Case Studies in Construction Materials
Case Studies in Construction Materials
Case Studies in Construction Materials
A R T I C L E I N F O A B S T R A C T
Keywords: Although 3D concrete printing (3DCP) is considered one of the most significant innovations in the
Limestone calcined clay cement construction sector, its large cement consumption remains an environmental concern. In
LC3 response, limestone calcined clay cements (LC3) have emerged as a promising alternative to
3D printing
Portland cement (PC) due to their potential for reducing environmental impact. While previous
3DCP
Rheology
studies have shown the influence of addition timing of superplasticizer (SP) on the fresh per
Superplasticizer formance of PC, its impact on LC3, particularly in the context of 3DCP, remains less understood.
This study assessed the effect of the SP addition time (either directly with the mixing water or
with a 10-min delay) on the rheology and printing-related properties of LC3 and PC. Rotational
rheometry and 3DP-related tests were conducted over two hours, besides hydration assessment
through thermogravimetric analysis (TGA). The results showed that adding SP directly to LC3 led
to significantly higher yield stress (1.2–2.5 times) and viscosity (14–59 % higher) values
compared to delayed SP addition within the same time frame. However, LC3 exhibited slower
rates of yield stress and viscosity increase over time in contrast to PC (with Athix structuration
rate approximately 92 % lower for LC3). These tendencies influenced printability performance.
While direct SP addition reduced PC’s open time from 100 to 30 min, it had no impact on LC3 ’s
open time, which remained at 80 min. TGA analysis yielded additional insights, highlighting that
hydrating LC3 samples required a greater free water content to achieve the same yield stress as PC
and this difference was attributed to the presence of calcined clay. These findings make contri
butions to the technical and scientific communities by enhancing comprehension of LC3 cement
fresh behavior and solidifying 3DCP as a disruptive construction method.
1. Introduction
Digital fabrication using 3D printing (3DP) for construction materials is rapidly expanding due to its numerous benefits, including
the elimination of formworks and the ability to create complex-shaped elements [1]. However, the extensive use of cement in 3D
concrete printing (3DCP) raises significant environmental concerns [2]. Consequently, there is an urgent need to explore eco-friendly
* Corresponding authors.
E-mail addresses: paulo.matos@udesc.br (P.R. de Matos), mtsouza@uesc.br (M.T. Souza).
https://doi.org/10.1016/j.cscm.2023.e02419
Received 11 July 2023; Received in revised form 17 August 2023; Accepted 21 August 2023
Available online 22 August 2023
2214-5095/© 2023 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
P.R. de Matos et al. Case Studies in Construction Materials 19 (2023) e02419
alternatives, primarily focusing on replacing Portland cement [3]. In this regard, limestone calcined clay cements (LC3) have emerged
as a highly promising solution [4].
Previous studies have documented significant advancements in the production of LC3 -based 3DP elements. Notably, Chen and
colleagues conducted comprehensive research on the influence of mix design on the fresh and hardened properties of 3DP LC3 ma
terials. Their findings shed light on the optimization of various factors in the production process. In Refs. [5–7], the authors assessed
the effect of the grade level of calcined clay and the clinker-calcined clay-limestone ratio on the fresh and hardened performance of
3DCP. The authors observed that by increasing the content of calcined clay and limestone in the mixtures, the buildability and stiffness
development improved significantly. However, it was noted that this increase led to a reduction in flowability. On the other hand, a
high replacement of cement with calcined clay + limestone had a negative impact on both compressive strength and hydration. As for
increasing the metakaolin content in calcined clay (i.e., the grade level), it had several positive effects such as enhancing extrusion
pressures, green strength, initial setting time, and compressive strength at different ages. These findings suggest that using
higher-grade calcined clay has the potential to greatly enhance the performance of printable cementitious materials. Long et al. [8]
evaluated the effect of using silica fume on the rheological properties and compressive strength of 3DP LC3 mortars. The presence of
silica fume in 5 wt% improved the yield stress, viscosity and structural recovery of the material. Tao et al. [9] proposed the use of
perforated fly ash cenospheres as a sand replacement material to improve the fresh and hardener performance of LC3 mortars. The
authors found that incorporating cenospheres resulted in a substantial reduction of 80 % in shrinkage strain. This reduction in
shrinkage strain was attributed to the cenospheres acting as internal curing agents within the mortars. Shantanu et al. [10] demon
strated that the rheological properties of the LC3 matrix played a more critical role in the first few minutes of printing (e.g., 5 min),
while the matrix-aggregate interaction became the key factor at later ages (>30 min). Besides mix design, the effect of printing pa
rameters on the performance of LC3 -based 3DCP was assesses by Chen et al. [11]. The authors varied the time interval between layers
deposition (from 20 s to 10 min) and the nozzle standoff distance (from 0 to 10 mm), evaluating the effects on the mechanical strength
and microstructure of 3DCP. According to the authors, reducing the time interval between layers was found to enhance bond strength
and reduce porosity. Conversely, the impact of increasing the nozzle standoff distance on bond strength was found to be limited.
Despite the growing interest in LC3 -based 3DCP, there are still technical issues that must be tackled. One of the major challenges for
the application of LC3 is controlling its fresh properties [12]. To address this challenge, polycarboxylate-based (PCE) superplasticizers
(SP) are commonly used as effective dispersing agents in both Portland and clay-containing cementitious systems [13]. The timing of
SP addition, whether simultaneous with mixing water or delayed, plays a crucial role in the rheology and hydration of PC [14]. Von
Daake and Stephan [15] and Uchikawa et al. [16] have shown that adding SP after a few minutes delays the hydration kinetics of PC to
a greater extent. Pott et al. [17] showed that adding a high content of SP directly (with the mixing water) can induce the undesired
formation of high ettringite contents within the first minutes of hydration. Valentini et al. [18] and de Matos et al. [19] showed that the
direct SP addition retards the conversion of the intermediate short-range ordered C-(A)-S-H to long-range ordered foil-like C-(A)-S-H,
while delayed SP addition prevents such retardation. However, the precise influence of these effects on LC3 is still not comprehensively
understood.
In our previous work [19], it was established that the timing of SP addition did not have a substantial impact on the hydration of
LC3 within the first 48 h, unlike PC. However, the effect of the SP addition time on the rheology of LC3 materials, especially for 3DCP
applications, remains unknown to the best of our knowledge. Thus, the motivation of the current work is to understand the effect of SP
addition time on the fresh properties of LC3 -based 3DCP materials. For this purpose, 3DCP mixes were produced with LC3 and PC and
SP was added either simultaneously with the mixing water or with a 10-min delay; the rheological and printing-related properties of
the mixes were assessed over the first two hours.
2.1. Materials
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P.R. de Matos et al. Case Studies in Construction Materials 19 (2023) e02419
Table 1
Mix proportions of the 3DCP produced.
Mix Portland cement (g) Extra calcium sulfate (g) Calcined clay (g) Limestone filler* (g) Sand (g) Water (g) Superplasticizer (g)
Two binders were used in this work: (i) an LC3 with a proportion of (clinker + calcium sulfate):CC:LF of 55:30:15 by weight; and (ii)
a commercial PC. In our previous study [19], it was observed that replacing both Portland cement (PC) and limestone calcined clay
cements (LC3) with an additional 1 wt% of gypsum resulted in the optimal sulfate content for these compositions. Therefore, in the
present study, the same additional gypsum content was utilized in order to maintain consistency with the previous findings and ensure
comparable experimental conditions. To produce the 3DCP, the water/binder (w/b) ratios of 0.4 and 0.3 (by weight) were selected for
LC3 and PC samples, respectively, to ensure comparable applicability. A binder:sand proportion of 1:1 by weight and a SP content of
0.3 wt% over the binder weight were fixed for all samples. Table 1 shows the detailed composition of the 3DCP mixes produced.
The 3DCP samples were produced in batches of 1 L using a 5 L mortar mixer with a capacity of 285 rpm. Each sample was prepared
with the SP added at two distinct moments: (i) together with the mixing water (referred to as “direct”); and (ii) with a 10-min delay
(referred to as “delayed”). For the “direct” method, the dry materials and 90 % of the water + SP were mixed for 1 min. After 10 min,
the remaining water was added, and the sample was mixed for another 1 min. For the “delayed” method, the dry materials and 90 % of
the water were mixed for 1 min. After 10 min, the remaining water + SP were added, and the sample was mixed for another 1 min. In
both cases, the SP was pre-mixed with the respective amount of water added together with it.
For cement hydration tests (described in Section 2.3.3), pastes with the same composition were prepared without sand. The same
mixing procedures were followed using a mortar mixer with a capacity of 650 rpm in 50 ml batches. The mixtures were prepared in
plastic containers and sealed until hydration was stopped at 20 and 120 min. To stop hydration, approximately 1 g of each paste was
immersed in 50 ml of isopropanol and stirred for 30 min. Due to the soft consistency of the pastes, there was no need for a grinding
process. Subsequently, the samples were filtered using a paper filter under low vacuum for about 10 min. After filtration, the samples
were dried in an oven at 40 ◦ C for 10 min. The dried samples were then stored in a desiccator containing silica gel until testing.
where τ is the shear stress (Pa); τ0,d is the dynamic yield stress (Pa); and γ̇ is the shear rate (s− 1).
The measurements were taken from 20 to 120 min every 20 min. For each measurement, a fresh portion from the same batch was
placed in the rheometer container 5 min before each measurement while the spindle was introduced into the sample 1 min before each
test begins; then, the static yield stress and flow curve measurements were conducted. While the flow curves provide information about
the dynamic yield stress, we specifically chose to focus on the static yield stress for the purpose of 3DPC studies, which is considered
more representative in this context [25–29]. The structural build-up of the 3DCP samples was assessed by determining the structur
ation rate over time (Athix) through two models: the linear model proposed by Roussel and Cussigh [30] shown in Eq. (2), and the
non-linear exponential model proposed by Perrot et al. [31] shown in Eq. (3):
τ0(t) = τ0,0 + Athix .t (2)
(3)
t
τ0(t) = τ0,0 + Athix .tc (etc − 1)
where τ0(t) is the yield stress (Pa) at a given elapsed resting time t (min); τ0,0 is the yield stress prior to flocculation (Pa), i.e., at t = 0;
and tc is the characteristic time obtained experimentally (min).
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P.R. de Matos et al. Case Studies in Construction Materials 19 (2023) e02419
Fig. 2. Shear stress vs. time curves for yield stress determination: LC3 mixes (w/b = 0.4) with direct SP addition in (a) and delayed SP addition in
(b); PC mixes (w/c = 0.3) with direct SP addition in (c) and delayed SP addition in (d). Note: measurements were recorded from 20 to 120 min every
20 min; the grey dashed line in (c) represents the shear stress capacity of the rheometer.
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P.R. de Matos et al. Case Studies in Construction Materials 19 (2023) e02419
Fig. 3. Yield stress evolution of the 3DCP samples over time. (a) linear fit from Roussel and Cussigh [30]; (b) exponential fit from Perrot et al. [31].
Note: *corresponds to a torque overload measurement, before reaching the yield stress of the sample.
Table 2
Structural build-up parameters of the 3DCP samples obtained by the linear and exponential models used.
Sample PC direct PC delayed LC3 direct LC3 delayed
interval during which it was possible to print a continuous filament measuring 200 mm in length, as proposed by Ma et al. [33].
where w40 ◦ C and w600 ◦ C are the weight of the sample at 40 and 600 ◦ C, respectively (in wt%).
The free water (FW) was calculated using Eq. (5), where w/b is the water/binder ratio (0.3 for PC and 0.4 for LC3) and CBW is the
value obtained from Eq. (4). Note that both CBW and FW were normalized to 100 g of fresh paste.
[ ]
w/b
FW = − CBW (5)
1 + w/b
Fig. 2 shows the shear stress vs. time curves of the 3DCP samples over time, while Fig. 3 shows the yield stress evolution of the 3DCP
pastes over time. Both datasets were fitted with the linear model given by Eq. (2) and the exponential model given by Eq. (3). The
results obtained from the data fitting process are summarized in Table 2. Notably, the exponential model demonstrated a significant
better fit (Fig. 3), especially for the PC samples. This is supported by the higher R2 values (See Table 2) and more consistent τ0,0 values.
For example, the linear fit yielded a τ0,0 of 58 Pa while the exponential fit yielded a τ0,0 of 797 Pa for the PC delayed sample. The first
recorded τ0 value (at 20 min) was 984 Pa, aligning more closely with the exponential model fit. In addition, the linear model yielded a
negative τ0,0 for the LC3 delayed sample, which lacks physical meaning. It is generally accepted that the τ0 increases linearly within the
first ~60 min of hydration [22,34,35] while the evaluation of longer time intervals requires non-linear models, as confirmed by our
findings.
Owing that the exponential model led to more coherent structural build-up parameters, those are discussed next. Although the LC3
and PC samples exhibited different rheological properties over time, the timing of SP addition had a similar impact on their structural
build-up parameters. Direct SP addition significantly increased the “non-flocculated” yield stress (τ0,0) in both systems, reaching a
value 2.4 times higher than that of the respective delayed SP samples for both binders. Additionally, the effect of the SP addition timing
on the structuration rate (Athix) was comparable for LC3 and PC, resulting in 1.2- and 1.0-times higher values, respectively, for direct SP
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P.R. de Matos et al. Case Studies in Construction Materials 19 (2023) e02419
Fig. 4. Correlation between the free water of pastes and the yield stress of 3DCP samples. Note: The "PC direct – 120 min" data is not shown since its
yield stress could not be measured.
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water to achieved a given yield stress compared to the PC samples. This finding aligns with previous reports [6,13,41] which show that
the very high SSA of calcined clays (here, 11.99 m2/g for CC vs. 1.83–2.56 m2/g for the other powder materials) leads to an increased
water requirement for achieving the target flowability. These results are also consistent with those reported by Jakob et al. [42], who
demonstrated that the gradual consumption of free water during cement hydration contributes to the loss of flowability over time,
along with flocculation [43]. It is worth warning that additional techniques are desirable to confirm the phase assemblage (and CBW)
of the samples, such as X-ray diffraction.
Fig. 5 shows the variation in plastic viscosity of the 3DCP pastes over time. The general trend for viscosity among the samples was
consistent with that of the yield stress. Specifically, the PC samples exhibited higher viscosity values compared to the LC3 samples, and
the direct SP addition led to higher viscosities when comparing samples produced with the same binder. In addition, the viscosity
values felt within the range of 4.0 ± 1.3 Pa.s for the LC3 mixes and 6.5 ± 2.2 Pa.s for the PC mixes. These values are comparable to
those reported by Zhang et al. [44] and Long et al. [8] for 3DCP samples. Although the presence of calcined clay (with high SSA) may
increase the viscosity of the mixture, the higher w/b ratio used for the LC3 samples compensated for it. In turn, the viscosity growth
over time did not follow the exponential trend of the yield stress growth especially for the LC3 mixes. Instead, the viscosity exhibited a
steadier growth. These results agree with the time-dependent plastic viscosity values reported by Long et al. [8] for PC and LC3 based
3DCP. The slower viscosity growth over time of LC3 becomes evident when comparing the LC3 direct and PC delayed samples. At
20 min, both samples had equivalent viscosities, but the latter displayed ~40 % higher viscosity values than the former for longer
resting times.
Fig. 6 shows the results of the 3D printing-related test, i.e., the buildability and printability of the 3DCP samples Fig. 7 provides
visual illustration of the samples during the printability test, while this illustration is shown in Fig. S1 for the buildability test.
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Regarding the LC3 samples, the timing of addition time did not have a significant impact on their printability. In turn, for the PC
samples, the direct SP addition significantly reduced the printability compared to delayed addition. from 90 to 30 min, When both
samples achieved a viscosity of ~7 Pa.s (as shown in Fig. 5), the direct SP addition reduced the printability from 90 to 30 min. On the
other hand, the specific viscosity threshold for printability was not clearly defined for the LC3 samples. From a practical standpoint, the
direct SP addition in LC3 3DCP was advantageous as it effectively doubled the buildability of the sample without harming the
printability (open time kept at 70 min). As for PC, direct SP addition further improved the buildability (from 10 to 34 layers) but came
at the cost of reducing the open time to one-third of the value found for delayed SP addition.
One can expect that increasing the materials’ yield stress would increase its buildability (i.e., the maximum achievable height that
can be printed with it), which did not occur to our samples. The plastic collapse theoretically occurs when the compressive load (σ),
given by σ = ρgh (where ρ is the material’s density, g is the acceleration due to gravity, and h is the height of the printed object),
overcomes the material’s yield stress. However, recent reports [45] showed divergences of 17–55 %. between the number of layers
predicted from rheometry results and measured in printed elements. In this scenario, a collective effort is being made to define what
is/are the most suitable test/s to assess the fresh properties of 3DCP, and ideally predicting its buildability [46].
4. Conclusion
In this work, the effect of the SP addition timing on the rheological and printing-related properties of LC3 and PC 3DCP was
investigated. It was found that the direct addition of SP resulted in higher yield stress and viscosity values compared to delayed SP
addition, which was observed for both LC3 and PC samples. However, LC3 exhibited lower yield stress and viscosity increase rates over
time compared to PC. Additional care must be taken in interpreting the results since PC and LC3 systems required different water
contents to achieve comparable applicability.
The SP addition time also influenced on the printability performance of the 3DCP samples. In PC samples, the direct SP addition
reduced the open time from 90 to 30 min in PC compared to delayed addition, while did not affect it for LC3 (which remained at
70 min). Regarding buildability, the direct addition of SP increased the number of successive layers compared to delayed addition. For
LC3 , the direct SP addition resulted in 20 successive layers, whereas for PC, it increased the number of layers to 34. Coupling TGA and
rheometry, it was observed that LC3 samples required a greater content of free water than PC samples to achieve a given yield stress.
This observation is consistent with the higher water demand of LC3 due to the presence of calcined clay.
The author declare that he has no known competing financial interests or personal relationships that could have appeared to in
fluence the work reported in this paper.
Data Availability
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P.R. de Matos et al. Case Studies in Construction Materials 19 (2023) e02419
Acknowledgments
The authors acknowledge the financial support from the following Brazilian governmental agencies: National Council for Scientific
and Technological Development – CNPq (grant number 403563/2021-6) and Coordination for the Improvement of Higher Education
Personnel – CAPES. The Multi-User Facility Infrastructure CMU/CCT/UDESC and Ms. Vanessa B. dos Santos are acknowledged for the
TGA.
Supplementary data associated with this article can be found in the online version at doi:10.1016/j.cscm.2023.e02419.
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