was covered by a layer of water,
this peak was eliminated, as according to the authors this water penetrated into the
paste at setting replacing the chemically used water and reducing thus the possible
cavitation phenomena. Also the fact that the AE energy was proportional to the mass
of the specimens, indicated that AE comes from the whole volume and not from
possible friction with the walls of the mould.
Recently another approach saw publicity (Bardakov and Sagaidak 2016), mainly
focusing on predicting the strength of concrete based on the AE acquisition rate
recorded at the first hours after mixing. A seemingly metal waveguide connected to
a 30–300 kHz sensor was inserted into the fresh concrete. AE was recorded from
the first minute and three distinct stages were recognized. Initially AE rate was very
high (stage I, first 4–5 h) attributed to “mobility” or mechanical displacement of the
mixture. As the water was consumed in hydration, the mobility (and the originating
AE) became gradually less until temporarily stopping at 10 h. The authors did not
consider other mechanisms as sources (dissolution of cement grains and formation of
hydration products) because their emissions were expected with low amplitude and
taking into account the high attenuation of fresh concrete, these signals would not be
recorded. However, shrinkage cracking is acknowledged as a possible source. The
2nd stage (between approximately 10–15 h) had very limited AE activity something
attributed to low energy sources like formation of calcium hydrosilicates which, how-
ever, are lost due to attenuation. The final stage showed an increase in AE attributed
to growth of crystallites in conditions of limited volume. With the above logic, the
AE slope of the 3rd stage was directly indicative of the intensity of structure for-
mation and giving eventually good correlations with the final compressive strength.
Correlations were also reasonable with the duration of the 2nd, “silent” stage, which
was inversely connected to strength, as according to the authors, longer silence meant
delay in hydration formation.
A similar approach was applied in Pazdera et al. (2014) based on relatively
broadband sensors placed on steel holders on top of the specimens for 28 days.
Here, the monitoring started after a period of 8 h and a similar trend of AE was
shown: initially high rate of activities followed by a gradual decrease which came
close to the temperature peak. After 24 h the specimens (100 × 100 × 400 mm)
were demoulded and the sensors attached again using steel waveguide and wax.
AE continued to register in low rates up until the end of the experiment. The main
result was that the mix exhibiting the least AE (one containing fly ash), exhibited
the highest compressive strength. This according to the authors was attributed to
less early age cracking which from one side increases the numbers of emissions
and at the same time decreases the strength. In another study of the same group
(Hoduláková and Topolár 2016), mortar was tested, showing, according to the
1 Acoustic Emission Characterization of Fresh Cement … 9

authors, that addition of microsilica possibly mitigates early age microcracking as

the AE amplitudes were lower than the reference sample.
In Qin et al. (2014) embedded cement-based piezocomposites with sensitivity up
to 600 kHz were applied for AE monitoring along with a broadband commercial
transducer fixed on a waveguide. The embedded sensor exhibited higher activity for
the first 12 h, attributed to better contact with the material, having peak frequen-
cies below 150 kHz. Based on the shape of the cumulative hits curve, three distinct
stages were suggested, namely the dormant period of low emissions, due to neg-
ligible microstructure development and heavy attenuation, followed by higher AE.
At this second stage a strong increase in temperature was also measured showing
the intensive hydration phenomena as well as shrinkage induced cracking. After the
temperature peak, the AE rate decreased. Then, the authors applied two embedded
sensors with distance of 2 m in a large-scale construction (foundation base element of
depth 2.5 m) and were able to linearly localize several hundreds of events, attributed
to the high temperature gradients that were measured inside the bulk of fresh concrete.
Recently, in Iliopoulos et al. (2016a) AE was monitored from the period just after
mixing (10 min) using 150 kHz resonant sensors on the external surface of the metal
mould. This approach led to many thousands of hits showing that the monitored
volume of the material is much larger than using a single waveguide. In this case, the
whole metal mould acted as a waveguide transferring the AE signals to the sensors.
The rate of emissions started at a very high value, being gradually decreased until
approximately 4–5 h. Concretes with high w/c ratio seemed to exhaust their activity
earlier, completing the 85% of their total activity in less than one hour, while for w/c
= 0.65, the same proportion was reached at almost 3 h. Concerning the aggregate
content, it was shown that high a/c (up to 5) led to reduced emissions compared to
cement paste (a/c = 0). The high AE activity for paste could be attributed to the lack
of multiple scattering and attenuation of the waves onto the aggregates, but more
likely to the higher amount of cement which contributes to the mobility through
settlement and is the chemically active compound. Apart from the total number
of emissions, in this study some qualitative features used previously for hardened
concrete were also examined. Parameters RA and AF show distinct trends, with high
w/c mixtures giving higher frequencies in average and shorter signals, something
more evident 3–4 h after mixing. AE activity and parameters during the first hours
correlated well with the 28 days compressive strength. Specifically, mixes with high
a/c ratio that exhibited the highest strength, had also the highest average frequency,
lower RA value between 4 and 6 h after mixing and lower AE activity in total when
fresh (Iliopoulos et al. 2016a). Excluding one outlier class a general trend is given in
Fig. 1.4. The result could be considered reasonable since high amount of early AE
activity is connected to increased settlement and therefore, excessive bleeding.
A multi-disciplinary approach was used in Dzaye et al. (2016). Apart from two AE
sensors of 150 kHz resonance attached directly on the mould of standard 40 × 40 ×
160 mm paste and mortar specimens (Fig. 1.5), capillary pressure measurements and
pulse velocity measurements were simultaneously taken on a separate specimen of
the same batch. Results showed that initially, as cumulative AE was increasing with
high rate, the capillary pressure was also building up. When AE was nearly saturated
10 D. G. Aggelis et al.

Fig. 1.4 Correlation between compressive strength of hardened concrete and the AE during the
fresh state (results from Iliopoulos et al. 2016a)

Fig. 1.5 AE monitoring of fresh paste in standard mould, taken from Dzaye et al. (2016)

for this initial stage and the increase was marginal (approximately at 3 h after mixing
of paste) the capillary pressure dropped suddenly indicating that air has entered
into the matrix. At the same time, ultrasonic pulse velocity and amplitude started
to rapidly develop indicating the setting time (or the point that an interconnected
network of hydration products has been built, see Fig. 1.6.
1 Acoustic Emission Characterization of Fresh Cement … 11

Fig. 1.6 AE cumulative curve and UPV development for a cement paste measured with the test
setup of Dzaye et al. (2016)

In addition, measurements in vertical mould of 200 mm height and cross section

of 40 × 40 mm with multiple sensors at different heights (Fig. 1.7) revealed that the
activity was higher for the bottom sensors showing that the initial hydrostatic pressure
is important. Furthermore, and in an effort to isolate AE producing mechanisms,
individual aggregates were let to drop from the top of the mold while an air hose
was separately used to produce air bubbles which rose from the bottom to the top

AE sensor

Magnetic clamp

Fig. 1.7 AE monitoring of fresh paste in vertical mould with sensors at different heights (Dzaye
et al. 2018)
12 D. G. Aggelis et al.

(Dzaye et al. 2018). It was found that both types of events could be well monitored
by the three AE sensors placed along the height of the mold of Fig. 1.7. There was a
positive correlation between the aggregate size and the AE energy release from the
impact, while the average amplitude due to air bubbles was approximately 6 dB lower
than the one from aggregate impacts but was still detectable. An interesting detail
is that aggregates impact in cement paste resulted in higher frequency than impact
of the same size aggregates in water-filled or empty mold. This was attributed to the
lower speed of the particles due to viscosity of the paste and therefore, shorter impact
contact time with the inner of the steel mould. The basic conclusion was that both
mechanical sources (aggregates impact and air bubble creation/movement) produce
waves that are well received by AE systems (Dzaye et al. 2018).
The early-age cracking was targeted in Topolár et al. (2017), as is the reason for
severe problems with the durability of concrete. Specifically mortars of different
w/c ratio were prepared and two AE sensors of frequency range 100–800 kHz were
attached to steel waveguides embedded in the material. The specimens were prismatic
with 1 m length and cross section of 100 × 60 mm. There, the AE activity started
at 1 h after mixing. The initial hits were attributed to “plastic setting” and early
microstructure formation, while the peak of AE rate came at 4 h. Duration and
amplitude of AE signals are also presented, without however, showing consistent
trends between the different w/c specimens as one of the specimens contained also
super-plasticizer. The activity continued with some silent stages up to 72 h when the
experiments were terminated.
In another recent study, paste, mortar and concrete prism specimens of dimensions
100 × 100 × 500 mm were monitored by AE sensors 15–20 min after mixing and for
72 h in plastic molds (Thirumalaiselvi and Sasmal 2019). Five broadband sensors with
range 100–900 kHz were placed along the top surface of the specimen, and one at the
base as reference. Activity started after 2–3 h for all material types. The highest AE
rate for paste came between 10 and 20 h (at 10 events/h), while for concrete the activity
peaked between 23 and 35 h at approximately 2.5 events/h. These peaks coincided
with the heat evolution period in each material. Overall the paste accumulated 120
events, concrete approximately half, while mortar was in between. Attenuation was
acknowledged as a crucial factor since simulations showed that it starts at high
values at time zero while strongly decreases further (at 22 h and later). Looking at
the frequency content, the band 0–100 kHz was always by far the most powerful for
the early stage, while later, the band of 100–200 kHz took over in content. According
to the presented analysis, four basic types of signals were classified, being related
to the CSH formation and emptying of capillary pores, chemical shrinkage while at
the end of monitoring, a cluster attributed to micro-cracking was also added, which
was stronger for concrete than for paste. As a general comment for this interesting
and detailed study, it presents many AE characteristics combined also with “active”
wave parameters (pulse velocity and attenuation) however, it does not present any
activity at the first 2 h, missing therefore, the process of settlement, which in other
studies results in thousands of AE signals within 2 h after mixing. This may be due
to the placement of the sensors directly on the surface of concrete, which initially,
as acknowledged, is very attenuative.
1 Acoustic Emission Characterization of Fresh Cement … 13

Assi et al. (2018), after discussing the lack of consensus in literature on the corre-
lation between AE signals and hydration mechanisms, reported the AE application
on fresh cement paste with the use of pattern recognition algorithms, combined with
analysis of wavelet energy distribution. Specimens were prisms of 38 × 38 × 110 mm
cast in Plexiglas molds with two different w/c ratios, i.e. 0.3 and 0.5. One relatively
wideband sensor (range from 200–900 kHz) was placed on each specimen, after
placing an acetate sheet of the free surface to increase the transmission of waves.
Results showed the highest amplitude signals came close to the “middle” stage where
the temperature peak was exhibited. While there was strong variation in cumulative
energies even of specimens of the same composition, it was seen that a sudden initial
increase was noted at the start of the “acceleration” stage, when temperature was
rising for all specimens. Main mechanisms considered as AE sources were crystal-
lization, formation of hydrates during the acceleration stage, chemical shrinkage and
related micro-cracking and delayed hydration at the deceleration stage. The authors
did not consider settlement as possible source maybe because the setup received
limited AE activity in the first minutes after mixing.
In the field of concrete admixtures Lefever et al. (2017) monitored the AE activity
during the standard shrinkage cracking ring test. Two 150 kHz resonant sensors were
placed on the inner side of the metal ring. In the reference mortar specimen, AE started
to be recorded after about 4 h in hand with the increase in shrinkage as measured by
strain gauges on the steel ring, while after approximately 4 days, the mortar rings
were cracked emitting very strong AE, simultaneously with the strain drop. A mix
containing super-absorbent polymers (SAPs) followed a different behavior, as it did
not exhibit strong shrinkage. This was attributed to the action of SAPs that at some
point release water during hydration. At the same time, AE started to be recorded at
very high rates (higher than the reference mix) at 7–8 h after mixing indicating the
release of water by the SAPs, showing how its sensitivity can be utilized to monitor
delicate processes in the microstructure.
Lastly, two interesting cases are reported by Ohtsu (2005). One concerns the
identification of consistency of roller-compacted concrete mixes. An AE sensor was
placed on the outer surface of the large cylindrical container of 48 cm diameter
and height 40 cm (“VS test apparatus”). The contained concrete was submitted to
vibration until bleeding water appeared on the surface. AE was continuously acquired
for all mixes in two stages, exhibiting a bilinear curve, first with high slope and
then with lower. This turning point was well related to the number of vibrations as
concrete with higher “VC value” (according to the authors the time until bleed water
is observed at the surface) exhibited this transition point earlier.
In a similar case also reported by Ohtsu (2005) AE was monitored by a sensor
applied on the external surface to estimate the compaction of the concrete mixes. The
concrete volume in the cubic container was of 30 cm side. During compaction by a
vibrator, AE was recorded in rates of more than 1000 hits/s until approximately 80 s.
Then AE rate decreased and stayed constant to values around 500 hits/s implying
according to the authors that compaction was completed, or that “the steady state”
was reached. Changing the w/c ratio from 0.45 to 0.60 did not have strong effect
14 D. G. Aggelis et al.

on the time to reach the fully compacted stage, but a stiffer mixture tested (called
“non-slump concrete”) exhibited this transition from high to low AE energy much
later.

1.4 Discussion

The above studies show that there is potential in AE monitoring of fresh cement-
based material, as it contributes to the understanding of the complicated processes
during hydration and also provides possible predictions for the final mechanical
properties. However, the explanations of the sources of AE are not consistent and
depend mainly on the assumptions allowed by the experience of the researchers and
the accompanying measurement conditions.
It is characteristic that some studies find positive correlation between the sum of
AE and final strength (Bardakov and Sagaidak 2016), while others find negative,
with specimens of low AE activity at the fresh state, possessing higher strength
at the hardened state (Pazdera et al. 2014; Iliopoulos et al. 2016a). These results
are not necessarily contradictive as the different setups may be sensitive to other
processes that take place at different times of curing (e.g. settlement at very fresh
age, shrinkage cracking or hydration formation later). However, they indicate that a
common understanding would be necessary to advance the field.
The basic mechanisms that are considered as sources in the literature are settlement
of cement, migration of water through the capillary pores and air bubbles, cavitation,
formation of hydrates, early micro-cracking, friction with the mould due to shrinkage,
while cracking on the aggregate-paste interphase has been considered (McLaskey
et al. 2007; Pease et al. 2003). These mechanisms may occur at different time zones
but they certainly exhibit overlapping windows.
A characteristic point of the monitoring is the temperature peak. In some of the
aforementioned studies, activity started or peaked at approximately that point, e.g.
(Van Den Abeele et al. 2009; Chotard et al. 2001). However, other studies (Bardakov
and Sagaidak 2016; Pazdera et al. 2014; Iliopoulos et al. 2016a; Dzaye et al. 2016;
Dzaye et al. 2018; Dzaye et al. 2020; Topolár et al. 2017) showed the large majority
of recorded hits earlier than that, leading to the conclusions that significant processes
(possibly of lower intensity and thus more difficult to register) occur from as early
as the mixing time, much before the chemical reaction of hydration and any heat
is developed. This type of mechanical sources has also been studied in relation to
AE for characterizing the deformation of granular media due to jamming of grains
and frictional slip of particles which release strain energy (Michlmayr and Or 2014).
However, differences in the acquisition equipment (including sensor sensitivity), the
coupling (with or without waveguide), the specimen size do not allow for robust
conclusions relatively to some trends. It could be mentioned though that in most
studies different stages are identified, the first of which is characterized by large AE
numbers while later AE gradually stops. In the most recent ones that are able to get
activity from the first moment of the test, meaning just after mixing, the AE curve
1 Acoustic Emission Characterization of Fresh Cement … 15

looks like the examples of Fig. 1.6, where a period of silence is found between the
initial high activity period and the moderate activity at the end (e.g. indicatively 5–8 h
in Fig. 1.6).
However, the work is still hardly enough to unambiguously explain the origin of
the AE activity and to contribute to specific open questions:
• Can the “setting time” be characterized by AE?
• Can the mixture proportion be reliably investigated?
• Can the influence of different type of admixtures or additives be evaluated?
• Can the suitability of a mixture be assessed in the first hours just by passive AE
monitoring (or combination of techniques)?
• Can the final properties be predicted by the AE activity of fresh cement-based
material?
• Can other AE parameters (apart from the hit number and possibly energy) seriously
assist the characterization?
• Can AE provide feedback to the complex modelling of processes taking place in
the microstructure of hydrating cement, basically can the different AE signals be
identified according to their source?
Finally, another serious issue is the contribution of wave propagation through
this changing medium. A certain excitation will be recorded with very different
characteristics after propagating through fresh heavily damping low velocity paste
or after propagation through stiff hardened cement (or concrete) what is well known
from ultrasound experiments at fresh and hardened concrete (Robeyst et al. 2009a,
b; RILEM 2011; Iliopoulos et al. 2016b; Popovics and Popovics 1998). In fact,
fresh concrete can be characterized as a “suspension” of particles (cement, sand,
aggregates, air bubbles) in water. The viscosity of the liquid matrix and its strong
mismatch with the stiff aggregates as well as the cavities induces tremendous amount
of damping and scattering attenuation. This has been demonstrated (Popovics and
Popovics 1998) and treated through multiple scattering models like the well-known
model of Waterman and Truell (1961), in studies aiming at ultrasonically examining
the material since the fresh state (Aggelis et al. 2005). In particular the presence and
content of air bubbles is crucial (Aggelis et al. 2005; Sayers and Grenfell 1993; Boutin
and Arnaud 1995; Robeyst et al. 2008). Even in very small volume percentages (i.e.
0.1%) they are responsible for severe signal distortion compared to de-aired paste and
a considerable delay in the rise of longitudinal and shear wave velocities (Zhu et al.
2011). They also cause very high scattering attenuation at moderate frequencies (i.e.
below 200 kHz) attributed to the “bubble resonance effect” which is more pronounced
in paste rather than mortar (Aggelis et al. 2005; Sayers and Grenfell 1993; Zhu
et al. 2011). On the other hand, sand and larger aggregates dominate the attenuation
behaviour through scattering above 300 kHz (Aggelis et al. 2005). It should also
be mentioned that, especially for the early ages, compaction is very important, as it
drastically reduces the air content and accelerates the settlement and better packing
of cement particles in the mix (Zhu et al. 2011). Later, with the progress of hydration
the material is gradually transformed to solid and thus in terms of wave propagation it
has been well treated as a water saturated porous solid medium through Biot theory
16 D. G. Aggelis et al.

(Sayers and Grenfell 1993; Zhu et al. 2011; Biot 1956). The transition between
different forms has also a crucial effect on the transmitted frequency content, which
for the same initial excitation, extends to much higher range after setting (De Belie
et al. 2005; Robeyst et al. 2009a, b).
An also quite important issue is that with the development of material stiffness,
other types of waves obtain significance. Initially after mixing the material supports
only longitudinal waves due to its liquid form. Later and with the increase of shear
modulus, shear and surface (Rayleigh) waves are also supported and actually may
take up more of the energy from the excitation (Graff 1991). Therefore, although
initially the acquired AE waveforms include only longitudinal wave components,
at later ages they may well contain contributions from all different wave modes,
with longitudinal dominating the early part of the signal and shear and Rayleigh
arriving later within the waveform. This effect may be more straightforward in case
the transducers are placed directly on the surface of the material, where the different
waves can even be separated based on the waveform shape and content (McLaskey
et al. 2007).
All above mentioned propagation effects are coupled to the AE results and there-
fore, so far, any discussion or conclusion on specific AE values (e.g. amplitude or
frequency of emissions) corresponding to a certain mechanism is inconclusive since
it is also a function of curing time that defines the damping and the stiffness of the
matrix. To support this, the following indicative simulations are presented. The geom-
etry of the simulations may be representative but not directly corresponding to any of
the above-mentioned literature studies. The external mould and the waveguide have
properties of steel (longitudinal velocity 6000 m/s, shear 3200 m/s, no damping),
while the cement paste obtains two different set of properties: one corresponding to
fresh (longitudinal velocity 800 m/s, shear negligible, high damping) and the other
corresponding to hardened (longitudinal 4000 m/s, shear 2100 m/s, low damping).
The excitation is in both cases one cycle of period 1 µs (basic frequency 1 MHz),
occurring at the same point, as shown in Fig. 1.8. In the same figure the displacement
fields after several µs are seen when the wave has already reached the waveguide.
In Fig. 1.9a one can see the difference between the received waveforms through the
sensor at the top of the waveguide despite the same excitation. The waveform through
hardened material exhibits much higher intensity and has seemingly longer duration
due to the limited damping of the materials that allows multiple reflections in this
simulation. On the other hand, the waveform through fresh material is much weaker
due to the lower elastic properties and the higher damping factor used. Figure 1.9b
shows the corresponding power spectra showing not only the tremendous difference
in magnitude but the loss of the higher frequencies in the case of fresh matrix. It is
indicative that when the material is fresh, the acoustic impedance mismatch between
paste and metal is huge, not allowing wave energy to propagate through the waveg-
uide, as it is almost entirely reflected back to the paste (see the arrow in Fig. 1.8a).
In Fig. 1.8b, a reflection is still obvious, but a considerable amount of energy enters
the waveguide.
Therefore, propagation through the medium should be seriously taken into account
when trying to interpret the AE results in this time-dependent material.
1 Acoustic Emission Characterization of Fresh Cement … 17

(a) Receiver (b) Receiver

Fresh paste Hardened

Waveguide

Waveguide
paste
Metal mold

Metal mold
Energy enters Energy re-
Most energy the wave- flected away
is reflected from the
away from waveguide
the wave-
guide

Excita on Excita on

Fig. 1.8 Snapshot of strain field through numerical simulations in hydrating paste. The external
dimensions of the mould are 80 × 80 mm and the thickness is 5 mm. The length of the waveguide
is 50 mm, a fresh (liquid) matrix, b hardened matrix

It is certain that combined experimental techniques are necessary. Recently such

a combination is realized in a collaborative project between VUB and UGent in
Belgium. Since AE may be of chemical (e.g. hydrate formation) as well as mechanical
(e.g. settlement, cracking) origin, measurements of temperature can enlighten the
ongoing degree of hydration, while the settlement can also provide information on
the mobility of the cement particles. Digital Image Correlation is also used to confirm
the onset of shrinkage cracking at the surface, while capillary pressure measurements
indicate when the paste has dried and air penetrates through micro-cracking. In any
case the fresh material is extremely attenuative (much more than hardened concrete)
and therefore, the experimental setup should be sensitive enough. Attaching multiple
sensors on the metal mould seems to be a good experimental solution to receive the
emitted activity. Even if, due to shrinkage, one surface of the specimen is detached
from the mould wall, others will remain in contact providing continuous information.
On another notice, localization of AE events in the volume of the material would
be very beneficial. This would help to clarify some cases, e.g. if an event is due
to the friction with or detachment from the mould it would be localized on the
concrete-mould interface. However, the tremendous attenuation of fresh cement paste
or mortar would not allow capturing the same event by as many as four sensors to
achieve 3D localization. As argued in Iliopoulos et al. (2016a) the attenuation of
fresh paste and mortar is of the order of 2 dB/mm depending also on the frequency
and composition. This means that for further propagation of 1 cm, the signal would
lose 20 dB which is a tremendous loss. Practically it would be extremely difficult
to record the same source by multiple receivers, taking into account that the sensors
occupy some physical dimension of mm or cm and cannot be placed very close to
18 D. G. Aggelis et al.

(a)

(b)

Fig. 1.9 a Simulated waveforms on the receiver of the geometry of Fig. 1.8 for hardened and fresh
matrix. b FFT of the same waveforms

each other. Even if that was possible, then the accuracy would not be sufficient as the
“gauge length” would be too small and comparable to errors in placement and signal
reception. Furthermore, the pulse velocity in such a medium may present variations
for different directions something that would contribute to the increase of errors.
1 Acoustic Emission Characterization of Fresh Cement … 19

1.5 Conclusions

AE monitoring is a field that can offer much to the characterization of cement-based

materials especially at the sensitive stage of curing. If during this early stage the mate-
rial is controlled, the possibility that later the performance is less than satisfactory
is crucially diminished. A lot of meaningful research efforts have emerged recently
showing the capability of the AE technique to correlate with different processes
of properties. These efforts, however, are all case-specific, meaning that geome-
tries, sensors, coupling types, monitoring periods are different. Some suggestions
for future research include:
• Careful selection of the experimental setup including records of environmental
conditions (ambient temperature, humidity, etc.) and concrete mixing process
(compaction).
• AE experiments using multiple sensors with varying frequency response functions
and varying positions, ensuring a good coupling throughout the experiments and
taking into account attenuation and acoustic impedance mismatches.
• Designing experiments that would physically isolate as much as possible the
different source mechanisms.
• Combination of multidisciplinary measurements to reduce the assumptions on
the behaviour of the material and create different correlations with AE to help
interpretation.
• Numerical simulation to understand the wave propagation in cementitious materi-
als and to examine in what way does the received wave after propagation through
cement and waveguide/mould correspond to the sources.
• A coordination in the field in order to steer the efforts in a common direction.

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