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properties
T. Ohji* and M. Fukushima
Porous ceramics are now expected to be used for a wide variety of industrial applications from
filtration, absorption, catalysts and catalyst supports to lightweight structural components. During
the last decade, tremendous efforts have been devoted for the researches on innovative
processing technologies of porous ceramics, resulting in better control of the porous structures
and substantial improvements of the properties. This article intends to review these recent
progresses of porous ceramics. Because of a vast amount of research works reported in this field
these days, the review mainly focuses on macro-porous ceramics whose pore size is larger than
50 nm. Followed by giving a general classification of porous ceramics, a number of innovative
processing routes developed for critical control of pores are described, along with some
important properties. The processes are divided into four categories including (i) partial sintering,
(ii) sacrificial fugitives, (iii) replica templates and (iv) direct foaming. The partial sintering, the most
conventional technique for making porous ceramics, has been substantially sophisticated in
recent years. Very homogeneous porous ceramics with extremely narrow size distribution have
been successfully prepared through sintering combined with in situ chemical synthesis. Carefully
tailored micro-structure (size, morphology and orientation of grains and pores, etc.) of porous
ceramics has led to unique mechanical properties, which cannot be attained even in the dense
materials. Various types of the sacrificial fugitives have been examined for obtaining well-tuned
shape and size of pores. The freeze-drying techniques using water or liquid as fugitive materials
have been most frequently studied in recent years. Controlling growth of ice during freezing has
led to unique porous structures and excellent performances of porous ceramics, e.g. excellent
mechanical behaviour for highly porous lamellar hydroxyl-apatite scaffolds. Numerous
approaches on the replica templates have been developed in order to produce highly porous
ceramics having interconnected large pores and sufficiently strong struts without cracks. Natural
template approaches using wood, for example, as positive replica, have been intensively studied
in these years and have realised highly oriented porous open-porous structure with a wide range
of porosity. As for the direct foaming technique, a variety of novel techniques which stabilise the
bubbles in ceramic suspension have been developed to suppress large pore formation, e.g.
evaporation of emulsified alkane droplets and use of surface-modified particles. We also briefly
review porous ceramics with hierarchical porosity (incorporation of macro-, meso- and micro-
pores), which have attracted much attention in both academic and industrial fields. Finally the
article gives the summary and discusses the issues to be solved for further activating the potential
of porous ceramics and for expanding their applicability.
Keywords: Ceramics, Pores, Processing, Properties, Permeability, Mechanical property, Foam, Review
Introduction
For structural applications of brittle ceramic materials,
National Institute of Advanced Industrial Science and Technology (AIST), pores are generally what to be eliminated because they
Anagahora 2266-98, Shimo-shidami, Moriyama-ku, Nagoya 463-8560, act as fracture defects and degrade the structural
Japan reliability, and therefore, ceramic engineers tried to
*Corresponding author, email t-ohji@aist.go.jp sinter ceramics to full density to attain high mechanical
5 Micro-structures and mechanical properties (flexural strength and fracture toughness) of porous silicon nitrides sintered
with 5 wt-%Yb2O3 at 1600, 1700, 1800 and 1850uC. ‘P’ denotes porosity52 (Reproduced with permission of Elsevier)
the fibrous grain formation. As the sintering tempera- nitrogen pressure of 1 MPa. The texture of porous
ture further increases, the micro-structure becomes silicon nitride with porosity of 14% is shown in Fig. 6.
coarser and the strength decreases with increasing The fibrous grains of silicon nitride are well aligned
fracture toughness (though the toughness values are toward the casting direction, and the pores, whose
still below 4 MPa m1/2). Porous b-Si3N4 ceramics were shapes are mostly plate-like along the same direction,
also fabricated by carbothermal reaction between silica exist among the grains. The anisotropic (fibrous grain-
and carbon.54 Micro-structure is controlled by varying aligned) porous silicon nitrides showed excellent
particle size of the carbon in this case. Tuyen et al.55 mechanical behaviour, when a stress is applied in the
fabricated porous reaction-bonded silicon nitride by alignment direction.53,57 Figure 7 shows the fracture
nitridation process at 1350uC and post-sintering at strength and fracture toughness of the anisotropic
1550–1850uC, which provides similar fibrous micro- porous silicon nitrides as a function of porosity,53,57 in
structure and high porosity. The duration time for comparison with those of the isotropic porous silicon
sintering had a significant effect on the micro-structure nitrides that were sintered at 1800uC by using a-Si3N4
and grain morphology. The fabrication process is and 5 wt-%Yb2O3.53,58 The anisotropic materials exhib-
advantageous due to the low cost of Si raw powder. ited very high strength above 1?5 GPa, and very high
One of the unique processing routes for porous fracture toughness above 17 MPa m1/2 in the porosity
ceramics with anisotropic micro-structure is tape-casting range below 5%. It should be noted that the toughness of
fibrous seed crystals or whiskers. For porous silicon the porous materials with porosities below 10% is
nitrides, b-Si3N4 seed crystals were mixed with sintering somewhat higher than that of the dense one (0%
additives as starting powders, and the green sheets porosity). These excellent mechanical properties were
formed by tape casting were stacked and bonded under due to enhanced crack shielding effects (bridging and
pressure.56 Sintering was performed at 1850uC under a pull-out) of aligned fibrous grains. Debonding was
lower cost of the overall materials. Kim and his flow directly through the pores. However, the prepara-
co-workers83,84 used hollow micro-spheres as sacrificial tion of such ceramics is complex because handling long
templates to make porous silicon carbide ceramics fibres such as thin wire or cotton thread is difficult.
synthesised from carbon-filled polysiloxane and others. Using short fibres or whiskers as the pore-forming agent
Using preceramic polymer and organic micro-spheres is an alternative that combines the advantages of
for fabricating porous ceramics allows use of the low- partially sintered porous ceramic and those of unidirec-
cost and/or near-net shaped processing techniques like tional pores. Yang et al.65 demonstrated formation of
extrusion and direct casting. They reported relatively rod-shaped pores in silicon nitride ceramics, using slip
high flexural strength for porous SiC ceramics (e.g. 60 casting of aqueous slurries of silicon nitride powder and
and 45 MPa at 40 and 50% porosity, respectively) and sintering additives with 0–60 vol.-% fugitive organic
very low thermal conductivity (2 W m21 K21, at y70% whiskers. Rheological properties of slurries were opti-
porosity).84 mised to achieve a high degree of dispersion with a high
Song et al.85 produced micro-cellular silicon carbide solid-volume fraction. Samples were heated at 800uC in
ceramics with a duplex pore structure by using expand- air to remove the whiskers and sintered at 1850uC in
able micro-spheres and PMMA spheres; which resulted nitrogen atmosphere to consolidate the matrix. Porosity
in the large pores and the small windows in the strut was adjusted in 0–45% by changing the whisker content
area respectively. This porous ceramics showed excel- in 0–60 vol.-%. The obtained porous silicon nitride
lent air permeability as shown in the section on ‘Gas contained uniform rod-shaped pores with random
permeability’. directions, exhibiting relatively high gas permeability
Diaz et al.93,94 fabricated porous silicon nitride in comparison with porous silicon nitride containing
ceramics by using a fugitive additive, corn starch equiaxed pores.157 Isobe et al.81,110 and Okada et al.86,87
(particle size: 5–18 mm). In order to obtain homoge- used carbon fibres (14 mm diameter and 600 mm length)
neous dispersion of the fugitives, the mixture slurry was or Nylon 66 fibres (9?5–43 mm diameter and 800 mm
kept in agitation by using a magnetic stirrer for a while, length) for pore-forming agent, and tried to align them
and then was frozen and dried under vacuum for sieving. by extrusion technique to produce porous alumina81,110
Kim et al.95 mixed various amounts of corn starch to and mullite86,87 ceramics with unidirectionally-oriented
(Ba, Sr) TiO3 powder to obtain (Ba, Sr) TiO3 porous pores. They showed that the pore sizes and porosities
ceramics. They found that depending on the porosity, can be controlled by varying the fibre diameter and fibre
the PTCR effect was 1–2 orders of magnitude improved content. The obtained samples showed better air
in comparison with the dense reference. permeability than the conventional porous materials
Chen et al.66 developed porous silicon nitride of used for filter applications.110 This technique can allow
equiaxed a-grains by using phosphoric acid (H3PO4) as the production of highly oriented porous ceramics by
the pore-forming agent and pressureless sintering of industrially favoured extrusion method.
relatively low temperatures techniques (1000–1200uC). Liquid phases such as water and oil, which are readily
On the other hand, Li et al.80 fabricated porous silicon sublimated or evaporated, are often used as pore
nitride with fibrous b-grain structure, using naphthalene forming agents.116–157 One of the most frequently
powder as the pore-forming agent and gas-pressure studied approaches in recent years is freeze-drying the
sintering of high temperatures above 1700uC. The water or liquid-based slurry to produce porous ceramics
bending strength of the former materials was 50– of unique structure.119–155 Figure 9 shows a schematic
120 MPa in porosity range of 42–63%, while that of illustration of the procedures which was employed by
the latter was 160–220 MPa in porosity of 50–54%. This Fukasawa et al.119–121, and a porous silicon nitride body
substantial difference in strength is most likely due to obtained thereby. When the bottom part of the slurry is
the micro-structural difference (equiaxed versus fibrous), frozen, ice grows macro-scopically in the vertical
which was similar to what we observed in Fig. 5. direction, and pores are generated subsequently by
Ding et al.49 used graphite as the pore-former to sublimation of the ice. Through sintering this green
fabricate mullite-bonded porous silicon carbide ceramics body, a porous ceramics with unidirectionally aligned
in air from SiC and a-Al2O3 through in situ reaction channels can be obtained; these channels contain smaller
bonding technique. Graphite is burned out to produce pores in the internal walls (Al2O3)119,120 or fibrous grains
pores and the surface of SiC is oxidised at high protruding from them (Si3N4).121 This method has
temperatures to SiO2, which, at further increased several advantages, including simple sintering process
temperatures, reacts with a-Al2O3 to form mullite without materials to be burnt out, a wide range of
(3Al2O3.2SiO2). SiC particles are bonded by the mullite porosity (30 to 99%) controlled by the slurry concentra-
and oxidation-derived SiO2. tion, applicability to various types of ceramics and
Long fibres such as cotton thread,96 natural tropical environmental friendliness without emitting harmful
fibre97 and metal wires109 are often used as pore forming products. In particular, porous scaffolds with ice-
agents for obtaining porous ceramics of through designed channel-like porosity have been intensively
channels. Zhang et al.96 produced porous alumina studied for a wide variety of applications including
ceramics with unidirectionally aligned continuous pores biomedical implants and catalysis supports.
(diameter: y160 mm) via the slurry coating of mer- The porosity of the porous materials obtained by using
cerised cotton threads. The pore size can be adjusted by this technique is a replica of the original ice structure. The
using cotton threads of different diameters, and the porous channels run from the bottom to the top of the
porosity can be controlled by changing the solids samples, and the pores most frequently exhibit an
concentration of the slurry. In this case excellent anisotropic morphology in the solidification plane.
permeability can be achieved for porous ceramics with Deville et al.128–131 investigated freeze casting of ceramic
unidirectional through channel pores, because gas can slurries, and particularly the relationships between the
processes using water or liquid as fugitive materials are filter smaller pollutants in the exhaust gases with less
advantageous in this viewpoint and have been very pressure drop. We presume that one of the effective
intensively studied in recent years. Controlling growth of solutions will be a hierarchically porous structure
ice during freezing leads to unique porous structures and incorporating well controlled macro-scaled cylindrical
excellent performances of porous ceramics. For exam- pores and micro- or nano-scaled whiskers grown from
ple, the highly porous lamellar hydroxyl-apatite scaf- the internal walls, which enable the fluid permeation and
folds via this approach are several times stronger than pollutant capture respectively.250,251
materials currently used for implantation. Also the Finally, it should be remarked that porous ceramic
freeze-dry-processed porous ceramics that have cylind- components are most frequently subjected to mechanical
rical through channels demonstrated the excellent loads and thermal shocks in their numerous applications
permeability. and that better structural reliability will be critically
The replica template techniques have been widely needed to further expand their applicability in future
used to fabricate porous ceramics with interconnected industries. Greater efforts will be made for ensuring the
large pores of high volume porosity. Porous polymeric mechanical reliability, such as enhancing neck growth
sponge such as polyurethane is the most typical among matrix grains and avoiding crack formation
synthetic template used for this process. However, due during fabrication. On the other hand, while pores are
to cracking struts during pyrolysis of the sponge, the generally believed to deteriorate the mechanical proper-
mechanical reliability is substantially degraded; a variety ties, this is not always true as seen in this review.
of approaches have been used to avoid the strut crack Carefully tailored porous micro-structures have a great
formation. Natural template approaches using wood, possibility to give rise to substantially improved or
for example, as positive replica, have been frequently unique properties that are not attained even in dense
used in these years and have realised highly oriented materials.
porous open-porous structure with a wide range of
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