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Additive Manufacturing 14 (2014) 110118

Light curing strategies for lithography-based additive manufacturing of

customized ceramics
Gerald Mitteramskogler a, , Robert Gmeiner a , Ruth Felzmann a , Simon Gruber b ,
Christoph Hofstetter a , Jrgen Stampfl a , Jrg Ebert c , Wolfgang Wachter c , Jrgen Laubersheimer c
a

Christian Doppler Laboratory for Photopolymers in Digital and Restorative Dentistry, Vienna University of Technology, Favoritenstrasse 9, 1040 Vienna, Austria
b Institute of Materials Science and Technology, Vienna University of Technology, Favoritenstrasse 9-11/E308, 1040 Vienna, Austria
c Ivoclar Vivadent AG, Bendererstrasse 2, 9494 Schaan, Liechtenstein
Available online 8 September 2014

Abstract
Lithography-based additive manufacturing (AM) is increasingly becoming the technology of choice for the small series or single unit production.
At the TU Vienna a digital light processing (DLP) system was developed for the fabrication of complex technical ceramics, requiring high levels
of detail and accuracy. The DLP-system used in this study creates a ceramic green part by stacking up layers of a photo-curable resin with a solid
loading of around 45 vol.% zirconia. After a thermal debinding and sintering step the part turns into a dense ceramic and gains its final properties.
The native resolution of the DLP process depends on the light engines DMD (digital mirror device) chip and the optics employed. Currently it
is possible to print 3D-structures with a spatial resolution down to 40 m. A modification of the light source allows for the customization of the
light curing strategy for each pixel of the exposed layers. This work presents methods to improve the geometrical accuracy as well as the structural
properties of the final 3D-printed ceramic part by using the full capabilities of the light source. On the one hand, the feasibility to control the
dimensional overgrowth to gain resolution below the native resolution of the light enginea sub-pixel resolutionwas evaluated. Overgrowth
occurs due to light scattering and was found to be sensitive to both exposure time and exposed area. On the other hand, different light curing
strategies (LCSs) and depths of cure (Cd ) were used for the 3D-printing of ceramic green parts and their influence on cracks in the final ceramic
was evaluated. It was concluded that softstart LCSs, as well as higher values for Cd , reduce cracks in the final ceramic. Applying these findings
within the 3D-printing process may be another step toward flawless and highly accurate ceramic parts.
2014 Published by Elsevier B.V.
Keywords: Additive manufacturing; Ceramic; Zirconia; Photopolymerization; Digital light processing

1. Introduction
Additive manufacturing (AM) technologies allow for the
resource-efficient fabrication of highly complex structures on
a layer-by-layer basis directly from 3D data [1]. For engineering applications, AMTs are used to produce near net-shaped
parts made of materials including unfilled polymers, metals or
ceramics. For the shaping of high strength oxide ceramics in particular, the most commonly used AM technologies are: fused

Corresponding author. +43 15880130857.

E-mail address: gerald.mitteramskogler@tuwien.ac.at
(G. Mitteramskogler).
http://dx.doi.org/10.1016/j.addma.2014.08.003
2214-8604/ 2014 Published by Elsevier B.V.

deposition modeling (FDM), selective laser sintering/melting

(SLS/SLM), laser engineered net shaping (LENSTM ), 3D
printing (3DP), direct ink writing (DIP), laminated object manufacturing (LOM), stereolithography (SLA), and digital light
processing (DLP) [2,3]. Table 1 briefly describes the mentioned
AM technologies and lists process-inherent assets and drawbacks. This review is based on recent literature and reflects the
authors opinions.
Using photochemical reactions triggered by light for the
shaping of a part, instead of thermal energy (SLS, SLM) or a
binder system (3DP), the photopolymerization-based technologies (SLA, DLP) offer several benefits in cases where a higher
feature resolution and surface quality are required. A solid part
is created on a layer-by-layer basis by photopolymerization of a
suspension of ceramic particles in a photosensitive resin. SLA

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111

Table 1
Survey of AM technologies for the manufacturing of structural ceramics; legend to symbols: + good, o average, poor.
Resolution

Surface
quality

Build
speed

Postprocessing

Production
costs

Mech.
properties

Process description

References

FDM

[18,19]

SLM SLS

LENSTM

3DP

DIP

LOM

SL DLP

Extruder and nozzle based

deposition system with a
thermoplastic
ceramicpolymer material
High power laser fuses a
polymerceramic composite
or directly sinters a ceramic
powder
Ceramic powder directly
injected into molten pool
created by high power laser
3D-jetting of organic blinder
on a ceramic powder bed
Direct ink-jet printing of a
ceramic containing ink
Placing of layers of a laser cut
ceramic green tape
Photocuring of ceramic
containing resin by a laser
light source or a LED

uses a laser scanner to cure thin lines of slurry and draw the crosssection of the part, whereas the DLP-system cures the whole
layer at once using a light mask, which is dynamically created
by a digital micromirror device. The state of the art for DLP systems are constant parameter light curing strategies (LCS), that
allow the operator to choose the light intensity (mW/cm2 ) and
the exposure time (s) depending on the polymerization characteristics of the slurry. After one layer is completed, a fresh layer
of slurry is coated and the process is repeated until the so-called
green part is built. Different to SLS, where the ceramic particles are shaped and sintered in one step, a green part built with
SL requires a thermal treatmentincluding a binder burnout
(debinding) and sintering stepto achieve a dense ceramic part
(Figs. 1 and 2).
Debinding rates need to be carefully adjusted to the volume
of the green part in order to avoid cracks in the final structure.
Besides a temperature treatment that is too fast, the fabrication
parameters of the green part could influence cracks in the final
structure. Bae and Halloran [4] showed in a study the influence of
fabrication parameters of a green part made by SLA on cracks in
the final ceramic. They conclude that residual monomer in gaps
in the light-curing pattern of the laser beam leads to cracks in

Fig. 1. Parts made of Al2 O3 fabricated by using the DLP-based 3D printing

technology presented in this paper.

[20,21]

[22]

[19]
[23,24]
[25,26]
[6,27]

the structure during thermal debinding. Rather than on flawless

debinding and sintering of green parts, most literature dealing
with ceramic SLA or DLP-systems focuses on the measurement
and calculation of the photopolymerization properties of slurry
compositions [57].
In the present work, we are the first to use a DLP-process
described by Rohner et al. [8] to test the influence of light curing parameters on cracks after debinding. On the one hand we
evaluate the influence of depth of cure (Cd )the polymerized
thickness of the slurry when light curing of a layeron cracks.
On the other hand, we test different light curing strategies
(LCS) used to minimize shrinkage strains from photopolymerization on their influence of cracks after debinding. LCS
to minimize shrinkage strains caused by photopolymerization
are known in the field of dental composites, exhibiting similar polymerization kinetics as ceramic slurries used for SL.
Shrinkage strains originate from the conversion of C C double
bonds, where the larger van der Waals inter-molecular spacing
is replaced by the smaller intramolecular covalent bonds [9].
Literature on dental composites explains shrinkage strains to be
one limiting factor for the performance of dental restorations
[1012]. One way to reduce the inherent shrinkage is by using
softstart LCS [1315]. Dewaele et al. [16] explain the reaction
kinetics of a softstart polymerization. A lower initial intensity
creates fewer polymerization centers and a more linear, less brittle polymer network. By delaying the gel-point before final high
intensity curing, the material is given the ability to accommodate viscous flow before the rigid network is created and thus
lowering shrinkage strains.
The utilized DLP-system projects images used for light curing of a layer at a native resolution of 40 m. In this work
we show that it is possible to improve the geometrical resolution of the green part without changing the projection optics,
reducing the overall building size of the 3D printer. In turbid

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Fig. 2. Green parts (a), sintered parts (b), and a cellular structure [28] made of ZrO2 (c) fabricated by using the DLP-based technology presented in this paper.

slurries, the light-cured geometry grows beyond the intentionally

exposed image by scatter light (overgrowth) that originates at the
resinparticle interface due to the materials different refractive
indexes [17]. We show that an exact control of the overgrowth
allows for a green part resolution below the native resolution of
the DLP-system, defined as the sub-pixel resolution.
2. Materials and methods
2.1. Ceramic DLP-system and customized LCS
The ceramic DLP-system (Fig. 3) is equipped with a special
coating deviceconsisting of a rotating mechanism and a coating bladeenabling the processing of highly viscous ceramic
slurries. The coating device provides a fresh layer of slurry and
the DLP-system selectively exposes the slurry to light at 460 nm
wavelength to initiate a radical photopolymerization. The DLPsystem adds the layers to fabricate the green part and typical layer
thicknesses range from 15 m to 100 m. A digital micromirror device (DMD) dynamically generates the images used for

light curing. The micromirrors reflect the light either toward the
material vat (on) or away from it onto a light absorber (off) to
create light or dark pixels. The DLP-system allows for the fabrication of green parts at an x/y resolution of 40 m. The size of
the building platform is 76.8 mm 43.2 mm. A binary bitmap
transfers the geometrical information of a layer to the DLPsystem and a sequence file determines the order and timing in
which the image is to be displayed and hence enables grayscales
of the image. When the micromirrors of the DMD are switched
on more frequently than off, the image appears to be brighter
(higher intensity). When the micromirrors are switched off more
frequently than on, the image appears to be darker (lower intensity). With a combination of multiple images and a sequence
file, grayscales for every single pixel of the exposed layer could
be created. The creation of the images and the sequence file
was performed in MATLAB (R2011b, The Mathworks Inc.,
MA). A standard pulse width modulation (PWM) algorithm was
used to convert an analog light intensity curve to a digital (on,
off) signal for the light engine. Sampling rates for the PWM
ranged from 20 Hz to 100 Hz, depending on the length of the
LCS.
2.2. Ceramic lled photocurable slurry

Fig. 3. Principle of the ceramic DLP-system by Gruber et al. (2011).

A photo-reactive suspension (slurry) was prepared based

on commercially available di- and monofunctional methacrylates. The slurry was a blend of 0.05 wt% of a highly reactive
photoinitiator, 2 wt% of a dispersant, an absorber, and 10 wt%
of a non-reactive diluent. A solid loading of zirconia powder
(TZ-3YS-E, Tosoh, Japan) up to 45 vol% was achieved. A homogeneous mixture was prepared by using a SpeedMixerTM DAC
150 FVZ (Hauschild, Hamn, Germany). The SpeedMixerTM is
based on the double rotation of the mixing cup (dual asymmetric centrifuge). Both the organic and the ceramic powder
were added in the cup and the mixing parameters were 2 min at
3500 rpm. The viscosity of the ceramic slurry was in the range
of 15 Pa s.

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113

gauge. To further investigate the influence of oxygen inhibition on Cd , the slurry was degassed under vacuum prior to the
investigation.
2.5. Inuence of LCS and Cd on cracks after thermal
treatment

Fig. 4. Overlays of the exposed test patterns (marked pixels) and the light cured
samples for the outside case (a) and the inside case (b).

2.3. Measuring geometrical overgrowth

Light scattering effects cause the curing of a larger area than
originally exposed by the DLP-system. The overgrowth was
defined as the originally exposed length subtracted from the
actually measured length. Fig. 4 shows overlays of the originally exposed images and the cured and cleaned samples for the
outside case (a) and the inside case (b). For the experiments,
the light intensity of the exposed pixels was kept constant at
13 mW/cm2 and the influence of exposure time (0.83.2 s) and
totally exposed area (0.163.96 mm side length) on the amount
of overgrowth was evaluated. For the inside case, the opening
side length was kept constant at 0.36 mm. After exposure of the
slurry the cured samples were cleaned and the respective dimensions were measured under a light microscope. The images were
evaluated using an image analysis software (ImageJ, National
Institutes of Health, USA).

As a testing geometry, cylindrical green parts of 10 mm in

diameter and height were fabricated using a layer thicknesses of
25 m. The reference parts were fabricated using a constant LCS
at 13 mW/cm2 light intensity and 1.5 s exposure time, yielding
a measured Cd of around 100 m. To evaluate the influence of
LCS on cracks after thermal treatment, we used constant (reference), exponential (exp 1, exp 2), and a softstart (softstart 1,
softstart 2) LCS to fabricate green parts (Fig. 5). To evaluate
the influence of Cd on cracks after thermal treatment, we fabricated green parts with the mentioned LCS at a Cd of 75 m and
150 m. To achieve different values for Cd the high-intensity
exposure times were varied accordingly. At least two cylinders
were fabricated for each group and qualitatively compared with
the reference.
2.6. Thermal analysis
After fabrication, the dimensional change of the green parts
with respect to an increase in temperature was analyzed using
thermomechanical analysis (TMA), 2940 Fa. TA-Instruments.
The samples were heated up from room temperature to 400 C
with a heating rate of 0.1 K/min. We evaluated the dimensional
change for the LCS (softstart and constant) and the different
values for Cd (75 m and 150 m) we used to fabricate the
green parts.

2.4. Measuring depth of cure (Cd )

We measured Cd for the given slurry at light intensities up
to 13 mW/cm2 and exposure times ranging from 0.5 s to 12 s.
The slurry was placed in a tray on top of the material vat at
a filling height of 1 mm and leveled with a blade. Circles of
10 mm in diameter were exposed and subsequently cleaned by
removing the excess slurry. Cd was measured with a micrometer

2.7. Thermal treatment

Fig. 6 shows the thermal treatment used in this study for
drying, debinding and the final sintering of the parts. Prior to this
study, TMA measurements were used to adjust the temperature
profile to the geometry of the green part.

Fig. 5. Exponential (exp(x) 1, exp(x) 2) and soft start (softstart 1, softstart 2) LCS compared to constant curing (reference). 100% light intensity equals 13 mW/cm2 .

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Fig. 6. Thermal treatment (drying, debinding, and sintering).

3. Results and discussion

3.1. Geometrical overgrowth
Figs. 7 and 8 show the measured overgrowth for the outside and the inside case calculated by subtracting the originally
exposed length by the actually measured length. At a given
light intensity of 13 mW/cm2 the overgrowth increases with both
exposure time and exposed area. For the outside case, light scattering causes the actual length to be higher than the original
length. For the inside case, it causes the actual length to be
smaller than the original length or even leads to a complete
closure of the opening. A peak could be observed for both the
outside and inside cases at 2 mm and at 4 mm side length, respectively. The higher amount of overgrowth for the inside case could
be explained by the larger amount of surface surrounding the
inner opening.
3.2. Depth of cure (Cd )
For the given slurry, an increase in exposure time causes an
increase in Cd , which is converging to a maximum value depending on the light intensity applied (Fig. 9). For the reference curing

parameters of 13 mW/cm2 light intensity and 1.5 s exposure

time, a Cd of around 100 m could be measured. The iso-energy
lines show that Cd is not linear with respect to the overall energy
applied but higher intensities are favored for increased Cd . To
evaluate the influence of oxygen inhibition, Cd was measured
for a degassed slurry and about three times greater values for Cd
could be observed (Fig. 10).
3.3. Inuence of LCS and Cd on cracks after debinding
Due to a certain level of translucency of the dense zirconia,
cracks within the sintered ceramic can be visualized by raying with visible light. The side view (a) and top view (b) of
a sintered reference specimen in front of a light source show
prominent horizontal and vertical cracks (Fig. 11). The horizontal cracks do not entirely follow the layerwise orientation
and therefore might not originate from delamination issues during 3D-printing. The horizontal crack patterns instead show
a stepwise crack propagation between the layers. Due to sintering of the loosely packed powder to a compact ceramic, a
dimensional shrinkage of around 20% occurred. Fig. 12 shows
light microscopy images of the rayed ceramic cylinders fabricated with the LCS presented aboveyielding a Cd of 100 m.

Fig. 7. Overgrowth of the outside length as a function of rectangle side length and exposure duration.

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115

Fig. 8. Overgrowth of the inside length as a function of side length and exposure duration.

Fig. 9. Measured Cd for different light curing parameters. The solid lines represent the results for the same intensity (iso-intensity); the dashed lines show the same
level of energy dose (iso-energy).

Using the shorter exponential LCS exp(x) 1 showed no clear

reduction of cracks compared with the reference constant LCS
(Fig. 12(a)). Longer times for the initial intensity increase
(exp(x) 2) prevented vertical cracks and led to only minor

horizontal cracks (Fig. 12(b)). Cylinders fabricated with the softstart LCS showed no vertical cracks and only smaller horizontal
cracks. The fewest cracks were observed for the LCS softstart 2
(Fig. 12(d)).

Fig. 10. Cd for degassed (dashed lines) and regular (solid lines) slurry.

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Fig. 11. Side view (a) and top view (b) of a sintered reference cylinder built with a constant light intensity curing protocol at 13 mW/cm2 light intensity and 1.5 s
exposure duration; lines mark the cracks visible within the ceramic.

To evaluate the influence of Cd on cracks after debinding, we

varied the high intensity curing time from originally 1.5 s to 0.8 s
and 2.5 s, yielding values for Cd of 75 m and 150 m respectively. At the same layer thickness of 25 m, cylinders fabricated
at a Cd of 75 m again showed structural cracks similar to the
reference part shown above. Using a Cd of 150 m and the constant LCS it was not possible to achieve flawless ceramics. The
combination of the softstart LCS and a Cd of 150 m resulted
in flawless specimens as seen in Fig. 13.

The curing of layer with the presented LCS softstart 2 can be

regarded as a double light exposure approach. The initial softer
polymerization at 1.3 mW/cm2 for 10 s allows for a certain level
of viscous flow of the slurry before the gel-point is reached.
A further reduction of shrinkage stresses might be achieved by
using even lower softstart intensities. As a drawback, the curing
of the layers turns into a time consuming process, since lower
light intensities require longer light exposure times for similar
curing results. The high-intensity light exposure at 13 mW/cm2

Fig. 12. Sintered specimens fabricated with exponential LCS exp(x) 1 (a) and exp(x) 2 (b) and softstart LCS softstart 1 (c) and softstart 2 (d). Lines of crack
propagation are highlighted.

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117

3.4. Inuence LCS and Cd on structural and thermal

properties

Fig. 13. Flawless cylindrical part fabricated with the LCS softstart 2 and a Cd
of 150 m.

for 2.5 s completes the curing of the slurry and ensures the bonding to the previous layer. We have concluded that a higher depth
of cure increases the bonding of the layers and improves the
structural properties of the final ceramic part.

We analyzed the fracture surface of green parts fabricated at

a Cd of 75 m and 150 m using scanning electron microscopy
(SEM) imaging. At a Cd of 75 m the fracture surface shows
signs of the layered manufacturing route (Fig. 14(a)). At a Cd
of 150 m the green structure seems homogeneous (Fig. 14(b)),
which might indicate improved interlaminar bonding of the single layers.
Thermomechanical analysis (TMA) of green parts with 4 mm
in diameter and height revealed a difference in dimensional
change over temperature. The dimensional shrinkage of the
green part is associated with evaporation of the diluent and pyrolysis of the organic. The escaping gaseous products pass through
the mesh of ceramic particles and the remaining polymer network. At higher temperature rates, trapped debinding gasses lead
to an increase in internal pressure of the green part visible as an
expansion in the TMA measurement. Using TMA, cracks during debinding of the green part can be seen as a peak in the rate
of shrinkage. Specimens fabricated with a softstart LCS showed
increased shrinkage compared with the specimens fabricated
with the constant LCS, see Fig. 15. The temperature at which a
major mass loss begins shifted to a higher temperature for the

Fig. 14. SEM micrographs of fracture surfaces of green parts fabricated at a Cd of 75 m (a) and 150 m (b).

Fig. 15. Result of TMA measurements. The samples were heated up to 400 C at a heating rate of 0.1 K/min.

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specimens at 150 m. This might be explained by a more rigid

network caused by longer exposure times, which increase the
activation energy needed for the evaporation of the diluent. The
higher amount of total shrinkage for parts fabricated with the
softstart LCS may be explained by a more rigid network after
photopolymerization, which causes higher levels of shrinkage
during the drying of the part.
4. Conclusion
This work presents a modification of a special DLP-system
used for the 3D-printing of ceramic green parts in order to
improve the geometrical accuracy, as well as the structural properties of the final structural ceramic part after debinding and
sintering. We found that light scattering within the ceramic filled
slurry causes a certain amount of widening of dimensions in
the final geometry and that this overgrowth is both sensitive
regarding overall exposure area and exposure time. We concluded that softstart LCS and higher values for Cd are preferred
for the successful thermal processing of a 3D-printed green part.
Softstart LCS are applied to reduce internal stresses originating from photopolymerization, whereas higher values for Cd
improve the interlaminar bonding of the layers.
To implement these findings in the DLP-system, the image
used for light curing of a layer could be split into a core image and
a contour image, which are light cured consecutively. At a certain
width of the contour the amount of overgrowth could be controlled by the light exposure duration. This approach achieves
a resolution below the spatial resolution of the DLP-system,
defined as sub-pixel resolution, without a loss in overall building
size. Besides the time-controlled curing of the contour images,
the core image of a layer could be light-cured with the presented
softstart LCS to improve the structural properties of the final
ceramic part.
Acknowledgments
The research presented in this paper was conducted at the
Technical University of Vienna. We gratefully acknowledge the
financial support from the Christian Doppler Laboratory for
Photopolymers in Digital and Restorative Dentistry and Ivoclar
Vivadent AG (Liechtenstein).
Appendix A. Supplementary data
Supplementary data associated with this article can be found,
in the online version, at doi:10.1016/j.addma.2014.08.003.
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