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Musat, V. a, B. b Teixeira, E. b Fortunato, R. C. C. b Monteiro, and P. c Vilarinho. "Al-doped ZnO thin films by sol-gel method." Surface and Coatings Technology. 180-181 (2004): 659-662. AbstractWebsite

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.

Ribeiro, A. S. M. a, R. C. C. b Monteiro, E. J. R. a Davim, and M. H. V. a Fernandes. "Ash from a pulp mill boiler-Characterisation and vitrification." Journal of Hazardous Materials. 179 (2010): 303-308. AbstractWebsite

The physical, chemical and mineralogical characterisation of the ash resulting from a pulp mill boiler was performed in order to investigate the valorisation of this waste material through the production of added-value glassy materials. The ash had a particle size distribution in the range 0.06-53μm, and a high amount of SiO2 (∼82wt%), which was present as quartz. To favour the vitrification of the ash and to obtain a melt with an adequate viscosity to cast into a mould, different amounts of Na2O were added to act as fluxing agent. A batch with 80wt% waste load melted at 1350°C resulting in a homogeneous transparent green-coloured glass with good workability. The characterisation of the produced glass by differential thermal analysis and dilatometry showed that this glass presents a stable thermal behaviour. Standard leaching tests revealed that the concentration of heavy metals in the leaching solution was lower than those allowed by the Normative. As a conclusion, by vitrification of batch compositions with adequate waste load and additive content it is possible to produce an ash-based glass that may be used in similar applications as a conventional silicate glass inclusively as a building ecomaterial. © 2010 Elsevier B.V.

Lima, M. M., and R. Monteiro. "Characterisation and thermal behaviour of a borosilicate glass." Thermochimica Acta. 373 (2001): 69-74. AbstractWebsite

The changes occurring during the heating of a borosilicate glass have been investigated by differential thermal analysis, dilatometric analysis and thermomechanical analysis. The thermal properties of this glass, such as glass transition temperature, dilatometric softening temperature and linear thermal expansion coefficient, have been determined. Viscosity measurements in the temperature range 898-1048 K were performed in a thermomechanical analyser equipped with a penetration attachment for isothermal measurement, and from the temperature dependence of viscosity a value of 290 kJ mol-1 was obtained for the activation energy for viscous flow. Devitrification of the glass was observed, specifically in finely powdered glass samples, where the precipitation of cristobalite was identified by X-ray diffraction. Glass powder compacts sintered by viscous flow and cristobalite precipitation reduced strongly the shrinkage rate. © 2001 Elsevier Science B.V.

Monteiro, R. C. C. a, C. F. a Figueiredo, M. S. a Alendouro, M. C. b Ferro, E. J. R. b Davim, and M. H. V. b Fernandes. "Characterization of MSWI bottom ashes towards utilization as glass raw material." Waste Management. 28 (2008): 1119-1125. AbstractWebsite

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.

Kullberg, A. T. G., A. A. S. Lopes, J. P. B. Veiga, and R. C. C. Monteiro. "Crystal growth in zinc borosilicate glasses." Journal of Crystal Growth. 457 (2017): 239-243. AbstractWebsite

Glass samples with a molar composition (64+x)ZnO–(16−x)B2O3–20SiO2, where x=0 or 1, were successfully synthesized using a melt-quenching technique. Based on differential thermal analysis data, the produced glass samples were submitted to controlled heat-treatments at selected temperatures (610, 615 and 620 °C) during various times ranging from 8 to 30 h. The crystallization of willemite (Zn2SiO4) within the glass matrix was confirmed by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). Under specific heat-treatment conditions, transparent nanocomposite glass-ceramics were obtained, as confirmed by UV–vis spectroscopy. The influence of temperature, holding time and glass composition on crystal growth was investigated. The mean crystallite size was determined by image analysis on SEM micrographs. The results indicated an increase on the crystallite size and density with time and temperature. The change of crystallite size with time for the heat-treatments at 615 and 620 °C depended on the glass composition. Under fixed heat-treatment conditions, the crystallite density was comparatively higher for the glass composition with higher ZnO content. © 2016 Elsevier B.V.

Soares, R. S. a, R. C. C. a Monteiro, A. A. S. a Lopes, M. M. R. A. a Lima, B. A. b Sava, and M. b Elisa. "Crystallization and microstructure of Eu3 +-doped lithium aluminophosphate glass." Journal of Non-Crystalline Solids. 403 (2014): 9-17. AbstractWebsite

A transparent Eu3 +-doped lithium aluminophosphate glass was prepared by melt-quenching technique. The thermal behavior of the glass was investigated by differential thermal analysis (DTA), the structure was studied by X-ray diffraction (XRD) and the morphology was observed by optical polarization microscopy and scanning electron microscopy (SEM). The activation energy of glass transition and the activation energy of crystallization and Avrami exponent have been evaluated under non-isothermal conditions from the data obtained by DTA at different heating rates. DTA curves exhibited an endothermic peak associated with the glass transition and two exothermic peaks. The mean value calculated for the activation energy of glass transition was 545 kJ mol- 1. The activation energy of crystallization was   400 kJ mol- 1 for the first exothermic peak and   170 kJ mol- 1 for the second peak. The Avrami exponent was   1 for both peaks indicating surface crystallization. XRD results showed that the main crystalline phase, aluminum metaphosphate, Al(PO3)3, and aluminum phosphate, AlPO4, were formed together with lithium barium phosphate, Li 3Ba(PO3)7, during the first exothermic peak and together with barium pyrophosphate, Ba2P2O7, during the second peak. Morphological study of heat-treated glass samples revealed microstructural features that confirmed a surface crystallization process. © 2014 Elsevier B.V.

Lopes, A. A. S. a, R. C. C. a Monteiro, R. S. a Soares, M. M. R. A. a Lima, and M. H. V. b Fernandes. "Crystallization kinetics of a barium-zinc borosilicate glass by a non-isothermal method." Journal of Alloys and Compounds. 591 (2014): 268-274. AbstractWebsite

The crystallization kinetics of a glass with a molar composition 40BaO-20ZnO-30B2O3-10SiO2 was investigated. The kinetic parameters, activation energy for crystallization (Ec) and Avrami exponent (n), were evaluated under non-isothermal conditions using the results obtained by differential thermal analysis (DTA) performed at different heating rates. DTA curves exhibited two overlapping exothermic peaks associated with the crystallization of the glass. Barium borate (BaB4O 7) was the first crystalline phase to be formed and it was followed by the formation of barium zinc silicate (BaZnSiO4), as identified by XRD. For the first exothermic peak, when the fraction of crystallization (χ) increased from 0.1 to 0.9, the local activation energy (E c(χ)) decreased from 700 to 500 kJ/mol, while for the second exothermic peak, Ec(χ) slightly increased from 490 to 570 kJ/mol. For the range of 0.1 < χ < 0.9, the local Avrami exponent (n(χ)) increased from ∼1 to 1.4 for the first exothermic peak and it decreased from ∼1.7 to 1.4 for the second exothermic peak. Observation by SEM of the microstructure of sintered glass samples revealed that crystallization started at the surface of glass particles, with growth of lamellar crystallites, that together with some quasi-spherical nano-sized crystallites progressed towards the inside of the glass at the highest sintering temperatures. The change of the local activation energy with the fraction of crystallization suggested that a multi-step kinetic reaction took place during sintering and crystallization of the glass. © 2013 Elsevier B.V. All rights reserved.

Lima, M. M. R. A., and R. C. C. Monteiro. "Crystallization of a borosilicate glass during sintering studied by dilatometry and XRD analysis." Materials Science Forum. 455-456 (2004): 212-215. AbstractWebsite

The crystallization of a borosilicate glass, when compacts of powdered glass were sintered under various conditions, was investigated by dilatometric and XRD analysis. The dilatometry results from non-isothermal sintering experiments until 800°C, performed at different heating rates (1, 2, 5, 8 and 10°C/min), revealed that the compacts started to shrink above ∼ 600°C and that the shrinkage decreased with the increase of the heating rate for temperatures up to ∼750°C. Above this temperature, and specifically when the samples were heated at heating rates < 5°C /min, the shrinkage was hindered, while samples heated at heating rates ≥ 5°C/min showed continuous shrinkage. XRD results showed that the formation of cristobalite had occurred during the sintering at the lowest heating rates and therefore, the presence of this crystalline phase was affecting the shrinkage of the compacts, inhibiting further sintering of the glass. The crystallization of the glass when sintered at a temperature in the range 700-850°C and hold at the selected temperature during various times was also analysed. XRD results showed that both cristobalite and quartz were present in glass compacts sintered under particular conditions (for example, after heating during 24h at 725°C and 765°C). Quartz dissolution took place when the glass samples were sintered at 850°C. At this temperature and whatever the sintering time, cristobalite was the only crystalline phase present in the sintered compacts.

Monteiro, R. C. C., F. P. Glasser, and E. E. Lachowski. "Crystallization of CaO-Al2O3-SiO2 and CaO-MO-Al2O3-SiO2 (M=Mg, Zn) glasses." Journal of Materials Science. 24 (1989): 2839-2844. AbstractWebsite

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.

Soares, R. S., R. C. C. Monteiro, M. M. R. A. Lima, and R. J. C. Silva. "Crystallization of lithium disilicate-based multicomponent glasses - Effect of silica/lithia ratio." Ceramics International. 41 (2014): 317-324. AbstractWebsite

Two glass compositions were prepared from the system SiO2-Li2O-K2O-ZrO2-P2O5 with different SiO2/Li2O ratio (2.39 and 3.39) and the crystallization behavior was investigated by differential thermal analysis (DTA), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The crystallization kinetic parameters (activation energy of crystallization and Avrami exponent) were evaluated by different methods from the data obtained by DTA performed at different heating rates. For both glasses, two exothermic peaks were observed in the DTA curves, and the crystallization peak temperatures increased with SiO2/Li2O ratio. XRD analysis revealed that the first peak corresponds to the crystallization of lithium metasilicate (Li2SiO3) and the second to the formation of lithium disilicate (Li2Si2O5). After heating the glasses at a temperature above the second crystallization peak (900 °C), both Li2Si2O5 and Li2SiO3 were found in samples having the lowest SiO2/Li2O ratio, whereas no Li2SiO3 was detected in samples with the highest SiO2/Li2O ratio. For both glasses, the value obtained by different methods for the activation energy of crystallization was in the range of 225-275 kJ mol-1 for the first exothermic peak and in the range of 425-500 kJ mol-1 for the second peak. The estimated Avrami exponent was close to 1 for the first exothermic peak, indicating surface crystallization, and close to 3 for the second exothermic peak, suggesting volume crystallization. This was confirmed by the morphological study made by SEM that showed needle-like crystals in the microstructure of samples with lithium metasilicate and granular crystals in the microstructure of samples having lithium disilicate. © 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

PerdigãO, J. a, A. M. b Pinto, R. C. C. c Monteiro, F. M. c Braz Fernandes, P. b Laranjeira, and J. P. c Veiga. "Degradation of dental ZrO 2-based materials after hydrothermal fatigue. part I: XRD, XRF, and FESEM analyses." Dental Materials Journal. 31 (2012): 256-265. AbstractWebsite

The aim was to investigate the effect of simulated low-temperature degradation (s-LTD) and hydrothermal fatigue on the degradation of three ZrO2-based dental materials. Lava, IPS, and NanoZr discs were randomly assigned to (1) Control-Storage in distilled water at 37°C; (2) Aging at 134°C for 5 h (s-LTD); (3) Thermocycling in saliva for 30,000 cycles (TF). XRD revealed that ZrO 2 m phase was identified in all groups but TF increased the m phase only for Lava. Under the FESEM, Lava showed no alterations under s-LTD, but displayed corrosion areas up to 60 μm wide after TF. We conclude that TF accelerated the degradation of Lava through an increase in the m phase and grain pull-out from the material surface.

Monteiro, R. C. C. a, S. J. G. a Alendouro, F. M. L. a Figueiredo, M. C. b Ferro, and M. H. V. b Fernandes. "Development and properties of a glass made from MSWI bottom ash." Journal of Non-Crystalline Solids. 352 (2006): 130-135. AbstractWebsite

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.

Monteiro, R. C. C., M. M. R. A. Lima, and C. S. Clemente. "Development of structural ceramics from fly ash and shale." Materials Science Forum. 587-588 (2008): 787-791. AbstractWebsite

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.

Monteiro, R. C. C., and M. M. R. A. Lima. "Effect of compaction on the sintering of borosilicate glass/alumina composites." Journal of the European Ceramic Society. 23 (2003): 1813-1818. AbstractWebsite

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.

Monteiro, R. C. C., C. S. Mota, and M. M. R. A. Lima. "Effect of dolomite addition on the densification of fly ash based ceramics." Materials Science Forum. 514-516 (2006): 1711-1715. AbstractWebsite

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.

Ferro, M. C. a, M. H. V. a Fernandes, and R. C. C. b Monteiro. "Effect of heat treatment on the microstructure of fly ash derived glass ceramics." Glass Technology. 46 (2005): 151-154. AbstractWebsite

Mixtures of fly ash, calcite and soda ash were prepared by keeping the amount of fly ash at 80 wt% and adding the other raw materials in order to obtain Na2O/CaO ratios of 1/3, one and three. On melting all mixtures led to black glassy materials. Several heat treatments were performed on these glasses at temperatures suggested by DTA. The crystalline phases precipitated during the heat treatments were identified by XRD on powdered samples and the microstructures of the obtained glass ceramics were observed by SEM. The formulations tended to precipitate pyroxene solid solutions and aluminium silicates of calcium and/or sodium, during the heat treatments. The glass ceramics mainly contained fine crystals. However some of the materials obtained from glasses with Na2O/CaO ratios of 1/3 and three had non-uniform microstructures. It is generally concluded that the microstructure of these crystallised glasses is critically dependent on both composition and heat treatment.

Lima, M. M. R. A., L. F. C. Braz, R. C. C. Monteiro, and JP Veiga. "Effect of phosphogypsum on the clinkerization temperature of portland cement clincker." Materials Science Forum. 730-732 (2013): 94-99. AbstractWebsite

Phosphogypsum (PG) is a pollutant residue resulting from the production of phosphoric acid in the phosphated fertilizers industry. About 180 millions of tons of PG are generated worldwide per year, which originates storage problems because of the environmental restrictions and the high costs of storage spaces. Taking into account the mineralizer properties of PG it has been studied a way to valorize this residue as an alternative material in the production of Portland cement clinker. The PG and the raw-materials (limestone, marl, sand and iron oxide) were chemical, mineralogical and thermally characterized by X-ray fluorescence (XRF), X-ray diffraction (XRD) and differential thermal analysis and termogravimetric analysis (DTA/TGA). After milling, the phosphogypsum was mixed with the raw-materials in different amounts up to 10% weight. The raw mixtures were submitted to two types of firing schedules, heating up to 1500°C without any holding time or heating up to 1350°C and holding for 20 minutes. After firing, the clinkers were analyzed by optical microscopy, milled and characterized in terms of chemical and mineralogical compositions. The clinkers were used to produce cement mortar according to NP EN 196-1 standard. The resultant test specimens were mechanically tested at 2 and 28 days according to the same standard. The obtained results show a reduction of about 140°C in the clinkerization temperature, when a raw mixture with 5% phosphogypsum was used. Standard clinkers, without phosphogypsum addition, which were fired at 1500°C, originated test specimens with a compressive strength of 48.1MPa at 28 days. Test specimens produced with clinker containing 5% phosphogypsum present higher compressive strength values at 28 days, being 55.1MPa for clinkers produced at 1500°C, and 49.4 MPa for clinkers produced at 1350°C. © (2013) Trans Tech Publications, Switzerland.

Musat, V. a, B. b Teixeira, E. b Fortunato, and R. C. C. b Monteiro. "Effect of post-heat treatment on the electrical and optical properties of ZnO:Al thin films." Thin Solid Films. 502 (2006): 219-222. AbstractWebsite

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.

Barbosa, A. R. J. a, A. A. S. a Lopes, S. I. H. a Sequeira, J. P. a Oliveira, A. b Davarpanah, F. b Mohseni, V. S. b Amaral, and R. C. C. a Monteiro. "Effect of processing conditions on the properties of recycled cathode ray tube glass foams." Journal of Porous Materials. 23 (2016): 1663-1669. AbstractWebsite

Cathode ray tube glass waste was used to produce glass foams by a powder sintering route. The glass waste powder was mixed with small amounts (5 and 8 wt%) of coal fly ash, which acted as foaming agent, and the compacts of the mixed powders were heated at different sintering temperatures in the range 600–800 °C for various dwell times (30–120 min). The effect of the different processing conditions on the microstructural characteristics (porosity, pore size and pore size distribution), mechanical resistance and thermal conductivity of the produced foams was investigated. The volume of pores tended to increase with sintering temperature and time, and glass foams (with a porosity higher than 50 %) were only achieved after sintering at 750 °C. The average pore size increased with sintering temperature and dwell time, and pore growth was particularly accentuated at 800 °C, where coalescence of the pores occurred, with a consequent decrease in compressive strength. Selected combinations of the sintering temperature, dwell time and foaming agent led to glass foams with a satisfactory microstructural homogeneity, which exhibited mechanical strength and thermal conductivity values similar to commercial foams used as thermal insulating materials. © 2016, Springer Science+Business Media New York.

Muşat, V. a, B. b Teixeira, E. b Fortunato, R. C. C. b Monteiro, and P. c Vilarinho. "Effect of thermal treatment on the properties of sol-gel derived Al-doped ZnO thin films." Materials Science Forum. 455-456 (2004): 16-19. AbstractWebsite

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.

Ferro, M. C. a, M. H. V. a Fernandas, C. F. M. L. b Figueiredo, M. S. J. G. b Alendouro, and R. C. C. b Monteiro. "Effect of TiO2 on the crystallization of fly-ash based glass-ceramics." Materials Science Forum. 455-456 (2004): 831-834. AbstractWebsite

A batch of coal fly-ash, soda and lime was melted, quenched to a glass and then devitrified, by one-step heating cycles, forming coarse fibrous microstructures with pores and cracks, resulting in low strength materials. The crystallization behaviour of the based glass was further studied by adding a nucleating agent, TiC2. The resulting structural and microstrutural changes were investigated by differential thermal analysis, scanning electron microscopy, x-ray diffraction, dilatometry and density measurements. The results indicated that the addition of TiO2 could provide a finer grained microstructure, suitable for the production of structural materials.

Nico, C. a, M. P. F. a Graça, M. b Elisa, B. A. b Sava, R. C. C. c Monteiro, L. a Rino, and T. a Monteiro. "Effects of ultraviolet excitation on the spectroscopic properties of Sm3+ and Tb3+ doped aluminophosphate glasses." Optical Materials. 35 (2013): 2382-2388. AbstractWebsite

Li2O-BaO-Al2O3-La2O 3-P2O5 glasses optically activated with rare earth ions with the 4f5, and 4f8 electronic configuration (Sm3+ and Tb3+, respectively) were analyzed by Raman spectroscopy, absorption, excitation photoluminescence, decay curves and temperature dependent photoluminescence. The spectroscopic characteristics of the as-prepared and heat treated samples at temperatures below and above T g were studied as well as their room temperature photometric properties under ultraviolet excitation. All the doped glasses exhibit typical signatures of the lanthanides in their trivalent charge state. For the samarium doped glass heat treated at 250 C (<Tg) the Sm2+ luminescence was also observed. The analysis of the luminescence efficiency was performed in the interval range of 14 K to room temperature, where the integrated intensity of the luminescence was found to decrease for the Sm 3+ and Tb3+ ions in the studied temperature range. Luminescence decay curves were found to be non-exponential for the 4G5/2 → 6H7/2 and 5D3 → 7F4 transitions of the Sm3+ and Tb3+ ions, respectively. The results strongly suggest the occurrence of energy transfer processes through cross relaxation phenomena, mediated by dipole-dipole interaction in all the studied samples. The decay of the 5D4 → 7F5 emission of the Tb3+ ions was found to be single exponential with a time constant of ∼3.1 ms. Based on the spectroscopic characteristics, models for recombination processes are proposed. The room temperature luminance photometric properties with ultraviolet excitation show that the samarium doped glasses have much lower luminance intensity (around 0.3 Cd/m2) when compared with the 6-7 Cd/m2 observed for the terbium doped ones. © 2013 Elsevier B.V. All rights reserved.

Nico, C. a, R. a Fernandes, M. P. F. a Graça, M. a Elisa, B. A. b Sava, R. C. C. c Monteiro, L. a Rino, and T. a Monteiro. "Erratum: Eu3+ luminescence in aluminophosphate glasses (Journal of Luminescence (2014) 145 (582-587))." Journal of Luminescence. 161 (2015): 465. AbstractWebsite
Nico, C. a, R. a Fernandes, M. P. F. a Graça, M. b Elisa, B. A. b Sava, R. C. C. c Monteiro, L. a Rino, and T. a Monteiro. "Eu3+ luminescence in aluminophosphate glasses." Journal of Luminescence. 145 (2014): 582-587. AbstractWebsite

With a 4f6 electronic configuration, europium ions in the trivalent charge state are known to be efficient activators in wide band gap matrices. Embedded in the aluminophosphate (Li2O-BaO-Al 2O3-La2O3-P2O 5) glasses the optically activated Eu3+ ions lead to intense room temperature orange/red luminescence with 16-23 Cd/m2 by using ultraviolet pumping. The as-prepared and heat treated europium doped glasses for temperatures below and above Tg were studied by room temperature Raman spectroscopy, absorption, photoluminescence excitation, temperature dependent and time dependent photoluminescence. When the samples are excited by 325 nm wavelength photons, an enhancement of the red luminescence intensity by ca. one order of magnitude was found to occur for temperatures between 14 K and 350 K, for all the doped glasses. On the other hand, by using resonant excitation on the 5L6 Eu3+ excited state (λexc 390 nm) the ion emission intensity was found to be nearly constant for temperatures up to 500 K. For higher temperatures a steeper decrease of the luminescence intensity occurs due to non-radiative competitive channels described by activation energies of ca. 235 meV and 450 meV by using 325 and 390 nm wavelength photons as excitation, respectively. The lifetime of the 5D0 level in these glasses is ca. 2.93 ms. A discussion of the thermal population and de-excitation mechanisms is performed. © 2013 Elsevier B.V.

Ferro, M. C., C. Leroy, R. C. C. Monteiro, and M. H. V. Fernandes. "Fine-grained glass-ceramics obtained by crystallisation of vitrified coal ashes." Key Engineering Materials. 230-232 (2002): 408-411. AbstractWebsite

Coal fly ashes have been vitrified by melting with Na2O and CaO as fluxing additives. Adequate heat treatments on the fly ash derived glass produced attractive dark green glass-ceramics. These glass-ceramics exhibited fine-grained microstructures consisting of esseneite and nepheline crystals, with average size below 200 nm, homogeneously dispersed in a residual glassy matrix. Several properties, such as density, thermal expansion coefficient, bending strength, hardness and brittleness index were determined and the correlation microstructure-properties is discussed. The results suggest that these coal ash-based glass-ceramics have potential applications as structural materials or as cladding materials.