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Ceramics in Asia

Synthesis, Properties and Applications of Cordierite Ceramics, Part 1

A. Chowdhury, S. Maitra, S. Das, A. Sen, G.K. Samanta, P. Datta

Anirban Chowdhury is a post-graduate research student working in the area of sol gel ferroelectrics for his PhD at the Institute for Materials Research, University of Leeds, UK. He earned his BTech in Ceramics from the College of Ceramic Technology, University of Calcutta and MTech in Materials Science from IIT Kanpur. He received the prestigious ORS award and a Tetley & Lupton Scholarship for 20052008.


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Fig. 1 Structure of cordierite [5]

As an engineering material, cordierite has many applications in different fields exploiting its unique electrical, mechanical and thermal properties. The synthetic aspect of cordierite is of constant interest to researchers. Elucidation of its structure and establishing the properties of its structure has always been considered a fascinating subject by researchers. In the present paper these different aspects of cordierite are briefly reviewed. Keywords: Cordierite, processing, properties, applications

1 Introduction
Cordierite (2MgO2Al2O35SiO2) is an important naturally occurring ceramic material, which is popular especially for its unusually low thermal expansion coefficient, low thermal mass, low dielectric loss factor, low density, volume resistivity and high thermal shock resistance. Cordierite is isostructural with beryllium. It is found in two structural forms, namely, the orthorhombic (low temperature form) symmetry, which is more common, and the hexagonal symmetry, which is also known as indialite. The structure of cordierite is characterized by six-membered rings and is built up from SiO4 and AlO4 tetrahedra. These tetrahedra form six (cation) membered or four (cation) membered rings [1], as shown in Fig. 1.

Some properties of this multiphase oxide are given below [24]: Density 2.02.53 g/cm3 Melting point 1470 C Thermal expansion coefficient from 25 to 1000 C 1.42.6 106/K Youngs modulus 139150 GPa Flexural strength at room temperature 120245 Relative dielectric constant 5.0 (K and tan at 1 MHz) Typical thermal expansion curves are shown in Fig. 2. The expansion is small and anisotropic. The c axis expansion is negative, while the a axis expansion is positive and therefore the re-

sultant volume expansion is negligibly small (with an aggregate thermal expansion of about 0.9 106/K from room temperature to 800 C). With elevated temperatures, the increased thermal motion of the atoms of cordierite is accommodated primarily by twisting and rotation of the rings. The relationship between thermal expansion and crystal structure of cordierite has been discussed by Hochella and Brown [5]. Cordierite is widely used in the whiteware industries as kiln furniture because of its abovementioned properties. It also has advanced applications as electrical insulators, high performance resistors, heating element supports, burner tubes,feed-through insulators,special furnace shapes, exhaust catalyst supports, filters and many more that are discussed here. For engineering applications, it is usual to control purity and reproducibility by utilizing synthetic cordierite.

2 Mineralogical aspects

Cordierite is a magnesium aluminium silicate (Mg2Al4Si5O18) mineral. It belongs to the class of silicates and the subclass of cyclosilicates (andalusite-sillimanite-kyanite group).Although, it is not a very popular mineral from the geological point of view, its gemstone variety, which is called iolite, is well known among gemstone collectors and fanciers. Cordierite was known and used as a gemstone in Sri Lanka long before the French geologistmineralogist Pierre Louis Cordier accurately described it in 1809. Cordierite was identified as a specific mineral and named in 1813. Apart from iolite, the other varieties of cordierite found are bloodshot iolite and praseolite. The unusual blue-violet colour of cordierite is attractive Fig. 2 Typical thermal expansion curves of cordierite [5] and can be compared


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with a light blue sapphire of purplish tint. This is the reason why cordierite is sometimes called "water sapphire". Different colours of cordierite crystal available are blue, greyish blue, violet blue, grey, yellow, brown, green (rare), etc. One of the most notable characteristics of cordierite is its strong pleochroism, or colour changing ability. Generally, it is strongly trichroic. When viewed from one direction, the crystal or gemstone may appear blue or blue-violet. But as the crystal or gemstone is rotated in another viewing direction, the colour will appear yellowish gray to light blue. The Mg-rich variety shows as pale yellow, pale blue, and violet blue and the Fe-rich variety shows as colourless and violet. Its index of refraction varies in between 1.521.57. Its birefringence ranges from 0.005 to 0.018 and dispersion is 0.017. Its optical character is biaxial positive, but often it is negative. The crystals may be colourless or transparent to translucent. It has some opalescence resembling star sapphire. It has a vitreous lustre. The cleavage is poor in one direction and the fracture is subconchoidal. Its hardness is 77.5, specific gravity is approximately 2.3 and streak is white. It reacts slightly with concentrated acids, but more readily dissolves in HF. The crystal habits include rare prismatic crystals that are usually massive, or in compact grains embedded in metamorphic schists and gneisses. They are also found as pebbles and grains in alluvial deposits.The minerals associated with cordierite are almandine, corundum, andalusite, biotite and feldspars. The inclusions in cordierite crystals are clouds of very small zircon crystals surrounded by interference colours rimmed with intense yellow and hematite platelets in parallel orientation. Its notable occurrences include Sri Lanka; India; Burma; Madagascar; Middlesex Co., Connecticut and the Yellowknife area of the Northwest Territories of Canada.It is a very common mineral in Sweden as it is a component in many Swedish schists, found in central Sweden. It is of relatively low cost, has good electrical insulation properties, moderate mechanical properties and temperature resistance, and can readily be formed into a variety of shapes. It can be made in high volume through cost-effective extrusion or dry-pressing methods. through various routes. The effects of different additives like TiO2, ZrO2, ZnO, SrO, B2O3, etc. on the densification of cordierite have also been studied extensively. During powder preparation of cordierite the kinetics of heat treatment can also have a significant effect on its densification. Cordierite can be synthesized by firing traditional ceramic raw materials like clay, talc, silica and alumina at 13401450 C.But this process does not yield theoretically dense bodies as they cannot be fired to maturity due to excessive formation of glass from talc and clay and because of the fact that cordierite incongruously melts at 1460 C to give mullite. To overcome this problem, a cordierite composition is pre-calcined to grog (talc + alumina) and then combined with clay. Sometimes, the batch composition is melted and after fabrication of the desired shape directly from the melt or glass, the amorphous shape is devitrified to yield a cordierite monolith [6]. The conventional formation of cordierite involves two stages. Firstly, a small amount of cordierite is formed at 1275 C through the solid-state reaction of mullite, protoenstatite and cristoballite the decomposition products of talc and kaolinite. In the second stage, a glassy phase appears at 1335 C from the reaction of previously formed cordierite and the remaining cristoballite and protoenstatite. The bulk of the cordierite is then formed by the reaction of the melt with mullite. Cordierite forms at lower temperatures (1140 C) when clinochlore and kaolinite are reacted [7]. Al(NO3)39H2O and colloidal silica by co-precipitation method and studied its sintering. In other works, Han and Park [1112] synthesized and sintered cordierite from metal alkoxides,using Si(OC2H5)4Al(OC3H7)3Mg(OC2H5)2 by the sol-gel method. Densification of this powder compact, which was studied by using the precursor powders calcined at 900 C for 2 h, improved at the sintering temperature of 800900 C. An alkoxide sol-gel route was developed by Tsai [13] to prepare stoichiometric cordierite fibers. X-ray diffraction analysis revealed that non-aged and aged fibrous gels all remained amorphous at 800 C, but began crystallizing into -cordierite and -cordierite at 900 C and 1050 C, respectively. Single-phase -cordierite fibers were obtained at 1300 C. Heating the non-aged fibers yielded denser microstructures with fine grain sizes of 0.2 and 0.4 m,whereas the aged fibers exhibited porous microstructures following heating at 1300 C.A higher heating rate and aging treatment resulted in higher open porosity of the fired fiber. Petrovic et al [14] synthesized alkoxy-derived cordierite gels from tetraethylorthosilicate (TEOS), aluminium isopropoxide and magnesium ethoxide. TEOS was partially hydrolyzed at molar ratios H2O/TEOS = 1.2 in the presence of HCl as catalyst.At first -cordierite crystallized in a three dimensional growth at 9501000 C with a small amount of spinel. The transformation of - to -cordierite began at about 1100 C and that of - to cordierite occurred at above 1300 C. The overall activation energy of the crystallization of cordierite is 580 81 kJ/mol. Fukui et al [15] studied the effect of prehydrolysis on the structure of a complex alkoxide as a cordierite precursor and its crystallization behavior. Here complex alkoxides were synthesized as cordierite precursors by reaction of pre-hydrolysed TEOS with Al and Mg alkoxides and the effect of prehydrolysis on alkoxide structure was analyzed by IR, 27Al and 29Si NMR spectroscopies. It was observed that, for temperatures at the lower end of the range of -cordierite formation, an increase in the water ratio of prehydrolysis was effective because Si-O-Al bondings were introduced into the Mg-Al-Si complex alkoxides. Moon and Kim [16] prepared a cordierite ceramic with a thermally stable pore structure by a simple modification of a sol-gel reaction of alkoxide precursors, synthesized from Mg metal or Mg-acetate, Al(i-Opr)3 and partially pre-

3.1 Synthesis from kaolin by solid state reactions

P. Grosjean [8] studied the talc-clay reaction of different sources and he found 30 mass-% talc and 70 mass-% clay to be an optimum composition as it showed minimum thermal expansion at 1000 C in all test samples fired at 1330 C. Khabas et al [9] studied the synthesis of cordierite in mixtures of magnesia and clay raw materials recovered from deposits in Siberia. The raw materials were mechanically activated using a vibratory centrifugal mill. The synthesis can be brought to completion at lower temperatures under mechanical activation conditions using a cordierite addition.

3 Processing of synthetic cordierite 3.2 Synthesis by solution technique

Many researchers have tried to synthesize cordierite from different starting materials Han and Park [10] synthesized cordierite from inorganic compounds like Mg(NO3)26H2O,

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hydrolyzed Si(OEt)4. The crystallization of -cordierite began at 900 C and -cordierite formed in between 10501250 C. Lee and Kriven [17] synthesized homogenous and stable amorphous type cordierite powder by a solution-polymerization route using polyvinyl alcohol (PVA) solution as polymeric carrier. The bulky, long chain polymeric precursor changed into a very soft and porous powder after calcination at 800 C for 1 h. The calcined powder was attrition milled to get a 30 nm size amorphous cordierite powder with a high specific surface area (181 m2/gm).A dense powder having a relative density of 99 % and a CTE value of 2.1 106/C was found in the process. Awano et al [18] studied the effects of grinding on the synthesis of cordierite where a precursor gel derived from colloidal processing was ground. The calcined ground powder enhances the homogeneity of the resulting powder and causes the accumulation of internal energy as crystal strength; consequently the densities of the sintered bodies increase and the optimum temperature range widens. by the presence of crystalline particles in the fly ash, which jeopardized the viscous flow densification mechanism. These materials have good machinability.

3.5 Other synthetic techniques

Many researchers have worked on the synthesis of cordierite honeycombs and foams through different routes. Oliveira et al [27] fabricated cellular cordierite foams using the polymer foam replication process, where a polyurethane template was infiltrated with slurries containing appropriate binders and ceramic particles, followed by the removal of excess slurry, burning out of the polymer to leave a ceramic replica of the polyurethane and, finally, high temperature sintering. Rheological studies showed that optimum dispersion and stabilization conditions were achieved for aqueous slurries containing 40 vol.-% solids, 2 mass-% bentonite and 0.8 mass-% dispersant. The struts had an angular cross-section and cracks were seen along the cell edges and the cell walls. The density of the sintered foams was 20 % of the struts density. The volumetric shrinkage was approximately 30 % and the linear shrinkage appeared to be isotropic. The synthesis of cordierite from various pre-cursor materials via different routes such as solid-state reaction, solution technique, and viscous flow densification has been reviewed in this part. The sol-gel process has been proved as the low temperature densification process. Cordierite densification occurs gradually from to to at 900, 1100 and 1300 C respectively. The prehydrolysis of the complex alkoxides in sol-gel processing was effective. Geothermic wastes have been shown as a non-conventional source of raw material for the synthesis of cordierite glass-ceramics. The precursor compositions were altered in many cases by the addition of different additives B2O3 as flux; TiO2 as nucleant,and ZrO2 have been used to improve the fracture toughness. The relation between thermal expansion and crystal structure has also been discussed.

3.4 Effect of additives on cordierite synthesis

Low temperature synthesis of cordierite had been tried by Sumi et al [22] from kaolinite and magnesium hydroxide mixtures with boron oxide addition. Boron oxide (B2O3) was added in the form of magnesium borate (2MgOB2O3). The addition of B2O3 promoted densification at 850900 C and accelerated the crystallization of -cordierite. The authors found that the specimen with 3 mass-% B2O3, that was fired at 950 C showed a linear thermal expansion coefficient of ~ 3 106 K1, a bending strength of >200 MPa, and a relative dielectric constant of 5.5 at 1 MHz. Finally, they concluded that these cordierite ceramics may be used as substrate materials for semiconductor interconnection. Torres and Alarcon [23] reported that additions of TiO2 as nucleant and B2O3 as flux to a chosen glass in the cordierite primary phase field of the CaOMgOAl2O3SiO2 quaternary system favoured the crystallization of cordierite as the only crystalline phase with hexagonal prismatic morphology.But the presence of Na2O and K2O as fluxes suppresses its crystallization. This can lead to new glazes for floor tiles with improved mechanical and optical properties. Jung et al [24] studied the effect of pure or stabilized ZrO2 addition on the sintering of cordierite-based ceramics. As ZrO2 content is increased, MOR, fracture toughness, and bulk density of the cordierite ceramics increased along with a decrease in the thermal expansion coefficient. El-Kheshen [25] studied the effect of alumina addition (15 vol.-%) on cristoballite formation in cordieritic glass-ceramic composites prepared from pyrex borosilicate glass and silica. The cristoballite formation decreased with the addition of alumina due to a strong reaction between Al3+ of alumina and K+ of pyrex borosilicate glass. Hence, the material has a low thermal expansion coefficient. A new route for the solid-state reaction synthesis of cordierite with and without the use of a flux was followed by Malachevsky et al [26] by varying the sintering temperatures between 900 and 1400 C. Bi2O3 was proved to be a useful additive for lowering the temperature needed for the reaction to take place.

3.3 Synthesis of cordierite glassceramics

Geiss et al [19] showed that a glassy phase of cordierite can be retained by a rapid quench from the melt and then a fine powder can be prepared by the granulation of the quenched glass. The resultant powder compact can be fully densified by a viscous flow sintering mechanism at a temperature between the glass transition temperature (810 C) and the softening point (860 C). Furthermore crystalline cordierite can be obtained by annealing at a higher temperature. Diaz et al [20] described a new route of cordierite synthesis from geothermic wastes, as the geothermic plants produce a variety of waste materials, which can be purified and used as a non-conventional source of raw materials for making glass ceramics. Two cordierite materials were synthesized by means of de-vitrification time-temperature treatment. TiO2, ZrO2, ZnO, and SrO were used as additives. Boccaccini et al [21] fabricated cordieriteglass matrix composites from fly ash and waste glass. Commercial alumina platelets were reinforced to improve the wear resistance of the material.For fly ash contents up to 20 mass-%,nearly fully dense compacts could be fabricated at a low sintering temperature (650 C). For higher fly ash contents, the densification was hindered

4 Properties of cordierite ceramics

The general properties of cordierite ceramics have been discussed previously in this paper. These key properties of cordierite have made it suitable for various applications. Many researchers have studied the effects of different additives and their amount of additions during the synthesis of cordierite ceramics on the development of these properties. The properties required for any particular application have been developed through proper selection of raw ma-


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terials, mixing them in definite proportions, using additives in definite amount, etc. Different processes of synthesis will lead to the acquisition of definite properties in the cordierite ceramics. Some of these have been discussed in the previous section and will be discussed further in this section. shown to be chiral in nature and the chirality direction is fixed. The sandwich fillingappears in two shapes a thick,well-defined domain at low temperatures and a thin layer of wetting at high temperatures. Matos et al [31] studied the structure of polymeric and polymer-derived ceramic cellular cordierite foams using two different approaches, which were compared. The authors measured the morphological aspects of both structure from images acquired by optical and electron microscopy. In what concerns the cell structure, a relation was observed either in the proportion of the closed faces or in the size distributions of the cells. Average cell diameters ranged from 575 to 715 m in the ceramic foams and 715 to 920 m in case of polymeric foams. The size distributions of the ceramic cells were narrower than those of the respective polymer templates. The authors established a relation between the final ceramic structures and the respective templates and also explained the mechanical behaviour of the foams obtained. Diaz-Mora et al [32] investigated the activation energy and activation enthalpy for crystal growth and viscous flow in a cordierite glass-ceramic by using experimental growth rates and viscosity data. They concluded that the bond breaking and molecular reorientation required for crystallization is comparable to the atomic transport mechanism involved in viscous flow and hence viscosity data may be used to estimate crystal growth rates in glasses. pared the mechanical behaviour of cordieritemullite honeycombs with that of commercial cordierite foam with and without rubber encapsulation. While impact testing, the energy absorption of both the honeycomb and the foam increased upon rubber encapsulation. The rubber-encapsulated honeycomb had shown a substantial decrease in energy absorbed parallel to the channel walls, as opposed to an increase in the perpendicular direction.The foam absorbed less energy than the honeycomb. The critical stress decreased in the honeycomb but increased in foam upon rubber encapsulation.

4.1 Structural evolution

Logvinkov et al [28] analyzed the thermodynamic relation G = f(T) for solid-phase reactions between stoichiometric components of the MgOAl2O3SiO2 system and considered the thermodynamic conjugation of solid-phase reactions.It was shown that the structural changes in the crystal lattice of cordierite should be considered as arising from compositional changes in the corresponding solid solutions rather than from polymorphous transformations. The authors discussed the thermodynamic instability of cordierite and proposed a diagram for phase relations in the subsolidus of the MgOAl2O3SiO2 system. Torres and Alarcon [29] reported the structural evolution of loosely compacted equimolar cobalt-magnesium cordierite glass powder (MgCoAl4Si5O18) with annealing time at temperatures between 900 and 1100 C. The first crystalline phase formed was -cobalt containing cordierite, which transformed to -cordierite with longer annealing. The -cordierite grew by a dendritic mechanism along the particle surface, and the nucleation and growth of -cordierite occurred within the -cordierite dendrites. At the beginning of this transformation, some mullite and cobalt-magnesium aluminate spinels were detected which disappeared on further annealing.After long annealing at 1100 C, some ordering for Al and Si in tetrahedral sites had taken place, indicating some transformation to -cordierite (orthorhombic). After short annealing at 1100 C, the fully crystallized microstructure developed was -cordierite with columnar or linear features.Below Tc,cordierite shows an unusual domain pattern consisting of walls, which are not well oriented along elastic soft directions due to a low spontaneous strain and low anisotropy energies.Hence,there is a competition between the wall due to strain and the wall due to local interactions, which leads to the formation of sandwich walls, an intermediate between these two wall types.Blackburn and Salje [30] tried to simulate the formation of the sandwich walls using an atomistic computer model. These walls are

4.3 Thermal properties

Hasselman et al [36] studied the effect of 15 vol.-% particulate diamond reinforce-ment on the thermal conductivity of a cordierite matrix as a function of diamond particle size from room temperature to 700 C. The thermal conductivity increases with increasing particle size to a maximum of ~75 % for a mean particle size of 50 m. The particle effect was more pronounced at lower than at higher temperatures. The effect of particle size and temperature was attributed to an interfacial thermal barrier, possibly resulting from interfacial phonon scattering, with a positive temperature dependence on interfacial thermal conductance. Garcia et al [37] applied the laser flash method for measuring the thermal diffusivity of highly porous cordierite materials. Errors in the calculation due to the surface roughness were reduced by attaching two thin Cu layers to both surfaces of the samples.Nandi [38] observed the thermal expansion behaviour of boron doped cordierite glass ceramics, where 1, 2, and 3 mass-% B2O3 showed negative expansion in the temperature range of 100300 C. The expansion of the undoped cordierite was positive.A relative decrease in the degree of negative expansion was observed as the B2O3 concentration increased. Johnson et al [39] tried to establish correlations between the cordierite content, processing temperature and CTE values of the samples.A maximum cordierite content of 90 % was achieved for sintering at 1693 K (4 h soaking) corresponding to a lowest CTE of 0.74 106 / K. The authors also showed that the bulk thermal expansion of cordierite honeycombs increases on CaO doping due to the absence of micro-cracks, but the axial anisotropy is reduced. Thermal shock resistance is an important property that predicts the life of cordierite ceramic products in ther-

4.2 Phase transformation and mechanical properties

Yue et al [33] reported that a small amount of B2O3 and P2O5 was found to promote the cordierite to -cordierite transition in low temperature sintered cordierite glass-ceramics prepared by a sol-gel-process.At the higher concentration, the transition occurs at high temperature due to the formation of MgO-P2O5 based compounds. The material has a dielectric constant of less than 5.5 and low dissipation factor, however, the amount of B2O3 and P2O5 has no effect on these properties. Oh et al [34] studied the reaction kinetics, melting endothermal, nucleation and crystallization behaviour of cordierite glasses containing up to 5 mass-% nitrogen by using combined heat flux differential scanning calorimetry and thermo-gravimetric analysis. The authors also discussed the effect of AlN on the stability of the melt, microstructures and the container materials. Jain et al [35] com-

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mal environments used for automobile pollution control as catalytic converters or as diesel particulate filters.Das et al [40] presented a comparative study on the thermal shock resistance of extruded cordierite honeycombs calculated by using CTE, MOE, MOR, etc.
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4.4 Electrical and dielectric properties

Freer and Owate [41] studied some electrical properties of certain cordierite glass ceramics in the system SiO2MgOAl2O3TiO2. High crystallinity, good surface finish, and homogeneous microstructure yielded high break down strength. Sarkar et al [42] studied the effects of firing temperature and test frequency on the dielectric properties of nickel-cordierite,silver-cordierite and titanium-cordierite samples after firing. The values of the dielectric constant and dielectric loss decreased with increasing test frequencies and increasing firing temperature.A low dielectric constant of 2.2 was observed for the nickel-cordierite samples.Wu and Huang [43] studied the effect of crystallization on microwave dielectric properties of stoichiometric cordierite glasses containing B2O3 and P2O5,where two glasses containing 5 mass-% B2O3/ 5 mass-% P2O5 and 7.5 mass-% B2O3/ 7.5 mass-% P2O5 were studied.Both glasses were sintered to nearly full density at temperatures as low as 860 C. Finally the authors concluded that cordierite glass containing cordierite possesses better microwave properties than glassy phase and -cordierite. Concerning the mechanical properties additions of B2O3 and P2O5 in definite proportion have shown an effect on the transition of cordierite from to form at different temperatures. The effect of diamond reinforcement with varying particle size on the thermal conductivity and the alteration of thermal expansion co-efficient of cordierite with the addition of B2O3 has been discussed.In respect of electrical properties,high crystallinity, good surface finish, and homogeneous microstructure yielded high break-down strength. From the studies it can be seen that cordierite glass containing -cordierite possesses better microwave properties than glassy phase and -cordierite.

[1] Ikawa, H., Otagiri, T., Imai, O., Suzuki, M., Urabe, K., Udagawa, S.: J. Amer. Cer. Soc. 69 (1986) [6] 492498 [2] Advanced Technical Ceramics, Edited by

Received: 16.03.2005 (To be continued)


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