Assessing the fresh properties of printable cement-based

materials: High potential tests for quality control

Citation for published version (APA):
Roussel, N., Buswell, R. A., Ducoulombier, N., Ivanova, I., Kolawole, J., Lowke, D., Mechtcherine, V., Mesnil, R.,
Perrot, A., Pott, U., Reiter, L., Stephan, D., Wangler, T., Wolfs, R. J. M., & Zuo, W. (2022). Assessing the fresh
properties of printable cement-based materials: High potential tests for quality control. Cement and Concrete
Research, 158, Article 106836. https://doi.org/10.1016/j.cemconres.2022.106836

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 Cement and Concrete Research 158 (2022) 106836

Contents lists available at ScienceDirect

Cement and Concrete Research

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

Assessing the fresh properties of printable cement-based materials: High

potential tests for quality control
Roussel Nicolas a, *, Buswell Richard b, Ducoulombier Nicolas c, Ivanova Irina d,
Kolawole John Temitope b, Lowke Dirk e, Mechtcherine Viktor d, Mesnil Romain f,
Perrot Arnaud g, Pott Ursula h, Reiter Lex i, Stephan Dietmar h, Wangler Timothy i, Wolfs Rob j,
Zuo Wenqiang a
a
Navier Laboratory, Gustave Eiffel university, Paris, France
b
School of Architecture, Building and Civil Engineering, Loughborough University, United Kingdom
c
XtreeE®, Rungis, France
d
Institute of Construction Materials, TU Dresden, Dresden, Germany
e
Institute of Building Materials, Concrete Construction and Fire Safety (ibmb), Technische Universität Braunschweig, Braunschweig, Germany
f
Ecole des Ponts ParisTech, Marne-La-Vallée, France
g
Univ. Bretagne-Sud, UMR CNRS 6027, IRDL, Lorient, France
h
Department of Civil Engineering, Building Materials and Construction Chemistry, Technische Universität Berlin, Berlin, Germany
i
Institute for Building Materials, ETH Zurich, Zurich, Switzerland
j
Department of the Built Environment, Eindhoven University of Technology, Eindhoven, the Netherlands

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

Keywords: In the absence of a formwork, printable materials are expected to quickly increase their consistency in order to
Yield stress resist the self-weight of the structure being printed. Resolving this rheological requirement with the printing
Elasticity process is the key to successful printing. It is therefore necessary, from a material design, from a process design
Digital fabrication
and from a daily quality control point of view, to have the ability to measure the relevant fresh properties.
3D printing
Because of the range of stresses of interest, there only exist a few standard tests in literature allowing for such an
assessment while some new ones were developed in the last decade. The present paper aims at presenting some of
these tests along with some preliminary data supporting their ability to capture the material properties of interest
while discussing the remaining and related open research questions.

1. Introduction and background
For decades, the cement-based materials research community has
been divided into two distinct sub-communities. On one hand, there
were researchers focusing on hardened pastes, mortars or concrete
properties. The elastic modulus, creep behavior, strength along with
some porous material features such as porosity, permeability and
various diffusion coefficients were reported by these researchers [1a].
The modelling of cracking, creep, durability and service life both at the
level of the material and of the structure were also conducted. On the
other hand, other researchers focused their works on assessing the fresh
properties and rheological behavior of cement-based materials using
some tests described [1b]. The effect of solid volume fraction on fresh
and rheological properties, the colloidal interactions between cement
grains, the viscous dissipation in the interstitial fluid [2] and the origins
of thixotropy and aging in such reactive suspensions were investigated
by these authors [3]. They were in parallel understanding how organic
macromolecules (i.e. admixtures) were allowing for the tuning of these
fresh properties [4] and how industrial processing may impose some
specific rheological requirements on the material [5–7].
Despite the fact that both hardened and fresh materials contain
cement, water and some other coarser rigid mineral particles, they do
not have many things in common from a physical point of view [8].
Hardened cement-based material are brittle, viscoelastic porous solids
[1a], while fresh cement-based materials are dense, non-Newtonian
granular suspensions [2]. At the level of the paste (or matrix), hard­
ened materials display an unsaturated porosity typically around 20 to
30% while the fresh ones have almost-fully saturated porosities typically

* Corresponding author.
E-mail address: nicolas.roussel@ifsttar.fr (R. Nicolas).

https://doi.org/10.1016/j.cemconres.2022.106836
Received 26 November 2021; Received in revised form 24 March 2022; Accepted 8 May 2022
Available online 2 June 2022
0008-8846/© 2022 Elsevier Ltd. All rights reserved.
R. Nicolas et al.
around 50 to 60%. But, more than anything, the stresses required to
drastically modify their structure (i.e. cracking for hardened materials or
flow onset for fresh ones) are extremely different. For hardened mate­
rials, strength ranges from some hundreds of kPa for mortars to up to
around 100 MPa for high strength concretes while, for fresh materials,
yield stress ranges from a few tens of Pa for self-compacting products to
several thousands of Pa for stiff concretes (Cf. Fig. 1).
The interface between these two communities was the setting of the
material with strength ramping up from some tens or hundreds of Pa to
some tens of MPa in a matter of several hours. Despite the abundant
literature on the chemical aspects related to setting [9–11], this perco­
lation phenomenon was only barely studied as a whole from a me­
chanical point of view. This can be explained by the lack of tools
allowing for the assessment of such a large variation in mechanical
properties over such a short time span. Such tools should indeed have
been able to cover a range of around 5 to 6 orders of magnitude, which is
unreachable for most force sensors. According to [12], the Vicat needle
is able to cover a range of strength of around one order of magnitude
while ultrasound seems to be the only device allowing for a rough
assessment of the full material phase change. However, according the
best knowledge by authors in [13], some values were provided that are,
at this stage, only qualitative and can only be related to strength or
elasticity through some empirical calibration.
On each side of the above interface, the two communities developed
some mechanical quality-control oriented and research-lab focused
tests. From the above, it can therefore be concluded that some standard
and/or technical recommendations do exist to measure, on one side,
strengths between several hundreds of kPa and some tens of MPa and, on
the other hand, yield stresses between around 10 Pa and a few kPa.
In parallel, a few decades ago, additive manufacturing, sometimes
called 3D printing, attracted a lot of attention and interest within the
manufacturing industry. It took one more decade before attempts to
integrate this type of shaping processes to the concrete industry were
first reported [14,15]. This new type of concrete processing is getting
away from the standard formative approach (i.e. shaping with a mold/
formwork) [16] and is offering an enhanced freedom of shape along
Fig. 1. Range of relevant values for consistency/yield stress or mechanical strength for cement-based materials.
2
Cement and Concrete Research 158 (2022) 106836
with potential gains in productivity. It is moreover anticipated that this
freedom of shape may allow for some material saving by lifting the
shape limitations induced by a formative approach and which prevent
from the manufacturing of concrete elements with optimal structural
design.
Nevertheless, such shaping processes impose many new constraints
on the material being printed. These include, but are not limited to,
some rheological requirements on the material in its fresh state [17–19].
The specificity of these requirements, as discussed below, is that they not
only impose the value of the material yield stress (or elastic modulus)
after mixing but also the evolution of this value over time.
It was indeed shown in [17] that there exists a minimum value for the
material yield stress at the nozzle level required for a proper control of
the extruded layer cross section. This value seems to be related to the so-
called “printability” property. This critical value is expected to scale
with the gravity-induced stress at the level of one layer of material. It is
moreover expected to be around a couple hundreds of Pa for standard
centimetric layers. Then, while the printing process goes on, the gravity-
induced stress in the first printed layer increases. This, in turn, requires
that the printed material yield stress increases with time accordingly. In
addition, the overall deformation of the structure being printed has to
stay within some tolerance related to the geometric conformity of the
manufactured element. This imposes some further requirements on the
material rigidity and its evolution with time. Finally, it was shown that,
for slender elements being printed vertically, self-weight buckling be­
comes the dominant failure mechanism [20]. Avoiding it requires again
the material rigidity (elastic moduli of the fresh material) and strength
(yield stress) to stay above some critical values. All the above re­
quirements on the evolution of the material yield stress and elasticity
with time seems to be related to the empirically defined and so-called
“buildability” property.
The orders of magnitude of these requirements were roughly
assessed in [17,21,22]. It can be concluded from this exploratory paper
that the range of interest for the yield stress of a printable material and
its evolution in time shall be between a couple hundreds of Pa and a few
hundreds of kPa (Cf. Fig. 1).
R. Nicolas et al.
Such a range of yield stress creates several issues. First, this range is
crossing the zone where the two research communities identified above
never developed any mechanical tests. Moreover, this range spreads
over almost four orders of magnitude. Such a large spread questions the
possibility of having one unique test allowing for capturing the mate­
rial's fresh properties and their evolution with time. Finally, depending
on its kinetics, the yield stress values evolution may be extremely fast
and delicate to assess properly. This is expected to be specifically the
case of many extrusion-based additive manufacturing technologies
where the material is accelerated through the timely addition and
dispersion of a chemical compound [23–25]. Such materials may see
their yield stress double in a matter of a couple tens of seconds or a
couple of minutes. Sampling the material could then prove extremely
sensitive. It may therefore become necessary to distinguish between the
assessment of the initial material yield stress and the assessment of its
long-term structuration rate (i.e. the yield stress increase rate) as defined
in [3,26]. Finally, the picture is made even more complex as it was
suggested that, in this range of fresh properties, some material may
display some frictional (and not therefore purely plastic) behavior
[20,63,68,69].
Within this frame, the RILEM technical committee TC-PFC “Perfor­
mance requirements and testing of fresh printable cement-based mate­
rials” was created in 2020. It aims at developing a set of technical
recommendations for the testing and quality control of fresh printable
materials. To reach this goal, around 100 international experts from
around 30 countries started to identify and select some high-potential
tests that would be able to screen the range of yield stress materials
discussed above. In addition to being relevant from a measurement point
of view, these tests shall fulfill a number of practical requirements such
as being acceptable from a cost point of view, being based on standard
equipment or requiring a low volume of material. These tests should be
simple, robust and generic enough to be applicable to the wide variety of
printable materials and also.
In a second step, these tests are expected to go through an extensive
inter-laboratory comparison and, for the most promising ones, to be
provided with a dedicated and detailed testing recommendation.
The present paper aims at presenting some of these pre-selected tests
and some preliminary data supporting their ability to capture the ma­
terial yield stress/elasticity at the level of the nozzle and/or its evolution
with time after deposition.
2. Gravity-driven rheometry for extrusion-based additive
manufacturing with concrete
Applying a stress and measuring the resulting deformation or
detecting flow onset is a very common way to assess the yield stress of
materials from nature or industry. Applying a stress may however
require some expensive and fragile equipment such as a rheometer or a
loading device. Nevertheless, it is possible to make use of a simple source
of external stress in cement-based materials: the one induced by gravity.
It is specifically relevant for additive manufacturing where the stress of
interest to be resisted during printing is the gravity-induced stress (i.e.
induced by the self-weight of the structure). Finally, it can be reminded
here that it is also a gravity-induced stress that competes with yield
stress in the universal slump test [27]. The slump test can however not
always be applied to printable materials as, on one hand, it is limited to
yield stress values lower than around 4 kPa [28] and, on the other hand,
for accelerated materials, the time required to fill the conical mold with
a robot would prevent from the exact measurement of the yield stress at
the level of the extrusion nozzle. The competition between the
destructuration of the material induced by the Abrams cone filling and
the structuration of the material in the zones at rest shall moreover result
in a very non-reproducible procedure and would therefore be very much
operator dependent. In the last decade, several techniques of gravity-
driven rheometry were developed in parallel with the development of
extrusion-based additive manufacturing techniques. We present two of
3
Cement and Concrete Research 158 (2022) 106836
these techniques below.
2.1. Inline rheometry: the “slugs test”
The slugs-test was introduced by Ducoulombier et al. [29]. It is based
on the analysis of the extensional flow [30] that occurs at the nozzle
level when the extruder axis is vertical and far above the ground. With
pasty materials such as printable material, this situation leads to a
discontinuous flow typology and to the formation of so-called slugs (see
Fig. 2). It was shown in [30] that the slugs' shape relates to the rheo­
logical properties of the extruded material. In the case of a yield stress
fluid, there exists a simple relation between the yield stress at the nozzle
τ00, the slug mass MS, gravity acceleration g and the nozzle cross section
area A. This allows for a simple yield stress assessment at the nozzle
level, which is very promising for inline printable materials quality
control.
This test can be applied to any cement-based material as long as the
yield stress contribution to apparent viscosity remains higher than the
purely viscous one and as long as the nozzle diameter remain small
compared to the slug length [29]. An analytical first-order relation be­
tween the average mass of a slug and yield stress can then easily be
derived from a Von Mises plasticity criterion and writes:
gM
τ00 = √̅̅̅ S (1)
3A
where MS is the average mass of the slugs and A is the cross section of the
nozzle. A deeper analysis of this extensional flow can be found in [31]. In
practice, however, the above relation has proven to be sufficient to
capture the variations of interest for a successful quality control of the
yield stress at the nozzle and therefore of the resulting geometry of the
printed layer [29].
Three different data series are used below to illustrate the test po­
tential. All studied mixes were chosen to exhibit a non-thixotropic and
non-aging behavior, allowing for the use, in parallel, of standard yield
stress measurement techniques. In the two first series, obtained at
Navier Laboratory, the yield stress measured by the slugs test was
compared to yield stress values computed from traditional slump tests
[27]. The third series was obtained at Loughborough University and the
slugs test measurements were compared with vane tests measurements
[32] similar to the ones described in Section 3. The average and the
standard deviation of the yield stress value for each mix are computed
and given in Table 1. A very promising correlation is found between
slugs test yield stress values and the reference ones as shown in Fig. 3.
These results suggest that the slugs test may provide for an efficient
inline quality control tool at the printing nozzle level. As it does not
require any sampling, it could even apply to highly accelerated mate­
rials. It could, in industrial practice, allow for a daily fine-tuning of the
printable material yield stress and therefore of the geometrical confor­
mity of a printed layer.
Finally, it was suggested in [29] that the standard deviation in the
measured slugs masses could relate to the homogeneity of the material
being extruded. Such a feature would, in turn, allow for the control of
the mixing and/or dispersing quality level of the printing unit.
2.2. Other potential gravity-driven tests
As discussed previously, the slugs test appears to be a promising tool
for assessing the extensional yield stress of printable concrete
[29,31,33,34]. As printable materials most often display a plastic Von
Mises criterion, shear rheological parameters can be directly derived
from the slugs test extensional flow typology [21,35]. However, for
stiffer mixes used, for instance, in the infinite brick deposition strategy
[17], the slugs test could reach a limit and may not be sufficient to obtain
the whole picture of the material rheological behavior. This is specif­
ically critical when the contribution of granular friction in high solid
R. Nicolas et al. Cement and Concrete Research 158 (2022) 106836

Fig. 2. Illustration of the “slugs” formation at the level of the printing nozzle (reproduced from [29]).

Table 1
Experimental data including reference yield stress measurements and slugs tests measurements. Standard error defining the confidence interval was computed for 95%
fractile.
Navier manual experiments Navier automatic experiments Loughborough automatic experiments

Average yield stress computed from slump τc (Pa) 170 260 500 300 190 410 1380
Standard error (Pa) (95% interval) 40 50 100 60 50 80 70
Average yield stress computed from vane test τc (Pa) 715 462 356 1104
nb of test 4 4 4 4
Standard error (Pa) (95% interval) 55 22 19 64
Flow rate (g/s) 3.5 3.9 3.3 7 15 12 22 23.8 13.1 14.8 98.1
Nb of experiments/slugs 4 4 4 24 30 22 39 22 20 15 27
Average yield stress computed from slugs test τ00 (Pa) 210 290 530 350 270 400 1350 787 401 318 1170
COV (%) 4.5 4 6.5 11.5 16.2 30 14 20.5 11.5 14.7 11.6
Standard error (Pa) (95% interval) 10 11 34 20 20 50 60 38 11 12 27

content mixes may turn the plastic criterion into a pressure-dependent
one [35,36]. Flow onset may then vary with the type of stress applied
to the material: compression, tension or shear.
In order to supplement tensile measurements such as slug tests, other
geometrical configurations may be used to obtain additional informa­
tion on the material rheological behavior. For example, Jacquet et al.
[35,36] proposed to study the deformation and cracks occurrence on a
material filament exiting a printer nozzle horizontally aligned. Such a
configuration is able to induce a combination of shear and bending in
the filament. The video recording of the deformation was then used to
compute the elastic modulus and/or the critical strain of the material.
Examples of such a test is shown in Fig. 4.
3. Flow onset measurements
The gravity-driven tests presented in the previous section offer po­
tential ways to easily assess the yield stress at the level of the printing
nozzle. However, as discussed in the Introduction and background sec­
tion, for a complete quality control of the material, it is also required to
assess the speed and magnitude of the yield stress development with
time and therefore the ability of the printable material to be printed
without a failure of the element being manufactured.
As printable material's yield stress is evolving quickly with time and
since sampling the material and then placing it into the rheometer may
take time, it can be expected that short term measurements using
rheometers could prove unreliable. However, it can be assumed that,
after longer resting times, the influence of sample handling becomes
neglectable.
Rotational rheometry has been intensively used in the recent past for
assessing the so-called “structural build-up” of cement-based materials
[37]. Predominantly, Constant Rotational Velocity (CRV) test, also
referred to as Constant Shear Rate (CSR) test, was used for this purpose
[18,38–41]. In a single CRV test, a low value of constant rotational ve­
locity is applied to the material until flow onset occurs. Flow onset is
detected by the reaching of a peak or of a plateau in stress or torque on
the stress or torque vs. testing time graph [3,26], see Fig. 5 [42]. This
peak value or plateau value corresponds to the yield stress of the ma­
terial. Such a test is then repeated after various time intervals at rest, i.e.
without shearing the material, in order to observe the evolution of the
material yield stress over time.
Due to the thixotropic nature of cement-based materials, the results
of flow onset measurements are prominently sensitive to the shear history
of the tested sample [43,44]. The time, at which the sample is sheared
prior to a flow onset measurement, and the intensity of this shearing
affects the resultant static yield stress and its growth rate [44–46].
Generally, it can be recommended to keep the shear history of the tested
sample as close to the application conditions as possible. If rheological
measurements are conducted simultaneously with the printing process
for the purpose of quality control, a sample can be received directly from
the nozzle of the printer. Moreover, for stiff mixes, such pre-shearing can

4
R. Nicolas et al.
Fig. 3. Comparison between the slugs test with some reference rheological test (partially reproduced from [29]).
Fig. 4. Gravity-driven test - filament bending out of a horizontal nozzle.
create irreversible shear localization at the interface between the
rotating probe and the tested material. In the absence of pre-shear, a zero
flow onset measurement is reported to be still required in order to enable a
proper positioning of the rotating probe in the sample before the main
testing sequence [42]. This measurement is not taken into account in the
data analysis, but enables to establish a better contact between the
rotating probe and the tested material.
Another key part of such a testing protocol lies in the selection of the
applied Constant Rotational Velocity (CRV). Its value is rheometer- and
material-dependent and results from a compromise between decreasing
the material viscous contribution to the measured torque and the need to
reach the material critical shear strain (highlighted by the maximum
torque) during a reasonable duration of the test. This compromise may
evolve with the stiffening of the material over time [42,44,47]. A large
variety of applied rotational velocities or shear rates, which can differ by
a couple orders of magnitude, are therefore reported in literature. For
5
Cement and Concrete Research 158 (2022) 106836
instance, while testing printable mortars with various devices and ge­
ometries, Perrot et al. [18] applied a CSR of 0.001 s− 1, Benamara et al.
[39] used 0.01 s− 1, and Panda et al. [38] performed flow onset mea­
surements at 0.1 s− 1. This range of rotational velocities is still today a
very open research question.
To evaluate the structural build-up of printable materials over time,
single-batch approach is commonly implemented, i.e. multiple flow onset
measurements are successively conducted on the same sample
[18,38,39]. This protocol is opposed to multi-batch approach, which
implies the use of an individual sample for each age of the material [17].
The implementation of a multi-batch approach requests multiple cells
and multiple rotors; the rotors must be immersed in all samples at the
same time and kept motionless until the required resting time is reached
[42]. A similar protocol was applied by Khayat et al. [48] for flowable
mortar and concrete, while the torque was measured by a dial indicator-
type torque wrench. However, the single-batch approach has clear
R. Nicolas et al. Cement and Concrete Research 158 (2022) 106836

Fig. 6. Static yield stress evolution over resting time described by

various models.
Fig. 5. Representative curves resulting from a single flow onset measurement
by means of CRV test; T is the torque, Tmax is the maximum torque, Teq is the
equilibrium torque, Nap is the applied CRV, Nef is the effective rotational ve­ applied as an alternative to rheometers, especially under the field
locity, td is the test duration [42]. conditions [48,54].

benefits, since it is less labor-, time- and material-consuming. However, 4. Penetration tests
a single-batch protocol creates a risk of underestimating the structura­
tion rate due to the successive multiple disturbances of the sample When it comes to the assessment of yield stress evolution with time,
during testing. To some extent, this risk can be minimized by stopping flow onset measurements, despite the fact that they are better docu­
the flow onset measurement right after the peak or the appearance of the mented than many other consistency tests, are limited, on one hand, by
plateau [42]. their destructive nature and, on the other hand, by the rather low
In flow onset measurements, torque values are obtained as raw data. maximum torque typically available. They provide therefore a picture of
For coaxial cylinders and vane rheometers, Eq. (2) can be applied to the material evolution that is limited in time (only data points at given
compute the yield stress τ0 in Pa after a given time of rest from the time intervals are available) and in magnitude.
measured value of torque T at the peak in Fig. 5 [49]. As discussed in the introduction, the material phase change that we
are concerned with here covers the same range of strength as the one
τ0 =
T
(2) covered during the setting process of typical cement-based products (See
2πhr2 + n2πr3 /3 Fig. 1). Therefore, in the last decade, researchers naturally tried to adapt
the penetration test family normally used to assess setting to the study of
where h and r are the height and the radius of the rheometer probe in m,
printable material with time. Within this frame, some specific fast and
respectively; n = 1 if the contribution of the bottom surface of the probe
slow penetration tests were developed and applied to printable materials
is accounted for, and n = 2 in the case when the contributions of its top
[24,55–58,59b,59c].
and bottom surfaces are considered.
During a penetration test, a probe (in most cases, needles, cones or
The values of τ0 obtained from several consecutive flow onset mea­
spheres) penetrates the material at a given velocity. The force required
surements are then plotted versus the resting time, which equals the time
for the probe penetration is recorded as a function of time.
period from the moment when the sample is left at rest to the moment at
The advantage of this method is that, in the case of low penetration
which a CRV test is conducted. The obtained data can then be fitted with
velocities, the rheological behavior can be assessed continuously during
one of the existing thixotropy models from literature [26,50,51] as
a long test duration (up to several hours).
illustrated in Fig. 6.
Similarly to flow onset measurements using rotational rheometers
Several challenges and limitations should be kept in mind while
(see previous section), the probing tool penetration velocity is a first
assessing the yield stress evolution with time of printable materials by
order parameter of the test. The penetration velocities reported in
rotational rheometry:
literature varies between a couple mm/min to a couple thousandths of
mm/min [12,41,55]. Such a large range suggests that various regimes
- Due to their high yield stresses, these materials are prone to so-called
and therefore various material behaviors are assessed. It can be expected
“plug flow” when tested in wide-gap rheometers [52]. It must
that, at high penetration velocities, there could exist a viscous contri­
therefore be kept in mind that the computed shear strain may deviate
bution to the measured force. On the other hand, at extremely low
from the real strain applied to the material [42].
penetration velocities, it can be expected that flow onset is never
- Pre-shearing of stiff (and often concentrated) printable materials
reached as the material structuration is faster than its destructuration.
might result in the formation through shear induced particle
Such measurements are expected to provide information on the visco-
migration [53] of a thin fluid layer at the interface between the
elastic “solid” behavior of the material. They can also be seen as the
rotating probe and the material. Subsequent flow onset measure­
creep of an aging material. In this regime, viscous effects are expected to
ments conducted on the same sample may then show underestimated
be extremely high as they involve the so-called “solid viscosity” of the
torque values.
material (i.e. the material viscosity below its yield stress). The non-
- Most of the currently available rheometers have torque limitations,
viscous stress that can be computed is expected to always stay lower
which do not allow to investigate the yield stress of printable ma­
than the yield stress of the tested sample. Finally, for intermediate
terials over long resting times [17]. Possibly, torquemeters can be

6
R. Nicolas et al. Cement and Concrete Research 158 (2022) 106836

penetration velocities, one can expect to measure a force that is, in this
regime, independent of velocity itself. In this regime, this force is ex­
pected to be proportional only to the yield stress of the material.
As all the above regimes are expected to capture the consistency
increase (in its broadest definition) of the material, they are all able to
provide information of the underlying changes in the material micro-
mechanical features as a function of time.
From a practical point of view, during the test, care must be taken to
ensure that the penetration probe always has the same effective area.
This means that the material must be stiff enough so that the gap above
the penetration probe does not close [55]. For more liquid materials, the
evaluation must consider that the effective surface area of the penetra­
tion probe may increase with time.
The measured force can be translated into a yield stress (or non-
viscous stress) using various relations. These relations assume that the
probe is large when compared to the material coarsest particles and
considers mostly some non-pressure dependent plastic behavior (i.e.
non-frictional). In some early works [12,60], the yield stress is calcu­
lated at first order by simply dividing the measured force by the surface
of the penetration probe. Another approach is based on the work of
Wünsch for a falling-sphere viscometer [60]. This work was applied by
Pott et al. to the slow penetration test [55]. It was shown that yield stress
τ0 and plastic viscosity ηp must fulfill, at any time, the following
equation:
√̅̅̅̅̅̅̅
τ0 d τ0 d F
1 + 1.874 + 1.152 − =0 (3)
ηp v ηp v 3πηp vd

with the measured Force F in N, the penetration velocity v in m/s, the

diameter of the spherical probe d in m.
To solve the Eq. (3), two measurements at different velocities are
therefore necessary. This approach applies well to very low penetration
velocities as illustrated in Fig. 7(b) and correlates well with yield stresses
obtained from a rheological test.
A second approach for computing the yield stress from the measured
force originates from the field of soil mechanics and was proposed by
Reiter [41]. It can be used from a single recording of the penetration
force with time in the yield stress range of 1–200 kPa, the lower limit
given by a depth dependency simplification and the upper limit by the Fig. 7. a) Comparison of the yield stress determined by a fast and slow pene­
material behavior transition to frictional. The equation for the calcula­ tration test, compressive strength and rheometer with a vane paddle (adapted
tion of the yield stress τ0 is Eq. (4). from [61]). b) Comparison of the results of a slow penetration test penetration
test and rheometry (reproduced from [55]).
F
τ0 = (4)
αN c S To this end, various researchers have adopted compression tests for
fresh printable materials [20,58,62–64]. Similar to the well-known test
with the penetration force F in N, the penetration cross-section area S in
on hardened concrete, rock or soil [65,66], the so-called uniaxial un­
m2, the dimensionless cohesion bearing capacity factor Nc (identified as
confined compression test (UUCT) is based on a (vertical) compression
being equal to 9 for a conical tip) and αd a dimensionless factor ac­
of the sample until failure. Usually the test is performed displacement-
counting for penetration depth (increasing from 1 to approximately 1.9
controlled, although a load-controlled test is also possible, on cylindri­
with depth) [61]. This approach is illustrated in Fig. 7(a).
cal specimens of various sizes with a height-to-diameter ratio between 2
and 2.5. Since in 3D printing the evolution of the material properties is
5. Uniaxial compression tests
of interest, this destructive test is repeated at several specimen ages on
multiple specimens. Typical failure patterns are shown in Fig. 8, dis­
All methods presented above were aiming at assessing yield stress.
playing a transition from plastic failure (bulging) towards brittle failure
This value is critical to the printing process as it drives both the geom­
(shear failure plane) as specimen age increases.
etry control of each layer and the overall plastic collapse of the element
The recorded force and displacement graphs can be converted into
being printed. However, as stated in the Introduction and background
material stress-strain relations (Cf. Fig. 9), which provides insight into
section, for geometry control purposes and for stability issues, there also
the material stiffness (the slope of the initial curve), and the uniaxial
exist some requirements on the elastic modulus of the material and its
compressive strength, also called green strength (its peak value). This
evolution over time. Yield stress and elastic modulus (at least shear
critical stress is expected to be proportional to the yield stress of the
modulus) are expected to be related through the value of the critical
material. Such measurements were compared with other experimental
shear strain at which flow onset occurs. This critical strain is known to
procedures in [67].
change slowly over time [62].
Due to the fresh state of the material, however, the resulting spec­
To fully capture the material elasto-plastic behavior over time, it is
imen deformations are of a much larger order of magnitude (several %
therefore necessary to assess, in addition to its yield stress, either its
strain can be expected, in contrast to hardened material). As such, an
critical strain or its elastic modulus.
‘engineering’ stress-strain approach may result in some overestimation

7
R. Nicolas et al.
Fig. 8. Failure patterns as observed in UUCT tests on specimens with increasing age (reproduced from [13]).
Fig. 9. Stress-strain relations derived from the results of UUCT on specimens
with increasing age (reproduced from [20]).
of material properties. Instead, ‘true’ stress-strain values should be
derived by considering the actual specimen dimensions throughout the
test. To this end, standard testing procedures have been adapted to
accommodate the fresh material state, by monitoring displacements
through optic measurements such that the natural deformation behavior
is not restrained.
If the test is to be used to assess the material behavior of printed
bodies, it is critical that the sample represents the material state as
accurately as possible so that the response is not over- or under­
estimated. This means that the samples for the UUCT must be produced
and treated in the same way as the material for 3D printing, considering
e.g. specimen compaction and scale.
6. Conclusions
In the absence of a formwork, printable materials are expected to
quickly increase their yield stress and elastic modulus in order to resist
the self-weight of the structure being printed. Resolving this rheological
requirement with the printing process is the key to avoiding plastic
collapse on one hand and buckling instability on the other hand. It is
therefore necessary, from a material design, from a process design and
from a daily quality control point of view, to have the ability to measure
the above rheological parameters and their evolutions with time.
The present paper presents some high potential tests along with some
preliminary data supporting their ability to capture the above material
8
Cement and Concrete Research 158 (2022) 106836
properties while discussing the remaining and related open research
questions. Based on the list of tests presented in this paper, the following
conclusions can be drawn.
1. The slugs test allows for a simple and robust inline assessment of the
yield stress at the level of the printing nozzle. It obviously does not
allow for the measurement of the material evolution with time but it
is reported to potentially allow, through the study of the slugs mass'
standard deviation, for the assessment of the material homogeneity.
2. Standard rotational flow onset measurements allow for the mea­
surement of the material's yield stress and its evolution in time. These
tests are however destructive (at least partially) and limited by the
maximum torque of the chosen device. Moreover, when the yield
stress evolution is fast, assessing the initial yield stress of the material
may prove impossible as the placement of the sample may strongly
affect the measurement. Finally, these tests are extremely sensitive to
the constant shear chosen to be applied to the sample in a way that is
not fully understood yet.
3. Penetration tests (either fast or slow) are a family of high potential
tests that have proven their ability to quantitatively measure the
yield stress evolution and its evolution with time. Similarly to rota­
tional flow onset measurements, they however strongly depend on
the probing tool velocity in a way that is still to be explored.
4. While the above tests allow for the assessment of yield stress, uni­
axial compression tests may allow for the assessment of the elastic
modulus of the material. They are however destructive by nature and
require, for their analysis, an independent measurement of the true
strain applied to the sample.
CRediT authorship contribution statement
Roussel Nicolas: Supervision/Writing - Original Draft
Buswell Richard: Review and editing
Ducoulombier Nicolas: Methodology/Writing - Original Draft/Re­
view and editing
Ivanova Irina: Writing - Original Draft/Review and editing
Kolawole John Temitope: Investigation/Methodology/Writing -
Original Draft
Lowke Dirk: Review and editing
Mechtcherine Viktor: Review and editing
Mesnil Romain: Review and editing
Perrot Arnaud: Writing - Original Draft/Review and editing
Pott Ursula: Investigation/Methodology/Writing - Original Draft
Reiter Lex: Investigation/Methodology/Writing - Original Draft
Stephan Dietmar: Review and editing
Wangler Timothy: Writing - Original Draft/Review and editing
Wolfs Rob: Writing - Original Draft/Review and editing
Zuo Wenqiang: Review and editing
R. Nicolas et al.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
References
[1] (a) K. Kovler, N. Roussel, Properties of fresh and hardened concrete, Cem. Concr.
Res. 41 (2011) 775–792, https://doi.org/10.1016/j.cemconres.2011.03.009;
(b) P. Bartos, M. Sonebi, A. Tamimi, Workability and Rheology of Fresh Concrete:
Compendium of Tests, RILEM Publications S.a.r.l, January 2002. Publisher:. (ISBN:
2-912143-32-2).
[2] N. Roussel, A. Lemaître, R.J. Flatt, P. Coussot, Steady state flow of cement
suspensions: a micromechanical state of the art, Cem. Concr. Res. 40 (2010) 77–84,
https://doi.org/10.1016/j.cemconres.2009.08.026.
[3] N. Roussel, G. Ovarlez, S. Garrault, C. Brumaud, The origins of thixotropy of fresh
cement pastes, Cem. Concr. Res. 42 (2012) 148–157, https://doi.org/10.1016/j.
cemconres.2011.09.004.
[4] P.C. Aïtcin, R.J. Flatt, Science and Technology of Concrete Admixtures, 2015,
https://doi.org/10.1016/C2015-0-00150-2.
[5] N. Roussel, Rheology of fresh concrete: from measurements to predictions of
casting processes, Mater. Struct. Constr. 40 (2007) 1001–1012, https://doi.org/
10.1617/s11527-007-9313-2.
[6] K.H. Khayat, W. Meng, K. Vallurupalli, L. Teng, Rheological properties of ultra-
high-performance concrete — an overview, Cem. Concr. Res. 124 (2019), https://
doi.org/10.1016/j.cemconres.2019.105828.
[7] G. De Schutter, D. Feys, Pumping of fresh concrete: insights and challenges, RILEM
Tech. Lett. 1 (2016) 76–80, https://doi.org/10.21809/rilemtechlett.2016.15.
[8] N. Roussel, H. Bessaies-Bey, S. Kawashima, D. Marchon, K. Vasilic, R. Wolfs, Recent
advances on yield stress and elasticity of fresh cement-based materials, Cem.
Concr. Res. 124 (2019), https://doi.org/10.1016/j.cemconres.2019.105798.
[9] J. Zhang, E.A. Weissinger, S. Peethamparan, G.W. Scherer, Early hydration and
setting of oil well cement, Cem. Concr. Res. 40 (2010) 1023–1033, https://doi.org/
10.1016/j.cemconres.2010.03.014.
[10] G.W. Scherer, J. Zhang, J.J. Thomas, Nucleation and growth models for hydration
of cement, Cem. Concr. Res. 42 (2012) 982–993, https://doi.org/10.1016/j.
cemconres.2012.03.019.
[11] J.W. Bullard, H.M. Jennings, R.A. Livingston, A. Nonat, G.W. Scherer, J.
S. Schweitzer, K.L. Scrivener, J.J. Thomas, Mechanisms of cement hydration, Cem.
Concr. Res. 41 (2011) 1208–1223, https://doi.org/10.1016/j.
cemconres.2010.09.011.
[12] D. Lootens, P. Jousset, L. Martinie, N. Roussel, R.J. Flatt, Yield stress during setting
of cement pastes from penetration tests, Cem. Concr. Res. 39 (2009) 401–408,
https://doi.org/10.1016/j.cemconres.2009.01.012.
[13] R.J.M. Wolfs, F.P. Bos, T.A.M. Salet, Correlation between destructive compression
tests and non-destructive ultrasonic measurements on early age 3D printed
concrete, Constr. Build. Mater. 181 (2018) 447–454, https://doi.org/10.1016/j.
conbuildmat.2018.06.060.
[14] S. Lim, R.A. Buswell, T.T. Le, S.A. Austin, A.G.F. Gibb, T. Thorpe, Developments in
construction-scale additive manufacturing processes, Autom. Constr. 21 (2012)
262–268, https://doi.org/10.1016/j.autcon.2011.06.010.
[15] B. Khoshnevis, Automated construction by contour crafting - related robotics and
information technologies, in, Autom. Constr. (2004) 5–19, https://doi.org/
10.1016/j.autcon.2003.08.012.
[16] R.A. Buswell, W.R.L. da Silva, F.P. Bos, H.R. Schipper, D. Lowke, N. Hack, H. Kloft,
V. Mechtcherine, T. Wangler, N. Roussel, A process classification framework for
defining and describing digital fabrication with concrete, Cem. Concr. Res. 134
(2020), https://doi.org/10.1016/j.cemconres.2020.106068.
[17] N. Roussel, Rheological requirements for printable concretes, Cem. Concr. Res. 112
(2018) 76–85, https://doi.org/10.1016/j.cemconres.2018.04.005.
[18] A. Perrot, D. Rangeard, A. Pierre, Structural built-up of cement-based materials
used for 3D-printing extrusion techniques, Mater. Struct. Constr. 49 (2016)
1213–1220, https://doi.org/10.1617/s11527-015-0571-0.
[19] T. Wangler, E. Lloret, L. Reiter, N. Hack, F. Gramazio, M. Kohler, M. Bernhard,
B. Dillenburger, J. Buchli, N. Roussel, R. Flatt, Digital concrete: opportunities and
challenges, RILEM Tech. Lett. 1 (2016) 67, https://doi.org/10.21809/
rilemtechlett.2016.16.
[20] R.J.M. Wolfs, F.P. Bos, T.A.M. Salet, Early age mechanical behaviour of 3D printed
concrete: numerical modelling and experimental testing, Cem. Concr. Res. 106
(2018) 103–116, https://doi.org/10.1016/j.cemconres.2018.02.001.
[21] V. Mechtcherine, F.P. Bos, A. Perrot, W.R.L. da Silva, V.N. Nerella, S. Fataei, R.J.
M. Wolfs, M. Sonebi, N. Roussel, Extrusion-based additive manufacturing with
cement-based materials – production steps, processes, and their underlying
physics: a review, Cem. Concr. Res. 132 (2020), 106037, https://doi.org/10.1016/
j.cemconres.2020.106037.
[22] A.S.J. Suiker, R.J.M. Wolfs, S.M. Lucas, T.A.M. Salet, Elastic buckling and plastic
collapse during 3D concrete printing, Cem. Concr. Res. 135 (2020), 106016,
https://doi.org/10.1016/j.cemconres.2020.106016.
[23] D. Marchon, S. Kawashima, H. Bessaies-Bey, S. Mantellato, S. Ng, Hydration and
rheology control of concrete for digital fabrication: potential admixtures and
cement chemistry, Cem. Concr. Res. 112 (2018) 96–110, https://doi.org/10.1016/
j.cemconres.2018.05.014.
9
Cement and Concrete Research 158 (2022) 106836
[24] L. Reiter, T. Wangler, A. Anton, R.J. Flatt, Setting on demand for digital concrete –
principles, measurements, chemistry, validation, Cem. Concr. Res. 132 (2020),
106047, https://doi.org/10.1016/j.cemconres.2020.106047.
[25] Y. Tao, A.V. Rahul, K. Lesage, Y. Yuan, K. Van Tittelboom, G. De Schutter,
Stiffening control of cement-based materials using accelerators in inline mixing
processes: possibilities and challenges, Cem. Concr. Compos. 119 (2021), https://
doi.org/10.1016/j.cemconcomp.2021.103972.
[26] N. Roussel, A thixotropy model for fresh fluid concretes: theory, validation and
applications, Cem. Concr. Res. 36 (2006) 1797–1806, https://doi.org/10.1016/j.
cemconres.2006.05.025.
[27] N. Roussel, P. Coussot, “Fifty-cent rheometer” for yield stress measurements: from
slump to spreading flow, J. Rheol. (N. Y. N. Y.) 49 (2005) 705–718, https://doi.
org/10.1122/1.1879041.
[28] N. Roussel, Correlation between yield stress and slump: comparison between
numerical simulations and concrete rheometers results, Mater. Struct. Constr. 39
(2006) 501–509, https://doi.org/10.1617/s11527-005-9035-2.
[29] N. Ducoulombier, R. Mesnil, P. Carneau, L. Demont, H. Bessaies-Bey, J.F. Caron,
N. Roussel, The “slugs-test” for extrusion-based additive manufacturing: protocol,
analysis and practical limits, Cem. Concr. Compos. 121 (2021), https://doi.org/
10.1016/j.cemconcomp.2021.104074.
[30] P. Coussot, F. Gaulard, Gravity flow instability of viscoplastic materials: the
ketchup drip, Phys. Rev. E Stat. Nonlinear, Soft Matter Phys. 72 (2005), https://
doi.org/10.1103/PhysRevE.72.031409.
[31] A. Geffrault, H. Bessaies-Bey, N. Roussel, P. Coussot, Extensional gravity-rheometry
(EGR) for yield stress fluids, J. Rheol. (N. Y. N. Y.) 65 (2021) 887–901, https://doi.
org/10.1122/8.0000241.
[32] P.V. Liddell, D.V. Boger, Yield stress measurements with the vane, J. Nonnewton.
Fluid Mech. 63 (1996) 235–261, https://doi.org/10.1016/0377-0257(95)01421-7.
[33] N. Ducoulombier, P. Carneau, R. Mesnil, L. Demont, J.F. Caron, N. Roussel, “The
Slug Test”: Inline Assessment of Yield Stress for Extrusion-Based Additive
Manufacturing, in: RILEM Bookseries, 2020, pp. 216–224, https://doi.org/
10.1007/978-3-030-49916-7_22.
[34] P. Carneau, R. Mesnil, N. Ducoulombier, N. Roussel, O. Baverel, Characterisation of
the Layer Pressing Strategy for Concrete 3D Printing, in: RILEM Bookseries, 2020,
pp. 185–195, https://doi.org/10.1007/978-3-030-49916-7_19.
[35] Y. Jacquet, A. Perrot, V. Picandet, Assessment of asymmetrical rheological
behavior of cementitious material for 3D printing application, Cem. Concr. Res.
140 (2021), https://doi.org/10.1016/j.cemconres.2020.106305.
[36] Y. Jacquet, V. Picandet, D. Rangeard, A. Perrot, Gravity Driven Tests to Assess
Mechanical Properties of Printable Cement-Based Materials at Fresh State, in:
RILEM Bookseries, 2020, pp. 280–289, https://doi.org/10.1007/978-3-030-
49916-7_29.
[37] P.F.G. Banfill, D.C. Saunders, On the viscometric examination of cement pastes,
Cem. Concr. Res. 11 (1981) 363–370, https://doi.org/10.1016/0008-8846(81)
90108-3.
[38] B. Panda, J.H. Lim, M.J. Tan, Mechanical properties and deformation behaviour of
early age concrete in the context of digital construction, Compos. Part B Eng. 165
(2019) 563–571, https://doi.org/10.1016/j.compositesb.2019.02.040.
[39] A. Benamara, A. Pierre, A. Kaci, Y. Melinge, 3D Printing of a Cement-Based Mortar
in a Complex Fluid Suspension: Analytical Modeling and Experimental Tests, in:
RILEM Bookseries, 2020, pp. 768–777, https://doi.org/10.1007/978-3-030-
49916-7_76.
[40] J. Kruger, Rheo-mechanics modelling of 3D concrete printing constructability.
https://scholar.sun.ac.za, 2019.
[41] L. Reiter, Structural Build-up for Digital Fabrication with Concrete - Materials,
Methods and Processes, 2019, https://doi.org/10.3929/ethz-a-010025751.
[42] I. Ivanova, V. Mechtcherine, Possibilities and challenges of constant shear rate test
for evaluation of structural build-up rate of cementitious materials, Cem. Concr.
Res. 130 (2020), https://doi.org/10.1016/j.cemconres.2020.105974.
[43] G. Ovarlez, F. Mahaut, S. Deboeuf, N. Lenoir, S. Hormozi, X. Chateau, Flows of
suspensions of particles in yield stress fluids, J. Rheol. (N. Y. N. Y.) 59 (2015)
1449–1486, https://doi.org/10.1122/1.4934363.
[44] I. Ivanova, V. Mechtcherine, Evaluation of Structural Build-Up Rate of
Cementitious Materials by Means of Constant Shear Rate Test: Parameter Study, in:
RILEM Bookseries, 2020, pp. 209–218, https://doi.org/10.1007/978-3-030-
22566-7_25.
[45] S. Ma, Y. Qian, S. Kawashima, Experimental and modeling study on the non-linear
structural build-up of fresh cement pastes incorporating viscosity modifying
admixtures, Cem. Concr. Res. 108 (2018) 1–9, https://doi.org/10.1016/j.
cemconres.2018.02.022.
[46] A. Pierre, A. Perrot, A. Histace, S. Gharsalli, E.H. Kadri, A study on the limitations
of a vane rheometer for mineral suspensions using image processing, Rheol. Acta
56 (2017) 351–367, https://doi.org/10.1007/s00397-017-0993-4.
[47] V.N. Nerella, M.A.B. Beigh, S. Fataei, V. Mechtcherine, Strain-based approach for
measuring structural build-up of cement pastes in the context of digital
construction, Cem. Concr. Res. 115 (2019) 530–544, https://doi.org/10.1016/j.
cemconres.2018.08.003.
[48] K.H. Khayat, A.F. Omran, S. Naji, P. Billberg, A. Yahia, Field-oriented test methods
to evaluate structural build-up at rest of flowable mortar and concrete, Mater.
Struct. Constr. 45 (2012) 1547–1564, https://doi.org/10.1617/s11527-012-9856-
8.
[49] G. Ovarlez, G. Ovarlez, Caractérisation rhéologique des fluides à seuil, 2011.
[50] A. Perrot, A. Pierre, S. Vitaloni, V. Picandet, Prediction of lateral form pressure
exerted by concrete at low casting rates, Mater. Struct. Constr. 48 (2015)
2315–2322, https://doi.org/10.1617/s11527-014-0313-8.
R. Nicolas et al.
[51] J. Kruger, S. Zeranka, G. van Zijl, An ab initio approach for thixotropy
characterisation of (nanoparticle-infused) 3D printable concrete, Constr. Build.
Mater. 224 (2019) 372–386, https://doi.org/10.1016/j.conbuildmat.2019.07.078.
[52] D. Feys, J.E. Wallevik, A. Yahia, K.H. Khayat, O.H. Wallevik, Extension of the
Reiner-Riwlin equation to determine modified Bingham parameters measured in
coaxial cylinders rheometers, Mater. Struct. Constr. 46 (2013) 289–311, https://
doi.org/10.1617/s11527-012-9902-6.
[53] J. Spangenberg, N. Roussel, J.H. Hattel, H. Stang, J. Skocek, M.R. Geiker, Flow
induced particle migration in fresh concrete: theoretical frame, numerical
simulations and experimental results on model fluids, Cem. Concr. Res. 42 (2012)
633–641, https://doi.org/10.1016/j.cemconres.2012.01.007.
[54] P. Estellé, C. Lanos, High torque vane rheometer for concrete: principle and
validation from rheological measurements, Appl. Rheol. 22 (2012), https://doi.
org/10.3933/ApplRheol-22-12881.
[55] U. Pott, D. Stephan, Penetration test as a fast method to determine yield stress and
structural build-up for 3D printing of cementitious materials, Cem. Concr. Compos.
121 (2021), https://doi.org/10.1016/j.cemconcomp.2021.104066.
[56] A. Szabo, L. Reiter, E. Lloret-Fritschi, T. Wangler, F. Gramazio, M. Kohler, R.
J. Flatt, ACDC: The Admixture Controlled Digital Casting and Its Application to
Thin Folded Concrete Structures, in: RILEM Bookseries, 2020, pp. 956–966,
https://doi.org/10.1007/978-3-030-49916-7_93.
[57] B. Mazhoud, A. Perrot, V. Picandet, D. Rangeard, E. Courteille, Underwater 3D
printing of cement-based mortar, Constr. Build. Mater. 214 (2019) 458–467,
https://doi.org/10.1016/j.conbuildmat.2019.04.134.
[58] I. Dressler, N. Freund, D. Lowke, The effect of accelerator dosage on fresh concrete
properties and on interlayer strength in shotcrete 3D printing, Materials (Basel) 13
(2020), https://doi.org/10.3390/ma13020374.
[59] (a) H. Kloft, H.W. Krauss, N. Hack, E. Herrmann, S. Neudecker, P.A. Varady,
D. Lowke, Influence of process parameters on the interlayer bond strength of
concrete elements additive manufactured by Shotcrete 3D Printing (SC3DP), Cem.
Concr. Res. 134 (2020), https://doi.org/10.1016/j.cemconres.2020.106078;
(b) Marie Bohuchval, Mohammed Sonebi, Sofiane Amziane, Arnaud Perrot, Effect
of metakaolin and natural fibres on three-dimensional printing mortar, Proc. Inst.
10
Cement and Concrete Research 158 (2022) 106836
Civil Eng. Construct. Mater. 174 (3) (2021) 115–128;
(c) M. Sonebi, M. Dedenis, S. Amziane, A. Abdalqader, A. Perrot, Effect of red
mud, nanoclay, and natural fiber on fresh and rheological properties of three-
dimensional concrete printing, ACI Mater. J. 118 (6) (2021) 97–110.
[60] E. Lloret Fritschi, Smart Dynamic Casting: A Digital Method for Non-standard
Concrete Structures, 2016.
[61] L. Reiter, T. Wangler, N. Roussel, R. Flatt, Slow penetration for characterizing
concrete during its digital fabrication.pdf, Submitted. (n.d.).
[62] L. Nachbaur, J.C. Mutin, A. Nonat, L. Choplin, Dynamic mode rheology of cement
and tricalcium silicate pastes from mixing to setting, Cem. Concr. Res. 31 (2001)
183–192, https://doi.org/10.1016/S0008-8846(00)00464-6.
[63] L.K. Mettler, F.K. Wittel, R.J. Flatt, H.J. Herrmann, Evolution of strength and
failure of SCC during early hydration, Cem. Concr. Res. 89 (2016) 288–296,
https://doi.org/10.1016/j.cemconres.2016.09.004.
[64] Y. Chen, S. Chaves Figueiredo, Z. Li, Z. Chang, K. Jansen, O. Çopuroğlu,
E. Schlangen, Improving printability of limestone-calcined clay-based cementitious
materials by using viscosity-modifying admixture, Cem. Concr. Res. 132 (2020)
1–37, https://doi.org/10.1016/j.cemconres.2020.106040.
[65] EN196-1, Methods of testing cement - part 1: determination of strength, Eur. Stand.
(2005) 1–33.
[66] ASTM, Standard Test Method for Unconfined Compressive Strength of Cohesive
Soil 1, in: ASTM Int., 2013, pp. 1–7.
[67] F.P. Bos, J. Kruger, S.S. Lucas, G. van Zijl, Juxtaposing fresh material
characterisation methods for buildability assessment of 3D printable cementitious
mortars, Cement Concr. Compos. 120 (2021) 104024, https://doi.org/10.1016/j.
cemconcomp.2021.104024.
[68] R. Wolfs, F. Bos, T. Salet, Triaxial compression testing on early age concrete for
numerical analysis of 3D concrete printing, Cement Concr. Compos. 104 (2019),
103344.
[69] Roshan Jayathilakage, Jay Sanjayan, Pathmanathan Rajeev, Direct shear test for
the assessment of rheological parameters of concrete for 3D printing applications,
Mater. Struct. 52 (2019) 12, https://doi.org/10.1617/s11527-019-1322-4.