Materials: Ffect of Accelerator Dosage On Fresh Concrete

materials
Article
The Effect of Accelerator Dosage on Fresh Concrete
Properties and on Interlayer Strength in Shotcrete
3D Printing
Inka Dressler * , Niklas Freund and Dirk Lowke
Institute of Building Materials, Concrete Construction and Fire Safety, TU Braunschweig,
38106 Braunschweig, Germany; n.freund@ibmb.tu-bs.de (N.F.); d.lowke@ibmb.tu-bs.de (D.L.)
* Correspondence: i.dressler@ibmb.tu-bs.de; Tel.: +49-531-391-5582

Received: 19 November 2019; Accepted: 8 January 2020; Published: 14 January 2020
Abstract: Recently, the progress in 3D concrete printing has developed enormously. However, for the
techniques available, there is still a severe lack of knowledge of the functional interaction of processing
technology, concrete rheology and admixture usage. For shotcrete 3D printing technology, we present
the effect of accelerator dosages (0%, 2%, 4% and 6%) on fresh concrete properties and on interlayer
strength. Therefore, early yield stress development up to 90 min is measured with penetration
resistance measurements. Deformation of layers under loading is investigated with digital image
correlation and a mechanical testing machine. One point in time (10 min after deposition) is examined
to quantify vertical buildability of elements depending on the accelerator dosage. Four different
interlayer times (0, 2, 5 and 30 min), which occur for the production of small and large elements
as well as due to delay during production, are investigated mechanically as well as quantitatively
with computed tomography regarding the formation of cold joints. With increased accelerator
dosage, an instantaneous increase in early age yield stress and yield stress evolution was observed.
An increase in interlayer time leads to a reduced strength. This is mainly attributed to the observed
reduced mechanical interlocking effect of the strands. Finally, a model to describe interlayer quality is
presented. In the end, advantages as well as limitations of the findings are discussed.
Keywords: additive manufacturing; shotcrete 3D printing; interlayer strength; bond; accelerator
1. Introduction
3D printing is proclaimed to be “the third industrial revolution” [1], as many believe it has the
potential to revolutionize all manufacturing processes. Even though cementitious building materials
such as concrete can theoretically be used to create elements of any shape, in today’s concrete
construction, simple shapes with a constant cross-section are largely used. This is due to the high
cost of freeform formwork on the one hand and the low degree of automation in construction on the
other hand. Compared to conventional production, 3D printing techniques hold an advantage for the
fully automated production of components of high geometric complexity-even for small quantities.
Therefore, 3D printing seems to be ideally suited for construction where piece production and geometric
complexity are common [2]. CNC-based and robot-controlled 3D printing processes in particular
offer the opportunity to minimize cost-intensive manual production. Freed from the constraints of
conventional manufacturing, the shape of structural elements can be tailored to various requirements
and functions. In contrast to traditional construction methods, particularly those used in concrete
construction, where a single type of material is poured into formwork, it may also be possible to
achieve functional grading (see, for example, [3]) by creating structural reinforced elements with
non-standard geometries and varying the material properties during the printing process. Generally
Materials 2020, 13, 374; doi:10.3390/ma13020374 www.mdpi.com/journal/materials

Materials 2020, 13, x FOR PEER REVIEW 2 of 20
Materials 2020, 13, 374 2 of 19

process. Generally speaking, this would lead to more economic, higher-quality construction
processes and more efficient material usage.
For this
speaking, large-scale
would lead additive
to more manufacturing in construction,
economic, higher-quality mainlyprocesses
construction extrusionand or more
shotcrete
efficient3D
printingusage.
material techniques, where the premixed cementitious material is extruded or sprayed in long
strands, are applied.
For large-scale In general,
additive two main strategies
manufacturing can be distinguished:
in construction, mainly extrusion (I) the deposition
or shotcrete 3Dofprinting
narrow
strands of several
techniques, wherecentimetres’
the premixed width, which are either
cementitious materialstitched to createor
is extruded thesprayed
desired in structure or used
long strands,
to build
are applied.a filigree formwork
In general, two main structure strengthened
strategies by an inner structure
can be distinguished: (compareofconcrete
(I) the deposition narrow printing
strands
[4–10]
of severaland contour crafting
centimetres’ width,[11–14])
which are and (II) the
either deposition
stitched to create of the
broaddesiredstrands of several
structure decimetres’
or used to build
awidth,
filigreewhich
formworkare used to build
structure the whole width
strengthened of thestructure
by an inner component in a single
(compare pass as
concrete a kind[4–10]
printing of ‘infinite
and
brick’ (compare, e.g., ConPrint3D [15,16]). The major advantage
contour crafting [11–14]) and (II) the deposition of broad strands of several decimetres’ width, whichof these techniques is the high
manufacturing
are used to buildspeed for creating
the whole width oflarge-sized
the component monolithic
in a singlestructures
pass as aaskind wellofas‘infinite
the building size of the
brick’ (compare,
produced
e.g., ConPrint3D elements.[15,16]). The major advantage of these techniques is the high manufacturing speed
High manufacturing
for creating large-sized monolithicspeed means the as
structures needwellforas atherapid structural
building size ofbuild-up
the producedof theelements.
deposited
material,
High as the stability of
manufacturing the printed
speed means the strand
needisfor based onstructural
a rapid the self-supporting
build-up offunction of thematerial,
the deposited concrete
due
as thetostability
the absence of theofprinted
a supporting
strandformwork.
is based onInthe addition to the inherent
self-supporting function stability
of theofconcrete
the strand,due theto
printed material also has to bear the load of the subsequent layers. To
the absence of a supporting formwork. In addition to the inherent stability of the strand, the printed enable the printed layer to bear
the loadalso
material of thehasnext layer
to bear thewithout
load of thecollapsing,
subsequent a minimum
layers. Toyieldenable stress is necessary
the printed [5,17–20].
layer to bear the Forloadthis
of
purpose, t defines the point in time when a subsequent layer can
the next layer without collapsing, a minimum yield stress is necessary [5,17–20]. For this purpose, tmin
min be applied to the existing layer
[20], seethe
defines Figure
point1.inAchieving
time whenthe minimum layer
a subsequent required can yield stressto
be applied is the
highly dependent
existing on the
layer [20], see mixtures
Figure 1.
composition
Achieving the and the used
minimum admixtures.
required In particular,
yield stress the use of set
is highly dependent on accelerators
the mixturessignificantly
composition changesand the
the setting behaviour of the concrete and enables, derived from this,
used admixtures. In particular, the use of set accelerators significantly changes the setting behaviour the manufacturing of largeof
building
the concrete heights.
and enables, derived from this, the manufacturing of large building heights.
However,to
However, tomake
makedeposition
depositiontechniques
techniquesmechanically
mechanicallycompetitive
competitivefor forcasting
castingof ofconcrete
concretehigh high
interlayer adhesion, e.g., the prevention of cold joints, is required [21].
interlayer adhesion, e.g., the prevention of cold joints, is required [21]. Therefore, the roughness of Therefore, the roughness of
the interface
the interface region
region isisrelevant,
relevant, which
which isispredominantly
predominantly determineddetermined by by mixture
mixture composition
composition (e.g., (e.g.,
aggregate size, cement, water–cement-ratio, admixtures). Moreover,
aggregate size, cement, water–cement-ratio, admixtures). Moreover, time delay between two layers, time delay between two layers,
whichoften
which oftenresults
resultsfrom
fromthe theproduction
productionprocess
processitself,
itself,isisimportant
importantsince sincelimited
limitedinterlocking
interlockingoccurs occurs
afteraacritical
after criticalresting
restingtimetime[22].
[22].For
Forthethecontinuous
continuousproduction
productionof ofvarious
varioussized sizedelements,
elements,the thenozzle
nozzle
willapply
will applythe the adjacent
adjacent layer
layer within
within several
several secondsseconds
up toup to aminutes.
a few few minutes. When production
When production stop occurs,stop
occurs,
the the adjacent
adjacent layer willlayer will be several
be applied appliedminutes
several minutes
up to a few up to a few
hours hours later.
later.
It is important to investigate the effect of yield stress development as wellas
It is important to investigate the effect of yield stress development as well as the
the effect effect of
of different
different accelerator dosages on the quality of the layer interlocking.
accelerator dosages on the quality of the layer interlocking. For this purpose, a maximum yield stress For this purpose, a maximum
yieldthus,
and, stress and, thus, delay
a maximum a maximum
time tmax delay
needtime tmaxdefined.
to be need toThis be defined.
represents Thisanrepresents
upper limit anwith
upper limit
regard
with regard to the interlayer strength
to the interlayer strength quality, Figure 1. quality, Figure 1.
Figure 1. Principle of yield stress development over time with and without set-accelerator as well as
Figure 1. Principle of yield stress development over time with and without set-accelerator as well as
the open window for processing shotcrete indicated by tmin and tmax.
the open window for processing shotcrete indicated by tmin and tmax.
Materials2020,
Materials 2020,13,
13,374
x FOR PEER REVIEW 3 3ofof20
19
Although the progress in 3D concrete printing has developed enormously [23], there is still a
Although
severe lack of the progressofinthe
knowledge 3Dfunctional
concrete printing
interactionhasofdeveloped
processingenormously
technology, [23], thererheology
concrete is still a
severe
and admixture usage. This paper presents for Shotcrete 3D Printing (SC3DP) technology the effectand
lack of knowledge of the functional interaction of processing technology, concrete rheology of
admixture
a range of usage.
acceleratorThisdosages
paper presents
(0%, 2%,for 4%,Shotcrete 3D Printing
6%) on fresh concrete(SC3DP)
properties technology theevolution)
(yield stress effect of a
range
and onof interlayer
acceleratorstrength.
dosages (0%, 2%, 4%, 6%) on fresh concrete properties (yield stress evolution) and
on interlayer strength.
2. Shotcrete 3D Printing (SC3DP) Technology
2. Shotcrete 3D Printing (SC3DP) Technology
SC3DP is a novel additive manufacturing method using an automated wet-mix shotcrete process
SC3DP
[24–26]. It isis assigned
a novel additive
to the open manufacturing
space depositionmethod 3D using
printing an technologies
automated wet-mix shotcrete
and is especially
process
designed[24–26].
for theItmanufacturing
is assigned to the open spacecomponents,
of large-scale deposition 3D printing
Figure 2. Due technologies
to the varyingandnozzle
is especially
angle
designed
from 0° for the manufacturing
to 180°, of large-scale
full three-dimensional components,
processing Figure 2. Due
are achievable. The to the varying
resulting nozzleofangle
geometry the
from 0◦ topath
printed 180◦can, fullbethree-dimensional
varied by different processing are achievable.
process parameters such The resulting
as nozzle geometry
distance of the
and path printed
velocity.
path can the
Unlike be varied
extrusionby different
method,process
SC3DPparameters
uses high such as nozzle
kinetic energydistance
for the and path velocity.
application Unlike
of concrete.
Specimens
the extrusionmanufactured
method, SC3DP withusesthishigh
technology show an
kinetic energy forincrease of contact
the application of surface
concrete. between the
Specimens
layers, which allows
manufactured with this a good interlocking
technology show effect [27]. Forof
an increase this reason,surface
contact the usebetween
of high kinetic energy
the layers, can
which
lead toa good
allows the minimization
interlockingof cold[27].
effect jointsFor[28].
thisHowever,
reason, the due usetoofthe
highproduction without
kinetic energy cansupporting
lead to the
formwork, theofSC3DP
minimization as well
cold joints as the
[28]. extrusion
However, dueprocess
to theare based on awithout
production self-supporting
supportingof the printed
formwork,
material. The contrary requirements, which are caused by the pumping
the SC3DP as well as the extrusion process are based on a self-supporting of the printed material. process and the required
pumpability
The on the one hand
contrary requirements, whichand the subsequent
are caused rapid structural
by the pumping process and build-up as well
the required as pursued
pumpability on
interlayer
the one hand strength
and theon the other hand,
subsequent rapid necessitate the targeted
structural build-up use as
as well of pursued
admixtures (e.g., superplasticizer
interlayer strength on the
and set
other accelerator)
hand, necessitate [18,27]. Compressed
the targeted air is applied
use of admixtures in superplasticizer
(e.g., the nozzle to spray andthe
set pumped
accelerator)concrete.
[18,27].
Moreover, admixtures may be induced in the nozzle, which are homogeneously
Compressed air is applied in the nozzle to spray the pumped concrete. Moreover, admixtures may distributed by thebe
compressed
induced in theair.nozzle, which are homogeneously distributed by the compressed air.
Figure2.2.Digital
Figure DigitalBuilding
Building Fabrication
Fabrication Laboratory (DBFL) at
Laboratory (DBFL) at Technische
Technische Universität
Universität Braunschweig,
Braunschweig,
Germany (© Institute of Structural Design Technische Universität Braunschweig), compare [25,29].
Germany (© Institute of Structural Design Technische Universität Braunschweig), compare [25,29].
3. Effects on Interlayer Strength
3. Effects on Interlayer Strength
It is commonly known that the bond between two layers in 3D-printing is a prerequisite to avoid
It is commonly known that the bond between two layers in 3D-printing is a prerequisite to avoid
weak spots and anisotropy (e.g., [21,22,30–32]). There are two main factors influencing the interface
weak spots and anisotropy (e.g., [21,22,30–32]). There are two main factors influencing the interface
bond between two concrete layers [33]:
bond between two concrete layers [33]:
(a)
(a) mechanical
mechanical effect:
effect: mechanical
mechanical bonding relies solely
bonding relies solely on
on the
the physical
physicalattributes
attributesofofthe
thelayers,
layers,e.g.,
e.g.,
micro roughness of substrate, cohesion and friction coefficients of the layers and age
micro roughness of substrate, cohesion and friction coefficients of the layers and age of the of the bottom
strand
bottomasstrand
well asasrheological properties
well as rheological of the single
properties layers
of the single[31,32].
layersThe inability
[31,32]. of the layers
The inability of theto
interlock
layers to lead to a reduced
interlock lead to a contact
reducedarea and area
contact herewith to a reduced
and herewith interlayer
to a reduced adhesion.
interlayer adhesion.
(b) chemical effect: chemical bonding occurs if the hydration and chemical
(b) chemical effect: chemical bonding occurs if the hydration and chemical bonding of bonding of particles
particles
occurs
occursin inbetween
between two
two layers
layers [31].
[31].
Materials 2020, 13, 374 4 of 19
Moreover, it is possible that there are further factors, such as homogeneity, affecting interface
bond. However, these factors have not been systematically investigated yet.
Up to now, the effect of interlayer strength in the context of 3D printing has mainly been observed
with extrusion-based techniques. Anisotropic behaviour was observed for mechanical strength of
3D-printed specimen [34–37], which is attributed to the oriented interface properties [38]. In [39],
a flexural strength of a cement-based mortar with a water-to-binder-ratio of 0.42 for layers oriented
perpendicular to a loading direction of 10.1 MPa was reported, whereas, for layers with parallel
orientation, a reduced flexural strength of 5.3 MPa (approximately 48% strength loss) was determined.
The anisotropic effect was found to be more distinct for tensile strength than for compressive strength,
which indicates that the increase in interlayer strength could be due to the increase in contact surface,
e.g., due to interlocking, of the layers [32]. The positive effect of an increase in contact area on interlayer
strength has also been identified by [40,41].
A reduction of flexural strength with interlayer time in between the manufacturing of two layers
was explained with a higher amount of pores/voids [41], microcracks at the interface as well as drying
and plastic shrinkage [31,39]. In the latter, a reduction in flexural strength has been reported for
specimen with a water-binder-ratio of 0.42 when the interlayer time in between the layers increased
from one minute to ten minutes (up to 45% strength loss) or even one day (up to 85% strength loss),
whereas, in [41], an interlayer strength reduction of 89% for a 10 minutes-interlayer time and 97% for
60 minutes-interlayer time was reported for a mortar with a water-cement-ratio of 0.36 for a printing
speed of 3 cm/s. In addition, reference [9] stated that there is a time window for geopolymer mortars in
which the interval time has negligible effect on interlayer strength, whereas, outside of the window,
the negative effects are significant. In [42], it is found that an increase in water–cement ratio has a
positive effect on relative interlayer strength for an interlayer time of two hours. For a specimen with a
water–cement ratio of 0.40, the relative interlayer strength was reported to be nearly 100% (compared
to monolithic specimen), whereas it dropped to below 60% for a specimen with a water–cement ratio
of 0.20. Therefore, extremely localized drying is assumed to be the origin of a drop in bond strength in
particular for flowable mortars with low water-to-cement ratios since evaporated liquid is not replaced
quickly enough by liquid from the inner part of the layer. Herewith, a weak region with less hydrated
cement than in the rest of the layer is prevalent. This could be complemented by the finding that
moisture content of the bottom layer has an effect on interlayer strength, where a higher moisture
content led to an increase in interlayer strength within the investigated boundary conditions [30,43].
The usage of silica fume in mixture composition (positive effect) [44], decrease in aggregate size
and aggregate-to-cement ratio (positive effect) [45] were found to affect interlayer strength. In addition,
a high structuration rate of the material is negatively affecting interlayer strength of geopolymer
mortars [9]. In [46], it is stated in the context of distinct-layer casting of self compacting concrete that
the thixotropic behaviour should remain under a certain threshold value to allow subsequent layers to
mix. This means that there is a critical timeframe for each mixture composition, which is influenced
by factors such as particle packing, cement type [47], or admixtures [48], in order to enable a high
interlayer bond.
In addition to this, the process of applying the layer has been identified to affect interlayer
strength. In [34], it is stated that there is no significant effect on interlayer strength of 3D printed
concrete when the distance from the nozzle to layer is changed. By contrast, [49] found an increase
of the nozzle height to have a negative effect on interlayer strength of geopolymers mortars. This is
supported by [9], who measured the same correlation and found additionally the mixture composition
as an influencing factor when varying the nozzle distance. Reference [41] investigated the effect of
printing speed on interlayer strength. They measured a strength reduction of approximately 50% when
increasing the printing speed from 1.7 cm/s to 3 cm/s and explained the effect with an increase in voids
and a decrease in surface roughness of the contact area in between the layers. In [28], the interlayer
adhesion is compared for extrusion- and SC3DP-technique. For the same material, the mechanical
strength (expressed in flexural and compressive strength) of the SC3DP-specimen is higher than that
Materials 2020, 13, 374 5 of 19
induced kinetic energy, which leads to a reduced air void content (expressed in a higher density) and
herewith higher strength.
of extruded
The findingsspecimen. Thisthe
regarding is assumed
effects ontointerlayer
be due to strength
higher induced
are notkinetic
alwaysenergy, which leads to a
consistent—compare
reduced air void content (expressed in a higher density) and herewith higher strength.
[23]. In addition, there are nearly no data available on systems with significant structural build-up as
The findings
it is prevalent regarding the effects
in SC3DP-technology. The on interlayer strength
development are not always
of fundamental theoriesconsistent—compare [23].
is necessary to explain
In addition, there are nearly no data available on systems with significant structural
the observed effects regardless of a specific mixture composition. Moreover, coherent testing build-up as it is
prevalent in SC3DP-technology. The development of fundamental theories is necessary
procedures regarding the production of the specimen (e.g., geometry of specimen, loading direction) to explain the
observed
need effects regardless
to be established to makeofresults
a specific mixture composition.
comparable in the future.Moreover, coherent testing procedures
regarding the production of the specimen (e.g., geometry of specimen, loading direction) need to be
4. established
Materials and to make results comparable in the future.
Methods
4. Scope
4.1. Materials and Methods
and Concept of Experimental Investigation
4.1.The
Scope and Concept
presented of Experimental
investigations Investigation
pursued the goal to determine the effect of accelerator dosage and
the time gap in between two strands of shotcrete on (a) vertical buildability and (b) interlayer
The presented investigations pursued the goal to determine the effect of accelerator dosage and
strength, e.g., mechanical performance. Both accelerator dosage and interlayer time are assumed to
the time gap in between two strands of shotcrete on (a) vertical buildability and (b) interlayer strength,
have an effect on the properties of the contact area in between the layers.
e.g., mechanical performance. Both accelerator dosage and interlayer time are assumed to have an
In line with this, a multi-scale approach is chosen for the investigations of shotcrete layers with
effect on the properties of the contact area in between the layers.
variations in the content of accelerator (0%, 2%, 4%, 6%) and interlayer time in between two strands
In line with this, a multi-scale approach is chosen for the investigations of shotcrete layers with
(0 min, 2 min, 5 min, 30 min). On a macroscopic level, the fresh properties (yield stress evolution over
variations in the content of accelerator (0%, 2%, 4%, 6%) and interlayer time in between two strands
time, deformation under loading, geometry) as well as hardened properties (compressive and 3-
(0 min, 2 min, 5 min, 30 min). On a macroscopic level, the fresh properties (yield stress evolution
point-bending-tests) are investigated. On a microscopic level, the interlayer zone is investigated in
over time, deformation under loading, geometry) as well as hardened properties (compressive and
more detail on drilling cores using micro-computed-tomography (µCT) and image post-processing.
3-point-bending-tests) are investigated. On a microscopic level, the interlayer zone is investigated in
The manufacturing process is divided into two steps. In the first step, three layers are sprayed
more detail on drilling cores using micro-computed-tomography (µCT) and image post-processing.
over a length of 1200 mm, which corresponds with an approximate sample height of 10 cm. For
The manufacturing process is divided into two steps. In the first step, three layers are sprayed
mechanical investigations on the printed layers in fresh state, one half of the sample was removed
over a length of 1200 mm, which corresponds with an approximate sample height of 10 cm. For
after completion and transported to the testing machine for deformation measurements under
mechanical investigations on the printed layers in fresh state, one half of the sample was removed
loading. The remaining half of the sample was left in the working space of the printer. After a
after completion and transported to the testing machine for deformation measurements under loading.
designated interlayer time ∆t (0 min, 2 min, 5 min, 30 min), three additional layers are sprayed on the
The remaining half of the sample was left in the working space of the printer. After a designated
remaining 600 mm as a second manufacturing step. A total sample height of approximately 200 mm
interlayer time ∆t (0 min, 2 min, 5 min, 30 min), three additional layers are sprayed on the remaining
and a width w of approximately 125 mm is targeted. On the sixth strand, the yield stress
600 mm as a second manufacturing step. A total sample height of approximately 200 mm and a width
measurements with a penetrometer are performed. An overview of the principle of sampling is
w of approximately 125 mm is targeted. On the sixth strand, the yield stress measurements with a
shown in Figure 3.
penetrometer are performed. An overview of the principle of sampling is shown in Figure 3.
Figure 3. Principle of sampling: production of three long layers and subsequently three short layers.
Figure 3. Principle of sampling: production of three long layers and subsequently three short layers.
The series of investigation are named as indicated in Table 1. Every experiment reveals the
The series of investigation are named as indicated in Table 1. Every experiment reveals the
accelerator dosage in percent and-if relevant-the interlayer time ∆t in between layer three and four in
accelerator dosage in percent and-if relevant-the interlayer time ∆t in between layer three and four in
minutes. Each experiment is repeated twice.
minutes. Each experiment is repeated twice.
Materials 2020, 13, 374 6 of 19
Table 1. Overview of the experiments with variations in accelerator dosage (a) and interlayer time (t).
Interlayer Time
Accelerator Dosage
0. Min 2. Min 5. Min 30. Min
0% Accelerator a0t0 a0t2 a0t5 a0t30
4.2. Materials and Mixture Preparation

The material used in this series of experiments consists of an Ordinary Portland Cement (OPC,
CEM I 52.5) and a quartz sand with a maximum grain size of 3.15 mm. A detailed overview of all used
components and chemical admixtures is given in Table 2.
Table 2. Mixture compositions of used mortar.
Components Value Unit

Portland Cement (CEM I 52.5) 600 kg/m3
Ground limestone 97 kg/m3
Aggregate, d = 0–3.15 mm 1258 kg/m3
Water 270 kg/m3
Stabilizer 0.1 M.-%
PCE superplasticizer 0.3 M.-%/cement
Alkali-free set accelerator 0–6 M.-%/cement
For the experiment, batches of 75 L are prepared in a pug pill mixer (Mader WM Jetmix 125/180,
Erbach, Germany). The regime in the compulsory mixer is basically divided into two phases:
I. Water was put into the mixer. For 2 min, all components are added continuously into the mixing
container while the mixing tool was rotating. The order of addition was set as follows: a dry
premixed mixture of cement, ground limestone and stabilizer is added, followed by the dry
premixed aggregates. Moreover, superplasticizer was added constantly over the entire 2 min.
II. Continuous mixing for a further 2 min.
4.3. Methods
4.3.1. Material Processing and Test Specimens

For material processing, a small lab-scale SC3DP unit is used (Smart Additive Manufacturing
Material Investigator—SAMMI, manufactured inhouse). SAMMI contains an x–z-linear axis with
maximum gantry speed of up to 5 m/min, Figure 4. The shotcrete material is produced outside of
the working space with a pug mill mixer and pumped (Mader WM Variojet FU, Erbach, Germany)
through a hose to a shotcrete nozzle. Inside the nozzle, the concrete is torn up by air twice—firstly with
pressurized air only and secondly with pressurized air and-if applicable - accelerator, compare also [50].
The parameters for the experiments at hand are as follows:
Discharge rate of concrete pump: 0.8 m3 /h,

Hose: 5 m, diameter: 35 mm,
Volume air flow: 45 m3 /h,
Working distance (nozzle to specimen): 20 cm,
Gantry speed: 4.5 m/min.
After being manufactured, all specimens are stored in an air-conditioned environment at 20 ◦ C

and 65% relative humidity until the investigation of mechanical properties.
Materials
Materials2020, 13,13,
2020, 374x FOR PEER REVIEW 7 7of of
19 20
Figure 4. Experimental setup for the Smart Additive Manufacturing Material Investigator (SAMMI)
forFigure 4. Experimental
Shotcrete setup forexperiments.
3D-printing (SC3DP) the Smart Additive Manufacturing
x–z-linear Material Investigator (SAMMI)
axis with a nozzle.
for Shotcrete 3D-printing (SC3DP) experiments. x–z-linear axis with a nozzle.
4.3.2. Investigations on Fresh Properties
4.3.2. Investigations on Fresh Properties
The consistency of fresh concrete properties is measured and documented by the slump test
(according
The to DIN EN 12350-2
consistency of fresh[51]; cone dimensions:
concrete properties isheight measured= 300and mm,documented
bottom diameterby the= slump
200 mm, test
top diameter =
(according to100
DIN mm).
EN This test[51];
12350-2 examines
cone the vertical slump
dimensions: heightof=the 300concrete
mm, bottom by filling it into =a 200
diameter slumpmm,
cone
topand removing
diameter = 100 it. mm).
For quality control,
This test a sample
examines the is taken from
vertical slump each mixed
of the batch before
concrete filling
by filling the pump.
it into a slump
coneA and
handheld
removing shotcrete
it. Forpenetrometer
quality control, (Mecmesin,
a sample isWest taken Sussex,
from eachUK) mixed
is usedbatch
to discontinuously
before filling the
investigate
pump. the penetration resistance evolution of fresh concrete from 5 to 90 min after deposition.
The penetrometer
A handheldneedle shotcreteused has a diameter
penetrometer of 3 mm, West
(Mecmesin, a cylindrical
Sussex, height
UK) is of 12.5tomm
used and a cone
discontinuously
height of 2.5 mm.
investigate According to
the penetration [52,53], penetration
resistance evolution ofresistance
fresh concrete is correlated
from 5 to to 90
yield
minstress
afterof cement
deposition.
paste and mortar when a sufficiently large needle is used. Therefore,
The penetrometer needle used has a diameter of 3 mm, a cylindrical height of 12.5 mm and a cone the yield stress is calculated
according
height ofto2.5 [52].
mm. ForAccording
each pointtoin[52,53],
time, five repetitions
penetration are conducted
resistance in the centre
is correlated to yieldofstress
the specimen.
of cement
Theand
paste height
mortarof every
whenlayer is measured
a sufficiently largewith a ruler
needle afterTherefore,
is used. deposition. theMoreover,
yield stress theis width is
calculated
determined
according and used
to [52]. Fortoeach
calculate
pointthe stressfive
in time, in the specimenare
repetitions under loading.
conducted in the centre of the specimen.
ToThe
quantify
heightthe ofshape
everystability
layer isof the manufactured
measured with a ruler strands,
aftertwo 30 cm long
deposition. segments
Moreover, arewidth
the used, is
Figure 3. Theseand
determined segments,
used toconsisting
calculate theof three
stresslayers
in theeach,
specimenare loaded
underinloading.
a testing machine (Zwick/Roell
Z020, Ulm, Germany)
To quantify theafter
shape a defined
stabilitytime
of the period of t1 = 10 strands,
manufactured min aftertwo deposition
30 cm long with a testingare
segments speed
used,
ofFigure
2 N/s up to a force
3. These of 1000
segments, N to simulate
consisting of three thelayers
additional
each, are load wheninapplying
loaded a testing 50 additional
machine layers.
(Zwick/Roell
The loadUlm,
Z020, is applied
Germany) to theafter
specimen
a definedovertimea length
period ofof20t1cm and
= 10 min can be recalculated
after deposition with to stress overspeed
a testing the
loaded width
of 2 N/s up to of athe specimen.
force of 1000 TheN toselected
simulatesettings of the load
the additional loadapplication
when applying are representative
50 additional for a
layers.
typical printing
The load progress
is applied to theof specimen
a wall with a height
over a length of approximately
of 20 cm and can 1.5bemrecalculated
within 10 min. In order
to stress overtothe
ensure
loadeda constant
width ofload introduction,
the specimen. Theeach specimen
selected wasofloaded
settings the load with a preloadare
application of approximate
representative 40for
N. a
The deformations
typical printingof the printed
progress of a strands
wall with are aquantified
height of by an optical measuring
approximately system
1.5 m within 10(Aramis,
min. In orderGOM,to
Braunschweig,
ensure a constant Germany). This system each
load introduction, is composed
specimen of was
two loaded
cameras, which
with record of
a preload theapproximate
deformation40 onN.
the basis
The of previously
deformations of defined
the printedreference
strands points
are (pixel
quantifiedlength by=an 142optical
µm) [54]. Reference
measuring points
system were
(Aramis,
attached
GOM, to the testing machine
Braunschweig, (for validation,
Germany). This system GOM, is Braunschweig,
composed of Germany) two cameras, and inserted
which recordon sticksthe
into the layer interface
deformation on theduring basis the production process,
of previously defined Figure
reference 7a. Thus,
pointsinformation
(pixel length on the deformation
= 142 µm) [54].
ofReference
the individualpoints layerswerecanattached
be obtained to intheaddition
testingtomachine
the overall (fordeformation.
validation, GOM, Braunschweig,
Germany) and inserted on sticks into the layer interface during the production process, Figure 7a.
Thus, information on the deformation of the individual layers can be obtained in addition to the
overall deformation.
Materials 2020, 13, 374 8 of 19
4.3.3. Investigations on Mechanical Properties

In order to examine mechanical properties prisms perpendicular to the layer direction are cut.
The prisms were cut approximately 3 weeks after production. In order to minimize the impact of
cutting, a fine saw blade was used. Since a prism length of 160 mm with a central ∆t-interface could not
be realized for every sample, the side-length ratio was scaled to a length of 125 mm (20 × 20 × 125 mm3 ).
The prisms are tested after 28 days of standardized storage in a 3-point bending test. The previously
created ∆t-layers were positioned in the middle so that the highest bending moment was applied
at this interface. After finishing the bending tests, the remaining halves of the specimens are tested
for compressive strength. In order to obtain a comparison to monolithic samples for all accelerator
dosages (0%, 2%, 4%, 6%), material is removed from the nozzle during the tests and subsequently
cast into prism moulds. The conventionally produced samples are stored together with the printed
specimens under standardized conditions (20 ◦ C, 65% r.H.) and are tested after 28 days.
4.3.4. Investigations on Interlayer Characteristics

To investigate the interface between two layers on a microscopic scale, drilling cores (diameter
30 mm) are taken from the specimen. Since baryte powder is placed in between layers 3 and 4
during production of the layers, the interface with baryte powder can be examined in more detail [55].
The specimen is placed into a µCT and 3D scanned (GE phoenix, Boston, MA, USA, voltage: 160 kV,
current: 230 µA, number of images: 1000, image average: 3, filter: 0.1 mm Cu, exposure: 500 ms for all
specimen, voxel edge length: 33.7 µm). From the X-ray projections of each specimen, the volumetric
image is obtained by applying a 3D reconstruction algorithm with the software phoenix datos|x2
(GE Sensing & Inspection Technologies, Boston, MA, USA). The software VG studiomax 2.2 (Volume
Graphics, Heidelberg, Germany) is used to convert the reconstruction to RAW-files. Matlab 2018b
(Mathworks, Natick, MA, USA) is used for postprocessing of the RAW-files with a customized script.
The script segments the baryte powder, which represents the interlayer, with a threshold approach.
Then, the interlayer is reduced to one scalar height value z at every coordinate (x,y) along the base
area. Therefore, the thickness is reduced to one voxel by using its median z-coordinate as the boundary
position. Then, the segmented discrete points are bilinearly interpolated via a mesh and the generated
data are saved in a 2D array. Then, further analysis of the interlayer is performed, Figure 5. Here,
the (interpolated) real contact surface area Ac (mm2 ) is divided by the basic surface area A0 (mm2 ) to
quantify the local effective interlayer in the 2D array with an interface tortuosity I (-):
Ac
I= (1)
A0
The mean interface tortuosity I (-) is calculated for the middle interface of each drilling core
according to Equation (1). The lower the coefficient, the weaker the interlocking effect. If the mean
interface tortuosity approaches 1, there is no mechanical interlocking in between two layers. This factor
is mathematically similar to a 3D-tortuosity, which is usually used to describe the structure of cracks [56].
Materials 2020, 13, 374 9 of 19
Figure 5. Method to investigate the interlayer exemplified for two experiments with various content in
Figure 5. Method to investigate the interlayer exemplified for two experiments with various content
accelerator: (a) 3D scan of a drilling core, (b) interlayer between strand three and four (white line) and
in accelerator: (a) 3D scan of a drilling core, (b) interlayer between strand three and four (white line)
(c)
andcalculation of the
(c) calculation ofinterface tortuosity.
the interface tortuosity.
Furthermore, the micro

Furthermore, the roughness𝑅Ra of
microroughness ofaaprinted
printedlayer
layer (before
(before applying
applying thethe subsequent
subsequent layer)layer)
was determined on the top layers of specimen a0 to a6 by means of a digital microscope
was determined on the top layers of specimen a0 to a6 by means of a digital microscope (Keyence, (Keyence,
VHX-2000D,
VHX-2000D,magnification
magnification 30 30 ××20)
20)since
sinceininliterature
literature micro
micro roughness
roughness waswas found
found to affect
to affect interlayer
interlayer
strength,
strength, compare [41]. Therefore, a profile in the printing direction is taken from two specimens per per
compare [41]. Therefore, a profile in the printing direction is taken from two specimens
accelerator
acceleratordosage
dosage with
with aa total
total measurement
measurementdistance l of
distancel of 120
120 mm.mm. Then,
Then, thethe
meanmean vertical
vertical deviation
deviation
Z(x)
Z(x)of
ofthe
thesurface
surface from an ideal
ideal smooth
smoothsurface
surfaceisisdetermined
determined according
according to to
DINDINENENISOISO
42874287
[57]:[57]:
1 Z l
𝑅 = 1 |𝑍 𝑥 |𝑑𝑥 (2)
Ra = 𝑙 Z(x)dx (2)
l 0
5.5.Results
Results and
and Discussion
Discussion
5.1.
5.1.Fresh
Fresh Properties
Properties
The
Theslump
slump tests carried out
tests carried outasaspart
partofofquality
qualitycontrol
control give
give sufficient
sufficient uniform
uniform values.
values. TheThe average
average
slumpwas
slump wasmeasured
measuredtotobe be2323mmmmwith
witha astandard
standarddeviation
deviationofof5 mm.
5 mm.According
AccordingtotoDIN DINEN EN 12350-[51],
12350-2
2 [51],
the usedthe used material
material can be can be classified
classified into theinto the category
category S1 (plastic
S1 (plastic concrete).
concrete).
Anincrease
An increasein in yield
yield stress
stress over
over time
time is observed for all sprayed
sprayed strands,
strands,Figure
Figure66As Asexpected,
expected, an
an increase
increase in accelerator
in accelerator dosageleads
dosage leadstotoan
anincrease
increase ofof initial
initialyield
yieldstress
stressasas
well as as
well slope of the
slope yield
of the yield
stress evolution. After 90 min, the yield stress of a6 (6% accelerator, 1710.4 kPa)
stress evolution. After 90 min, the yield stress of a6 (6% accelerator, 1710.4 kPa) is approximately is approximately 15
15times
timeshigher
higher than
thanthethe
yield
yieldstress of the
stress sprayed
of the sprayedlayers without
layers withoutaccelerator (a0, (a0,
accelerator 110.9 kPa).kPa).
110.9 Obviously,
Obviously,
the (alkali-free) accelerator provides rapid stiffening of the concrete, as it is
the (alkali-free) accelerator provides rapid stiffening of the concrete, as it is desired for SC3DP desired for SC3DP to to
enable a fast vertical building progress. This is mainly attributed to aluminium sulphate, which reacts
enable a fast vertical building progress. This is mainly attributed to aluminium sulphate, which reacts
with calcium and produces ettringite and aluminium hydroxide [58,59]. Besides the general effect of
with calcium and produces ettringite and aluminium hydroxide [58,59]. Besides the general effect of
accelerating admixtures, spraying could enhance accelerator reactivity and C3A hydration [60] and
accelerating admixtures, spraying could enhance accelerator reactivity and C3 A hydration [60] and
could lead herewith to a faster yield stress evolution in early ages compared to extruded material.
could lead herewith to a faster yield stress evolution in early ages compared to extruded material.
Moreover, yield stress evolution might be affected by evaporation from the specimen’s surface.
Moreover, yield stress evolution might be affected by evaporation from the specimen’s surface.
Materials 2020, 13, 374 10 of 19
Figure 6. Yield stress evolution over time after deposition of sprayed strands containing 0% (a0), 2%
Figure
(a2), 4%6.(a4)
Yield
andstress evolution
6% (a6) over time after deposition of sprayed strands containing 0% (a0), 2%
of the accelerator.
(a2), 4% (a4) and 6% (a6) of the accelerator.
The results of the loading tests show a clear correlation between the accelerator dosage and the
The results
deformation of the
of the loading
printed tests
layers. show
For a clear correlation
investigating between
the transfer the
of force accelerator
between two dosage
concreteand the
layers,
deformation of the printed layers. For investigating the transfer of force between two
the focus was placed on the lowest interlayer (between strands 1 and 2), which is the layer with the concrete layers,
the focus
highest wasinplaced
load on the lowest
real components. Forinterlayer (between
an accelerator dosagestrands
of 0%,1the
andapplied
2), which
loadisofthe layer
1000 N, with
whichtheis
highest load in equivalent
approximately real components. For an accelerator
to manufacturing processdosage
of a 1.5ofm0%, thewall
high applied load
within 10of 1000
min, N, which
results in a
is approximately
deformation of 2.9equivalent
mm. By usingto manufacturing process
the 2% accelerator, theofmaximum
a 1.5 m high wall withindecreased
displacement 10 min, results
by morein
a deformation
than 60% to 1.2ofmm.
2.9 mm. By using
A further the 2%inaccelerator,
increase the maximum
the accelerator dosage to displacement
4% and 6% is decreased
accompaniedby more
by a
than 60%
further to 1.2 mm.
decrease A further
in total increase
settlement to 0.8in and
the accelerator dosage to 4%
0.5 mm, respectively. and3 6%
Table is accompanied
gives a summary ofby thea
further decrease
measured in total
settlements forsettlement
a loading of to 1000
0.8 and
N. 0.5 mm, respectively. Table 3 gives a summary of the
measured settlements for a loading of 1000 N.
Table 3. Total deformation of lowest layer for a loading of 1000 N (equal to 50 additional layers or a
wall
Tablewith a height
3. Total of approximately
deformation of lowest1.5 m) 10
layer formin after deposition.
a loading of 1000 N (equal to 50 additional layers or a
wall with a height of approximately 1.5 m) 10 min after deposition.
Accelerator Dosage Total Deformation of Lowest Layer at a Load of 1000 N
Accelerator 0% Dosage Total Deformation of Lowest 2.9 mmLayer at a Load of 1000 N
0%2% 2.9 mm
1.2 mm
2%4% 0.8
1.2 mmmm
4%6% 0.5 mm
0.8 mm
6% 0.5 mm
Since the loaded samples have process related varying widths, the force increase is converted into
Since
a stress the loaded
increase via thesamples
measuredhave process geometry.
specimen related varying widths, the
The previously force increase
described effect ofisaccelerator
converted
into a stress increase via the measured specimen geometry. The previously
dosage on deformation can thus be converted into an effect on deformation modulus Ed (slope described effect of
accelerator
the dosage
stress–strain on deformation
curve) of the fresh can thus be
concrete, converted
Figure into an effect
7b. Accordingly, theon deformation
results show anmodulus
increase Eofd
(slope of themodulus
deformation stress–strain
by a curve)
factor ofofapprox.
the fresh14 concrete, Figure 7b. Accordingly,
from a0 (unaccelerated, 0.27 MPa) tothea6results show an
(6% accelerator,
increase
3.66 MPa).of deformation
Particularly modulus
clear is theby step
a factor
from ofa0approx.
to a2, 14 fromisa0accompanied
which (unaccelerated,by 0.27 MPa) to a6
a displacement
(6% accelerator,
difference of about3.66 MPa).
2 mm at 30Particularly clearit is
kPa. Therefore, the
can bestep
statedfrom
thata0 to a2,
rather which
low is accompanied
accelerator dosages leadbytoa
adisplacement difference
significant reduction inof about 2deformation.
material mm at 30 kPa.Thus,Therefore,
a fasterit can be stated
vertical that progress
building rather low is accelerator
achievable.
dosages lead
In the to a significant
presented reduction
experiments, in material
the point in timedeformation.
when a subsequent Thus, alayer
fasteris vertical building
applicable to an
progresslayer
existing is achievable.
without collapsing (tmin ) is always exceeded. However, it is assumed that this point
In is
in time thehighly
presented experiments,
dependent the point indefined
on the individually time when maximuma subsequent layerdisplacements
permissible is applicable ofto the
an
existing layer
produced without collapsing (tmin) is always exceeded. However, it is assumed that this point in
element.
time is highly dependent on the individually defined maximum permissible displacements of the
produced element.
Materials 2020, 13, 374 11 of 19
(a) (b)
Figure7. 7. Optical
Figure Optical measurement
measurement of of interlayer
interlayer displacement;
displacement; Specimen
Specimen with
with inserted
inserted reference
reference
components(a),
components (a), Displacement–stress
Displacement–stress curve
curveand
anddeformation modulus
deformation of the
modulus of first interlayer
the first for a0for
interlayer to
a0a6
to10
a6min
10 minafterafter
deposition (b). (b).
deposition
5.2.
5.2.Interlayer
InterlayerCharacteristics
Characteristicsand
andMechanical
MechanicalProperties
Properties
The
Theresults
resultsof
of the
the compressive strengthtests
compressive strength testsshow
shownono noticeable
noticeable correlation
correlation between
between the
the set-
set-accelerator dosage
accelerator dosage andand
thethe resulting
resulting 28d-compressive
28d-compressive strength
strength of 3D-printed
of 3D-printed specimens,
specimens, Table
Table 4. 4.
Table4.4.28d
Table 28dcompressive
compressivestrength
strengthfcfcof
of3D-printed
3D-printed specimens.
specimens.
Accelerator
Accelerator Dosage
Dosage Averaged CompressiveStrength
Averaged Compressive Strength
fc fc Standard
Standard Deviation
Deviation σfc σfc
0%
0% 59.9N/mm
59.9 N/mm2 2 3.4
3.4 N/mm
N/mm 2 2
2%
2% 64.8N/mm
64.8 N/mm22 2.8
2.8 N/mm
N/mm 2 2
4%
4% 66.0N/mm
66.0 2
N/mm2 4.6
4.6 2 2
N/mm
N/mm
6% 65.7 2 2
6% 65.7N/mm
N/mm2 3.0 N/mm
3.0 N/mm2
The
The results
results of the
of the effect
effect of interlayer
of interlayer time ontime on flexural
flexural strengthstrength and interface
and interface tortuosity
tortuosity for sprayed for
sprayed concrete a0 to a6 as well as the flexural strength of conventional casted specimens
concrete a0 to a6 as well as the flexural strength of conventional casted specimens are shown in Figure 8. are shown
in Figure
First 8. First
of all, one of all,
can see thatone can see
flexural that flexural
strength strength ofspecimens
of the accelerated the accelerated specimens
is reduced by 0.9 is
toreduced
1.8 N/mm by2 ,
0.9 to 1.8 N/mm 2, when the material is applied by SC3DP (with interlayer time 0 min) compared to
when the material is applied by SC3DP (with interlayer time 0 min) compared to the conventional casted
the conventional
specimens (compactedcasted viaspecimens (compacted
poking, indicated withviaa poking, indicated
solid line). with a strength
The flexural solid line).
of The flexural
the sprayed
strength (solid
specimen of thesymbols),
sprayed specimenwhere the(solid
load symbols),
is appliedwhere thetoload
parallel is applied
the layer parallelcharacterises
orientation, to the layer
orientation, characterises the interlayer quality. With an interlayer time of more than 0 min, a
the interlayer quality. With an interlayer time of more than 0 min, a reduction of flexural strength of
reduction of flexural strength of 3D printed specimen, i.e., a reduction of interlayer quality, is
3D printed specimen, i.e., a reduction of interlayer quality, is observed. Interestingly, the decrease
observed. Interestingly, the decrease is particularly pronounced with short interlayer times (0–5 min).
is particularly pronounced with short interlayer times (0–5 min). With a long interlayer time of
With a long interlayer time of 30 min, there is no further significant reduction of flexural strength.
30 min, there is no further significant reduction of flexural strength. For example, for a0t5, a reduction
For example, for a0t5, a reduction in flexural strength of 21% (1.2 N/mm2) and for a0t30 a reduction
in flexural strength 3of 21% (1.2 N/mm ) and for a0t30 a reduction of 22% (1.2 N/mm3 ) is observed
2
of 22% (1.2 N/mm ) is observed compared to a0t0. A similar behaviour has been observed for the
compared to a0t0. A similar behaviour has been observed for the extrusion process (compare Section 3).
extrusion process (compare Section 3). With regard to a practical application, this means that
With regard to a practical application, this means that interlayer times of less than 2 min should be
interlayer times of less than 2 min should be envisaged for path planning in order to avoid a
envisaged for path planning in order to avoid a significant (more than 20%) loss in interlayer strength.
significant (more than 20%) loss in interlayer strength. However, from the foregoing, a maximum
However, from the foregoing, a maximum interlayer time (tmax ), which represents an upper limit with
interlayer time (tmax), which represents an upper limit with regard to the interlayer strength quality,
regard to the interlayer strength quality, is not distinctively assignable. This point in time is highly
is not distinctively assignable. This point in time is highly dependent on the individually defined
dependent on the individually defined maximum sufferable reduction in interlayer strength.
maximum sufferable reduction in interlayer strength.
ToTounderstand
understandthe theunderlying
underlyingmechanisms
mechanismsofofthe theobserved
observedbehaviour
behaviour of of interlayer strength over
interlayer strength over
time,
time,thethe
interface tortuosity
interface tortuosity of the drilling
of the cores
drilling was was
cores determined, Figure
determined, 8 (empty
Figure symbols).
8 (empty The mean
symbols). The
interface tortuosity of the drilling cores ranges from I = 1.37 to 2.29 (-). As with flexural
mean interface tortuosity of the drilling cores ranges from I = 1.37 to 2.29 (-). As with flexural strength strength (filled
(filled symbols), the interface tortuosity tends to decrease as interlayer time increases. The lower the
Materials 2020, 13, 374 12 of 19

symbols), the interface tortuosity tends to decrease as interlayer time increases. The lower the initial
yield
initialstress
yield of the layer,
stress of thethe morethe
layer, deformation can take place
more deformation andplace
can take thus higher
and thusinterlayer
higher tortuosity
interlayer
can be achieved.
tortuosity can be With increasing
achieved. With accelerator dosages and
increasing accelerator increasing
dosages andinterlayer
increasingtimes, the initial
interlayer times,yield
the
stress of the underlying layer increases. As a result, a lower interlayer tortuosity and herewith
initial yield stress of the underlying layer increases. As a result, a lower interlayer tortuosity and a lower
interlayer aquality
herewith lowerisinterlayer
generated.quality
Therefore, measured flexural
is generated. strength
Therefore, on theflexural
measured specimenstrength
correlates
onwith
the
the interface
specimen tortuosity,
correlates withFigure 9.
the interface tortuosity, Figure 9.
Figure 8. 28 d flexural strength fct of monolithic specimen and specimen with various interlayer
times as well as according interface tortuosity I of (a) a 0%, (b) a 2%, (c) a 4% and (d) a 6% (for each
Figure 8. 28 d flexural strength fct of monolithic specimen and specimen with various interlayer times
accelerator dosage, a minimum of six drilling cores and seven prisms is evaluated) depending on the
as well as according interface tortuosity I of (a) a 0%, (b) a 2%, (c) a 4% and (d) a 6% (for each
interlayer time.
accelerator dosage, a minimum of six drilling cores and seven prisms is evaluated) depending on the
interlayer time.
Materials
Materials 2020,
2020, 13,
13, x374
FOR PEER REVIEW 13
13of
of 20
19
Figure 9. Linear correlation (dashed line) of mean flexural strength and mean interface tortuosity of
Figure Linear
drilling9.cores correlation
from (dashed
the printed line) of mean flexural strength and mean interface tortuosity of
specimen.
drilling cores from the printed specimen.
Figure 9. Linear correlation (dashed line) of mean flexural strength and mean interface tortuosity of
Since micro
drilling roughness
cores from tends
the printed to increase with increasing accelerator dosage, Figure 10. Since the
specimen.
Since micro roughness tends to increase with increasing accelerator dosage, Figure 10. Since the
basic mixture, e.g., the granulometric characteristic, is the same for all experiments, it is presumed
basic mixture, e.g., the granulometric characteristic, is the same for all experiments, it is presumed
that Since micro
the micro roughnesscorrelates
roughness tends to increase
with the with
yieldincreasing
stress of theaccelerator
material.dosage, Figure 10.
In the spraying Since the
process, the
that the micro roughness correlates with the yield stress of the material. In the spraying process,
basic mixture,
material volumee.g.,receives
the granulometric characteristic,
the same kinetic energy.isHowever,
the same for all experiments,
material with a higher it is presumed
content of
the material volume receives the same kinetic energy. However, material with a higher content of
that the micro
accelerator roughness
needs a higher correlates
energy to with thethe
reach yield stress
same of of
level thecompaction
material. Inas the spraying with
a material process, the
a lower
accelerator needs a higher energy to reach the same level of compaction as a material with a lower
material
content ofvolume receives
accelerator. Thisthe same
leads to akinetic
rougherenergy.
surface.However,
However,material
there is nowith a higherbetween
correlation content theof
content of accelerator. This leads to a rougher surface. However, there is no correlation between
accelerator needs and
micro roughness a higher energy
flexural to reach
strength theinterface
or the same level of compaction
tortuosity, Figures as11 aand
material
12. Thiswith a lower
means that,
the micro roughness and flexural strength or the interface tortuosity, Figures 11 and 12. This means
content of accelerator.
in the SC3DP process, This
theleads to a rougher
mechanical bondsurface.
betweenHowever, thereisis induced
two layers no correlation
less bybetween the
the micro
that, in the SC3DP process, the mechanical bond between two layers is induced less by the micro
micro roughness
roughness and flexural
generated on the strength
free surfaceor theduring
interface
thetortuosity,
production Figures
of the11bottom
and 12.layer
This means
than bythat,the
roughness generated on the free surface during the production of the bottom layer than by the tortuosity
in the SC3DP
tortuosity process,
generated by the
the mechanical
imprinting of bond between
particles duringtwothe layers is induced
application of theless by the micro
subsequent layer.
generated by the imprinting of particles during the application of the subsequent layer. Here, micro
roughness
Here, micro generated
roughness on plays
the free surfacerole
a minor during the production
regarding interlayerofstrength
the bottom layer than
compared by the
to interface
roughness plays a minor role regarding interlayer strength compared to interface tortuosity, which
tortuosity
tortuosity,generated by thethe
which depicts imprinting of particles
macro roughness of during the application
the interlayer of the subsequent
and corresponds layer.
with a vertical
depicts the macro roughness of the interlayer and corresponds with a vertical interlocking-amplitude
Here, micro roughness plays a minor role regarding interlayer strength
interlocking-amplitude of up to 4.3 mm. The interlocking effect of interface tortuosity is several compared to interface
of up to 4.3 mm. The interlocking effect of interface tortuosity is several magnitudes higher than micro
tortuosity,
magnitudes which
higher depicts the macro
than micro roughness
roughness. of the interlayer
The characteristic of theand corresponds
interlocking with a vertical
is depending on the
roughness. The characteristic of the interlocking is depending on the yield stress of the lower layer
interlocking-amplitude
yield stress of the lowerof up (deformability,
layer to 4.3 mm. Thewhich interlocking effect of interface
is time-dependent) and hastortuosity
therefore is several
a superior
(deformability, which is time-dependent) and has therefore a superior effect on the flexural strength for
magnitudes
effect on thehigher
flexuralthan microfor
strength roughness. The characteristic
SC3DP specimen, Figure 13.of the interlocking is depending on the
SC3DP specimen, Figure 13.
yield stress of the lower layer (deformability, which is time-dependent) and has therefore a superior
effect on the flexural strength for SC3DP specimen, Figure 13.
Figure 10. Micro roughness of the surface layer of specimen containing 0% (a0), 2% (a2), 4% (a4) and
6% (a6) of accelerator.
Figure
Materials 2020,10.
13,Micro
x FOR roughness of the surface layer of specimen containing 0% (a0), 2% (a2), 4% (a4) and
PEER REVIEW 14 of 20
Figure 10. Micro roughness of the surface layer of specimen containing 0% (a0), 2% (a2), 4% (a4) and
Materials 2020, 13, 374 14 of 19
Figure 11. No correlation between initial micro roughness and flexural strength of an interlayer time
of 0 min.
Figure 11. No correlation between initial micro roughness and flexural strength of an interlayer time of
0Figure
min. 11. No correlation between initial micro roughness and flexural strength of an interlayer time
of 0 min.

Figure 12. No correlation between initial micro roughness and interface tortuosity for an interlayer
time of 0 min.
time of 0 min.
time of 0 min.
Figure 13. Reduction of Interface tortuosity with increasing yield stress. Exemplary shown for the
specimen
Figure 13.a0–a6 with interlayer
Reduction time
of Interface 5 and 30 with
tortuosity min. increasing yield stress. Exemplary shown for the
specimen a0–a6 with interlayer time 5 and 30 min.
5.3. Modeling Interlayer Strength

In view of the above considerations, it should be possible to quantitatively describe the flexural
strength of the SC3DP specimen with dependence on interface tortuosity, which encompasses all
relevant boundary conditions. Therefore, a mechanical model is proposed based on an approach of
Materials 2020, 13, 374 15 of 19
5.3. Modeling Interlayer Strength

In view of the above considerations, it should be possible to quantitatively describe the flexural
strength of the SC3DP specimen with dependence on interface tortuosity, which encompasses all
relevant boundary conditions. Therefore, a mechanical model is proposed based on an approach of
Walraven [61] for the stress transmission in cracks in the direction of crack:

σ = σpu Ax + µ·A y , (3)
with σpu = 5.83 fcc0.63 (4)
Here, σpu (N/mm2 ) is the yielding strength of the matrix depending on uniaxial compressive
strength of concrete fcc (N/mm2 ), Ax (-) and A y (-) are the projected contact areas for a crack in x- and
y-directions, µ = 0.5 (-) is the coefficient of friction.
Based on Equations (3) and (4), the model is adopted to the case at hand. The interlayer is
considered as weakened area and is therefore the relevant location for stress transmission during
flexural strength tests. Therefore, stress σ is replaced by flexural strength fct (N/mm2 ). Moreover, the
projected contact areas are-due to isotropy reasons-replaced by the interface tortuosity I (-) between two
layers. A dimensionless coefficient ε (-) is used as model shift factor between crack–stress transmission
and determination of interlayer quality:
fct = σpu ·I·ε (5)
It can be shown that a good agreement exists between the model according to Equation (5) when
using a model shift factor ε = 0.037, Figure 14.
Figure 14. Correlation (dark grey dashed line) of measured and calculated flexural strength. Calculations
are based
Figure 14.onCorrelation
a modification
(darkof Walraven’s
grey dashedmodel forof
line) stress transmission
measured in cracks. Bright
and calculated greystrength.
flexural dashed
line indicatesare
Calculations thebased
rangeon
of acertitude (0.75×
modification ofand 1.25×). model for stress transmission in cracks. Bright
Walraven’s
grey dashed line indicates the range of certitude (0.75× and 1.25×).
From the above, it is concluded that the macro roughness of the interlayer, expressed as interface
From I,
tortuosity theis above,
a key parameter to describe
it is concluded that theinterlayer quality. of
macro roughness The
theinterface tortuosity
interlayer, is as
expressed affected by
interface
yield stressI,and
tortuosity is a herewith accelerator
key parameter dosageinterlayer
to describe and pointquality.
in time The
of application of the subsequent
interface tortuosity layer.
is affected by
Moreover, the compressive strength is relevant, which is interrelated to flexural strength of
yield stress and herewith accelerator dosage and point in time of application of the subsequent layer.concrete.
Moreover, the compressive strength is relevant, which is interrelated to flexural strength of concrete.
6. Conclusions and Outlook
6. Conclusions and Outlook
This contribution focusses on the effect of accelerator dosage and interlayer time on fresh concrete
properties and interlayer strength in Shotcrete 3D Printing (SC3DP). In the experimental investigations,
This contribution focusses on the effect of accelerator dosage and interlayer time on fresh
the accelerator dosage is varied from 0% to 6%. A severe increase in yield stress after deposition
concrete properties and interlayer strength in Shotcrete 3D Printing (SC3DP). In the experimental
investigations, the accelerator dosage is varied from 0% to 6%. A severe increase in yield stress after
deposition and in yield stress evolution over time is observed when adding accelerator. This enables
a higher vertical building rate, which is highly relevant for practical applications. By using a 2%
accelerator, the deformation in the lowest layer is reduced significantly from 2.7 mm to 0.8 mm
compared to the unaccelerated material for an applied stress of 30 kPa. By using a 6% accelerator, the
Materials 2020, 13, 374 16 of 19
and in yield stress evolution over time is observed when adding accelerator. This enables a higher
vertical building rate, which is highly relevant for practical applications. By using a 2% accelerator,
the deformation in the lowest layer is reduced significantly from 2.7 mm to 0.8 mm compared to the
unaccelerated material for an applied stress of 30 kPa. By using a 6% accelerator, the deformation of
the lowest layer is even reduced to 0.3 mm. By calculating the deformation modulus Ed , the effect of
accelerator dosage on the mechanical properties of fresh concrete could be quantified. For material
with 6% accelerator compared to a 0% accelerator, the deformation modulus is about 14 times higher.
An increase in accelerator dosage leads to an increase in yield stress evolution. A clear correlation
of yield stress and resulting interlayer strengths is found. In order to quantify and explain this effect,
mechanical performance tests as well as additional µCT-images of the interlayer zones are carried out.
Since various time spans may occur before the application of a subsequent layer, four interlayer times
(0, 2, 5 and 30 min) are examined. Based on the computed tomography results, an interface tortuosity,
which is a parameter describing the interlocking of the layer’s interface, could be determined for each
setup. Independent from the accelerator dosage, the largest decrease in interlayer strength is observed
for interlayer times between 0 and 5 min. For longer interlayer times (5 to 30 min), no further significant
reduction of interlayer strength is measured. With regard to a practical application, an interlayer time
of less than 2 min is recommended, which needs to be considered e.g., for path planning in order to
avoid a significant loss in interlayer strength. By including the analysis of µCT-results, a correlation
between decreasing interlayer strength and decreasing interlayer tortuosity is noticed. Thus, it can
be stated that, in SC3DP, the interlayer strength is significantly influenced by interlayer tortuosity.
Varying interlayer tortuosity is deduced to the initial yield stress of the underlying layer to which a
subsequent layer is applied. Interlayer tortuosity is higher and herewith a higher interlayer quality is
generated, when short interlayer times are prevalent.
Finally, to quantify the overall mechanical performance of SC3DP elements, a model is developed
depending on compressive strength and interface tortuosity. These findings can be used to improve
interlayer strength in the future, e.g., by purposefully manipulating the interlayer roughness by process
parameters. In this particular field, further studies are envisaged.
Author Contributions: Conceptualization, I.D., N.F. and D.L.; methodology, I.D., N.F. and D.L.; investigation, I.D.
and N.F.; resources, D.L.; writing—original draft preparation, I.D. and N.F.; writing—review and editing, I.D., N.F.
and D.L.; visualization, I.D. and N.F.; supervision, D.L.; funding acquisition, D.L. All authors have read and agree
to the published version of the manuscript.
Funding: This research received no external funding.
Acknowledgments: The APC was funded by Publication Fund of Technische Universität Braunschweig.
Conflicts of Interest: The authors declare no conflict of interest.
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© 2020 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access
article distributed under the terms and conditions of the Creative Commons Attribution
(CC BY) license (http://creativecommons.org/licenses/by/4.0/).

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Keywords: additive manufacturing; shotcrete 3D printing; interlayer strength; bond; accelerator

Materials 2020, 13, 374; doi:10.3390/ma13020374 www.mdpi.com/journal/materials

Materials 2020, 13, 374 2 of 19

4.2. Materials and Mixture Preparation

Table 2. Mixture compositions of used mortar.

Components Value Unit

4.3.1. Material Processing and Test Specimens

Discharge rate of concrete pump: 0.8 m3 /h,

After being manufactured, all specimens are stored in an air-conditioned environment at 20 ◦ C

4.3.3. Investigations on Mechanical Properties

4.3.4. Investigations on Interlayer Characteristics

Furthermore, the micro

Materials 2020, 13, x FOR PEER REVIEW 12 of 20

Materials 2020, 13, x FOR PEER REVIEW 15 of 20

5.3. Modeling Interlayer Strength

5.3. Modeling Interlayer Strength

with σpu = 5.83 fcc0.63 (4)

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