Design and additive manufacturing of periodic ceramic architectures

Giovanni Bianchi*, Sandro Gianella ¥, Alberto Ortona*

¥ EngiCer Sa, Balerna, Switzerland

* MEMTI - SUPSI, Manno , Switzerland

Abstract
Cellular ceramics are attracting material solutions for high temperature applications because of their
outstanding effective properties. Even though ceramic foams are already widely industrially
employed, they show scattered properties because of their randomness and fragility. Moreover there
are few parameters which can be varied in order to engineer their properties.
We first show how, through finite element simulations, periodic cellular ceramics can be designed
upon user’s requirements.
Then, thanks to additive manufacturing (AM), the aforementioned numerical domains can be
readily transformed into physical objects. Among many AM techniques nowadays available, we
developed an original method in which polymeric lattices templates are produced by 3D printing,
further coated by replica with ceramic slurries and finally heat treated. The advantage of this
technique is its flexibility. Practically any ceramic material already produced in bulk form can be
realized.
We then present some case study where we were able to design and produce components for the
concentrated volumetric solar receivers, thermal protections for aerospace entry vehicles, and heat
exchangers.

Published on Journal of Ceramic Science and Technology (Göller Verlag GmbH)

1. Introduction
Porous ceramics are a category of hybrid materials composed by a ceramic constituent and empty
1
space usually filled by a gas. This material architecture confers to the resulting structure unique
property-to-density ratios 2. Indeed such material configurations are quite common in nature often
3
related to organic components. Examples of natural porous solids are bones, wood, sponges and
pumice stones produced during volcanic eruptions. Engineers have adopted these structures, made
4, 5
of different materials, in many applications such as: hot and cold filtering , noise reduction 6,
shock absorption 7, mechanical2 , thermal insulation5 and a wide range of high temperature
applications 8 some of them detailed in the following paragraphs.
In this paper we will focus on hybrid materials characterized by a continuous ceramic solid phase
and macro voids 9 more in particular, due to its outstanding high temperature properties, on macro
10 11, 12
porous SiC . Ceramic foams can be produced in several ways the principal methods are:
direct foaming, gelation-freezing, burn out of fugitive pore formers and, last but not list, replica of a
sacrificial plastic foam13. A plastic foam (usually polyurethane) is soaked into a slurry composed
by ceramic powders, plastic binders and solvents. Then the excess slurry is removed by squeezing.
The result is a green foam which has a layer of slurry around its struts. This green body is then
thermally treated (sintering for oxides) to obtain the final component. In the case of SiSiC, the body
is pyrolysed at 1000°C in inert atmosphere and then infiltrated with molten silicon in vacuum at
1500°C 14.
Slurry replica 13 of oxide ceramics is by far the most industrialized method, its huge development is
15, 16
due to the molten metals filtration for the metal casting industry . Millions of pieces are every
year used to filter different kind of metal alloys before their casting.
In applications such the one described before, the randomness of a ceramic foam architecture is a
huge advantage 17-19.

This very randomness could be, on the other hand, a limiting factor. The polyurethane foams used
as templates are deriving from a liquid phase in which, before its polymerization, gas bubbles of
different size are growing inside. Because of that, the struts, i.e. the skeleton of these foams, are
random in shape, length, distribution and orientation in the space (Figure 1). As a consequence, the
20
local properties of the porous body dramatically change along its volume. Foams’ properties are
thus calculated using homogenization techniques in which the selected volume has to be rather large
21-23
in terms of number of pores in order to be treated as a representative one . Moreover using

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homogenization techniques doesn’t account on the boundaries at which cells and struts are
interrupted by machining: this operation has an huge influence on the overall properties of the
macro porous ceramic component with a discrete volume 24, 25 (Figure 1).

Figure 1 Stress distribution (blue low, red high) from the FEM analysis of a random foam under
compression (left)23 and bending (right) 26.

According to users’ requirements, to be fully reliable, macro porous ceramics components should
be realized as structures with a repeatable architecture.
With random foams this is impossible.
Another issue in random ceramic foams is the shape of their struts; this has huge consequences in
23
foams’ mechanical properties . Replica is accomplished employing polyurethane foams which,
because of their manufacturing process 5, have their struts with piercing corners. At the end of the
process each ceramic strut presents an hollow shape with sharp corners imposed by the former
polyurethane foam. Sharp corners act as notches from where, under mechanical or thermal loading,
a crack can easily propagate (Figure 2) 27.

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Figure 2 Crack propagating from the sharp corner of an hollow strut produced by replica of a
polyurethane foam

All these issues could be solved if a periodic cellular architecture with smooth, regular and
interconnected struts would exist.
This need was met with the advent of additive manufacturing.
Additive manufacturing or 3D printing is a near to net shape production technique developed
several years ago which allows the assembly of a material starting from a CAD model. The main
advantage of this technique is that it can allow the direct production of components whose shape is
impossible to realize with the conventional manufacturing methods. This is especially true for
porous materials. Presently this technique is industrially mature for metallic and plastic materials
while it is still in a development phase for ceramics. Our idea was thus to combine plastic AM, the
most mature, with replica 28.
The following paragraphs of this paper will describe how CAD files of cellular architectures are
generated and how they can be converted into ceramic objects. Finally some application in different
industrial fields will be reviewed.

2. CAD lattice generation

Lattice structures can increase the properties of a porous material by orders of magnitudes 1, 29. The
repetitive unit cell of these structures (Figure 3) can be designed from topological studies
(tetrakaidecahedron), inspired from crystallography (octet) , or developed on porpoise (Gibson and
Ashby cell) 2.

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Figure 3 Different unit cells and the relevant lattices obtained by CAD modelling

One can immediately see in Figure 3 that the first two structures already solved the problem of
having unconnected struts (Figure 1), this feature rises the mechanical properties of the resulting
20
structures . The next advantage is that the struts can be designed to overcome the problems
highlighted in the introduction 22, 27, 30. We tested several strut’s shapes, but the easiest solution is to
assign to the strut a cylindrical shape which will be, depending on the following transformation
technique, a tube or a solid bar. If for any reason the cell chosen doesn’t allow to have unconnected
external struts, we developed a software tool which cuts the numerical domain while keeping the
struts connected (Figure 4). To do this, solid lattices were made and cut in desired form (Figure 4,

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left). NX (Siemens, Munich, D) application-programming interface (API) was used together with a
MATLAB script (The Mathworks, Inc., Natick, MA) to convert all the nodes and edges into spheres
and cylinders. (Figure 4, right)

Figure 4 Numerically solving the problem of unconnected struts in a rotated cube configuration
adapted to fit a cylindrical volume (Ehsan Rezaei’s PhD thesis - ongoin).

If the problem is to fit a given volume with cells allowing cells’ distortion, another MATLAB script
can solve it (Figure 5). This code receives a meshed structure as the input and converts the structure
into any of tetrakaidecahedron, cubic or octet lattice. This code basically can be further developed
for any cell type, which can fit into a hexahedron.

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Figure 5 A numerical way to mesh with a given unit cell (a tetrakaidecahedron in this case) a
specific volume (Ehsan Rezaei’s PhD thesis - ongoin).

Once the numerical model has been designed, it can be utilized to simulate its behaviour in different
applications. Mechanical, thermal, fluid dynamic, electromagnetic simulations have been used to
optimize the performance of a porous component 17, 20, 22, 23, 25, 30-32.

3. Additive manufacturing of period cellular architectures

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Figure 6 A representation of the two AM processes described in this paper sketching the evolution
of a generic strut cross section. Aside there are corresponding pictures of real samples. On the left
a SiSiC Weaire–Phelan structure obtained by the replica of a 3D printed plastic template. On the
right the production steps of an Al2O3 periodic architecture obtained by 3D printing a slurry.

33, 34
There are several methods to build a porous ceramic architecture by AM . Two different
techniques were utilized in this work to transform a CAD file into a ceramic periodic cellular
architecture . They can be both considered as two step manufacturing methods, in the sense that 3D
printing was utilized to produce green bodies which were subsequently thermally treated to
transform them into ceramics. We are studying these two techniques because they are
complimentary in terms of printing volume capability, resolution and ceramic powder choice.

3.1. 3D printing and replica

A plastic periodic architecture is 3D printed by stereolithography and then used as template for a
following replica process (Figure 6 left) 13.

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This simple method allows the production of virtually any pore architecture with different slurries
28
and thus different final ceramic material . SiSiC ceramics were produced by molten silicon
infiltration of carbon bonded SiC particles but, as an example, also graphite based architectures can
35
be produced . For details regarding materials and methods this technique we encourage the
interested reader to go through our previous work 28.
The advantages of this method are that large bodies can be realized, the material which is added by
replica wraps the sacrificial template conferring higher mechanical properties to the final porous
architecture 11, 28 and finally the surface of the ceramic end product is very smooth.
Drawbacks are also present and will be hereunder described.
There are dimensional deviations of the strut shape from the nominal CAD file due to the replica
deposition phase which is gravity dependant because of the slurry viscous movements before its
consolidation. Slurry viscosity is the cause of probably the biggest disadvantage of this technique:
due to its high values (because of the high solid loading) small windows, and thus small cells, will
be occluded. Since one feature of a porous body in several applications is its large surface area
(which is exponentially increasing with the decreasing the cell size) this technique cannot be
applied to produce porous bodies with surface area bigger than 2000 m2·m-3.
A peculiarity of the replica process, which can be considered as an advantage or ad disadvantage
depending on the application, is that ceramic struts are hollow due to disappearing of the polymeric
template upon pyrolysis.

3.2. Stereolithography
The slurry receipt comprises photo polymeric resin TPGDA (Allnex, Luxenburg, Luxenburg)
mixed with ceramic powders (av. Diameter 2 m) 42 vol% (Nabaltec, Schwandorf, Germany) and
UV Photoinitiator: Irgacure 819 1.2 wt% (BASF, Ludwigshafen, Germany). Slurry was thoroughly
36
mixed by ball mixing for 24h with zirconia balls D=8.5mm, 30 vol%. . The green cellular
architectures were then built layer by layer (Figure 6 right) projecting with UV light a sequence of
images with a dark background obtained by slicing the CAD file of the object. Printing was
performed with a 3DL Printer – HD 2.0 (Robot Factory, Mirano, Italy). Parameters were set as
following: slice thickness: 0.05 mm, slice exposure time: 1.1 s. This technique is well suited to
produce porous bodies because, when slicing them, the projected area to be cured at each shot is
confined in small regions. A well cured, monomer-free slurry with highly packed and well
37-39
dispersed powders will result in a more dense layer-less bulk ceramic after sintering . 3D
printing large bulk ceramics with low surface-area-to-volume ratio (e.g. a sphere) is indeed the most

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challenging goal at the present time. The advantages of this technique are: final geometries
(provided that the distortions upon sintering are limited) do adhere to their nominal CAD ones,
small features can be printed (the present resolution is in the range of tens of microns) and thus
small struts and consequently cells can be realized, the process is completed in two steps.
Disadvantages are the followings. After slicing the CAD file, this technique selectively cures
regions of the slurry by projecting UV light on it. Once one slice is cured, the system moves ahead
and a new layer is printed on top of the previous one. This step-wise production method limits the
accuracy in reproducing tilted objects because slices’ thickness cannot be infinitesimal. The result is
the so called stair-casing effect (Figure 6 right) where printed objects present an zig-zag surface. In
ceramic materials this phenomenon can be highly detrimental under load because it acts as a notch
40
and thus as stress concentration points. This issue has been recently solved for plastic AM .
Printing area and printing time are two other technological issues which will be solved as the
knowledge in this techniques increases. The biggest limitation is that not all the powders can be
employed to make a UV curable slurry. Slurries with several ceramic powders are not UV curable
simply because they reflect or absorb the UV radiation. In our work we used Al2O3 which is easy to
print.

4. Applications
The following paragraphs shortly present some application of periodic cellular architectures for
high temperature, harsh working conditions. They are the outcome of research projects whose
results can be disclosed. Other applications, developed under an agreement of non-disclosure, will
be omitted.

4.1. Porous burner

The porous burner used in this work is based on the stabilization of the combustion process within
19
a porous medium where a flameless combustion takes places in its empty spaces . Si-SiC porous
architectures are fundamentals components for flame stabilization technology, because they can
guarantee the system functionality in oxidative conditions at high temperatures (~ 1400 °C) for
41
several thousand hours . With the use of Si-SiC lattice it is possible to further stabilize the flame
having a better temperature uniformity (Figure 7).

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Figure 7 A lattice glowing at ~ 1400°C on a CH4/air porous burner 42.

In industrial application with SiSiC ceramic foams the power is mostly limited to 1 MW/m2 , with
SiSiC cellular ceramics made of periodic architectures output power can be increased. Furthermore
the major improvement of this solution over the random foams is during the transient regime of
switching ON and OFF the burner. Rapid heating and cooling will lead to lower local failures
because of thermal shock. As a consequence, the problem of local stress concentration because of
the weaker struts into a foam (Figure 1) is clearly reduced.

4.2. TPS
Innovative thermal protection solutions (TPS) for space vehicles entering planets’ atmospheres
43
were developed within the FP7 European research project THOR (www. http://thor-space.eu/) .
44
One of them was exploiting a sandwich structured ceramic matrix composite with its core
working as active cooling system (Figure 8). A prototypic leading edge for plasma wind tunnel
tests was designed, its core, made of ad hoc cellular ceramics, was realized by AM and joined to
CMC skins 45.

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Figure 8 Top: Cooling gasses flow simulation inside the leading edge. The colour bar shows the
static temperature [K] on the leading edge surface according to this flow path. Bottom: the cellular
architecture developed for the active TPS solution above.

Following an extensive test campaign active cooling TPS proved to be an effective way to lower
outside temperatures of re-entry vehicles’ hottest parts31.

4.3. Catalytic supports

A lattice with rotated cubes as unit cell (Figure 9) was developed within the FP7 BioRobur
European research project (http://www.biorobur.org/).

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Figure 9 One slice (20 mm thick, 250 mm diameter) of a SiSIC periodic architecture based on a
rotated cube cell top right.

The BioRobur project focused on green hydrogen production by direct biogas auto thermal
reforming (ATR). The novelty is based on the use of period architectures as catalyst support for the
ATR reaction. ATR was favored by the ability of SiSiC periodic cellular materials to disperse the
heat axially in the reactor 46, 47.

4.4. Heat exchange

Tubular Si-infiltrated SiCf/SiCm composites with a periodic architecture inside were fabricated by
the electrophoretic deposition of matrix phases followed by Si-infiltration for concentrated solar
receiver applications 48, 49. Cellular ceramics were produced by the above mentioned method.
Results show that, by using engineered porous architectures such as cubic cells inside a tube (Figure
10), the heat transfer performance in operative conditions increased ~ 4 times in respect of a hollow
tube 50.

Figure 10 Top: the solution adopted enhance heat exchange with engineered porous architectures.
Bottom: Camera view of the inside of the tube during preliminary tests in a high temperature

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experimental apparatus. The image shows the inlet of the tube with an air mass flow of 5 g·sec-1
while the outer tube walls are kept at 1280°C

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5. Conclusions
Ceramic foams are nowadays employed in several industrial fields. These porous architectures
show several limitations in high tech applications where materials have to be engineered. These
limitations consist in the lack of design ability and local properties variations because of foam’s
randomness. These problems were overcome with the advent of ceramic AM. Thanks to this near to
net shape technique periodic cellular ceramics can be deigned, their performances simulated and
finally produced close to their nominal dimensions. This paper shows the outcome of a long-term
research work in this field, dedicated to the complete production cycle of these architectures.

6. Acknowledgements
This work is the result of the effort of several people who were hard working on the topic in the last
years. We would like to thank them one by one:
Simone Pusterla , Claudio D’Angelo and Ehsan Rezaei for CAD models generation and thermo
mechanical simulations, prof. Maurizio Barbato and Luca Ferrari for thermo fluid dynamic
simulations, Oscar Santoliquido for the Al2O3 lattices manufacturing.

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