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ACI MATERIALS JOURNAL TECHNICAL PAPER

Title No. 116-M22

Mechanical Properties of Cement-Based Materials and


Effect of Elevated Temperature on Three-Dimensional (3-D)
Printed Mortar Specimens in Inkjet 3-D Printing
by Pshtiwan Shakor, Shami Nejadi, Gavin Paul, Jay Sanjayan, and Ali Nazari

Three-dimensional (3-D) printers have the potential to print can easily change the compressive strength of the elements.
samples that can be used as a scaffold for a variety of applications Developing a technique to improve the mechanical behavior
in different industries. In this paper, cement-based materials of 3-D-printed structural elements becomes a crucial part of
including ordinary portland cement, calcium aluminate cement research in the field of 3DP technologies.
(passing 150 µm [0.0059 in.] size sieve), and fine sand were inves-
In inkjet 3DP, the powder particles and the layer thick-
tigated as the cement-based materials in inkjet 3-D printing. Prism
ness have a significant influence on the shape of the printed
specimens were printed for the three-point bending test; and cubic
specimens were printed for the uniaxial compressive strength test. specimens. Farzadi et al. (2014) discovered that the powder
Prism samples were printed along different directional axes (X, Y, particles influence the thickness of specimens. It was found
and Z). The tests were conducted at different saturation levels that specimens with a higher resolution were obtained in a
(water-cement ratio [w/c]) as represented by S100C200, S125C250, thin layer scaffold. However, they discovered that the layers
S150C300, and S170C340. The prism specimens were cured in should be thicker than the largest particle size of the powder.
water for 7 and 28 days while cubic specimens were cured in Moreover, the materials that could be used for printing
Ca(OH)2 and water for 7 and 28 days at the same ambient tempera- the scaffold in a powder-based method are plaster, cement,
tures. In general, the results changed according to the directional cement mortar, metal, and ceramic (Utela et al. 2008;
axes of the prisms. However, following water curing, the cubic Shakor et al. 2017b; Feng et al. 2015b). For instance, Pegna
samples were heated up to 40°C (104°F) in an oven and a higher
(1997) categorized the additive manufacturing processes
compressive strength was evident compared to the samples which
and discussed the selective aggregation of the reactive bulk
were only cured in the room-temperature water. The wettability test
for both powders has been conducted in the presented study. material to fabricate a large solid structure. Pegna’s speci-
mens consisted of placing layers of reactive materials (port-
Keywords: cement-based materials; mechanical properties; three- land cement) over layers of silica material. In Pegna’s tests,
dimensional (3-D) printing; variable temperature and direction (X, Y, Z). two options were proposed to bind the materials in a solid-
free fabrication: 1) the binder is placed and the blanket is
INTRODUCTION activated; or 2) the binder is used as a blanket. The structures
Techniques in rapid prototyping have improved dramat- built with sand and portland cement were activated by water
ically in recent years from the old-style manufacturing of vapor. The resulting material was heavier than the normal
complex components to include works of medical treat- cast and yet it had the same compressive strength.
ment, food, and the automobile and architecture industries In recent decades, various technologies have been
(Lipson and Kurman 2013). The use of three-dimensional developed to implement additive manufacturing in the
(3-D) printing (3DP) technology has been progressively construction industry. These techniques can be broadly
integrated into the field of building and construction (Shakor divided into two categories: extrusion printing and powder-
et al. 2018). based printing (that is, inkjet printing or binder jetting).
Recent studies are mostly focused on the characteristics of
3-D-printed layers of cementitious materials, their mechan- Extrusion printing technique
ical properties, and finite element modeling. According to The extrusion printing technique involves extruding
these studies, different directions of layers in compression cementitious material from a nozzle, which is mounted on a
tests and flexural tests generate different results. Cubic spec- framework, to print structural elements layer by layer—for
imens produced using these methods tend to have similar example, concrete printing, designed by Le et al. (2012) and
failure features (that is, an hourglass-shape in the X, Y, and contour crafting, established by Khoshnevis et al. (2001).
Z directions) but yield a compression strength and elastic Furthermore, the extrusion printing for the cement mortar
modulus which are highest in the X-direction. Based on the has been optimized and developed by Shakor et al. (2017a).
compression tests and stress-strain relationship, 3-D printed,
powder-based materials are described as orthotropic materials ACI Materials Journal, V. 116, No. 2, March 2019.
MS No. M-2018-183.R1, doi: 10.14359/51714452, received May 27, 2018, and
(Feng et al. 2015a). The results show that the printing direc- reviewed under Institute publication policies. Copyright © 2019, American Concrete
tion elicits an important effect on the load-bearing capacity Institute. All rights reserved, including the making of copies unless permission is
obtained from the copyright proprietors. Pertinent discussion including author’s
of the specimen. Therefore, a corresponding enhancement closure, if any, will be published ten months from this journal’s date if the discussion
is received within four months of the paper’s print publication.

ACI Materials Journal/March 2019 55


One example is concrete printing that was used to examine
the hardened properties of high-performance printed
concrete in relation to the implementation of a 9 mm (0.35 in.)
diameter-printing nozzle. It was found that the compressive
strength of the printed samples in different directions was
between 75 and 102 MPa (10,877.8 and 14,793.8 psi) (Le
et al. 2012). The perpendicular load direction was the highest
compressive load, while in a conventional mold, the cast
cube had a compressive strength of approximately 107 MPa
(15,519 psi). Furthermore, they stated that the printed
concrete had a higher density, approximately 2350 kg/m3
(146.71 lb/ft3), compared to the control cast cube, which was
approximately 2250 kg/m3 (140.46 lb/ft3). This could have
been due to the gentle vibration of the concrete as it flowed
from the nozzle. Furthermore, small pumping extrusions
Fig. 1—3-D printer main components while printing cubic
during printing reduced the void ratios, which resulted in an
samples.
increase in density.
this paper, printable cementitious materials are prepared by
Powder-based printing technique (inkjet printing) blending portland cement, calcium aluminate cement, fine
The powder-based printing, also known as inkjet printing sand and lithium carbonate.
(3DP binder jetting), is another additive manufacturing
technique that creates precise scaffolds with complicated RESEARCH SIGNIFICANCE
geometries. The materials is bonded by dropping binder The significance of this research was using an inkjet 3DP
fluid (or “toner”) selectively into a powder bed, which binds printer to fabricate various specimens from cementitious
the powder where it impacts, as shown in Fig. 1. Jee and powder. The paper also studied various post-processing
Sachs (2000) proposed a visual simulation and developed procedures, which can be applied for the 3DP specimens
a geometric model of surface texture designs applied to a to gain higher strength in construction applications. More-
fabricated model. over, investigations on the mechanical properties of the 3DP
Post-processing procedures are crucial when fabricating samples along different directional axes have been described.
3DP specimens. Vorndran et al. (2011) claimed that there The two main compressive strength and three-point bending
was a post-hardening process after printing a specimen and tests have been studied with different dimensions and
that it was possible to increase the compressive strength up different saturation (water-cement ratio [w/c]) levels. Inkjet
to 35 MPa (5076.32 psi) for newberyite and up to 10 MPa 3DP is work based on the flowability of powder and wetta-
(1450.38 psi) for struvite. The shrinkage level was found to bility in the powder; these aspects have been discussed in
be 5 to 7% compared to the original model. In this study, this paper.
the primary attempt is to use post-processing techniques to
increase the strength of the 3DP objects. EXPERIMENTAL INVESTIGATION
Many studies have investigated the use of powders in Standard tests (according to ASTM C293 and ASTM
conjunction with the inkjet 3-D printer. For example, Klam- C39) were conducted in the experimental program to deter-
mert et al. (2010) investigated the application of magne- mine the flexural and compressive strength of the printed
sium ammonium phosphate (struvite) with a neutral setting scaffolds (ASTM C39 2001; ASTM C293/C293M 2002). In
reaction by printing farringtonite (Mg3(PO4)2) powder with addition, the samples were examined for the effects of heat,
ammonium phosphate solution as a binder. After long curing, the impacts of different curing conditions, and the influences
the achieved compressive strength was approximately 2 to of printing along different directional axes. There were three
7 MPa (290.075 to 1015.26 psi). In another example, Shakor main factors that affected the printed samples including the
et al. (2017b) replaced the cement mortar powder with material components, sample preparation/3DP parameters,
gypsum hemihydrate so as to enable resulting parts to be and the curing parameters.
used in construction applications.
In the present study, the influence of different saturation Material components
levels with different curing conditions and the effects of Powder preparation—The samples were fabricated by
X, Y, and Z directions on the flexural strength in 3DP were mixing CAC (6.78 kg [239.15 oz]), OPC (3.22 kg [113.58 oz]),
investigated in addition to the mechanical properties of the fine sand (0.5 kg [17.63 oz]), and lithium carbonate (0.45 kg
specimens. Predominantly, this study presents a novel meth- [15.87 oz]), which made up the total weight of the powder.
odology in its use of cementitious material for the require- Two types of cement, calcium aluminate cement (CAC)
ments and demands of the commercially available gypsum (Al2O3 ≥ 37%, CaO ≤ 39.8%, SiO2 ≤ 6%, Fe2O3 ≤ 18.5%),
powder (3-D printer consumer powder) by using 3DP ordinary portland cement (OPC) conforming to AS 3972
technology. In addition, this study proposes to increase the general purpose type (C3S, C2S > 70%, C3A > 4%, C4AF >
number of different types of materials that can be used by 10%) and fine sand (SiO2 ˃ 90%, Australia—maximum size
powder-based 3-D printers in the construction industry. In of approximately 300 µm [0.011 in.]), were used to create

56 ACI Materials Journal/March 2019


Table 1—Details of 3-D-printed and manual mixture specimens (60 x 5 x 5 mm) for flexural strength
Number of samples
Specimens CAD dimension, mm Printed direction 7 days 28 days
S100C200 60 x 5 x 5 X,Y,Z 1 3
S125C250 60 x 5 x 5 X,Y,Z 1 3
S150C300 60 x 5 x 5 X,Y,Z 1 3
S170C340 60 x 5 x 5 X,Y,Z 1 3
S100C200 60 x 5 x 5 Manual mixture 1 1
S125C250 60 x 5 x 5 Manual mixture 1 1
S150C300 60 x 5 x 5 Manual mixture 1 1
S170C340 60 x 5 x 5 Manual mixture 1 1

Note: 1 mm = 0.039 in.

Table 2—Details of 3-D-printed specimens for compressive strength


Number of samples
Specimens CAD dimensions, mm Curing method 1 day 7 days 28 days
Green Part 20 x 20 x 20 — 3 3 3
S100C200 20 x 20 x 20 Water 3 3 3
S125C250 20 x 20 x 20 Water 3 3 3
S150C300 20 x 20 x 20 Water 3 3 3
S170C340 20 x 20 x 20 Water and Ca(OH)2 0 9 9

Note: 1 mm = 0.039 in.

Table 3—Details of 3-D-printed specimens (70 x 10 x 4 mm) for flexural strength


Number of samples
In (YZ 0,90°) directions
Specimens CAD dimensions, mm Printed sample in YZ plane 7 days 28 days
S100C200 70 x 10 x 4 YZ 0° YZ 90° 2 6
S125C250 70 x 10 x 4 YZ 0° YZ 90° 2 6
S150C300 70 x 10 x 4 YZ 0° YZ 90° 2 6
S170C340 70 x 10 x 4 YZ 0° YZ 90° 2 6

Note: 1 mm = 0.039 in.

a total of 110 specimens for the mechanical tests (refer to (<10%), vinyl polymer (<20%), and plaster (<90%) which
Tables 1, 2, and 3). Lithium carbonate (Li2CO3) (reagent was applied without further sieving.
grade by American Chemical Society) was mixed to accel- The particle size distribution of the powders was measured
erate the setting time of the mortar. The prepared specimens by using a laser diffraction particle size analyser. All powder
were divided into two batches of 54 samples for the compres- samples were measured three times to determine the D10,
sive strength test and 56 samples for the flexural strength D50, and D90 values, which designate that 10, 50, and 90%
test and each value is presented as an average (approximate of the particles were less than those sizes (refer to Fig. 2).
standard deviation). For each test, three specimens were The layer thickness was approximately 0.1 mm (0.0039 in.)
printed, which are the minimum requirements for making according to the setting of the 3-D printer, which determines
and curing samples according to the Australian standard (AS each layer while spreading through the roller (refer to Fig. 3).
1012.8.3 2015). The mixture ratio was the closest ratio to a The surface area test for the powder specimens was
gypsum powder. The gypsum powder is the recommended performed with a multipoint surface area analyser (BET
powder that is supplied by the inkjet printer supplier. In the analysis). In addition, the bulk density was determined
present study, the gypsum powder has been compared with according to ASTM C29.
cement mortar (modified powder). It should be noted that Binder characterization—A fluid solvent was used as an
the gypsum powder was chiefly calcium sulfate hemihydrate adhesive during the 3DP process. The binder was a commercial
(CaSO4·0.5H2O), also known as plaster of Paris (Zhou et clear liquid solution with a viscosity close to pure water. The
al. 2013). The gypsum powder was used for the delicate formation of the binder was mostly water with 2-Pyrrolidone
models. The powder was a combination of carbohydrate (Farzadi et al. 2014).

ACI Materials Journal/March 2019 57


Sample preparation and 3DP parameters rapid prototype machine and it revealed anisotropic charac-
Literature on inkjet 3DP parameters—The inkjet 3DP teristics in the compressive strength results of the specimens.
could be adjusted only for different saturation levels (binder/ According to Lin et al. (2015), the extrusion 3DP samples
volume ratio) or the w/c. Recently, new products from the could achieve a compressive strength of approximately 10 to
same company have made it possible to adjust the sample 20 MPa (1450.38 to 2900.75 psi) after 2 hours and approxi-
thickness layers in addition to saturation levels. The thick- mately 50 to 60 MPa (7251.89 to 8702.26 psi) after 28 days.
ness and saturation levels of the specimens had a significant The setting time of concrete was between 20 and 60 minutes
effect on the porosity and stability of the samples’ green after using lithium carbonate as an accelerator. However, the
parts. The appropriate time to remove a green part from the main differences observed in powder-based printer samples,
unbounded powder depends on the duration of drying in compared to extrusion printing, were the saturation levels
the powder bed and saturation levels. Green parts (uncured for the core and shell of the structure. Szucs and Brabazon
objects) can be defined when a binder (liquid) is added to the (2009) claimed that an increase in the saturation level of
powder and reacts to build a printed scaffold (Gibbons et al. printed samples could improve the mechanical properties
2010). Additionally, evaporation of the printing liquid plays of the structure. Based on the same study, the stiffness and
a crucial role. The saturation levels of the printer can be compressive strength of the 3DP samples rise at a higher
adjusted according to the outer and inner scaffold, which are sintering temperature. Moreover, sintering can reduce the
known as the shell and core, respectively. The ratio of binder specific surface area and increase the porosity of the sample.
to powder materials influences the degree of unification and They discovered that the obtained mechanical properties
consolidation. Furthermore, the layer thickness determines were still not sufficient for load-bearing applications. In this
the infiltration and final resolution of the printing liquid. The study, to harden the powder for the cubic samples, a higher
saturation levels are presented in Table 4. saturation level is used to produce a 3DP part. It is expected
Lee et al. (2007) studied the compressive strength values that the customized powder will be stronger than the powder
in different rapid prototyping (RP) machines. Fused deposi- that is commercially available.
tion modelling (FDM) and the inkjet 3DP were assumed as a From the literature review, it is evident that existing
research recognized the critical role played by layer thick-
ness and the binder saturation level. For instance, Lu and
Reynolds (2008) created a complex shape from TiNiHf
shape memory alloy (SMA). Furthermore, they have found
that a particle diameter 35 µm (0.0013 in.) printing sample
with a 170% binder saturation level has the highest struc-
tural mesh integrity. In general, a printing layer thickness

Table 4—Description of saturation levels,


consumed binder, and time taken to build cubic
(20 x 20 x 20 mm) sample
Sample Sample Binder/ Duration,
name description volume ratio Binder, mL min
Shell: 100,
S100C200 0.244 3.24 8.55
Core: 200
Shell: 125,
S125S250 0.305 3.74 8.66
Core: 250
Shell: 150,
S150C300 0.366 4.24 8.88
Core: 300
Shell: 170,
Fig. 2—Particle size distributions of gypsum and S170C340 0.415 4.66 9.00
Core: 340
CAC&OPC powders. (Note: q3 is unit standing for loga-
rithm of percentage of total particles; 1 µm = 0.000039 in.) Notes: 1 mL = 0.033 fl oz; 1 mm = 0.039 in.

Fig. 3—Layer explanation and powder/binder interaction between layers.

58 ACI Materials Journal/March 2019


Fig. 4—(a) Cubic specimens (20 x 20 x 20 mm [0.78 x 0.78 x 0.78 in.]); and (b) prism specimens (60 x 5 x 5 mm [2.36 x 0.19 x
0.19 in.]).

Fig. 5—Different plane in 3DP software for each axis (X, Y, Z); prism (70 x 10 x 4 mm [2.7 x 0.39 x 0.15 in.]) presented in
plane of YZ 0° and YZ 90°.
of 35 µm (0.0013 in.) and binder saturation level of 170% rotated 90 degrees (thickness of scaffold parallel to X-direc-
were found to be the optimum requirements when printing tion); refer to Table 3 and Fig. 5 for more details.
samples using a TiNiHf 3-D mesh scaffold. To measure the mechanical properties of the printed
Preparation of 3DP parameters—The specimens were scaffolds, uniaxial compressive strength was performed
sketched using computer-aided design software to prepare at a loading rate of 0.03 kN/s (6.74 lb/s). In this study,
for printing through the inkjet 3DP. In Fig. 4 to 6, the cubic uniaxial compressive strength was conducted only in the
samples with dimensions of 20 x 20 x 20 mm (0.78 x 0.78 x X-orientation.
0.78 in.) and two prism specimens with dimensions of 60 x
5 x 5 mm (2.36 x 0.19 x 0.19 in.) and 70 x 10 x 4 mm (2.75 x Curing conditions
0.39 x 0.15 in.), are shown. The curing process and conditions are another important
A cartridge was used as a print head by the inkjet printer aspect of 3DP for this application. The last process of printing
with a surface tension of 45 dynes/cm (0.00025 lb/in.) and is post-hardening. Post-hardening in 3DP has three alterna-
viscosity of 1.35 cP (0.0009 lb/ft.s) similar to the work that tives: wax, super glue, and epoxy. These could be applied
has been done by Utela et al. (2008). Figure 5 illustrates the as a dip, drizzle, and spray, respectively. However, the
different plane and directions of the printed samples for the cementitious powder has different processes for curing. In
flexural strength test. Table 1 present the flexural strength of this study, water was used to cure the cement powder. Some
specimens, while Table 2 presents the specimen’s compres- samples were cured with 5% calcium hydroxide (Ca(OH)2)
sive strength details. Table 3 presents the flexural strength dissolved in the total weight of water. Table 5 summarises
details of specimens with dimensions 70 x 10 x 4 mm the dimensions and weight of the S170C340 sample in
(2.75 x 0.39 x 0.15 in.). the different curing scenarios with water and 5% calcium
Other specimens, with dimensions of 70 x 10 x 4 mm hydroxide. As shown in Table 5, the specimens in water
(2.75 x 0.39 x 0.15 in.), were also fabricated for flexural increase their dimensions when they were cured for 7 and 28
strength at the same saturation levels of shell and core days. Specifically, if a sample was cured in water with 5%
(refer to Fig. 6). They were printed in two orientation calcium hydroxide after drying in an oven for approximately
degrees in the YZ plane: (i) YZ 0° (width of scaffold parallel an hour at 40°C (104°F), the original dimensions changed
to X-direction of the printer); and (ii) YZ 90°, when it was by 2 ± 0.22 mm (0.078 ± 0.008 in.), which means the dimen-

ACI Materials Journal/March 2019 59


Fig. 6—(a) Prism specimen (70 x 10 x 4 mm [2.7 x 0.39 x 0.15 in.]) YZ 90°; and (b) prism specimens (70 x 10 x 4 mm [2.7 x
0.39 x 0.15 in.]) YZ 0°.
Table 5—Curing method of S170C340 in water and
5% of Ca(OH)2 after drying at 40°C in oven
Sample Dimensions, mm Weight, g
descrip- Curing
tion method 7 days 28 days 7 days 28 days
Water 20.94 x 21.53 x
15.85 16.55
(40°C) 20.64 22.07
Water and
S170 5% of 22.37 x 22.05 x
16.60 16.85
C340 Ca(OH)2 22.19 22.1
(40°C)
Green
Fig. 7—Steps of penetrating water-based liquid into gypsum 21.12 x 20.83 12.64
parts
powder: (a) impact time of droplet on surface of powder; (b)
penetration processes of liquid on powder after 16 seconds; Notes: 1 mm = 0.039 in.; 1 g = 0.035 oz; °F = (°C/1.8) + 32.

and (c) absorbing most of liquid into powder. conduct the drop penetration test. Therefore, a binder droplet
sional rate increased by 6%. According to the study of Pfister with a volume of approximately 60 μL (0.002 fl oz) was
et al. (2004), when comparing 3-D bioplotting to 3DP, the dropped by a 1 mL (0.000033 fl oz) medical syringe (25-gauge
maximum elongation was found to be four times greater needle), which was placed over the powder surface.
and the maximum flexural strength was three times higher. In the following test, frame-by-frame shots by a high-
The swelling of the 3-D bioplotting matrix was 14% smaller speed camera were used to both determine the drop penetra-
than in 3-D printing by water. As another example, Seitz tion time and examine the complete drop penetration process
et al. (2005) used hydroxyapatite (HA) powder to fabricate as it has been prepared in previous studies (Hapgood et al.
3-D printed specimens. They found that the dimensions of 2002; Nguyen et al. 2009; Zhou et al. 2014). The starting
printed parameters were 3% smaller than the dimensions of point was indicated as an impact point to the surface when
the real model. the droplet first touches the powder bed surface. Thereafter
the end-point was determined as the time when completely
Wettability and drop penetration test liquid was diminished under the surface of the powder bed.
This test has been conducted using two different methods.
One of the methods uses the contact angle goniometer RESULTS AND DISCUSSION
method, while another method uses the high-resolution Powder characterization
camera to investigate the penetration time of the drop of The particle size of the gypsum powder has a similar size
liquid on the powder bed of the printer. Figure 7 shows how to 67%CAC & 33%OPC powders. The most widely used
a contact angle goniometer has been used for this inves- method of describing particle size distribution is a D value,
tigation, to capture image frames of each test at a rate of and D90 values are equal to 127.11 µm (0.005 in.) for CAC
60 frames/second. In Fig. 8, the second approach used a and 38.46 µm (0.0015 in.) for OPC powders. The surface
high-speed video recorder, operating at 240 frames/second, area and bulk density of both powders are shown in Table 6.
to capture images of the path a single binder droplet as it The main goal of this research is to fabricate a stronger
penetrated the powder bed. For each of the powders and sample. However, in the authors’ earlier study, Shakor et al.
methods, the test was replicated three times. (2017b), the gypsum powder was modified and the w/c for
A single droplet of binder was used for depositing and the manual mixture was investigated. According to the exper-
consequently penetrating the powder bed. The powder bed imentation results, it has been shown that it was not possible
was prepared in the printer before the process of drop fall to obtain consistent and acceptable mechanical properties in
penetration. After the process was completed, the build the produced printed samples. In the previous study, it was
chamber was taken out of the 3-D printer and was used to also found that the maximum compressive strength reached

60 ACI Materials Journal/March 2019


Fig. 8—Illustration of drop penetration test setup.
8.26 MPa (1198.01 psi) after 28 days when the samples Table 6—Properties of gypsum and cementitious
were only cured in water. In the current research, the curing powders
medium of the printed sample was changed to gain better
Powder properties Gypsum CAC, OPC
outcomes. Although the green samples should have enough
strength to hold their shape while handling and removing Surface area, m2/g 0.999 1.021
the excess material, it was initially concerning when it was Bulk density, g/cm 3
0.912 0.79
discovered that they did not have high compressive strength. Note: 1 m2/g = 307.42 ft2/oz; 1 g/cm3 = 0.578 oz/in.3.
In addition, dimensional accuracy was another concern.
The 3DP samples did not have the exact dimensions of the increase in the layer thickness requires a higher saturation
original CAD design model. To examine and monitor the level to ensure complete cohesion between the layers. In this
overall parts of the fabricated cubic and prism specimens for work, the fast-axis mounted print head, which was set on a
compressive and flexural strength, the external dimensions default speed, can build two to four layers in 60 seconds.
of each sample were measured accurately using a digital In addition, the three-point bending test equipment was
calliper with an accuracy of 0.01 mm (0.00039 in.). The custom made to test the flexural strength of 3DP specimens
weight of the specimen was also measured on a precision by ignoring friction which shows the flexural test setup.
scale with an accuracy of 0.001g (0.000035 oz). According to ASTM C29, flexural strength is approximately
10 to 20% of the compressive strength value. This depends
Effects of 3DP parameters on the size, volume, and type of the coarse aggregates that
This research also investigates how the saturation settings were used. The samples with 60 x 5 x 5 mm (2.36 x 0.19 x
influence the strength of the cement component powder. It 0.19 in.) were put on a simply supported edge with the exact
was obvious that the flexural strength in the X-direction had dimensions being 50 mm (1.97 in.) center to center. To eval-
the highest strength (approximately 6.21 MPa [900.68 psi]) uate the flexural strength of printed specimens, manually
because it required the least number of layers to construct in mixed samples were prepared with the same dimensions and
this direction compared to the other directions (axes) (refer compacted. It is noted that flexural strength in the manual
to Fig. 6). This is consistent with the study by Farzadi et al. mixture at a saturation level of (S125C250) was recorded
(2014). This was due to the acceptable coincidences between as the highest result among all the specimens, at approxi-
layers in this direction where the movement is parallel to mately 9.77 MPa (1417.02 psi) (refer to Fig. 9). This result
the printer head. For illustration, Castilho et al. (2011) stated suggests that, due to decent vibration in the normal mixture,
that the 3DP scaffold stiffness decreases when the number the outcomes were higher than the 3-D-printed samples. The
of elementary units (layers) increases. This suggestion was dimensions of the specimen were found to have a signifi-
also put forward by Vaezi and Chua (2011). Therefore, in the cant impact on the results. The specimens were produced in
present study, a similar thickness was used. The literature accordance with printer constraints, similar to those of Feng
also supports the case that a higher saturation level leads to et al. (2015b), who conducted their samples in a similar way.
a higher compressive strength. Experimental work by Vaezi The specimens 60 x 5 x 5 mm (2.36 x 0.19 x 0.19 in.)
and Chua (2011) found that increasing the binder satura- were tested for flexural strength and the results are shown
tion level from 90 to 125% increases the sample’s flexural in Fig. 10.
and tensile strengths, which has been also confirmed by the Furthermore, other samples with dimensions of 70 x 10 x
presented study. 4 mm (2.75 x 0.39 x 0.15 in.) were subjected to a three-point
The existing work uses the layer thickness print 0.102 mm bending test to measure the bending strength. In Fig. 11 and
(0.004 in.), while most of the particle sizes used are less than 12, the results of the bending strength test are illustrated
0.1 mm (0.0039 in.). According to Withell et al. (2011), an with the sample in the YZ plane is 0 degrees (called YZ 0°);

ACI Materials Journal/March 2019 61


Fig. 9—Flexural strength of manual mixture cementitious
prism specimens. (Note: 1 MPa = 145 psi.)
Fig. 11—Flexural strength of cementitious prism samples
when tested in YZ 0º. (Note: 1 MPa = 145 psi.)

Fig. 12—Flexural strength of cementitious prism samples


Fig. 10—Flexural strength of cementitious printed prism when tested in YZ 90º. (Note: 1 MPa = 145 psi.)
tested in different directions (X, Y, and Z) and saturation tion (3.22 ± 0.12 MPa [467.02 ± 17.4 psi]) but overall still
levels. (Note: 1 MPa = 145 psi.) had less strength than YZ 0°. It was noted that this specimen
refer to Fig. 5. When the sample rotates 90 degrees in the was more fragile than specimens printed in the other printed
YZ plane, it is called YZ 90°. The finding of the prelimi- plane. This was because printing in YZ 90° takes longer and
nary flexural strength test concerning the YZ 0° samples was leaves a large number of voids between the particles of
that the strength of bending increases when the saturation the powder.
level is increased. Figure 13 shows that the maximum peak Research by Vlasea et al. (2015) discovered that the
point of bending strength of YZ 0° was 7.25 ± 0.11 MPa different layer orientation had an effect on the mechanical
(1051.52 ± 15.95 psi). It can be seen that the sample printed properties of the printed scaffold. Similarly, Castilho et al.
in the plane YZ 0° can resist more bearing loads because (2013) produced almost the same results. In the present
it needs less time to print the samples than those that are work, all the cubic samples were tested parallel to the X-
printed in YZ 90°. Also, the largest part printed in the X- direction (0°), except for the prisms, which were tested in
direction or plane of YZ 0° has stronger mechanical proper- different directions.
ties than when printed in the other directions. Previous work
by Withell et al. (2011) agreed that the X-direction YZ 0° has Effects of curing parameters
the best results for flexural strength. The present research found that the curing parameters
Figure 12 illustrates the optimum bending strength YZ 90° had a significant impact on the mechanical properties of the
at S150C300. It was recorded as the highest point of deflec-

62 ACI Materials Journal/March 2019


Fig. 13—Cementitious cube: (a) sample under uniaxial
compressive strength test; and (b) after removal from
uniaxial compressive strength test.
materials’ composition. All the tests used a universal testing
machine (50 kN [11,240.44 lb]), as shown in Fig. 13.
Figure 14 shows how the 3DP samples changed under
high temperature in two types of curing scenarios. Compres-
sive strength was examined according to ASTM C39. In the
present study, the highest compressive strength was recorded Fig. 14—Compressive strength of cementitious cube at
(14.68 ± 0.43 MPa [2129.15 ± 62.36 psi]) when compared different curing conditions and saturation level S170C340.
to other recorded samples that were cured without drying at (Note: 1 MPa = 145 psi.)
high temperature (4.81 ± 0.86 MPa [697.63 ± 124.73 psi]).
These are explained in more detail in Fig. 15. For instance,
in the study by Ma et al. (2015), carbon powders with small
particle sizes were used as a solution binder. Then it was
found that the bending strength of the samples was very low,
but after pre-sintering, this doubled.
The 3DP sample (S170C340) had the highest result in
compressive strength when cured for 28 days in water and
then dried for approximately 1 hour at 40°C (104°F) in the
furnace. The tests were conducted in the laboratory with
samples which were dried in the laboratory oven at 40°C
(104°F) for approximately 1 hour and then left to cool to
room temperature. The samples were cured for 28 days in
water blended with 5% Ca(OH)2, which yielded weaker
compressive strength than the samples that had been cured
in water only. This might be due to the Ca(OH)2 not helping
to fill the gaps between the particles. As shown in Table 5,
the sample cured in Ca(OH)2 had larger dimensions and a
heavier weight. This means that the samples in Ca(OH)2
became larger, increasing the voids and not providing any
reactions with the Ca(OH)2. Goto and Roy (1981) found
that the curing temperature and w/c influenced the pore size Fig. 15—Compressive strength of cementitious cube at
distribution, the porosity, and the permeability of the cement different saturation level and curing in normal temperature
paste. However, the samples by Goto and Roy (1981), which water. (Note: 1 MPa = 145 psi.)
were cured at 60°C (140°F), had a smaller total porosity than
land cement and is related to the strength in cement-based
the samples cured at 27°C (80.6°F). Goto and Roy (1981)
materials.
also claimed that tricalcium silicate (C3S), when cured at
Figure 15 shows the compressive strength for the cubic spec-
a higher temperature, becomes larger in size than when
imens (S100C200, S125C250, S150C300, and S170C340),
cured at a lower temperature at an early age. In addition,
which used different saturation levels while retaining the same
Sandor (1986) emphasized and proofed that the compressive
curing scenarios. It was observed that the maximum compres-
strength of the sample is improved when the exterior holds
sive strength was 4.81 ± 0.79 MPa (697.63 ± 114.57  psi)
less wetness than the interior. Moreover, Patel et al. (1996)
when it was not dried in the oven. Hence, this emphasises that
discovered that the thickness of the calcium silicate hydrate
high-temperature curing has a more significant effect on the
(C-S-H) rims in paste increased from 5 to 25 mm (0.196 to
mechanical behavior of materials.
0.98 in.) at 20 and 80°C (68 and 176°F), respectively, at 28
There are several factors that led to the compressive
days age. C-S-H is the basic product of the hydration of port-
strength results, as shown in Fig. 15, where some specimens
did not develop effectively for the 7- and 28-day curing ages.

ACI Materials Journal/March 2019 63


Fig. 16—Interior (core) and exterior (shell) for same satura-
tion levels in 3DP sample.
Firstly, the binder used in this preparation is not pure water,
which affects the final mechanical strength of the mortar.
Secondly, the samples had orthotropic properties despite Fig. 17—Comparison of compressive strength of 3DP
being as isotropic as normal mortar. Moreover, porosities cement mortar cube in different sizes.
were prominent among the particles due to their free-flowing compressive strength results in the conventional mixture
nature. Layer processes made complete shapes, which also for the different dimensions of cube mold can make an
created open pores between layers. Another point to consider enormous difference due to the compaction, porosity, and
is the hydration process. Figure 16 shows how all particles particle size distribution, as explained by Hamad (2017) and
did not hydrate at the same time in the same saturation level Majeed (2011). On the other hand, for the 3DP specimens,
because the dispersion of the binder on the powder was not the compressive strength increases with 14% while the 3DP
distributed evenly (some parts of the powder were wet, and cube changes dimensions from 20 x 20 x 20 mm (0.78 x
some others were still dry). Accordingly, it was observed 0.78 x 0.78 in.) to 50 x 50 x 50 mm (1.96 x 1.96 x 1.96 in.),
that when they were put in the water for curing, the unhy- which is contrary to the prepared conventional mortar cube.
drated particles released from the hydrated particles. The For further understanding the anisotropic properties of the
combined particles resulted in better bonds, and the C-S-H 3DP cube, this work required further examination and extra
bonds became stronger. However, they did not have enough study. Additionally, the produced 3DP scaffold continuously
strength for structural purposes. This is further evidenced changed its properties and dimensions over time or in a vari-
when Parr et al. (2005) and Patel et al. (1996) samples’ able environment such as medium conditions, temperature
gained better mechanical strength after being heated in the and humidity (Farzadi et al. 2015).
oven because it helped the C-S-H or C-A-H to form a
better bond. Wettability and drop penetration
Additionally, the normal cement mortar is usually cast The wettability and drop penetration tests were conducted
under compaction or vibration, resulting in higher strength for the gypsum powder and CAC&OPC powder (modified
than the 3DP samples due to the removal of voids. In the powder). In this test, it has been observed that both test
3DP process, there was no such compaction. methods provided similar outcomes for the penetration time
Most notably, CAC (6.78 kg [2.2 lb]) and lithium of the water-based droplet into the powder.
carbonate (0.45 kg [0.99 lb]) in the powder quickly set the Figure 18 shows the test results for the gypsum powder
sample at an early age with a higher strength than normal and modified powder for both the contact angle goniom-
cement. However, as shown in Fig. 15 and corroborated by eter methodologies. It presented that drop penetration time
Ann and Cho (2014), the development of later-age strength takes longer to absorb the whole drop binder in the gypsum
(28 days) is negatively affected. powder, with an average value of 55.24 ± 5.4 seconds,
Two sizes of the 3DP samples are presented in Fig. 17. while the absorption of the whole drop takes less time in the
The result shows that the samples of 20 x 20 x 20 mm modified powder (cementitious powder), where the average
(0.78  x 0.78 x 0.78 in.) have a slight difference in their value was 3.70 ± 1.4 seconds. For each powder, the test was
compressive strength, with the standard mortar cube sample repeated three times. Each of the trials has been indicated in
50 x 50 x 50 mm (1.96 x 1.96 x 1.96 in.). This study needs different color lines in Fig. 18.
further investigation to find the differences in all three axes Figure 19 shows the test results with the images of the
when compared with conventional mortar mixture. Due to droplet penetration taken by the high-speed camera for both
the consistency of the printing layer and binder distribu- powders. The binder drop penetration in this method has
tion on powder bed, there was little difference in stiffness similar results to the goniometer method. In this approach,
between the two different printed dimensions. However, the the drop penetration average value time in gypsum powder

64 ACI Materials Journal/March 2019


Fig. 18—(a) Penetration time per volume (µL) consumed by gypsum powder; and (b) penetration time per volume (µL)
consumed by CAC&OPC powder. (Note: 1 µL = 0.000033814 fl oz.)
was approximately 55.93 ± 0.66 seconds, while the drop The wettability test is used to find how the structural form
penetration average value time for the modified powder was is made and the coherence between the printed part occurred.
1.28 ± 0.07 seconds. These experiments were also delin- The coherence of 3-D-printed objects is mainly dependent
eated by Hapgood et al. (2002) and Zhou et al. (2014). The on the strength of the bond between particles, and how the
significant differences in penetration time happened due to droplet binds to the particles. The morphology of the parti-
agglomeration in the modified powder. Agglomeration is cles and the presence of interparticle pores could be another
when the modified powder is naturally packed more closely reason for differences incoherence. Cement particles may
in the powder bed than the gypsum powder. In other words, provide an additional reason, and according to Kirchberg
gypsum powder distributed as a homogeneous powder and et al. (2011) fine particles increment the contact angle and
the CAC&OPC (modified) powder distributed as a hetero- decrease the powder’s wettability. Figure 2 clearly shows the
geneous powder during the preparation for the bedding layer peak particle sizes in gypsum powder that is inclined to have
and testing for the droplet penetration. finer particles than CAC&OPC powder.
The earlier studies by Nguyen et al. (2009) used two types
of powder with different particle sizes for the hydrophobicity CONCLUSIONS
and hydrophilicity. They discovered that the smaller-sized This paper described the modification to the inkjet 3-D
particle has hydrophobic properties. That study also showed printer, which operates by using low-cost cementitious
that the penetration time increased as a result of adding the powder materials. This powder can be used in construction
fine particles powders to the mixture powder. Hence, this work as it is fit-for-purpose and affordable. This study has
research agrees with the same study that has been done demonstrated reasonable mechanical strength which, with
by Hapgood et al. (2003). In all the previously conducted further investigation, can potentially help enable the produc-
investigations into the penetration time, evidence shows tion of large structural elements. This study also describes the
that the hydrophobic phenomena will occur in the finer influence of various parameters and how they can affect the
powder particles. The literature thus agrees with the results quality of the sample. Moreover, experimental results were
that are presented in this paper. In Fig. 2, it was shown that presented by producing a higher compressive strength when
the gypsum powder has a smaller particle size than that of curing in a furnace while using the CAC&OPC powder. The
CAC&OPC. compressive strength under different curing conditions and
As further evidence, Fuhr et al. (2013) showed that the drying at high temperatures was also discussed. Comparisons
fungi penetration time increases with decreasing the pore were made with other samples of 5% Ca(OH)2 dissolved in
size in the wood. In the presented study, it was observed water and 100% water. Experimental tests were conducted
that gypsum powder has a smaller pore size than cementi- on flexural strengths in different 3DP directions, which
tious powder. Another study, performed by Tschapek (1984), showed that samples printed along the X-directional axis had
stated that the porosity in the soil helps the water easily pass the highest flexural strength. In addition, the compressive
through the soil particles (hydrophilic soil). strength for the cube increased by 14% while the dimensions
Further study should be conducted to better understand the of the cube changed from 20 x 20 x 20 mm (0.78 x 0.78 x
phenomenon for the drop penetration through two different 0.78 in.) to 50 x 50 x 50 mm (1.96 x 1.96 x 1.96 in.). There-
powders. The porosity between particles has a great effect on fore, when the size of the cube increases, the compressive
the droplet penetration in the powder, which is led to droplet strength of the specimen increases as would occur contrary
penetrating the unpacked surface faster. in a conventional mortar cube mold. The penetration time
This experimental work revealed that the water-based for gypsum powder and CAC&OPC powders has also been
droplet on gypsum powder particles took longer to investigated in this research, which led to the conclusion
completely penetrate the surface. that the heterogeneous powder quickly absorbs liquid into
the powder due to the higher porosity among its particles.

ACI Materials Journal/March 2019 65


Fig. 19—Images from video recording for penetration time per drop of binder in gypsum powder and CAC&OPC powder.
Future work should focus on analyzing the various ACKNOWLEDGMENTS
percentages of Ca(OH)2 in water and employing various The authors would like to acknowledge that the experimental program
of this study has been conducted in the Smart Structures Laboratory at the
temperatures or steam conditions. Finally, it is also necessary Swinburne University of Technology and the Civil and Structural Engi-
to evaluate larger particle sizes of fine sand in the powder. It neering Laboratory at the University of Technology Sydney.
is important for researchers to use distilled water instead of
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presentations, webinars, and ACI Raleigh, October 25-29,
Center & Raleigh
education documents at either no or NC, USA
Marriott
2020
minimal cost. ACI and its subsidiaries
are always accepting the submission
of papers for potential publication and
distribution. More information about
ACI’s conventions, technical presentations
and documents, and calls for papers can
be found at www.concrete.org.

For more information visit Concrete.org   

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