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Alendouro, M. S. J. G. a, R. C. C. a Monteiro, C. F. M. L. a Figueiredo, R. M. S. a Martins, R. J. C. a Silva, M. C. b Ferro, and M. H. V. b Fernandas. "Microstructural characterization and properties of a glass and a glassceramic made from municipal incinerator bottom ash." Materials Science Forum. 455-456 (2004): 827-830. AbstractWebsite

A glass was made using bottom ash produced by a Portuguese municipal solid waste (MSW) incinerator. The bottom ash was the single batch material used in the formation of the glass, which was obtained through a conventional melt-quenching method. The glass was then converted to glass-ceramic for further recycling to construction materials. After submitting the glass samples to several heat treatments, between 820 and 1050°C and during different times, it was verified that the optimum heat treatment schedule for the ceramization of the glass was at 1000°C for 10h, as confirmed by microstructural observation and by X-ray diffraction. The major crystalline phases precipitated in the glass-ceramic were wollastonite (CaSiO3) and diopside (Ca(Mg,Al)(Si,Al)2O6). Microstructural analysis of the glass-ceramic revealed that the crystalline phases were present as dendrites and fiber-like structures that were homogeneously distributed in the material. The glassceramic showed good mechanical properties with a hardness of 5.6 MPa and a bending strength of 101 MPa. This material had a density of 2.8 gcm-3 and a thermal expansion coefficient of 9.10-6°C-1. The glass and the glass-ceramic showed an excellent chemical stability against leaching in acidic solution and in alkaline solution. In summary, both the glass and the glass-ceramic have good chemical and mechanical properties and can, therefore, be applied as construction materials.

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.

Barbosa, A. R. a, A. a Lopes, R. a Monteiro, and F. b Castro. "Use of different inorganic solid wastes to produce glass foams." Wastes: Solutions, Treatments and Opportunities - Selected Papers from the 3rd Edition of the International Conference on Wastes: Solutions, Treatments and Opportunities, 2015. 2015. 25-30. Abstract

Cathode Ray Tube (CRT) waste glasses produced from dismantling TV sets were used to prepare glass foams by a simple and economic processing route, consisting of a direct sintering process of mixtures of CRT waste as glass powder with different foaming agents (coal fly ash and limestone quarrying residues). The influence of firing temperature, amount and type of foaming agent on the apparent density, pore size distribution and compressive strength have been studied. The aim of the work was to investigate the possibility to obtain glass foams using exclusively wastes as starting materials, and therefore replacing the conventional raw materials. © 2015 Taylor & Francis Group, London.

Davim, E. a, M. H. V. a Fernandes, and R. C. C. b Monteiro. "Glass-ceramics produced from incinerated municipal solid waste." Glass Technology: European Journal of Glass Science and Technology Part A. 48 (2007): 164-167. AbstractWebsite

A homogeneous black coloured glass was obtained by melting the bottom ashes produced by a municipal solid waste incinerator at 1300°C for 2 h without any chemical additives. Based on thermal analysis data glass-ceramics were produced by heat treating the glass, doped with additional TiO2 as a nucleating agent, at temperatures between 870 and 1000°C. The crystalline phases precipitated during the heat treatments were identified by powder XRD and the microstructures were examined using SEM. After a heat treatment at 900°C for 2 h, the glass was converted into a fine grained glass-ceramic with uniform microstructure. The major crystalline phases precipitated in the glass-ceramics were augite (Ca(Mg,Fe)Si2O6), gehlenite (Ca2Al2SiO7) and clinopyroxene (Ca(Ti,Mg,Al)(Si,Al)2O6). Preliminary evaluation of the mechanical and chemical properties of the bottom ash glasses and glass-ceramics suggest that they have potential to compete with existing natural and commercial outdoor cladding materials.

Drasovean, R. a, R. b Monteiro, E. b Fortunato, and V. c Musat. "Optical properties of cobalt oxide films by a dipping sol-gel process." Journal of Non-Crystalline Solids. 352 (2006): 1479-1485. AbstractWebsite

Cobalt oxide thin films were prepared by using the dipping sol-gel process. The films were deposited onto glass slides, starting from methanolic solution of cobalt acetate Co(CH3COO)2 · 4H2O. The effects of film thickness and sol concentration on structural and optical properties were studied. Structural analyses of Co3O4 films were performed by X-ray diffraction. The film thickness was varied by using different withdrawal speeds and the number of dipping-heating cycles. It was found that the grain size increases with the number of dipping N. The results point out to some compacting effect that increases with the number of dippings: the films exhibit direct and indirect optical transition, absorption coefficients are of the order of 104 cm-1, and upon annealing the absorption coefficient increases. © 2006 Elsevier B.V. All rights reserved.

Drasovean, R. a, R. b Monteiro, and M. c Cherif. "Structure and morphology study of cobalt oxide doped silica nanocomposite films." AIP Conference Proceedings. Vol. 1203. 2010. 483-488. Abstract

Cobalt oxide doped silica films were synthesized by a dip-coating technique. Initial compounds were cobalt acetate Co(CH3COO)2-4H 2O and tetraethoxysilane Si(OC2H5)4. The chemical composition was studied by X-ray diffraction and UV-Vis spectroscopy. The morphology analyses were carried out by means of atomic force microscopy. The average diameter of cobalt oxide dispersed particles increases with the molar ratio Co:Si and with the aging time of the initial colloidal solution. © 2009 American Institute of Physics.

Elisa, M. a, B. A. a Sava, I. C. a Vasiliu, R. C. C. b Monteiro, J. P. B. Veiga, L. a Ghervase, I. a Feraru, and R. a Iordanescu. "Optical and structural characterization of samarium and europium-doped phosphate glasses." Journal of Non-Crystalline Solids. 369 (2013): 55-60. AbstractWebsite

The work deals with optical and structural properties of aluminophosphate glasses from Li2O-BaO-Al2O3-La 2O3-P2O5 system containing Sm 3 + and Eu3 + ions. X-ray fluorescence (XRF) has been used to establish the elemental composition of these materials. The influence of Sm3 + and Eu3 + ions on the optical properties of these glasses has been investigated in relation with their structural characteristics. The optical behavior of these materials has been studied by ultra-violet-visible (UV-Vis) spectroscopy, revealing absorption maxima specific to the doping ions. Structural information via vibration modes was provided by Fourier Transform Infrared (FTIR) absorption spectra evidenced as POP symmetrical and asymmetrical stretching vibration modes, POP bend, PO 2- symmetrical and asymmetrical stretching vibration modes, PO stretching vibration mode and POH water absorbance. Raman spectra acquired by 514.5 nm laser excitation disclosed peaks specific to metaphosphate network. Information about the elemental compositional homogeneity of Sm 3 + and Eu3 +-containing glasses as well as about the defects of the doped-glasses is revealed by scanning electron microscopy/energy dispersive spectrometry (SEM/EDS). Fluorescence spectroscopy measurements put in evidence important fluorescence peaks found at 596 nm and 643 nm for Sm 3 + ions in phosphate matrix and 611 nm and 700 nm in the case of Eu3 +-doped glass. © 2013 Elsevier B.V.

Elisa, M. a, B. A. b Sava, A. c Volceanov, R. C. C. d Monteiro, E. e Alves, N. e Franco, F. A. f Costa Oliveira, H. g Fernandes, and M. C. g Ferro. "Structural and thermal characterization of SiO2-P2O5 sol-gel powders upon annealing at high temperatures." Journal of Non-Crystalline Solids. 356 (2010): 495-501. AbstractWebsite

This study deals with SiO2-P2O5 powders obtained by sol-gel process, starting from tetraethoxysilane (TEOS) as precursor for SiO2 and either triethylphosphate (TEP) or phosphoric acid (H3PO4) as precursors for P2O5. In the case of samples prepared with H3PO4, TG-DTA data showed an accentuated weight loss associated to an endothermic effect up to about 140 °C, specific for the evaporation of water and ethylic alcohol from structural pores, and also due to alkyl-amines evaporation. Sol-gel samples prepared with TEP exhibited different thermal effects, depending on the type of atmosphere used in the experiments, i.e. argon or air. XRD analysis revealed that annealed sol-gel samples prepared with H3PO4 showed specific peaks for silicophosphate compounds such as Si3(PO4)4, Si2P2O9, and SiP2O7. XRD results for annealed sol-gel samples prepared with TEP indicated mainly the presence of a vitreous (amorphous) phase, which could be correlated with SEM images. The presence of SiO2 in the sample might be expected. Thus, we have searched for any SiO2 polymorph possible to crystallize. Only potential peaks of cristobalite were identified but some of them are overlapping with peaks of other crystalline phosphates. SEM analysis indicated a decrease of the amount of crystalline phases with the increase in the annealing temperature. © 2009 Elsevier B.V. All rights reserved.

Elisa, M. a, B. A. a Sava, I. C. a Vasiliu, R. C. C. b Monteiro, C. R. a Iordanescu, I. D. a Feraru, L. a Ghervase, C. c Tanaselia, M. c Senila, and B. c Abraham. "Investigations on optical, structural and thermal properties of phosphate glasses containing terbium ions." IOP Conference Series: Materials Science and Engineering. Vol. 47. 2013. Abstract

{Aluminophosphate glasses belonging to the Li2O-BaO-Al 2O3- La2O3-P2O 5 system doped with Tb3+ were prepared and investigated. Methods as Induced Coupled Plasma-Mass Spectrometry (ICP-MS), Induced Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) and X-ray diffraction (XRD) have been used to establish the elemental composition of these vitreous materials. The influence of the Tb3+ ions on the optical properties of the phosphate glasses has been investigated in relation with the structural characteristics of the vitreous matrix. The optical behavior has been studied by ultra-violet-visible (UV-Vis) spectroscopy, revealing electronic transitions specific for terbium ions. Fluorescence spectroscopy measurements have been performed by excitation in the UV and visible domains (377 nm and 488 nm) which resulted in the most significant fluorescence peaks in the Vis domain (540 and 547 nm). Structural information via vibration modes were provided by Fourier Transform Infrared (FTIR) absorption spectra in the 400-4000 cm-1 range. Absorption peaks specific for the vitreous phosphate matrix were put in evidence as P-O-P symmetrical and asymmetrical stretching vibration modes, P-O-P bend, PO2- symmetrical and asymmetrical stretching vibration modes

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.

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.

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.

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.

Kullberg, A. T. G., A. A. S. Lopes, J. P. B. Veiga, M. M. R. A. Lima, and R. C. C. Monteiro. "Formation and crystallization of zinc borosilicate glasses: Influence of the ZnO/B2O3 ratio." Journal of Non-Crystalline Solids. 441 (2016): 79-85. AbstractWebsite

Different glasses based on the ZnO-B2O3-SiO2 system, with a ZnO content ≥ 60 mol% and a fixed SiO2 content (20 mol%), were synthesised using a melt-quenching method. Glass samples with zinc oxide concentrations as high as 65 mol% were prepared successfully without deteriorating the glass-forming ability. The glass samples were submitted to controlled heat-treatments, and the effect of the ZnO/B2O3 molar ratio on the formation of crystalline phases within the glass matrix was investigated by means of differential thermal analysis (DTA), X-ray diffraction (XRD) and scanning electron microscopy (SEM). DTA results indicated that the glass transition and the onset crystallization temperatures of the studied glasses tended to increase with the increment on the ZnO/B2O3 ratio. XRD data showed that the zinc binary crystalline phases, willemite (Zn2SiO4), a zinc orthosilicate, and zinc borate (Zn3B2O6) could be present in the crystallized glasses, depending on the heat-treatment conditions. The formation of willemite was promoted by an increasing ZnO/B2O3 ratio. Microstructural observations performed by SEM indicated that under controlled experimental parameters (glass composition, heat-treatment temperature and time) the precipitation of nanocrystals within the glass matrix can be achieved, resulting in transparent and translucent willemite glass-ceramics. © 2016 Elsevier B.V. All rights reserved.

Lapa, N. a, R. a Barbosa, S. a Camacho, R. C. C. b Monteiro, M. H. V. c Fernandes, and J. S. a Oliveira. "Leaching behaviour of a glass produced from a MSWI bottom ash." Materials Science Forum. 514-516 (2006): 1736-1741. AbstractWebsite

This paper is mainly focused on the characterisation of a glass material (GM) obtained from the thermal treatment of a bottom ash (BA) produced at the Municipal Solid Waste (MSW) incineration plant of Valorsul. By melting the BA at 1400°C during 2 hours, and without using any chemical additives, a homogeneous black-coloured glass was obtained. The thermal and mechanical properties of this glass were characterised. The thermal expansion coefficient, measured by dilatometry, was 9-10 × 10-6 per °C and the modulus of rupture, determined by four-point bending test, was 75±6 MPa, which are similar values to those exhibited by commercial soda-lime-silica glasses used in structural applications. The chemical and the ecotoxicological leaching behaviour of the GM were also analysed. The GM was submitted to a leaching procedure composed of 15 sequential extraction cycles. A liquid/solid (L/S) ratio of 2 1/kg was applied in each cycle. The leachates were filtered through a membrane of PTFE (porosity: 0.45 μm). The filtered leachates were characterised for different chemical parameters and for an ecotoxicological indicator (bacterium Vibrio fischeri). The GM was also submitted to a microwave acidic digestion for the assessment of the total metal content. The crude BA was also submitted to the same experimental procedures. The GM showed levels of chemical emission and ecotoxicity for V. fischeri much lower than those determined for the crude BA. Similar characterisation studies will be pursued with the glass-ceramics produced by adequate thermal treatment of the glass, in order to investigate the effect of the crystallization on the final properties.

Leroy, C. a, M. C. a Ferro, R. C. C. b Monteiro, and M. H. V. a Fernandes. "Production of glass-ceramics from coal ashes." Journal of the European Ceramic Society. 21 (2001): 195-202. AbstractWebsite

Coal fly ashes produced by an extinguished power plant in the north of Portugal have been melted with addition of CaCO3 and Na2CO3 to obtain glasses. One of the formulated compositions was selected for further studies and it was possible to manufacture glass-ceramics by crystallizing the parent glass through adequate time-temperature schedules. The macroscopic appearance, microstructure, mechanical, thermal and chemical properties indicated that these materials are quite attractive for cladding applications, exhibiting in some cases better performances than the conventional ceramic tiles.

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.

Lima, M. M. R. A. a, R. C. C. a Monteiro, M. P. F. b Graça, and M. G. c Ferreira Da Silva. "Structural, electrical and thermal properties of borosilicate glass-alumina composites." Journal of Alloys and Compounds. 538 (2012): 66-72. AbstractWebsite

Borosilicate glass-alumina composites with (1 - x) Glass + x Al 2O 3 (x = 0, 5, 10, 25 vol.%) were prepared and the effect of Al 2O 3 addition on the structural, electrical and thermal characteristics was investigated. XRD patterns revealed the presence of cristobalite (SiO 2) in sintered borosilicate glass and that the addition of Al 2O 3 hinders cristobalite formation. This behavior is due to the diffusion of some Al 3+ ions from alumina to glass, which leads to changes in glass structure and composition as identified by SEM/EDS. Cristobalite was undetected in composites containing 10% Al 2O 3 that attained the lowest thermal expansion coefficient value (∼4.6 × 10 -6 °C -1). Conductivity (dc and ac) increased with the amount of Al 3+ ions present in the glass structure as modifiers and formers. Dielectric constant values, in the range 5.0-7.2, increased with Al 2O 3 addition and the values of loss tan δ (1.5-2.1 × 10 -2) indicate that these materials are good insulators. © 2012 Elsevier B.V. All rights reserved.

Lima, M. M. R. A., and R. C. C. Monteiro. "Shrinkage behaviour of borosilicate glass-Al2O3 composites during isothermal sintering." Materials Science Forum. 514-516 (2006): 648-652. AbstractWebsite

The effect of rigid inclusions on the densification during isothermal sintering of glass matrix composites was investigated. Mixtures containing borosilicate glass powder and 0, 5, 10 and 25 vol. % alumina (Al 2O3) particles were prepared and powder compacts isostatically pressed at 200 MPa have been used. The sintering behaviour of the samples heated at 800°C during various times was investigated through density measurement, axial and radial shrinkage measurements. The microstructure was analysed by SEM and the crystalline phases present in the sintered composites were identified by XRD. The relative density of the isothermally treated borosilicate glass-Al2O3 composites decreased significantly with the increase in Al2O3 content because the presence of rigid inclusions retarded the densification of the compacts. The borosilicate glass exhibited anisotropic shrinkage behaviour, showing a radial shrinkage higher than the axial shrinkage and isotropic shrinkage was favoured by Al2O3 additions. Sintered glass showed a dense microstructure with some spherical closed pores. The microstructure of composites with 5 vol. % Al2O3 revealed that most of the pores were filled by capillary flow of the glass. The microstructure of composites with higher Al2O3 additions showed dense areas together with interconnected pores, which appeared at the sites of large glass particles in the green compacts.

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.

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.

Lima, M. M. R. A., and R. C. C. Monteiro. "Viscous sintering in a glass-alumina system." Materials Science Forum. 587-588 (2008): 143-147. AbstractWebsite

The densification during sintering of borosilicate glass matrix composites with 25 vol. % alumina (Al2O3) particles was investigated. The powder compacts, isostatically pressed at 200 MPa, were sintered at a temperature within the range 800-1000° C and maintained at this temperature during various times. The sintering behaviour of the composites was investigated by density measurement and by axial and radial shrinkage measurements. The crystalline phases present in the sintered composites were identified by XRD and the microstructure was analyzed by SEM. For temperatures up to 900°C, the relative density of the composites increased continuously with sintering temperature and sintering time, while for higher temperatures, the density increased rapidly and then slowed down to achieve a nearly constant value after sintering the composites for 30 minutes. The composites exhibited isotropic shrinkage behaviour when sintered at 800°C and 850°C, but at higher temperatures slightly higher axial shrinkage than radial shrinkage was observed. The shrinkage behaviour and microstructural characteristics of the composites indicate that densification during sintering can be attributed to the viscous flow of the borosilicate glass.

Lima, M. M. R. A., F. M. Braz Fernandes, and R. C. C. Monteiro. "Study of the crystallization of a borosilicate glass." Key Engineering Materials. 230-232 (2002): 157-160. AbstractWebsite

The crystallization of a commercial borosilicate glass powder has been studied in the temperature range 750-900°C. Crystal growth was investigated by high temperature XRD and cristobalite precipitation was identified. Glass devitrification exhibited a characteristic incubation period that decreased with increasing temperature: 25-30 min at 750°C, 9-12 min at 775°C, 5-10 min at 810°C, and 0-5 min at 840°C. Cristobalite is an unfavorable transformation product in terms of thermal expansion behavior. The precipitation of cristobalite in sintered glass compacts was confirmed by dilatometric analysis, where the increase in thermal expansion coefficient due to the presence of cristobalite and its transition from the tetragonal to the cubic phase were verified. Correlation between the XRD results and the dilatometric data from sintered glass compacts showed the partial dissolution of cristobalite when the glass was heated at the highest temperatures.

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.

Lopes, A., P. Nunes, P. Vilarinho, R. Monteiro, E. Fortunato, and R. Martins. "Study of the sensing mechanism of SnO2 thin-film gas sensors using hall effect measurements." Key Engineering Materials. 230-232 (2002): 357-360. AbstractWebsite

Hall effect measurements are one of the most powerful techniques for obtaining information about the conduction mechanism in polycrystalline semiconductor materials, which is the basis for understanding semiconductor gas sensors. In order to investigate the correlation between the microscopic characteristics and the macroscopic performances exhibited by undoped tin oxide gas sensors deposited by spray pyrolysis, Hall effect measurements were performed at different temperatures, from room temperature up to 500 K, and in the presence of two different atmospheres, air and methane. From these measurements, it was possible to infer the potential barrier and its dependence with the used atmosphere. The obtained results were analysed in terms of the oxygen mechanism at grain boundaries on the basis of the grain boundary-trapping model. In the presence of methane gas, the electrical resistivity decreases due to the lowering of the inter-grain boundary barrier height.