Mechanical properties and coefficient of thermal expansion of β-eucryptite sintered by microwave technique

[ES]: La técnica de sinterización no convencional de microondas permite obtener materiales de ß-eucriptita en estado sólido cristalino con densidades cercanas a la teórica (~99 %). Se ha observado una diferencia considerable en estos materiales respecto a la técnica convencional en términos de densificación, microestructura, coeficiente de expansión térmica y propiedades mecánicas. Los valores de dureza y módulo de Young obtenidos mediante sinterización por microondas a 1200 ºC-5 min han sido relativamente altos, 6.8 GPa y 101 GPa, respectivamente, en comparación con el material obtenido mediante horno convencional (3.9 GPa y 58 GPa, respectivamente). Los datos dilatométricos obtenidos, incluyendo el intervalo de temperatura criogénica (-150 ºC a +150 ºC), muestran un coeficiente de expansión térmica controlado y negativo en todo el rango de temperaturas. La combinación de un calentamiento rápido junto con la reducción drástica en el tiempo de ciclo y el ahorro energético, hace que la técnica de microondas sean una clara alternativa a otro tipo de calentamientos.[EN]: Microwave non-conventional sintering technique allows obtaining fully dense glass-free β-eucryptite bulk material (∼99 %). A considerable difference in the densification, microstructure, coefficient of thermal expansion behaviour and mechanical properties, between conventional and non-conventional sintered specimens was observed. The hardness and Young’s modulus values obtained by microwaves at 1200 °C-5min have been relatively high, 6.8 GPa and 101 GPa, respectively, compared to conventional sintering (3.9 GPa and 58 GPa, respectively). Very low thermal expansion materials have been obtained in a wide temperature range including cryogenic temperatures (from -150 ºC to 150 ºC). The high heating rate along with the lower energy consumption makes microwave technique a clear alternative to other types of sintering methods.Los autores desean agradecer el apoyo financiero recibido de la UPV dentro de los proyectos SP20120621 y SP20120677 y, al gobierno español a través del proyecto (TEC2012-37532-C02-01). A. Borrell, agradece al Ministerio de Ciencia e Innovación su contrato de Juan la Cierva (JCI-2011-10498).Peer Reviewe

Effect of microwave sintering on microstructure and mechanical properties in Y-TZP materials used for dental applications

The aim of this work is to study the application of microwave sintering to consolidate yttria-stabilized zirconia polycrystalline (Y-TZP) ceramics commonly applied in dentistry, so as to obtain highly dense materials and fine microstructure with shorter sintering cycles. Three Y-TZP materials are considered: two commercially available for dental applications and one laboratory studied powder. Microwave sintering was carried out at 1200 and 1300 degrees C for 10 min and conventional sintering at 1300 and 1400 degrees C for 2 h. Relative density, Vickers hardness and fracture toughness values for sintered samples were determined. Microwave sintering results, generally, in improved mechanical properties of the materials in terms of hardness and fracture toughness compared to conventional sintering and, in some cases, at lower sintering temperatures. A finer grain microstructure (final grain size < 250 min) was obtained with microwave sintering for both commercial materials. Fracture toughness values differ significantly between sintering techniques and chosen parameters. These results suggest that microwave heating can be employed to sinter Y-TZP commercial ceramics for dental applications obtaining improving the mechanical properties of the materials with a very important time and energy consumption reduction. Crown Copyright (C) 2015 Published by Elsevier Ltd and Techna Group S.r.l. All rights reserved.The authors would like to thank the financial support received from Universidad Politecnica de Valencia under Project 5P20120677 and Ministerio de Economia y Competitividad (MINECO) and co-funded by ERDF (European Regional Development Funds) through the Project (IEC2012-37532-C02-01). A. Borrell acknowledges the Spanish Ministry of Science and Innovation for her Juan de la Cierva Contract (JCI-2011-10498) and the Generalitat Valenciana for the financial support under Project GV/2014/009. A. Presenda acknowledges the Generalitat Valenciana for his Santiago Grisolia program scholarship (GRISOLLV2013/035). The authors would also like to acknowledge Prof. Dr. M. F. Sold from the Faculty of Medicine and Odontology at the Universidad de Valencia for supplying the commercial materials.Presenda, Á.; Salvador Moya, MD.; Penaranda-Foix, FL.; Moreno, R.; Borrell Tomás, MA. (2015). Effect of microwave sintering on microstructure and mechanical properties in Y-TZP materials used for dental applications. Ceramics International. 41(5, Part B):7125-7132. https://doi.org/10.1016/j.ceramint.2015.02.025S71257132415, Part

Fabrication of near-zero thermal expansion of fully dense beta-eucryptite ceramics by microwave sintering

Microwave heating is proposed as non-conventional technique for the sintering of optimal lithium aluminosilicate compositions of &#946;-eucryptite system. The coefficient of thermal expansion and mechanical properties of the sintered samples has been studied under the influence of microwave heating. The ad hoc synthesized &#946;-eucryptite together with the microwave sintering technique developed in this work open the opportunity to produce breakthrough materials with low or negative coefficient of thermal expansion and excellent mechanical properties, as a Young s modulus of 110 GPa. The combination of rapid heating with low energy applied by the microwave technology (eco-friendly process) and the dramatic reduction in cycle time allows densification without glass phase formation. Results of the coefficient of thermal expansion of the &#946;-eucryptite ceramics presented here under cryogenic conditions will be of value, for example, in the future design of new composite materials for space applicationsThe authors would like to thank Dr. Emilio Rayon for performing the nanoindentation analysis in the Materials Technology institute (ITM) of the Polytechnic University of Valencia (UPV) and your financial support received of UPV under Projects SP20120621 and SP20120677 and Spanish Government through the Project MONIDIEL (TEC2008-04109). A. Borrell, acknowledges the Spanish Ministry of Science and Innovation for a Juan de la Cierva contract (JCI-2011-10498) and SCSIE of the University of Valencia.Benavente Martínez, R.; Borrell Tomás, MA.; Salvador Moya, MD.; Garcia-Moreno, O.; Penaranda-Foix, FL.; Catalá Civera, JM. (2014). Fabrication of near-zero thermal expansion of fully dense beta-eucryptite ceramics by microwave sintering. Ceramics International. 40(1):935-941. https://doi.org/10.1016/j.ceramint.2013.06.089S93594140

Microwave sensor system for continuous monitoring of adhesive curing processes

A microwave sensor system has been developed for monitoring adhesive curing processes. The system provides continuous, real-time information about the curing progress without interfering with the reaction. An open-coaxial resonator is used as the sensor head, and measurements of its resonance frequency and quality factor are performed during cure to follow the reaction progress. Additionally, the system provides other interesting parameters such as reaction rate or cure time. The adhesive dielectric properties can also be computed off-line, which gives additional information about the process. The results given by the system correlate very well with conventional measurement techniques such as differential scanning calorimetry, combining accuracy and rate with simplicity and an affordable cost. © 2012 IOP Publishing Ltd.The authors thank Rut Benavente Martinez for her assistance in the DSC experiments. The contract of BG-B is financed by the Ministry of Science and Innovation of Spain, through the 'Torres Quevedo' Sub-programme, which is also co-financed by the European Social Fund (ESF). This work has been financed by the Ministry of Science and Innovation of Spain through the project MONIDIEL (TEC2008-04109).García Baños, B.; Catalá Civera, JM.; Penaranda-Foix, FL.; Canós Marín, AJ.; Sahuquillo Navarro, O. (2012). Microwave sensor system for continuous monitoring of adhesive curing processes. Measurement Science and Technology. 23(3). https://doi.org/10.1088/0957-0233/23/3/035101S233Jost, M., & Sernek, M. (2008). Shear strength development of the phenol–formaldehyde adhesive bond during cure. Wood Science and Technology, 43(1-2), 153-166. doi:10.1007/s00226-008-0217-2Costa, M. L., Botelho, E. C., Paiva, J. M. F. de, & Rezende, M. C. (2005). Characterization of cure of carbon/epoxy prepreg used in aerospace field. Materials Research, 8(3), 317-322. doi:10.1590/s1516-14392005000300016Chen, J., & Hojjati, M. (2007). Microdielectric analysis and curing kinetics of an epoxy resin system. Polymer Engineering & Science, 47(2), 150-158. doi:10.1002/pen.20687Sernek, M., & Kamke, F. A. (2007). Application of dielectric analysis for monitoring the cure process of phenol formaldehyde adhesive. International Journal of Adhesion and Adhesives, 27(7), 562-567. doi:10.1016/j.ijadhadh.2006.10.004Núñez, L., Gómez-Barreiro, S., Gracia-Fernández, C. A., & Núñez, M. R. (2004). Use of the dielectric analysis to complement previous thermoanalytical studies on the system diglycidyl ether of bisphenol A/1,2 diamine cyclohexane. Polymer, 45(4), 1167-1175. doi:10.1016/j.polymer.2003.12.024Lefebvre, D. R., Han, J., Lipari, J. M., Long, M. A., McSwain, R. L., & Wells, H. C. (2006). Dielectric analysis for in-situ monitoring of gelatin renaturation and crosslinking. Journal of Applied Polymer Science, 101(5), 2765-2775. doi:10.1002/app.21631Cordovez, M., Li, Y., & Karbhari, V. M. (2004). Assessment of Dielectrometry for Characterization of Processing and Moisture Absorption in FRP Composites. Journal of Reinforced Plastics and Composites, 23(4), 445-456. doi:10.1177/0731684404031980Das, N. K., Voda, S. M., & Pozar, D. M. (1987). Two Methods for the Measurement of Substrate Dielectric Constant. IEEE Transactions on Microwave Theory and Techniques, 35(7), 636-642. doi:10.1109/tmtt.1987.1133722Fioretto, D., Livi, A., Rolla, P. A., Socino, G., & Verdini, L. (1994). The dynamics of poly(n-butyl acrylate) above the glass transition. Journal of Physics: Condensed Matter, 6(28), 5295-5302. doi:10.1088/0953-8984/6/28/007Givot, B. L., Krupka, J., & Belete, D. Y. (s. f.). Split post dielectric resonator technique for dielectric cure monitoring of structural adhesives. 13th International Conference on Microwaves, Radar and Wireless Communications. MIKON - 2000. Conference Proceedings (IEEE Cat. No.00EX428). doi:10.1109/mikon.2000.913931Canos, A. J., Catala-Civera, J. M., Penaranda-Foix, F. L., & Reyes-Davo, E. (2006). A novel technique for deembedding the unloaded resonance frequency from measurements of microwave cavities. IEEE Transactions on Microwave Theory and Techniques, 54(8), 3407-3416. doi:10.1109/tmtt.2006.877833Marks, R. B., & Williams, D. F. (1992). A general waveguide circuit theory. Journal of Research of the National Institute of Standards and Technology, 97(5), 533. doi:10.6028/jres.097.024Harrington, R. F. (1967). Matrix methods for field problems. Proceedings of the IEEE, 55(2), 136-149. doi:10.1109/proc.1967.5433Baker-Jarvis, J., Janezic, M. D., Domich, P. D., & Geyer, R. G. (1994). Analysis of an open-ended coaxial probe with lift-off for nondestructive testing. IEEE Transactions on Instrumentation and Measurement, 43(5), 711-718. doi:10.1109/19.328897Taylor, B. N. (1994). Guidelines for evaluating and expressing the uncertainty of NIST measurement results. doi:10.6028/nist.tn.1297Casalini, R., Corezzi, S., Livi, A., Levita, G., & Rolla, P. A. (1997). Dielectric parameters to monitor the crosslink of epoxy resins. Journal of Applied Polymer Science, 65(1), 17-25. doi:10.1002/(sici)1097-4628(19970705)65:13.0.co;2-tPreu, H., & Mengel, M. (2007). Experimental and theoretical study of a fast curing adhesive. International Journal of Adhesion and Adhesives, 27(4), 330-337. doi:10.1016/j.ijadhadh.2006.06.004Harper, D. P., Wolcott, M. P., & Rials, T. G. (2001). Evaluation of the cure kinetics of the wood/pMDI bondline. International Journal of Adhesion and Adhesives, 21(2), 137-144. doi:10.1016/s0143-7496(00)00045-2Garcia-Banos, B., Canos, A. J., Penaranda-Foix, F. L., & Catala-Civera, J. M. (2011). Noninvasive Monitoring of Polymer Curing Reactions by Dielectrometry. IEEE Sensors Journal, 11(1), 62-70. doi:10.1109/jsen.2010.2050475He, Y. (2001). DSC and DEA studies of underfill curing kinetics. Thermochimica Acta, 367-368, 101-106. doi:10.1016/s0040-6031(00)00654-7Núñez-Regueira, L., Gracia-Fernández, C. A., & Gómez-Barreiro, S. (2005). Use of rheology, dielectric analysis and differential scanning calorimetry for gel time determination of a thermoset. Polymer, 46(16), 5979-5985. doi:10.1016/j.polymer.2005.05.06

Microwave technique: An innovated method for sintering beta-eucryptite ceramic materials

Trabajo presentado al 13th International Ceramics Congress celebrado en Montecatini Terme (Italia) del 9 al 17 de junio de 2014.Microwave sintering has emerged in recent years as a new, fast, cheap and green technology for sintering a variety of materials. The main advantages of microwave heating can be summarized as follow: reduced processing times, energy costs and environmental benefits. Nevertheless, understanding how this specific heating drives to obtain ceramic materials with a combination of unique, structural and functional properties is the big challenge. The present work shows the different and improved properties achieved with beta-eucryptite nanocomposite ceramic materials by microwave heating in respect of the conventional method. Microcracking evolution in addition to the microstructure of the sintered materials along the several thermal cycles have been studied. Mechanical properties related to this behaviour change dramatically. Thus, the microwave technique is a promising tool for sintering new materials by controlling the composition of the phases, chemical reactivity and nanostructure, using up to 70% less energy in the whole sintering process than conventional heating. This technique becomes part of the new and innovative technologies "eco-green".Peer Reviewe

High thermal stability of microwave sintered low-ε r β-eucryptite materials

Low-temperature sinterable microwave LiAlSiO-based solid-state material was investigated with regard to microwave dielectric properties as functions of the sintering temperature. β-eucryptite materials and alumina-reinforced β-eucryptite composites were sintered by microwave technology at 1100°C and 1200°C. The combination of fast heating and the dramatic reduction in cycle time, along with the non-conventional heating source, opens the way to produce materials with desired multifunctional properties. The microstructure and crystalline composition of the materials were characterised, and the mechanical, thermal and microwave dielectric behaviours were analysed. X-ray diffraction showed good chemical stability in materials without between-phase reactions during the microwave sintering process. The excellent mechanical (∼8 GPa of hardness and ∼100 GPa of Young's modulus), thermal (-0.23·10 K) and microwave dielectric properties (ε =4.10; Q=1494) were obtained from the LAS/AlO composites sintered at a very low temperature (1100°C). The results achieved show the possibility of designing ceramic nanocomposites at low sintering temperatures using microwave technology with near-zero thermal expansion coefficients, high mechanical and chemical stability and low dielectric properties.This work has been developed by different funded projects. The authors would like to thank their financial support: Project SP20120677 funded by the Polytechnic University of Valencia (UPV), Project TEC2012-37532-C02-01 (DINAWAVE) funded from Ministerio de Economía y Competitividad (MINECO) – Spanish government- and co-funded by ERDF (European Regional Development Funds) of European Union. Author A. Borrell, acknowledges the Spanish Ministry of Science and Innovation for her Juan de la Cierva contract (JCI-2011-10498),Peer Reviewe

Study of colored on the microwave sintering behavior of dental zirconia ceramics

The aim of this work is to study the physical, chemical, and mechanical properties of 3 mol% Yttria-stabilized Tetragonal Zirconia Polycrystalline (3Y-TZP) materials doped with varying amounts of iron oxide (0, 400, 800, and 1000 ppm). We carried out full dense consolidation using two different sintering methods: fast-microwave technology at 1200°C and 1300°C, and conventional furnace at 1400°C. It was observed an improvement in density and hardness values, as well as great fracture toughness, and more intense color was achieved resulting in more natural color, similar to that of human teeth, using the microwave technique at 1300°C compared to the conventional method. However, the microwave-sintered specimens exhibited an increase in zirconia grains size and high color intensity along with iron oxide content when compared to conventional process, where the grain size does not vary with the coloring agent content. The results obtained in this work suggest that microwave technology can produce an increase in sintering activity due to the different dielectric properties of 3Y-TZP materials doped with Fe2O3. Another interesting confirmed result is that the addition of Fe2O3 presents a high resistance to low temperature hydrothermal degradation producing a delay in the aging process.A. Borrell acknowledges the Spanish Ministry of Economy and Competitiveness for her RyC contract (RYC-2016-20915).Peer reviewe

Tribological and wear behaviour of alumina toughened zirconia nanocomposites obtained by pressureless rapid microwave sintering

Dense alumina toughened zirconia nanocomposites (ATZ, 3Y-TZP with 20 wt% Al2O3) were densified by non-conventional microwave sintering technology at relatively low temperatures (1200 and 1300 °C). The sintering method and its effect on densification, microstructure, mechanical properties and tribological behaviour were investigated. The outcomes demonstrated that the density rose as the sintering temperature was higher, and therefore the mechanical properties were enhanced, reaching a maximum hardness (18.4 ± 0.4 GPa) and fracture toughness (5.7 ± 0.3MPa· m1/2). In addition, the samples were subjected to a tribological test in dry and wet conditions, using artificial saliva. In both cases, the coefficient of friction and wear volume for samples obtained by microwave sintering are lower than conventional samples, with the wear volume being two times higher in dry conditions than in wet conditions.The authors are grateful to the Government of Valencia for the funding received for the project PROMETEU/2016/040. A. Borrell thanks to the Spanish Ministry of Economy and Competitiveness for her RyC contract (RYC-2016-20915). A. Dalmau acknowledges to the Valencia Government for the financial support (APOSTD/2017/051).Peer reviewe