Suplemento de la Revista Latinoamericana de Metalurgia y Materiales 2009; S1 (1): 353-363

DESIGN AND FABRICATION OF CELLULAR GLASS CERAMIC STRUCTURES FOR

FILTERING COMBUSTION GASES OF DIESEL ENGINES

A. Sarmiento1*, A.M. Montes1, D. Hotza2, A.P. Novaes de Oliveira2, J.A Escobar1

9 Este artículo forma parte del “Volumen Suplemento” S1 de la Revista Latinoamericana de Metalurgia y Materiales
(RLMM). Los suplementos de la RLMM son números especiales de la revista dedicados a publicar memorias de
congresos.

9 Este suplemento constituye las memorias del congreso “X Iberoamericano de Metalurgia y Materiales (X
IBEROMET)” celebrado en Cartagena, Colombia, del 13 al 17 de Octubre de 2008.

9 La selección y arbitraje de los trabajos que aparecen en este suplemento fue responsabilidad del Comité
Organizador del X IBEROMET, quien nombró una comisión ad-hoc para este fin (véase editorial de este
suplemento).

9 La RLMM no sometió estos artículos al proceso regular de arbitraje que utiliza la revista para los números regulares
de la misma.

9 Se recomendó el uso de las “Instrucciones para Autores” establecidas por la RLMM para la elaboración de los
artículos. No obstante, la revisión principal del formato de los artículos que aparecen en este suplemento fue
responsabilidad del Comité Organizador del X IBEROMET.

0255-6952 ©2009 Universidad Simón Bolívar (Venezuela) 351

 Suplemento de la Revista Latinoamericana de Metalurgia y Materiales 2009; S1 (1): 353-363

DESIGN AND FABRICATION OF CELLULAR GLASS CERAMIC STRUCTURES FOR

FILTERING COMBUSTION GASES OF DIESEL ENGINES

A. Sarmiento1*, A.M. Montes1, D. Hotza2, A.P. Novaes de Oliveira2, J.A Escobar1

1: Facultad de Ingeniería, Dpto. de Ingeniería Mecánica, Universidad de los Andes. Bogotá, Colombia
2: Grupo de Materiales Cerámicos y Vítreos – CERMAT, Universidad Federal de Santa Catarina UFSC. Florianópolis,
Brasil
* E-mail: andres.sarmiento.s@gmail.com

Trabajos presentados en el X CONGRESO IBEROAMERICANO DE METALURGIA Y MATERIALES IBEROMET

Cartagena de Indias (Colombia), 13 al 17 de Octubre de 2008
Selección de trabajos a cargo de los organizadores del evento
Publicado On-Line el 20-Jul-2009
Disponible en: www.polimeros.labb.usb.ve/RLMM/home.html

Abstract
An exploratory study was developed to determine the potential use of glass ceramic materials in the manufacture of
an open pore foam catalytic support for diesel soot filtration. This project determines the behavior of some mechanical and
morphological properties of a cellular glass ceramic structure according to three different variables of analysis: pore
density, type of ceramic suspension, and percentage of compression during the excess material removal stage. The
replication method was used based on polyurethane (PU) foam templates of 45 and 60 pores per inch (ppi). The parent
glass used corresponds to a system called LZSA (Li2O – ZrO2 – SiO2 – Al2O3). Best fabrication parameters were
determined to obtain LZSA foams with properties similar to those of commercial foams used for this application.
Keywords: Cellular structures, Glass ceramic, Replication method
Resumen
Se desarrolló un estudio exploratorio para determinar el potencial del material vitrocerámico en la fabricación de una
estructura celular porosa apta como soporte de catalizador para la filtración de material particulado en los gases de
combustión de motores diesel. Este proyecto determina el comportamiento de algunas propiedades mecánicas y
morfológicas de una estructura celular vitrocerámica de acuerdo a tres diferentes variables de análisis: densidad de poros,
tipo de suspensión cerámica y porcentaje de compresión en la etapa de remoción de material en exceso. El método de
réplica se implementó basado en espumas de poliuretano (PU) de 45 y 60 poros por pulgada (ppi). El material vítreo
utilizado corresponde al sistema llamado LZSA (Li2O – ZrO2 – SiO2 – Al2O3). Los mejores parámetros de fabricación se
determinaron para obtener espumas de LZSA con propiedades similares a espumas comerciales utilizadas en esta
aplicación.
Palabras Claves: Estructuras celulares, Vitrocerámico, Método de réplica

1. INTRODUCTION engine modification, and after-treatment

The diesel engine is becoming nowadays one of the
most popular vehicle engines due to developments
that have achieved high energetic efficiency levels
with limited pollutant emissions. However, diesel
emissions have specific pollutants such as NOx and
soot that can be very hazardous not only to human
life but also to the environment (1). Cancer,
cardiovascular, and respiratory problems as well as
water, air, and soil contamination, are some of the
effects of these toxic emissions (2).
In order to reduce soot emissions form diesel
engines several techniques are being developed.
Among these, fuel modification or fuel alternatives,
0255-6952 ©2009 Universidad Simón Bolívar (Venezuela)
technologies (3). The after-treatment technique
consists on filtering the soot with specially designed
ceramic traps that can be catalytic or non-catalytic
and honeycomb type or foam type. Catalytic foam
traps present an advantage over other types of
filtering systems since they are self-regenerating (4).
The morphology of this filter allows the soot to
make close contact with the catalyst, allowing its
combustion without any additional regenerating
equipment (1; 3; 4; 5).
Ceramic foams can be produced by several
techniques including the replication method, direct
foaming or the use of a sacrifice material. However
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Sarmiento et al.

the replication method is the most known and used the different stages of the replication method shown
in industry as well as investigation. The replication on the diagram in Figure 1.
method consists on impregnating polymeric foams
with a ceramic suspension followed by a thermal A
Parent Glass
cycle. This thermal cycle has to main functions: it C Ceramic slurry
degrades the polymeric foam and consolidates the
ceramic material, generating a replica of the original A
structure. Additives
Generally, ceramic materials are used in the
D
fabrication of catalytic traps because of their high B
thermal stability and good chemical compatibility Impregnation of
PU the PU foam
with most of the reactive material used for the foam with the slurry
catalytic activation. Alumina (Al2O3) or ZTA
(zirconia-toughened-alumina) foams with pore
densities from 55 to 65 ppi are commonly used for D

this specific application. However, these materials Extraction of

require high temperature cycles (up to 1600oC), excess material
making the production more expensive and complex
(6). In this work, glass ceramic is introduced as an E
alternative material for the fabrication of catalytic
Thermal cycle
foam traps given that it requires a less demanding
heat treatment cycle.
A glass ceramic is a polycrystalline solid with a Ceramic foam
residual vitreous phase. This material can be
considered as a non porous compound formed by Figure 1. Diagram of the replication method.
nanometric crystals randomly arranged on a vitreous
matrix (7). The glass material is transformed to glass A – Raw Material:
ceramic by a process of crystallization during an The glass ceramic system used in this work
applied thermal cycle. The number, kinetics, and corresponds to a LZSA (Li2O – ZrO2 – SiO2 –
final size of crystals depend on the temperatures Al2O3) system. This system was developed by the
reached (8). Since crystallization temperatures of a Federal University of Santa Catarina, Brazil (9)
glass ceramic do not exceed 900oC, the use of this where several studies have been made concerning
material reduces the end cost of the final product. foam replication based on this material (10; 11). The
This would be an affordable alternative for third raw material to produce the parent glass powder was
world countries in their search for a better melted at ~1500±5°C for 7 hours on a gas furnace.
environment. Then it was quenched in water generating glass frits
(9). These were reduced to d50=4.26x10-6 m by
This project determines the behavior of some
mechanical milling. Commercial additives such as a
mechanical and morphological properties according
binder and dispersant were used. These were
to three different variables of analysis: pore density,
bentonite (Colorminas - Brazil) and sodium silicate
type of ceramic suspension, and percentage of
(Merck) respectively.
compression during excess material removal stage.
Porosity, permeability, mechanical resistance, and
B – Polymeric Foam:
form retention were measured and compared to a
The polymeric foams used correspond to
commonly used alumina foam trap. Best fabrication
polyurethane (PU) reticulated foams with open cells.
parameters were determined to obtain LZSA foams
Two different cell densities were used: 45 and 60
with properties similar to those of commercial
pores per inch (ppi).
foams used for this application.

2. EXPERIMENTAL PROCEDURE C – Ceramic Suspension:

The ceramic suspension was prepared using a
2.1 Foam Fabrication planetary ball mill with a mixing time of 5 minutes.
The experimental procedure is presented based on The solid phase corresponds to 95 wt% of LZSA
354 Rev. LatinAm. Metal. Mater. 2009; S1 (1): 353-363
 Design and Fabrication of Cellular Ceramic Structures for Filtering
parent glass powder and 5 wt% of bentonite. The
liquid phase corresponds to 1 wt% sodium silicate
and 99 wt% alcohol-isopropyl as aqueous medium.
The use of this medium helps promote a thixotropic
behavior of the vitreous suspension, which improves
the impregnation of the polymeric foam (10). The
solid/liquid phase ratio in wt% was varied between
50/50, 55/45, and 60/40.
D – Impregnation and removal of excess material:
The PU foam samples were immersed on the parent
glass suspension and the excess slurry was removed
using controlled compression with roller equipment.
Each sample was passed four times through the
rollers and was rotated after each pass in order to
improve the distribution of the remaining slurry.
The compression percentage of the foam
corresponds to a variable in this project, and was
controlled with different roller separation. The
compression percentages used correspond to 35%,
50%, 60% and 70%. Samples were left to dry at
room temperature for 24 hours.
E – Thermal cycle:
Heat treatment of the samples was performed in a
three stage process in an electric furnace in air. The
first stage at 450oC holding for 1 hour at a heating
rate of 1oC/min is for the PU foam decomposition.
The second stage at 650oC holding for 10 min at a
heating rate of 5oC/min is for the densification and
sintering of the parent glass. The third stage at
800oC holding for 10 min at a heating rate of
5oC/min for the crystallization of the glass (9; 12).
2.2 Characterization techniques
A morphological characterization of the cellular
structures is done using SEM images. Samples were
prepared using and isometric cutter with a diamond
blade to obtain sectional views.
Permeability measurements were performed on an
air flow apparatus (Amscor Air Flow). Samples
were prepared in order to leave only the front and
back face permeable. Direct airflow measurements
were taken. Permeability was calculated according
to Forchheimer’s equation,
ΔP / L = ( µ / k1 ) V + ( ρ / k2 ) V2 (1)
where ∆P [Pa] corresponds to the pressure drop, L
[m] the sample thickness, μ [Pa s] the viscosity of
the fluid (in this case air), ρ [kg m-3] the density of
the fluid, and V [m/s] the volumetric flow rate per
Rev. LatinAm. Metal. Mater. 2009; S1 (1): 353-363
unit of cross sectional area measured from airflow
data (13). The constants k1 (Darcyan) and k2 (non-
Darcyan) include the structural properties of the
porous medium and are used to compare the
permeability between different media (14). The first
term of the right side of equation 1 is attributed to
laminar flow and the second term to turbulent flow.
Since we are working with Re below ~150 we can
drop the term associated with turbulent flow and
then the Darcyan permeability can be defined as
k1 = (µ·V) / (ΔP / L). (2)
Mechanical measurements were performed under
compressive force. To ensure a uniform distribution
of the load, samples were mounted over epoxy putty
that was flattened and left to harden. To ensure the
alignment of the sample with the applied force, a
steel ball was used between the upper end cap and
the flat head of the equipment as seen in Figure 2a.
Tests were performed using a standard uniaxial
testing apparatus (Instron Model 5586) at a
crosshead speed of 0.5 mm/min (15).
After the applied thermal cycle, a volumetric
contraction is evident. The homogeneity of this
contraction depends on several fabrication
parameters. In order to characterize this
phenomenon, form retention was measured as a
percentage of the side view angles average as seen
in Figure 2b. An angle of 90o corresponds to 100%
form retention.
Figure 2. (a) Sketch of the assembly used during
compression tests (b) Form retention (sample 45ppi,
50/50 and 50% compression).
Porosity measurements were taken via image
analysis. Samples were mounted in a black
pigmented polyester resin used as contrast material
to fill all the open cells. A porous face was exposed
and polished. Images were taken and analyzed using
the freeware ImageJ. Only one plane was analyzed
by sample.
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Sarmiento et al.

3. RESULTS AND DISCUSSION OF THE

FABRICATION OF GLASS CERAMIC (c) LZSA replica. External
FILTERS superior view

3.1 Morphological characterization of LZSA

replicas
A first approach allows identifying a morphological Superficial
difference between the internal structure and the clogged cells
external structure of the glass ceramic replicas.
Figure 3 shows a better replication process on the Identification
external surface compared to the internal section of of cell
the foams. A better replication process can be structures
established based on the following observations:

• Fewer closed porosity.

• Cell type structure can be identified such as
windows and strut configuration. Figure 3. Particular case of analysis of morphological
• Fewer collapsed areas and clogged areas can be differences between internal and external section of the
identified. foam. Sample of 60 ppi, 55/45, 60% (Images are in the
same scale).
(a) PU foam of 60 ppi
A possible hypothesis for this behavior is found on
the stage of extraction of excess material. Once the
foam is impregnated with the slurry, it is passed
through a set of rollers with a controlled gap
distance. The foam is compressed four times
through the rollers with rotation after every pass to
promote the homogeneity of the remaining
suspension. The first compression eliminates most
part of the suspension. The after compressions help
distribute the remaining slurry inside the foam, but
part of the superficial slurry remains on the surface
of the roller. This behavior generates a gradient of
ceramic material concentration, creating a different
morphology on the surface and the inside of the
foams.
Cells with no (b) LZSA replica. Internal Morphological images of the internal sections of the
structure. sectional view 45 and 60 ppi replicas are shown in Figure 4 and
Destroyed cells.
Figure 5 respectively. Areas of excessive clogging
and areas with no cell definition can be seen. This
Large behavior is more evident in foams with low
number of compression percentage and more viscous
clogged suspension. As seen in Figure 4, no combination of
cells. parameters shows a better replication process. On
the other hand, for the 60 ppi foams shown in Figure
5, samples (f) and (g) correspond to better
morphological replicas of the PU foam.

356 Rev. LatinAm. Metal. Mater. 2009; S1 (1): 353-363

 Design and Fabrication of Cellular Ceramic Structures for Filtering

50% 60% 70%

50/50

(a) (b) (c)

55/45

(d) (e) (f)

60/40

(g)

Figure 4. Morphological comparison of the glass ceramic replicas. 45 ppi foam. Suspension type Vs compression
percentage.

Rev. LatinAm. Metal. Mater. 2009; S1 (1): 353-363 357

Sarmiento et al.
50%
50/50
(a)
55/45
(d)
60/ 40
Figure 5. Morphological comparison of the glass ceramic replicas. 60 ppi foam. Suspension type Vs compression
percentage.
3.2 Permeability of the LZSA replicas
¡Error! No se encuentra el origen de la
referencia. shows results for 45 and 60 ppi. For
both cell size densities, the permeability shows an
incremental behavior with the increase of
compression percentage. This value can increase up
to one order in magnitude for both types of foams
while varying the compression percentage from
35% to 70%. With higher compression percentages,
the ceramic load on the foam decreases. This
reduces the probability of cell clogging and the
accumulation of ceramic material on the polymeric
struts, thus increasing its permeability. A
358
60% 70%
(b) (c)
(e) (f)
(g)
relationship between the permeability and the type
of ceramic suspension can also be observed. Higher
permeability values can be obtained with less
viscous suspensions. However, less viscous
suspensions sacrifice the morphological replication
of the polyurethane foam. This phenomenon can be
explained based on the morphological results
discussed previously. The fluid suspensions are not
capable of covering polymeric struts on the
impregnation stage, causing partial collapse and
generating permeability paths with less fluid energy
loss.
Rev. LatinAm. Metal. Mater. 2009; S1 (1): 353-363
 Design and Fabrication of Cellular Ceramic Structures for Filtering

Figure 6. Permeability results for the 45 and 60 ppi foams.

3.3 Mechanical characterization of the LZSA
replicas
¡Error! No se encuentra el origen de la
referencia. shows the results of the mechanical
characterization. A bad quality impregnation can be
caused by high compression percentages or low
viscosities of the ceramic suspension, causing cell
collapses and the reduction of the mechanical
resistance of the ceramic replicas. The mechanical
resistance of a cellular structure is related with the
longitude and thickness of the cell struts. If the
ceramic material is reduced, then the mechanical
resistance suffers a reduction as well. A variation in
compression percentage from 70% to 35% can
increase the compressive mechanical resistance
from ~1 MPa to ~7 MPa. Analyzing the
morphological results for the LZSA replicas, a
hypothesis can be established showing the incidence
of the clogged cells on the mechanical resistance of
the porous structure. A low compression percentage
generates highly clogged cell areas. These clogged
cells are interconnected forming a cellular structure
with struts equivalent to the size of filled cells. This
allows the distribution of the force, thus increasing
its mechanical resistance.
3.4 Porosity of the LZSA replicas
Porosity corresponds to another variable to be
considered in the characterization of the structures.
This property is mostly a function of the
compression percentage. The behavior is very
similar to the one of permeability; it increases with
an increase in compression percentage. The
variation of porosity can be significant, from ~65%
to ~95% with an increase in compression percentage
from 35% to 90%.
The influence of the pore density and viscosity of
the ceramic suspension on porosity is not
concluding from the samples obtained, as seen in
Figure 8.

Figure 7. Mechanical characterization results for the 45 and 60 ppi foams.

Rev. LatinAm. Metal. Mater. 2009; S1 (1): 353-363 359

Sarmiento et al.
Figure 8. Porosity characterization results for the 45 and 60 ppi foams.
3.5 Form retention of the LZSA replicas
Form retention becomes a problem when enlarging
the size of the samples. For catalytic trap application
it is important to have larger samples (minimum
frontal area ~2.3x10-3 m2) in order to test them on
real engine exhaust gases (1; 3; 16; 17). As seen in
Figure 9, form retention tends to worsen with an
increase in compression percentage during the slurry
removal stage. This can be attributed to the lack of
parent glass over the PU foam and the sintering
mechanism. This mechanism corresponds to viscous
flow. In the early stage of sintering, before the glass
transition temperature of the parent glass, the
microstructure of the material covering the
polymeric struts corresponds to a random arrange of
packed particles. After the glass temperature is
reached, a continuum viscous matrix is formed
Figure 9. Form retention of the 45 and 60 ppi foams.
360
which defines the densification stage. A lack of
parent glass in the foam would cause a severe
uncontrolled retraction during the densification
stage (8; 18).
3.6 Comparison with commercial ceramic
foams used as filtering devices
Figure 10 and Figure 11 show some characteristics
of the LZSA replicas (red markers) in comparison
with other ceramic foams reported in literature (4).
It can be observed that the values obtained with this
material follow the generalized trend of other
ceramic cellular structures. Mechanical resistance
values obtained are in the upper range but
permeability and porosity values enter the lower
range. However, the values obtained prove the
LZSA material as a viable option in the fabrication
of ceramic filters.
Rev. LatinAm. Metal. Mater. 2009; S1 (1): 353-363
 Design and Fabrication of Cellular Ceramic Structures for Filtering

Figure 10. Comparison of LZSA foam characterization results (red markers) and other ceramic foams (4). The variable of
analysis corresponds to the cell density (ppi).

Figure 11. Comparison of LZSA results (red markers) and other ceramic foams (4). The variable of analysis corresponds
to compression of the foam during the excess slurry removal stage.
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Sarmiento et al.
4. CONCLUSIONS
Porous structures were obtained from a glass
ceramic material for diesel engine particulate
filtering applications. In order to obtain properties
similar to those of commercial cellular structures of
alumina (Al2O3) or zirconia toughen alumina (ZTA)
(porosities between 80% and 90% and mechanical
resistance between 1 and 7 MPa (1; 15; 19; 20; 21)),
the fabrication parameters were chosen as follows: a
ceramic suspension of 50/50 (solid/liquid phase
ratio) and a compression percentage of 50% during
the excess removal stage. Although this combination
of parameter does not result on the best ceramic
replicas based on morphological analysis, it results
on a porous material with good mechanical
properties for this specific application. Form
retention with these parameters for both types of
foams, 45 and 60 ppi, is superior to 90%, having a
geometrical tolerance of ±2 mm.
The morphology of the ceramic replicas is
influenced by the process variables in a way that it
can generate a porous structure but without
replicating the polymeric structure. The best replicas
were found with the most viscous ceramic
suspension and the highest compression percentage.
This does not necessarily mean the best mechanical
properties.
On the replication method, the compression
percentage on the stage of extraction of excess
material affects in a very significant way the
mechanical properties of the resulting structure.
Therefore this must be considered one of the most
important variables to be controlled during the
replication process. High compression percentages
correspond to high porosity and permeability values,
with a reduction in mechanical resistance.
5. ACKNOWLEDGMENTS
The authors are grateful to the Federal University of
Santa Catarina, Brasil (UFSC) for their contribution
to this project. To the CIPP-CIPEM of los Andes
University, Colombia for their help.
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