Materials Letters 145 (2015) 250–252

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Materials Letters
journal homepage: www.elsevier.com/locate/matlet

A new source for production of ceramic filters

A.C. Carvalho a, F. Raupp-Pereira b, J.B. Rodrigues Neto b, A.P. Novaes de Oliveira b,n
a
Process Engineering, University of Joinville Region, Joinville, SC, Brazil
b
Glass–Ceramic Lab, Federal University of Sta Catarina, 88040-900 Florianópolis, SC, Brazil

art ic l e i nf o a b s t r a c t

Article history: A industrial solid waste from the process of precision casting by lost-wax was used and evaluated for the
Received 4 October 2014 production of ceramic filters. PU sponges (9.8 ppi) impregnated with a stable suspension were
Accepted 27 January 2015 successfully fired at 1550 1C/2 h so that filters well reproduced (9.5 ppi), and mechanically stronger
Available online 4 February 2015
(1.0 MPa) were obtained. The produced filters tested in industrial scale showed very good performances
Keywords: with good filtering efficiency (1.7 kg/s) for liquid cast iron.
Ceramic shell & 2015 Elsevier B.V. All rights reserved.
Wastes
Cellular ceramics
Ceramic filters

1. Introduction 2. Materials and methods

Cellular porous ceramics are commercially available for a wide
range of technological applications such as filters, membranes, cata-
lytic substrates and lightweight structural panels [1]. They are used
because of their functional properties, such as low thermal expan-
sion and thermal conductivity, high permeability and chemical
inertness. Cellular porous ceramics are prepared and consolidated
using several materials including cordierite, mullite, silicon carbide,
alumina, glasses as well as solid wastes [1–3]. The valorization of
wastes for the production of new materials has attracted great
interest of society and scientists, since they represent, mostly, loss of
raw materials characterized by a strong potential for reuse. Many of
these wastes have potential use and deserve investigation and study
[2,3], as it is the case of the ceramic shell from the lost-wax casting
process used in the production of metal parts. Among the applica-
tions that can be envisioned for the development of new products
from this waste it may consider the cellular ceramics for the
fabrication of filters for molten metals [4]. These filters have the
function of retaining any slag inclusions and/or sand and also
the flow control of liquid metal into the mold cavity [5]. These
filters are produced by the replication process that involves the
impregnation of a polymeric sponge with a ceramic suspension,
followed by firing in which occur the elimination of the polymer and
sintering of the ceramic structure [1]. This study aimed to develop
and to characterize ceramic filters produced from a ceramic waste
(generated by a Brazilian company which produces about 500 t per
year of ceramic shell) as an alternative raw material source.
n
Corresponding author. Tel.: þ 55 48 37214004.
E-mail address: antonio.pedro@ufsc.br (A.P. Novaes de Oliveira).
The ceramic shell (average size of 5 cm and humidity content of
0.6%) was crushed (o1 cm) in a mortar steel and then wet milled
in a porcelain mill containing alumina grinding media and water
for 90 min. The average particle size distribution of the milled
material was determined using a laser scattering particle size
analyzer (Master Sizer 2000, Malvern). The chemical characteriza-
tion was performed by X-ray fluorescence spectroscopy (XRF,
Philips PW 2400). To investigate the crystalline phases of the waste
and fired filters, powdered samples were analyzed using X-ray
diffractometry, XRD (Philips X’Pert) with Cu Kα radiation. A refrac-
tory composition, named CF (ceramic filter) has been prepared
(weight of dry solid) combining ceramic shell (87.5%) and kaolin
(12.5%). The refractory composition was formulated based on the
phase diagram of the Al2O3–ZrO2–SiO2 (ZSA) system. The kaolin,
supplied by Colorminas (Brazil), was added as a stabilizer (rheolo-
gical treatment) and mineralizer (heat-treatment). Specific details
of the formulated composition (CF) can be obtained in Carvalho
et al. [6]. Based on the ternary diagram of the ZSA system a tem-
perature range (1500–1650 1C) was defined to study the sintering
behavior of the formulated composition. The CF composition belongs
to the ZS–S–A3S2 composition triangle in which the softening starts at
about 1550 1C in the preliminary phase field, A3S2 (mullite, Al6Si2O13).
In a rheological study conducted previously [6], the CF composition in
the form of suspension with 80% solids was prepared and analyzed at
different concentrations of dispersant, from 0.25 to 1.5% (Darvan
821A, RT Vanderbilt Company, Inc.). The impregnation of polyur-
ethane (PU) sponges (INOAC Corporation—Japan) with 10 ppi for
the production of ceramic filters was performed by dipping them in
an optimized ceramic suspension (70% ceramic shell (
5 mm), 10%
kaolin (
6 mm), 20% water and 1.5 wt% dispersant). This dipping
process was repeated three times for each PU sponge, with an interval

http://dx.doi.org/10.1016/j.matlet.2015.01.131
0167-577X/& 2015 Elsevier B.V. All rights reserved.
 A.C. Carvalho et al. / Materials Letters 145 (2015) 250–252
of 10 min followed by a drying process (25 1C/24 h). After dying
process, the impregnated sponges were fired in an electric furnace
in oxidizing atmosphere (air) and atmospheric pressure in three
steps for the thermal degradation of the PU sponge, at a heating
rate of 0.5 1C/min up to 500 1C/1 h, pre-sintering at a heating rate
of 0.5 1C/min up to 1200 1C/1 h and sintering (1500 to 1650 1C/1
and 2 h) at a heating rate of 5 1C/min for consolidation of the
ceramic filters. The cooling rates were established by natural heat
loss. The cellular structure of the PU sponges and ceramic filters
were photographed such that through the images it was possible to
observe and to determine (Image J) the linear pore density and the
pore size. The bulk density of fired samples was measured by
applying the Archimedes’s principle (in distillated water at 25 1C)
in an analytical balance (Shimadzu AX200). The theoretical density
was measured by a He pycnometer (Quantachrome Ultrapycn-
ometer 1000 (LiMac)) on crushed fired cell struts. The relative
density was the ratio of the bulk density and the theoretical
density. Porosity was calculated from this relative density. The
compressive strength was determined (ASTM C133) by averaging
5 specimens (20  20  20 mm3), using a mechanical test machine
—EMIC DL 2000, with loading speed of 1.3 mm/min. Ceramic foams
subjected to thermal shocks by cooling them from 800, 1000
and 1200 1C/30 min in air (25 1C) or in water (25 1C) were also
mechanically tested (ASTM C133). Filters were also tested on an
industrial plant for the fabrication of gray cast iron parts (cast in
sand) which are ordinarily produced in the manufacturer with the
use of silicon carbide filters (7 ppi). The filtration capacity was
determined by taking the set weight after metal solidification and
the time (using a chronometer) to fill the mold with molten metal.
3. Results and discussion
The ceramic shell was classified as not hazardous as leaching
tests (NBR 10005/04). Chemical composition of the waste and
kaolin is shown in Table 1. From the table it is possible to observe
that the waste consists mainly of Al2O3, SiO2, ZrO2 and small
amounts of other oxides present in the raw materials used in the
production of the ceramic shell and/or in the molten metals. The
waste is constituted mainly of mullite (JCPDS 01-079-1454), zircon
(JCPDS 01-084-1560) and cristobalite (JCPDS 01-082-0512). Fired
Table 1
Chemical composition of raw materials. L.O.I: loss of ignition.
Raw materials Chemical composition (wt%)
Al2O3 SiO2 ZrO2 TiO2 Fe2O3 K2O Na2O Others
Ceramic shell 53.3 36.2 5.4 1.4 1.7 0.9 0.4 o 0.7
Kaolin 39.9 50.1 – – 0.5 0.9 – o 0.3
Fig. 1. PU sponge (a) and ceramic filter (b) fired at 1550 1C/2 h.
251
samples of composition CF showed, besides the phases identified in
the waste, zirconium aluminate (JCPDS 01-084-1560) and tridymite
(JCPDS 00-003-0227). The presence of tridymite may be associated to
the transition from cristobalite to tridymite formed at lower tem-
peratures. Fig. 1(a) and (b) show photos of a PU sponge which was
impregnated with the formulated suspension (CF) and of ceramic
foam fired at 1550 1C/2 h, evidencing the pore structures. Linear
pore density measurements showed that the PU sponge (Fig. 1(a))
has 9.870.9 ppi and the ceramic foam produced (Fig. 1(b)) has
9.571.1 ppi. The obtained ceramic filter was very well reproduced,
i.e., linear pore density slightly smaller ( 0.3 ppi). The pore size
behaves as a bimodal distribution. Even so, results showed a greater
incidence of pore sizes within the range between 1.5–2.5 mm and
3.0–4.0 mm indicating the filter reproducibility since 80% of the
pores are in the cited ranges. Fig. 2 shows the relationship between
compressive strength and relative density of ceramic filters fired at
different temperatures for 2 h. The compressive strength increases as
the firing temperature increases (1500–1650 1C). However, for cera-
mic foams fired at 1600 and 1650 1C the compressive strength was
about the same even if for samples fired at 1600 1C the dispersion
around the mean value was higher. Moreover, ceramic foams fired
at 1550 1C reached higher compressive strength values which can
be associated to the relative density of the ceramic foams and the
porosity of the struts. In fact, porosities of the ceramic filters (Fig. 2)
were 84.6% (1500 1C), 83.4% (1600 1C), 81.0% (1550 1C) and 83.0%
(1600 1C). Furthermore, ceramic foams with higher relative den-
sities but with high density struts showed higher compressive
strength values (1.0 MPa) as for samples fired at 1550 1C/2 h.
However, zircon melts at 1540 1C [7]. Thus, it is reasonable to
assume that the melted (at 1550 1C) reacts with the preexistent
mullite thereby enhancing the densification of the ceramic filter.
L.O.I
0.1
8.3 Fig. 2. Compressive strength (σc) of ceramic filters fired/2 h at different tempera-
tures as a function of relative density (ρrel).
252 A.C. Carvalho et al. / Materials Letters 145 (2015) 250–252
Fig. 3. Steps of fabrication of cast iron parts. (a) and (b) CF filter in the silica mold, (c) solidified metal parts with the CF filter and (d) solidified metal with the SiC filter,
(e) parts produced with the filter CF and (f) parts produced with the SiC filter.
Moreover, the eutetic temperature and chemical composition may
change [8]. The prepared composition (CF) according to chemical
analysis shows relatively high amounts of Na and K as well as Fe
oxides which can contribute to reduce the eutectic temperature of
the zirconium aluminate. So, it is reasonable to say that at tempera-
tures as 1600 and 1650 1C the eutectic phase melts producing
microstructures with secondary porosity originated from the expan-
sion of liquid glassy phases. Ceramic foams fired at 1550 1C/2 h and
subjected to thermal shocks showed compressive strengths at least
40% lower than those not submitted to thermal shocks. The filter
produced showed a filtration capacity slightly lower (1.7 kg/s) than
the commercial SiC filter (2.1 kg/s). This difference is related to the
lower pore density of the SiC filter (7 ppi). However, this low
filtration capacity was positive since the cast iron parts manufac-
tured showed better surface finishing (Fig. 3) as a result of a less
turbulent flow into the mold cavity. In this case, the metal parts
require a smaller number of finishing operations which means
saving of energy and materials.
4. Conclusions
The ceramic shell waste is a strong candidate for the production of
filters for metal casting. PU sponges (9.8 ppi) impregnated with
an optimized suspension (CF) were successfully fired at 1550 1C/2 h
so that filters well reproduced (9.5 ppi) and mechanically stronger
(1.0 MPa) were obtained. Filters put on industrial test showed very
good performances with good filtering efficiency (1.7 kg/s) of liquid
cast iron for the production of metal parts free defects with excellent
surface finishing.
Acknowledgment
Authors are grateful to FAPESC/CNPq (PRONEX T.O. no. 17431/
2011-9).
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