Regina Monteiro

The surfaces of cordierite and glass particles were modified by coating them with an alumina precursor using a precipitation process in the presence of urea. Scanning electron microscopy (SEM), high-resolution transmission electron microscopy, X-ray diffraction, electrophoresis, and rheological measurements were used to characterize the coated powders. SEM and transmission electron microscopy morphologies of the coated powders revealed that amorphous and homogeneous coatings have been formed around the particles. The morphology of the coated powders showed a coiled wormlike surface. The coating Al2O3 layer dominated the surface properties of the coated glass and cordierite powders. The influence of the coating layer on the processing ability of cordierite-based glass-ceramics substrates by tape casting was studied in aqueous media. It could be concluded that the coating of the powders facilitates the processing and yields green and sintered tapes with denser, more homogeneous microstructures compared with the uncoated powders.

The effect of initial compaction on the sintering of borosilicate glass matrix composites reinforced with 25 vol.% alumina (Al2O3) particles has been studied using powder compacts that were uniaxially pressed at 74, 200 and 370 MPa. The sintering behaviour of the samples heated in the temperature range 850-1150 °C was investigated by density measurement, axial and radial shrinkage measurement and microstructural observation. The density of the sintered composites increased continuously with temperature for compacts pressed at 74 MPa, while for compacts pressed at 200 and 370 MPa it reached the maximum value at 1050 °C and at higher temperatures it decreased slightly due to swelling. The results showed anisotropic shrinkage behaviour for all the samples, which exhibited an axial shrinkage higher than the radial shrinkage, and the anisotropic character increased with the initial compaction pressure. © 2003 Elsevier Science Ltd. All rights reserved.

The characterization of the bottom ashes produced by two Portuguese municipal solid waste incinerators (MSWI) was performed with the aim of assessing the feasibility of using this waste as raw material in the production of glass that can be further processed as glass-ceramics for application in construction. Density and particle size distribution measurements were carried out for physical characterization. Chemical characterization revealed that SiO2, a network glass former oxide, was present in a relatively high content (52-58 wt%), indicating the suitability for this waste to be employed in the development of vitreous materials. CaO, Na2O and K2O, which act as fluxing agents, were present in various amounts (2-17 wt%) together with several other oxides normally present in ceramic and glass raw materials. Mineralogical characterization revealed that the main crystalline phases were quartz (SiO2) and calcite (CaCO3) and that minor amounts of different alkaline and alkaline-earth aluminosilicate phases were also present. Thermal characterization showed that the decomposition of the different compounds occurred up to 1100 °C and that total weight loss was <10 wt%. Heating both bottom ashes at 1400 °C for 2 h resulted in a melt with suitable viscosity to be poured into a mould, and homogeneous black-coloured glasses with a smooth shiny surface were obtained after cooling. The vitrified bottom ashes were totally amorphous as confirmed by X-ray diffraction. The results from the present experimental work indicate that the examined bottom ashes can be a potential material to melt and to obtain a glass that can be further processed as glass-ceramics to be applied in construction. © 2007 Elsevier Ltd. All rights reserved.

Barium zinc borosilicate glasses with a molar composition xBaO-(60-x)ZnO-30B 2O 3-10SiO 2, where x ranged from 0 to 60 mol%, were prepared using melt-quenching method. The effect of BaO substitution for ZnO on the sintering, crystallization, and dielectric characteristics has been investigated. The behavior of the studied barium zinc borosilicate glasses was mainly determined by the relative amount of the structural modifier oxides (BaO and ZnO) and the ionic size, and field strength of the modifying cations (Ba 2+, Zn 2+). Increased amounts of BaO decreased both glass transition temperature and crystallization temperature, while increasing the relative dielectric constant. Sintering occurred before crystallization for glasses where substitution of BaO for ZnO was up to 30 mol%, but for higher substitution levels, crystallization occurred during the sintering process hindering densification. © 2012 The American Ceramic Society.

A uniform shiny black-coloured glass was obtained using bottom ash produced by a Portuguese municipal solid waste incinerator (MSWI). The bottom ash was the single batch material used in the formation of the glass, which was obtained by vitrification of the solid waste at 1400 °C for 2 h. Under these conditions, a homogeneous melt with an appropriate viscosity to be shaped was obtained, indicating the suitability of this waste material to be employed in the development of vitreous products. The characterization of the resulting glass was performed in order to assess its structural, physical, mechanical, thermal and chemical features. The glass had a density of 2.69 g cm -3, a hardness of 5.5 GPa, a fracture strength of 75 MPa, a thermal expansion coefficient of 9.5 × 10-6 °C-1 and it exhibited a very good chemical stability. In summary, the MSWI bottom ash glass has good mechanical and chemical properties and may, therefore, be used in several applications, particularly as a construction material. © 2005 Elsevier B.V. All rights reserved.

Fly ash from Tapada do Outeiro, a coal power plant in the north of Portugal, has been processed by a powder technology route in order to obtain durable and mechanical resistant ceramics. Dolomite (CaC03.MgC03) was added in different proportions to the waste material, from zero up to 10 wt%, and the effect of this addition on the densification behaviour of the fired samples was investigated by measuring the apparent density, the open porosity and the linear shrinkage. The powder mixtures were uniaxially dry pressed in a steel die and fired at temperatures ranging from 950 to 1150°C XRD and SEM were used to identify the phases present in the sintered materials and the degree of densification. The results revealed that added dolomite was responsible for the appearance of anorthite, an extra phase besides mullite and quartz, for an increase in the amount of liquid phase and for the swelling of closed pores at the highest firing temperatures. Significant morphological changes and phase transformations occurred during sintering and their effects on the physical-mechanical and leaching characteristics of the sintered materials were analyzed.

The possibility of using fly ash and shale as alternative raw materials for the production of structural ceramics was investigated. Fly ash is a by-product from coal-burning power plants, and shale is a sedimentary rock that if ground finely enough can exhibit a clay-like plasticity. Ceramic samples containing 10-50 wt% fly ash were formed from mechanical mixing of both kinds of powders that were packed and sintered in the temperature range 950-1200°C It was verified that powders with larger fly ash content exhibited lower packing density resulting in compacts with a lower sintered density. Although an increase in fly ash content was associated to a larger presence of porosity in the sintered samples, as confirmed by microstructural analysis, all studied compositions when sintered at the highest temperatures exhibited satisfactory values for water absorption (< 10%), for flexural strength (20-64 MPa) and for hardness (20-30 GPa) indicating that they have potential to be applied in the production of structural ceramics.

A range of CaO-Al2O3-SiO2 glasses have been prepared by fusion of pure starting materials in platinum crucibles. Compositions containing large amounts on network formers, Al2O3 and SiO2, are difficult to crystallize. If the amount of network former is reduced, glasses will self-nucleate and crystallize more readily, but the products of crystallization tend to react with water. This conflict has been partly resolved by adding MgO and ZnO and tailoring compositions so as to produce a phase, variously designated "Q" or "pleochroite", ideally Ca20Al32-2 vMg vSivO68, with v close to 4. Pleochroite crystallizes with a typically fibrous morphology. Preliminary experiments on fragments and melt-cast glass rods indicate that these compositions can be heat treated without deformation to yield highly crystalline, transparent ceramics. © 1989 Chapman and Hall Ltd.

In this work, the mechanical characterization of ceramic products processed from red clay with different amounts of added coal fly ash was investigated. Coal fly ash produced by power plants is a waste material that constitutes an alternative source of minerals for the production of traditional building ceramics, as it is a complex mixture of several oxides such as SiO2, Al2O3, CaO, Fe2O3, Na2O, TiO2, which are usually present in the composition of such ceramics. A powder technology and firing route was followed for the processing of the clay and coal fly ash based ceramics. Different proportions of waste (10, 25 and 50%, by weight) were added to red clay, and then the mixed powders were pressed to form compacts that were fired at a selected temperature in the range 850-1,150°C. The effects of waste content and of heating conditions on the microstructure and mechanical characteristics of the obtained materials were investigated. The density, porosity, water absorption, flexural strength, hardness and fracture toughness of the produced materials were evaluated. A comparison was made between the properties of the produced ceramics with those of traditional ceramic materials used in construction, e.g. floor or wall tiles, and it was observed that the clay based products with coal fly ash additions may be used in similar applications. © 2007 Springer Science+Business Media B.V.

This paper presents preliminary results on Al doped ZnO thin films prepared by the solgel method. The thin films were produced by a dip-coater technique on glass substrate, using zinc acetate dihydrate, aluminium chloride hexahydrate, 2-methoxyethanol and monoethanolamine as raw materials. The ZnO thin films were analysed by XRD, Hall effect and SEM measurements. In order to determine the influence of the thermal treatments on the film properties, a set of four different heat treatments (atmosphere and temperature) were studied. All the films are polycrystalline presenting a crystallographic c-axis orientation (002) perpendicular to the substrate. The best results were obtained for films pre-heated at 400°C and post-heated for 1 hour in air at 600°C, after annealing under a reduced atmosphere of forming gas, where a resistivity of 3.9×10-3 Ωcm, a Hall mobility of 34.1 cm2/Vs, a carrier concentration of 4.7×1019 cm-3 and an optical transmittance of 90% were achieved.

This paper presents the effect of post-heating temperature and atmosphere on the electrical and optical properties of ZnO:Al thin films prepared by the sol-gel method. The electrical properties of the n-type semiconductor thin films showed that for the final films, the values of carrier concentration ranged between 2.76 and 9.96 × 1019 cm- 3, the Hall mobility values between 7 and 34.1 cm2/V s and the resistivity values between 2.9 × 10- 3 and 5.0 × 10- 2 Ω cm, depending on the processing conditions. For the thin film doped with 2 wt.% Al, preheated at 400 °C and post-heated for 1 h in air at 600 °C, a resistivity of 2.9 × 10- 3 Ω cm has been reached after annealing under a reducing atmosphere of forming gas. The optical transmittance spectra of the only post-heated films and of the post-heated and annealed films showed a good transmittance (75-90%) within the visible wavelength region and some small effects of Al-doping concentration and annealing treatment in forming gas. © 2005 Elsevier B.V. All rights reserved.

The isoconversional methods (Friedman (FR), Flynn-Wall-Ozawa (FWO) and Kissinger-Akahira-Sunose (KAS)) were applied for evaluating the dependencies of the activation energy (E) on the mass loss (Δm) corresponding to the non-isothermal decomposition of two Zn acetate-based gel precursors for ZnO thin films whose preparation differs by the drying temperature of the liquid sol-precursor (125°C for sample A, and 150°C for sample B). Although both investigated samples exhibit similar decomposition steps, strong differences between E vs. Δm curves as well as among the characteristic parameters of the decomposition steps, directly evaluated from TG, DTG and DTA curves, were put in evidence. © 2007 Springer Science+Business Media LLC.

Transparent and conductive high preferential c-axis oriented ZnO thin films doped with Al have been prepared by sol-gel method using zinc acetate and aluminium chloride as cations source, 2-methoxiethanol as solvent and monoethanolamine as sol stabilizer. Film deposition was performed by dip-coating technique at a withdrawal rate of 1.5 cm min-1 on Corning 1737 glass substrate. The effect of dopant concentration, heating treatment and annealing in reducing atmosphere on the microstructure as well as on the electrical and optical properties of the thin films is discussed. The optical transmittance spectra of the films showed a very good transmittance, between 85 and 95%, within the visible wavelength region. The minimum resistivity of 1.3 × 10-3 Ω cm was obtained for the film doped with 2 wt.% Al, preheated at 400 °C and post-heated at 600 °C, after annealing under a reduced atmosphere of forming gas. © 2003 Elsevier B.V. All rights reserved.

Various metal oxide-silica nanocomposite films have been recently proposed as gas-sensitive materials. This paper presents results on cobalt oxide-SiO2 mesoporous nanocomposite thin films templated by a cationic surfactant. The films were deposited on glass substrate by dip-coating process, using [Co(CH3COO)2]·4H2O and tetraethoxysilane (TEOS) as starting materials. The effect of withdrawal speed, number of layers and thermal treatment on the crystalline structure, morphology, Co-doping states, optical, electrical and gas sensing properties of the thin films has been investigated using X-ray diffraction, atomic force microscopy, X-ray photoelectron spectroscopy, optical transmittance and room temperature photoreduction-oxidation data. © 2007 Elsevier B.V. All rights reserved.

The thermal decomposition and crystallization behaviour of a sol-gel precursor used for the preparation of c-axis oriented Al-doped ZnO thin films were investigated in the temperature range 20-600°C by TG-DTA, IR spectroscopy and XRD analysis. At low temperature, the formation of ZnO crystallites from the sol precursor, prepared by dissolving Zn(CH 3COO)2·2H2O and AlCl 3·6H2O in 2-methoxyethanol and monoethanol amine, takes place via zinc carbonate hydroxide (sclarite/hydrozincite) and occurs simultaneously with the decomposition of this intermediary compound, which occurs above 150°C. At 200°C, the crystalline structure is well defined in terms of ZnO hexagonal lattice parameters, although an important amount of residual organic compounds and water was not yet removed. Increasing the treatment temperature up to 300, 400 and 600°C leads to a gradual removal of the residual organic compounds and therefore to a small change of the ZnO crystalline structure in terms of lattice parameters and grain size.

The kinetics of crystallization of transparent and conductive high preferential c-axis oriented Aldoped ZnO thin films on Corning 1737 glass substrate from amorphous sol-gel precursor prepared using zinc acetate and aluminum chloride as cations source, 2-methoxiethanol as solvent and monoethanolamine as sol stabilizer has been investigated. The effect of preheating temperature on the values of the kinetic parameters and crystallization mechanism is discussed. Some data concerning the microstructure, the electrical and optical properties of the thin films are presented.

The thermoreactivity of a zinc acetate non-alkoxide solution used for the preparation of ZnO-based thin films was investigated in the temperature range 20-600°C by TG-DTA, XRD and SEM data. We found that the formation in air of ZnO crystallites from the sol-gel precursor occurs above 150°C simultaneously with the decomposition of an intermediary compound, most probably carbonate hydroxide (sciante and/or hydrozincite). At 200°C, the crystalline structure is well defined in terms of ZnO hexagonal lattice parameters, although residual organic compounds and water were not yet fully removed and an amorphous phase coexists. A kinetic investigation on the thermal decomposition of sol-gel precursor from DTA data using Kissinger differential equation is also presented. Apparent activation energy values of about. 100 kJ mol-1 corresponding to the non-isothermal decomposition of solid precursors in the temperature range 170-250°C have been found.

The paper presents the properties of zinc oxide thin films deposited on glass substrate via dip-coating technique. Zinc acetate dehydrate, ethanol and monoethanol amine were used as starting materials and N2 gas was used as thermal annealing atmosphere for film crystallization. The effect of withdrawal speed on the crystalline structure, morphology, zinc and nitrogen chemical states, optical, electrical and gas-sensing properties of the thin films has been investigated using X-ray diffraction, atomic force microscopy, X-ray photoelectron spectroscopy, optical transmittance and photoreduction-ozone reoxidation data. © 2007 Elsevier B.V. All rights reserved.