Materials & Design 209 (2021) 109981

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Materials & Design

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

Development of multicolor 3D-printed 3Y-ZrO2 sintered bodies by

optimizing rheological properties of UV-curable high-content ceramic
nanocomposites
Sang Hyun Ji a, Da Sol Kim a, Min Soo Park b, Doojin Lee c, Ji Sun Yun a,⇑
a
Energy & Environmental Division, Korea Institute of Ceramic Engineering and Technology, 101, Soho-ro, Jinju 52851, Republic of Korea
b
Department of Mechanical System Design Engineering, Seoul National University of Science and Technology, Seoul 01811, Republic of Korea
c
Department of Polymer Science and Engineering, Chonnam National University, Gwangju 61186, Republic of Korea

h i g h l i g h t s g r a p h i c a l a b s t r a c t

 UV-curable different-colored 3Y-ZrO2

resins with 50 vol% of ceramic were
prepared.
 Photocurability, viscosity, flowability,
and printability were investigated.
 Flexural strength was comparable to
that of conventionally manufactured
resins.
 Multilayered objects were
continuously 3D printed and
simultaneously sintered.
 The different-colored sintered bodies
exhibited a high relative density
(>99.90%).
 The all sintered bodies exhibited a
high flexural strength (>930 MPa).

a r t i c l e i n f o a b s t r a c t

Article history: UV-curable different-colored 3Y-ZrO2 ceramic nanocomposite resins with a ceramic content of 50 vol%
Received 31 March 2021 were prepared for supportless stereolithography 3D printing. Based on the correlation between the sol-
Revised 9 July 2021 ubility parameters of UV-curable organic resin systems and the rheological behaviors of highly loaded
Accepted 9 July 2021
ceramic nanocomposites, the physical properties of the different-colored 3Y-ZrO2 ceramic nanocompos-
Available online 16 July 2021
ite resins, such as photocurability, viscosity, flowability, and printability, were optimized for a support-
less 3D printing process. Thus, white, pink, yellow, and gray 3Y-ZrO2 ceramic nanocomposite resins
Keywords:
with optimum physical properties were prepared. The different-colored 3D-printed 3Y-ZrO2 objects sin-
Ceramic 3D printing
Sintering process
tered at 1450 °C for 180 min exhibited a high relative density of>99.90% and a high flexural strength
Rheological behavior of>930 MPa, which are comparable to those of commercial 3Y-ZrO2 manufactured by a conventional
Flexural strength ceramic process. In addition, gear-shaped objects with different-colored layers of ceramic resins were
Relative density successfully manufactured by continuous 3D printing and simultaneous sintering. This study paves the
way for innovation in the manufacturing of ceramic products by 3D printing as an alternative to the tra-
ditional ceramic process.
Ó 2021 The Author(s). 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/).

⇑ Corresponding author.
E-mail address: susubin@kicet.re.kr (J. Sun Yun).

https://doi.org/10.1016/j.matdes.2021.109981
0264-1275/Ó 2021 The Author(s). 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/).
S. Hyun Ji, D. Sol Kim, M. Soo Park et al.
1. Introduction
Additive manufacturing or 3D printing technology is used to
construct complex 3D structures in a sequential layer-by-layer
manner using polymers, metals, and ceramics [1,2]. Ceramic 3D
printing technology is one of the most promising and challenging
approaches for the fabrication of ceramic products having complex
structures, as it is quite difficult to achieve this by traditional
methods [3,4]. 3D printing can be carried out by various methods
such as fused deposition modeling, selective laser sintering, and
stereolithography. Among these, 3D printing using stereolithogra-
phy apparatus (SLA) has attracted considerable attention for man-
ufacturing ceramics with sophisticated and complex structures
[5,6].
3D printing is one of the steps in the manufacturing of ceramic
products. A green body (a 3D-printed object obtained before addi-
tional post-processes such as sintering and hardening) is printed
by the ceramic 3D printer, and it is then subjected to high-
temperature sintering to obtain a ceramic crystal structure. Com-
pared with traditional ceramic parts, ceramic 3D-printed green
bodies have a high polymer content and a weak binding force
between the layers due to the layer-by-layer fabrication process;
hence, optimization of the drying, debinding, and sintering pro-
cesses of the green body is important [7]. Furthermore, a ceramic
content as high as 40 vol% or more is required to maintain the sta-
bility and functionality of the ceramic products after high-
temperature sintering. However, the viscosity of the UV-curable
ceramic composite resins increases rapidly with increasing cera-
mic content, because of which 3D printing with a general SLA
device is difficult. Supportless 3D printing technology has been
explored to address this issue of high-viscosity ceramic composite
resins owing to their high ceramic content [8]. However, the rheo-
logical behavior of ceramic composite resins suitable for support-
less 3D printing needs to be investigated in depth, which would
allow the manufacturing of ceramic products of various colors
and shapes after the sintering process.
Organic dyes are generally introduced in UV-curable liquid
resins used in 3D printing for esthetical color reproduction or to
improve the green body resolution [9,10]. However, organic dyes
cannot be used in ceramic 3D printing resins as they are eliminated
during the high-temperature sintering process. In other words, to
manufacture multicolor 3D-printed ceramic sintered bodies, a
multicolor ceramic composite resin must be synthesized using
ceramic powders containing a small amount of ceramic dye
(rare-earth elements). The color of such ceramic dyes is well-
expressed upon subsequent sintering. Since the presence of a small
amounts of rare-earth elements in ceramic particles affects the
rheological behavior, photocurability, and printability of the cera-
mic composite resins, the physical properties of ceramic composite
resins containing ceramic particles of various colors need to be
optimized.
In this study, different-colored 3Y-ZrO2 ceramic nanocomposite
resins with a ceramic content of 50 vol% were fabricated using 1,6-
hexanediol diacrylate (HDDA) as the monomer, and the rheological
behavior and printability of the resins were optimized for support-
less 3D printing by controlling the amount of the diluent, butox-
yethanol (Bu). The 3D-printed objects prepared using the
different-colored 3Y-ZrO2 nanocomposite resins with optimum
rheological properties were densified and crystallized by sintering
at 1450 °C for 180 min, which resulted in increased strength and
well-expressed color. Furthermore, gear-shaped products with
different-colored layers were successfully obtained by continuous
3D printing and simultaneous sintering.
2
Materials & Design 209 (2021) 109981
2. Material and methods
White, pink, gray, and yellow 3Y-ZrO2 ceramic nanopowders
were purchased from Tosoh Corporation (ZpexÒ, Japan). To
improve the dispersibility of the ceramics in the photocurable liq-
uid resin, the surface of the colored 3Y-ZrO2 ceramic nanopowders
was functionalized with acrylate groups by coating with a silane
coupling agent, vinyltriethylsilane (Sigma-Aldrich, USA), by
hydrolysis/condensation reactions [11]. Different-colored 3Y-ZrO2
ceramic nanocomposite resins were prepared by vigorously mixing
the 3Y-ZrO2 ceramic nanopowders with HDDA (Sigma, USA), a
photoinitiator—phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide
(BAPO, Sigma-Aldrich, USA), a dispersant—BYK111 (BYK, Ger-
many), and a non-reactive diluent—Bu (Sigma-Aldrich, USA). The
compositions of different-colored 3Y-ZrO2 ceramic nanocomposite
resins and the sample designations based on the main control fac-
tors are presented in Table 1.
The multicolor 3Y-ZrO2 ceramic nanocomposite resins were
additive-manufactured with a layer thickness of 50 lm by sup-
portless 3D printing using a 405 nm UV LED light (12.7 mW). To
minimize problems such as layer separation and cracking during
the sintering process [7], the green body was vacuum dried at
25 °C for 24 h, and then calcined by a three-step debinding process
at 300, 380, and 700 °C. Subsequently, the multicolored 3D-printed
3Y-ZrO2 objects were sintered at 1450 °C for 180 min.
The viscosities of different-colored 3Y-ZrO2 ceramic nanocom-
posite resins were measured at shear rates of 10–50 s 1 using a
rheometer (MCR-502, Anton Paar, Austria), and the photopolymer
properties were measured by photo-differential scanning
calorimetry (Photo-DSC 204 F1 Phoenix, NETZH) at a wavelength
of 355 nm. The flowability of the ceramic resins was evaluated
from the distance traveled by 1 g of resin in 10 min while moving
down a 60° slope. The UV-curing rheological properties (G‘‘ (loss
modulus), G’ (storage modulus), and tand (loss tangent)) of the
ceramic resins were analyzed using a rheometer with a UV acces-
sory in the small amplitude oscillatory shear mode at a frequency
of 10 Hz. The printability of the ceramic resins was determined by
a three-interval thixotropy test (3ITT) performed using a rheome-
ter [12–15]. During the 3ITT of the ceramic resins, the G’ and G”
were measured under three strain intervals of 0.1%, 2%–10%, and
0.1%, and the degree of structural deformation (De), relative solid-
ity (Rs), and degree of recovery to relative solidity (Recs) were cal-
culated [14,15]. The microstructures of the sintered bodies were
analyzed by field-emission scanning electron microscopy (FE-
SEM, JSM-6700F, JEOL), after polishing the surface of the sample
with #4000 grit sandpaper. The samples of circular disk-shaped
sintered bodies with a diameter of approximately 20 mm and a
thickness of approximately 2 mm were prepared, and then the
biaxial flexural strength of the sintered bodies was measured using
a universal testing machine (AG-X plus, Japan) according to ASTM
C1161-18 and ASTM C1239 standards. Multiple measurements
were made to determine the reproducibility, and the average of
five measurements was taken for the biaxial flexural strength.
3. Results and discussion
For supportless 3D printing, the viscosity of the highly loaded
3Y-ZrO2 ceramic nanocomposite resins should be in the range of
20,000–30,000 mPa
s at a shear rate of 15.8 s 1 [7,8]; therefore, a
solvent such as a non-reactive diluent needs be added to the
nanocomposite resins. However, since the added solvents nega-
tively affect the 3D printing process, a good solvent needs to be
selected for the monomers. Hansen solubility parameters, which
S. Hyun Ji, D. Sol Kim, M. Soo Park et al.
Table 1
Compositions and control factor-based designations of multicolor 3Y-ZrO2 ceramic nanocomposite resins.
Control factor Sample name 3Y-ZrO2 HDDA (vol%)
Color (vol%)
Bu content WB0 White 50 50
WB5
WB7.5
WB10
Color YB5 Yellow 50 50
PB5 Pink
GB7.5 Gray
define the relationship between the dispersion solubility parame-
ter (dd), polar solubility parameter (dp), and hydrogen-bonding sol-
ubility parameter (dh), are generally used to screen the appropriate
solvent and functional monomer for ceramic dispersion systems
[16]. For most common solvents and organic molecules, dd is sim-
ilar and therefore negligible, and dp and dh are defined by a single
parameter, a = (dp2 + dh2)0.5, which is the distance from the origin
in a 2D relationship graph of dp and dh. Fig. 1 shows the 2D relation-
ship graph of dp and dh for HDDA (dp = 3.1, dh = 7.9, a = 8.5), Bu
(dp = 5.1, dh = 12.3, a = 13.3), methanol (dp = 12.3, dh = 22.3,
a = 25.5), isopropyl alcohol (dp = 6.1, dh = 16.4, a = 17.5), and etha-
nol (dp = 6.1, dh = 19.4, a = 21.3) [16,17]. To improve the rheological
behavior of the ceramic nanocomposite resins, Bu, whose a is clos-
est to that of the HDDA monomer, was considered the most effec-
tive non-reactive diluent.
The rheological behavior, photo-curing properties, and print-
ability of the white 3Y-ZrO2 ceramic nanocomposite resins with a
ceramic content of 50 vol% were determined according to the Bu
content; the results are shown in Fig. 2. As can be seen from the
viscosity curves according to a shear rate of Fig. 2(a), the 3Y-ZrO2
nanocomposite resins are shear-thinning fluids. Furthermore, the
spreading characteristics of the 3Y-ZrO2 nanocomposite resins
improved with a decrease in viscosity owing to the increasing Bu
content, as shown in the inset images of Fig. 2(a). As determined
from the flowability test (Fig. 2(b)), the moving distance increased
with increasing Bu content, indicating improved flowability.
Although the viscosity and flowability of WB0 and WB5 are suit-
able for supportless 3D printing, the samples are difficult to apply
because of their poor spreading characteristics. In contrast, WB10
demonstrated the optimum spreading characteristics for support-
Fig. 1. 2D relationship graph of polar solubility parameter (dp) and H-bonding
solubility parameter (dh) for the UV-curable monomer (HDDA) and various solvents
[16,17].
3
Materials & Design 209 (2021) 109981
Bu BAPO (wt% of monomer) BYK111 (wt% of ceramic)
(vol% of monomer)
0 2 2
5
7.5
10
5 4 2
5 2
7.5
less 3D printing. However, its high flowability (moving distance
of over 2 mm) prevented its application in supportless 3D printing.
WB7.5 exhibited optimal rheological properties such as viscosity,
flowability, and spreading characteristics for supportless 3D print-
ing. Fig. 2(c) shows the heat flow curves of the ceramic nanocom-
posite resins. With increasing Bu content, the amount of
exothermic heat and the slope of the curve increased, which sug-
gests a slight increase in the photopolymerization degree and ini-
tial curing rate. In other words, since Bu is a good solvent for the
nanocomposite resin system consisting of HDDA, the rheological
and photo-curing properties improved with an increase in the Bu
content.
Fig. 2(d) shows the tand (G‘‘ (loss modulus)/G’ (storage modu-
lus)) curves of the ceramic nanocomposite resins with different
Bu contents cured by UV irradiation. The UV-curing rheological
properties of WB0 and WB5 were not measured because of their
high viscosity and poor spreading characteristics. Before UV irradi-
ation, WB7.5 and WB10 exhibited a solid-like behavior (G” < G’,
tand < 1), and the tand of WB10 was lower than that of WB7.5,
as inter-particle interactions tend to decrease at an excessively
high solvent content. Upon 10 s of UV irradiation, the resins began
to cure, and tand rapidly decreased due to an increase in solid-like
behavior. In particular, the curing rate of WB7.5 was higher than
that of WB10, which is consistent with the photo-DSC results (inset
in Fig. 2(c)). After UV irradiation, the tand value of WB7.5 became
almost constant, which indicates enhanced solid-like behavior and
stable rheological characteristics because of sufficient photopoly-
merization. In contrast, the tand value of WB10 increased, which
is possibly because of insufficient time (10 s) for photopolymeriza-
tion, and the uncured resins gradually began to exhibit liquid-like
behavior under shear stress. Bu, a hydrogen donor, leads to the for-
mation of radicals as a type II photoinitiator, which is usually
slower than a type I photoinitiator [18]. Thus, although the degree
of photopolymerization increased with increasing the amount of
Bu, the curing rate of WB10 with a high amount of Bu was slightly
lower than that of WB 7.5.
3ITT enables the evaluation of the response and recovery of a
material under stress when the polymer networks break over time
[12–14]. For the successful 3D printing of objects without any
structural deformation, the material of the 3D-printed layer must
recover before the next layer is 3D printed. Therefore, 3ITT was
performed to evaluate the printability of the ceramic nanocompos-
ite resins [15]. The De-Rs and De-Recs phase diagrams derived from
the 3ITT results of the 3Y-ZrO2 ceramic nanocomposite resins are
shown in Fig. 2(e) and 2(f), respectively. As can be seen from the
De-Rs phase diagram (Fig. 2(e)), with increasing De, the Rs of
WB7.5 decreased slightly, whereas the Rs of WB10 decreased sig-
nificantly. In other words, the flow behavior of WB10 was influ-
enced by the shear strain; this can affect the stability during the
3D printing process. The Recs of WB7.5 and WB10 exhibited similar
tendencies with increasing De (Fig. 2(f)) and indicated the strong
recovery and high durability of the internal network structures.
Thus, WB 7.5 possessed the optimum rheological properties for
S. Hyun Ji, D. Sol Kim, M. Soo Park et al. Materials & Design 209 (2021) 109981

Fig. 2. Properties of 3Y-ZrO2 ceramic nanocomposite resins with different Bu contents: (a) viscosity, (b) flowability, (c) heat flow, (d) tand, and (e) De-Rs and (f) De-Recs phase
diagrams to assess printability.

supportless 3D printing. The physical properties of pink, gray, and The rheological behaviors, photo-curing properties, and print-
yellow 3Y-ZrO2 ceramic nanocomposite resins were similarly ability of white, pink, gray, and yellow 3Y-ZrO2 ceramic nanocom-
optimized. posite resins with a ceramic content of 50 vol% were analyzed; the

4
S. Hyun Ji, D. Sol Kim, M. Soo Park et al. Materials & Design 209 (2021) 109981

results are shown in Fig. 3. Since a small amount of a ceramic dye
(rare-earth element) was added to the 3Y-ZrO2 ceramic powders,
the rheological behavior of the ceramic nanocomposite resin was
different for different colors. The viscosities of WB7.5, YB5, PB5,
and GB7.5 were controlled at approximately 20,000–30,000 mPa
s
at a shear rate of 15.8 s 1 by controlling the amount of Bu. As
shown in Fig. 3(a), with increasing shear rate, the viscosities of
the different-colored ceramic resins remained almost constant. In
addition, the moving distances of WB7.5, YB5, PB5, and GB7.5 ran-
ged up to 1 mm, which indicates the good flowability of the

Fig. 3. Characteristics of different-colored 3Y-ZrO2 ceramic nanocomposite resins: (a) viscosity, (b) flowability, (c) heat flow, (d) tand, and (e) De-Rs and (f) De-Recs phase
diagrams to assess printability.

5
S. Hyun Ji, D. Sol Kim, M. Soo Park et al.
Fig. 4. Characteristics of sintered bodies of different-colored ceramic resins: (a) FE-SEM images, (b) relative density and grain size, and (c) flexural strength.
different-colored ceramic resins for supportless 3D printing (Fig. 3
(b)). The enthalpy change (DH) values of WB7.5, YB5, PB5, and
GB7.5, as determined from the heat flow curves, were maintained
in the range of 70–72 J/g by adjusting the BAPO content; thus, the
different-colored resins exhibited similar photo-curing properties
(Fig. 3(c)). Furthermore, the different-colored ceramic resins exhib-
ited similar rheological behaviors during UV irradiation, as deter-
mined from their tand curves (Fig. 3(d)). After UV irradiation, the
tand values of the different-colored ceramic resins became almost
constant, and the sufficiently UV-cured resins exhibited stable rhe-
ological behaviors. The tand value of GB7.5 was slightly lower than
those of the other colored resins because of the relatively high
polymer-particle interaction caused by the presence of cobalt
oxide in the gray 3Y-ZrO2 ceramic particles, which resulted in
reduced molecular movement in the polymer matrix [19]. Further,
as can be seen from the De-Rs and De-Recs phase diagrams in Fig. 3
(e) and (f), WB7.5, YB5, PB5, and GB7.5 have excellent printability.
Among the different-colored resins, GB7.5 has the best printability
owing to a stable internal network structure due to the presence of
cobalt oxide [19]. In other words, during the 3D printing process,
the different-colored ceramic resins will be structurally stable with
very low possibility of structural collapse. Thus, all the different-
colored ceramic resins exhibited suitable rheological behavior,
Fig. 5. Optical images of 3D-printed objects before and after sintering: (a) disc-shaped objects of different colors and (b) gear-shaped objects with layers of different-colored
ceramic resins.
6
Materials & Design 209 (2021) 109981
photo-curing properties, and printability for supportless 3D
printing.
The 3D printed green bodies of different-colored 3Y-ZrO2 cera-
mic resins were sintered under previously optimized sintering con-
ditions to minimize defects [7]. As can be seen from the FE-SEM
images in Fig. 4(a), the sintered bodies of WB7.5, YB5, PB5, and
GB7.5 have well-grown grains and distinct grain boundaries with-
out any micropores between the grains. In addition, the sintered
bodies of all the different-colored ceramic resins had a high rela-
tive density of approximately 99.95% and a large grain size of
approximately 2.7 mm (Fig. 4(b)). Moreover, the flexural strengths
of WB7.5, PB5, YB5, and GB7.5 were 994.1, 962.3, 961.8, and
936.3 MPa, respectively (Fig. 4(c)), which are comparable to that
of ZpexÒ (1038 MPa) manufactured by the traditional method
[20]. The results indicate the absence of defects such as layer sep-
aration and cracking, which are frequently caused by internal
stress generated during the drying and debinding steps performed
to remove solvents, residues, and polymers. Thus, the sintering
process led to 3Y-ZrO2 grain growth without the formation of
voids, resulting in defect-free structures.
The optical images of disc-shaped different-colored 3D-printed
ceramic resin objects before and after sintering are shown in Fig. 5
(a). The sintered bodies of WB7.5, YB5, PB5, and GB7.5 exhibited
S. Hyun Ji, D. Sol Kim, M. Soo Park et al.
approximately 50% volume shrinkage. The RGB color codes of the
different-colored sintered bodies extracted from the optical images
and the hex color codes obtained by converting the RGB color
codes are as follows: #F6F6F6 (R: 246, G: 246, B: 246), #FAF4C0
(R: 250, G: 244, B: 192), #FFD9EB (R: 255, G: 217, B: 235) and
#B1B1B7 (R:177, G: 177, B: 183) for WB7.5, YB5, PB5, and GB7.5,
respectively. Fig. 5(b) shows the optical images of gear-shaped
multicolor 3D-printed objects manufactured with four differently
colored layers before and after sintering. The gear-shaped objects
were manufactured by continuous 3D printing and simultaneous
sintering. The teeth of the gear were printed and sintered at a high
resolution without any defects. The original color of each layer was
well-expressed, and no separation was observed between the col-
ored layers. To develop the SLA 3D printing technology for fine
ceramics, small-sized ceramic products such as honeycomb cata-
lysts and heat exchangers have been 3D printed [21,22]. However,
the continuous 3D printing of different materials on a single
machine and the simultaneous sintering of a 3D-printed object
with different layer have not been studied extensively. The results
suggest the possibility of continuous additive manufacturing and
the simultaneous sintering of different ceramic materials and are
expected to significantly contribute to expanding the industrial
market of ceramic 3D printing.
4. Conclusions
Highly loaded 3Y-ZrO2 ceramic nanocomposite resins of various
colors, (white, pink, yellow, and gray) were manufactured, and
their rheological behaviors were optimized according to the Bu
content to determine the composition with optimal properties
for supportless stereolithography 3D printing. The different-
colored 3D-printed 3Y-ZrO2 objects were vacuum dried at 25 °C,
calcined in three steps at 300, 380, and 700 °C, and finally sintered
at 1450 °C for 180 min. The sintered bodies of different-colored
ceramic resins exhibited a high relative density (>99.90%) and high
flexural strength (>930 MPa), which are comparable to those of
ZpexÒ manufactured by the conventional process. Furthermore,
gear-shaped objects with layers of different-colored ceramic resins
were successfully 3D printed and simultaneously sintered, which is
a new technology rarely reported in the ceramic 3D printing field.
This study paves the way for the development of an innovative
continuous 3D printing and simultaneous sintering technology,
which can expand the market for ceramic 3D printing.
Author Contributions
Sang Hyun Ji performed the fabrication and characterization of
the ceramic nanocomposite resins, processed the experimental
data, performed the analyses, and drafted the manuscript. Da Sol
Kim performed the fabrication and characterization of nanocom-
posite resins. Min Soo Park performed the 3D printing process
and analysis. Doojin Lee performed the rheological analysis. Ji
Sun Yun was involved in planning and supervised the work and
contributed to data interpretation and writing of this manuscript.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Materials & Design 209 (2021) 109981
Acknowledgements
This work was supported by the Industrial Fundamental Tech-
nology Development Program (20011779, Development of high
dispersion nanocomposite manufacture/processing technology
and quantitative dispersion analysis technology) funded by the
Ministry of Trade, Industry and Energy (MOTIE) of Korea.
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