ISSN: 1070-0129 INTERNATIONAL MicROWAVE P| N Power = Instute = PROCEEDINGS CeLesratinG THE SOTH ANNIVERSARY OF THE Microwave Oven July 18-21, 1999 Doubletree Hotel National Airport Arlington, VA, USAINTERNATIONAL Microwave Power INSTITUTE Board of Governors 1998-1999 OFFICERS: President: Charies R. Buffer, Ph.D, Microwave Research Center, Marlborough, NH, USA Secretary: Per O. Risman, Microtrans AB, Landvetter, Sweden Treasurer: Mitchell Henke, P.E_, Lincoln Foodservice Products, Ft Wayne, IN, USA Executive Director: Robert C. LaGasso, IMP! Manassas, VA, USA DIRECTORS: David Baron, Holaday Industries, Inc., Eden Prairie, MN, USA Raber Blocksidge, Photonetics, Wakefield, MA, USA Neal Cooper, Enersyst Development Center, Dallas, TX, USA Richard N. Gedye, Laurentian University, Sudbury. ON, Ganada ‘Wayne Love, Arrow Pneumatic, Hickory Hills, IL, USA Joanne Prater. J&B Associates, Ostord, AL, USA CORRESPONDING MEMBERS: John M, Osepchuk, Ph.D., Full Spectrum Consulting, Concord, MA, USA Richard H. Edgar, Chelmsford, MA, USA 347TH AnNuaL Microwave Symposium Procram Cuairs Ben Adu Sarah Risch, Ph.D. | Fusion UV Curing Systems Science by Design Gaithersburg. MD, USA Chicago, IL, USA John M. Osepchuk, Ph.D. Full Spectrum Consulting | Concord, MA, USATABLE OF CONTENTS 34 Microwave Power Symposium Proceedings duty 18-21, 1999 * Aruincton, VA Ceramic Processing Session Chair: Milton Mathis, 3M + Microwave Synthesis ond Sintering of Pb (ZeTiN0 E Vaighyarathan, DAK, Ageawal, T-R. Shrout and R. Ros. Materials Research Laboraiory, Pennsyl State University, University Paek, PA, USA .. + Suidy ofthe Behavior Uf Ceramic Masertate Exposed ta Maceowaves Related to thetr Lattice ‘alia Gomez and Juan Aguilar, Universidat Autonoma de Nuevo Lec, Nuevo Ladi, MEKiCO -icncucsn Dielectric Properties Session Ch Stuart O, Nelson, U.S, Department of Agriculture + Bensity-dndependent Permittivicy Functions for Maisture Sensing in Foods and Agriculmeal Products ‘Samir Trabelsi, Andree} W. Kraszewski and Smart 0. Nelson, U.S. Department of Agriculwre. Athens, GA, USA... + Bicleciréc Constand of Lemit and Dry Pass Kailash Prasad Thakur and Wayne S, Holmes, Industrial Research Limited, Auckland, New Zeatand su + Use of Cereal Grain Pemmistvity For Sensing Moisture Content Stuart O, Nelson, Andrze] W. Keaszevski, Kurt C. Lawrence und Sumir Trabelsi, 0.8. Department of Ageiculuns, Athens, GA, USA 2 HERE and Microwave Power Sources Session Chair: Walter Van Loock, Universty of Ghent + HF Applicosor Manufacnuring Glass Epoxy Composite Picces Georges Roassy*,G. Parizot® and S, Basiard**, *Université Naney, Vandoeuvre les Nancy: Prance #* Renault SA. Guyancount, France oienine tira + Esfaed Magnetron dirarovemicnts and Faiture Mechanisms Steven. Dorak and Rober J, Rutherford, Burie Industries, Inc Lancaster; PA, USA... + Switeh Mode Power Supply with Pulsed Capability Paolo Balocchi, Marco Garuti and Mario Massa, ALTER. Reggio Emilia, Italy. Microwave Chemistry Session Ch vader S. Warma, TRIES, Sam Houston State University * Microwave-Aecelerated Solvent-Free Chetrcal Transformations Rajender $. Varina, Dalip Kurnar und Kannan P. Naicker. Departament of Chemiistry and TRIES, Sam Houston State University, Huatsville, Texas, USA + Rate Enhancement of Reactéos ly Micromaves. re Non-Thermal Effects Involved? Richard N. Gedye, Laumentian University, Sudbury, ON, Canad mn wsrsnceminntsiinni Microwave Heating and Drying Session Chair: Michael Drozd, Industrial Micra wave Systems + Analysis of the Electromaynetic Fields in Microwave Cavities and the Temperature Fields in Loads Using Finite-Difference Time Damain Method Seeny-Ho Cho, ¥. NM Lee, HJ. Kim, H.J. Kang, UG Electronics, Inc., Keamchen-Gu, Seoul, Korea... 1g af Epox Glass Composite Far the Car trdlusiry Georges Roussy*.G. Purizort and S. Bastard™™, “Université Naney, Vandoeuvre Fes Nancy, France Renault SA, GuyaGOUlt FIRES wpe paar * troaheemat Devine of Parous Ceramic Microspheres in Microwave Heated Fludised Bed G.D. Sizgek and E: Sizgek, Australian Nuclear Science and Technology. Menai, NSW, Australia cn + Regeneration of « Diesel Engine Particulate Fitter Using Microwave Heating ‘Gene A. Danka”, Richard Silberglitt*, A. Carl McDonald and Thornas M, Yonushoni + FM Technologies, Fairfax. WA. USA, ™Curnmins Engine Company, Inc, Colurbis, 3 a6TaBLE oF ConTENTS, CONTINUED 34'* Microwave Power Symposium Proceedings Polymer Processing Session Chair: Georges Roussy, Université Nancy * Welding of PVDF-Pipes with Microeaves Rudolf Emmeneh', Michael Jauss*, Volker Brautigam*™ and Peter Elsner*. *Praunhofer lastivute Chemical ‘Technology, Pfinztal, Geratany, **Universty of Stuttgart, Siitgant, Geamany = aS + Microwave or Radiofrequency Processes of Potymcication: State ofthe Art Albert Gourdenne, Laboratoire de Physico-Chimie des Hats Polyméres, Toulouse Codex, France a-acnunnerninqsnenineS? Waste Remidiation Session Chairs Nguyen Tram, Microwave Research Laboratory ~ Antenna-Based RF Hearing Teclnology for Soil Remediation SoL. Price’, R. S, Kascvich*. D. Wiberg**, M,C. Marley* and M. Warson**, *Kal Technologies, LLC. Portsmouth, NH. USA, **DAHL & Associutes, Inc., Linalakes, MN, USA + Recovering of Used! Solvent Using Mlcranave Energy VN. Tran, A. Sherwal snc H, King, RMIT, Melboume, Vietoria, Austalia bios tiae TTS + Microwave Recycling of Canfectionery W.N.Tren and A. Sherwal, RMIT, Metboume, Wietoria, Australia... san iat i 65 Posters + Combined lficrowave onit Hos Atr Drying of Onion in Comparison with the Drving Only by Microwaves and nly by Hos Ate LL Abhayawick*-**,:C. Laguerte*, W. Tauris, LM. Enerie*, A. Duguenoy**, *ISAB, Cagy Pontoise ceden. France. **ENSIA, Massy cedex, France isn Ai Hata + Development of a Prototype Microwave Fumace For Post-Combustion Stuiles of Ligntte Ashes P. Veranesi*, C. Laswell", C, Siligardi*, G.C, Pellacani* and E, Camea"®, *University of Modena and Reggio Emilia, Madesa, italy, "University ef Genes, Italy i "1 TRE Ko torsional Micsovave Power lasts 1999 Alighs served. Primed and hound in the United Stes of QD S===— America. No part of this book may bs reproduced oe utilized in amy form or by any means. electronic or mechanical SBS © closing photocopying, recording, orby uny information storage and retrieval system, without permission m writing VATA tom ihe publishers.MICROWAVE SYNTHESIS AND SINTERING OF Pb(Zr.Ti)O;, B. Vaidhyanathan, D.K. Agrawal*, T.R. Shrout, and R. Roy Materials Research Laboratory, The Pennsylvania State University. University Park, FA 16862, ABSTRACT A facile, fast and clean microwave synthesis and sintering of Pb(Zr,Ti)O, (PZT) has bees demonsteated The combined use of microwave energy and non-sfoichiometrc precursors is found #0 enhance the reaction rates astonishingly and the solid state symthesis of single phase P27 has been accomplished in just few seconds. at temperatures as low as 600°C. For the first time partially stabilized zirconia has been identified as a better stating material for the microwave enhanced synthesis of PZT. Miccowave sintering of PZT is found t0 provide better densification in shorter duration even at lower temperatures, INTRODUCTION Lead zirconium titanate, PbZry »:Ti; «3 (PZT) belongs to the ferroelectric family of ABO, perovskite stroctures!? PZT a solid solution of antiefertoelectric Ph2O) and ferroelectric PLTIO, is very suitable for many industrial apzlications. such ax transducers, electro-optic modulators, sensors etc Conventional synthesis of lead based zirconates and titanstes involves long reaction times (owing to slow diffusion rates in the solid state), necessitates intermittent grinding and often requires stepmvise heating of the charue for several hours", Conventional sintering of P7T also sutfers ftom the problems of excessive PbO loss at high emperatures and the associated emvicommental Razand Te has been found recently that 2 wide variety of chemical reaetions can be accelerated by microwave irradiation'* ‘The major advantages are lower reaction temperatures and shorter processing times compared to conventional symhesis procedures. We envisaged that the enhanced reaction Kinesis and the lower processing fempesetures associated with microwave process can greaily simplify the PZT syathesis end sintering and can help in minimizing the PbO foss. Here we report 2 novel microwave assisted procedure forthe symbests and simering of PZT using, reduced oxide precursors. It is demonstrated thatthe combined use of microwave eneray and norestotchiometric precursors can enhance the reaction rates astonishingly and the sold state synthesis of P2T can be accomplished in just few seconds at temperatures much lower than required for eonventianal processes. It is found that the use of panally stabilized zirconia (PSZ) as a staring material for PLT synthesis leads to different ceaction pathways combined with higher kinetics EXPERIMENTAL, A modified commercial micronave system ( Amana, Redaiange Model No: RC/M4SE) operating at 2.45 GHz with a maximum power curput of 2W was employed for this study. Nonestoichiometric Ti; used a a precursor was prepared by reducing TiO; at 100°C for + hours in forming gas (25% Ns and $% H.) atmosphere’. Four sets of different precursors for the synthesis af PbZio.nTinaxO, were prepared, (i) mixing PbO, ZrO, and oxygen deficient nutile TiO,,, (PZT), (tt) mixing PbO, partially yeira (5 mos) stabilized Ziteonia and TiO; (PZT2), (ii) mixing POO, Zs0% and TiO; (PZT3) and tiv) mixing PLO, partially stabil XP2T4) in their metal cation stoichiometric ratio. The powders were ‘cald pressed in the form of discs of 1 25 cm diameter and the weight of pellets was maintained 2.5 gms each PZT! and PZT4 samples were hested in microwaves in flowing N; atmosphere to avoid possible oxidation of TIO, while the PZT2 ane PZT3 were peacessed én ait The-lemperature of the sarmples. was measured using a Pu(Pt-(O86Rh) thermocouple and often the values are confirmed by an infrared Pyremeter The phase identification was dane by powder X-ray diffraction For microwave sintering, nt of an aeryloid resin binder was added to the as prepared PZT powder before compaction. ISI-DS130 ‘dual stage SEM has heen used 1o investigate the micrastructure ofthe sintered PZT ceramicsRESUL: AND DISCUSSION ‘The X-ray diftaction results of the ‘owave prepared PZT samples with different precursar oxides viz P2T).P2T2, ECTS and PETS are listed in Table {This evident from Table I (company PZT and PZTS) that the presence of non-stoichiometric T:O,,, in the reaction mixture clearly enhances the formation of Table I. X-ray Diffraction Results of the Microwave Prepared PZT Samples with Different Precursor Oxides COMPOSITION | TEMPERATURE | STRUCTURAL PHASES PRESENT (Peer tecend making 5008S PbO (major); PoZrO3; TO2; PT PZTi co00c PZT (major; minor impurities (PHO + 204+ TiO, 7o0eC Par PEE (raajor); POO: ZOD PZT: very lide amounts of PRO, ZO Par PZT2 over (Pho + Psz-Ti0 LS PEO (major; PUTIOS; ZrO, PEE PZzr3 600°C PRO; PLZrOs; ZO2i PZT (PHO + Ze THO) TOC rar 500°C PZT (major); PbO: ZrO PZT GO08C. PZT (major); PbO; ZrCr2 (PhO+PSZ+ THO.) ee mee PZT 5 the major phase (more than 95%) even at 600°C. while the P2T3 composition gives single phase PZT only at T00C. “This could be corvelaied with the differences in the microwave wssoeption characteristics of reguler TiOs and redaced ‘TiO. Its found that non-stoichiometric TIO absorbs more efficiently’, the heating rate is higher, and also etiains much higher temperature {-1O00"C) that stoichiometric TiO; The high microwave absorption could be ducto the large umber af defects (wbich in tum increases the dielecatc oss) present in the rutile TiO is also clear from table Uthat the use of PSZ (partially stabilized vicconia) for PZT Synthesis enhances the reaction rate drastically (compare PZT2 and PZT3) and also lowers the reaction temperature. It is noticed that when PSZ is used as a reactant, PZT was fund fo be the major phase even at S00°C, while the usage ‘of regular ZrO requires 700°C to obtain single phase PZT. Also-ax lower temperatures, PZT3 shows PHO. PbTiO, and ZrO, as the major phases indicating that the reaction path-ways are altered by the use of PSZ (PZ12 composition}. Iris further confirmed (see PZT2 and PZTA in table I) that whenever PSZ is used, PZT was found to be the major phase even at temperatures as low as SOU'C while the usc of regular Zirconia leads to other undesirable phases. Thus the use af PSZ enhances the reaction rate (which could be ‘due to enhanced diffusion in the microwave field owing to the presence of large mumber of vneancies in the ‘cubic Huorite structure), reduces the reaction tempereture and also provides alternative reaction path-ways for the formation OF PZT. It is interesting to note hese that the conventional synthesis of P2T using the same precursor oxides provides single phase PZT only for PZTI and PZT3 compositions that too iwhenhheated-at 800°C for 4 hourn ‘The fact that PZT2 and PZT do noe provide PAT under the same conditions in conventional procosting, clearly indicates that the-meckanism of formation of PZT is very different in the microwave process and. unambiguously suggests that.a non-thermal mechanism is operative s38 % Toverene! Oonany azae Figure 1. Effect of temperature om the density Figure 2. SEM of microwave sintered PZT of PET ceramics Sincering of PZT veramics was carried out berween 1000 1200°C and the variation of sintered density as 4 function of temperature is depicted in figure 1. The sintered density was found to increase with increasing Temperature as well as with microwave exposure time Araund 96% densification has been achieved for PET sampley fora souk pertod of ust LOminutes at 1200°C in microwave sintering Its interesting to note here that even after 2 hours of sintering at the same temperature provide only 91% densification fot PZT in the conventional procs ‘Also the reduction in processing tire in the microwave method greatly minimizes the PbO lox» (almost ta half) compared to conventional sintering. The SEM photograph of the microwave sintered PZT sample is given in fagure 2 Uniform, non-porous microstructure with well faceted erystallites cesulted in microwave sintering CONCLUSIONS PZT has been prepared! using a facile microwave assisted procedure at temperatures ax low as 600°C By having one of the constituent precursors as a ngp-stoichiometric oxide, it was possible 10 achieve several fold enhancements in the reaction raies and single phase PZT resulted in just few seconds, The LusSae oF non-alnichiometiie precursors also leads to different reaction pathways far the formation of PZT The microwave method! is found to be simple, clean, energy efficient and much superior far the sintering of PZT eetamics compared wo conventional processes REFERENCES |. Jaffee, B., Cook, WR and Jaffe, Hi Piczoelectric Ceramics., Academic Press, New York, (1971) ‘Amin, A,, Newnham, RUE, Cross, I.E. and Cox, DE, 1981, Phonomenological and structural study of 2 low-temperature phase transition in the lead zirconate-ead vtanate cysiem, J Solid State Chem , 37. 28.255, Glazer, AM., Mabud, SA. and Clarke R. 1978, Powder profile refinemem of lead zirconate tikanste at several temperatures, Acta Cryst, B34, 1060-1065,4 Cheng P Agrawal DK. Kometneni: S. Mathis, MUD and Roy. R_ 1997, Microwave processing of WO-Co composites and ferrois tiunates, Mater Res, Innovat.. 1, 44-82 5. Rao, KJ, Vaidhyanathan. B., Ganguli. Mand Ramakrishnan, PA. 1S), Synthesis of Inorganic ‘Solids using Micrbwaves. Cheri, Mater 11, 882-895 6 Veidhyanathas, B Sirgh. AP. Agrawal, DIK. Strout, T.R an Roy, R 1990, Dramatic microwave effects in PET synthesis Enhanced Kinetics and Changed Mechanioms, J. Amer Ceram Soc. “communicated,STUDY OF THE BEHAVIOR OF CERAMIC MATERIALS EXPOSED TO MICROWAVES RELATED TO THEIR LATTICE [atin Gémey, Juan Aguilar Universidad Auténorna-de Nuevo Leon, Apariado Postal 076 F, San Nisoliis de los Garza, Nuevo Len ffet5(h Méxiew ABSTRACT ‘This i & summary oF @ study about the behavior of n90 kinds Of ceramic materials, peroyskite (CazrO; and Bais) and spinel (MgAl:0z and 2nAls0s), processed by means of microwaves at about 200°C. The chosen variables were: mass. ‘compact degree of the reactives and the applied power. The aim was to relate the Behavior of the exposed materials te thsir auice INTRODUCTION ‘There fas been mny discussions ghoul the mechanism that governs the microwave energy absorption, although ‘pale losses, fon jump relaxation and ohmic effect [Binner, 1993] have been proposed, the real contribution of cach mechanism is still unknown. this study we compared CazrO, against BaTiO, (perovskites), ond NAgAlLO, against ‘YnAL,O, (spinels: The results show thatthe role of the:specics themselves ago mre important thas the ftice tha they conform Permskite ‘Sone iowié ceramiés are complen, they are trased of a cubic system with more than. two types’ of ions within the unitary cell. Both, the actahedral and tetrahedral sites are either partially or fully accupied by ions. The lattice of the calcium zirconate is w perovskite, in which the tons Ca" and O* are combined for conforming a compact eubic lattes with the Zr locaied over the oetahedral sites. Each oxygen ts surrounded by Ca at the canter of the unitary fice centered cubic cell where the Z+*" is coordinated with six O° Spinel ‘The Spinel structure is based over a super Intice made of oxygen fons in a fhoe centered eubie cell with just one fraction of ths oetaheral and tetraedral sites occupied. The compounds with an stoichiometry ABO. an whiek A and B- cations are 2+ and 3+ respectively, are par of the spinct structure, The unitary spine! enntains eight face centered cubic suiblaniees of oxygen. Half af the cetahedral ster and one eighth of the tetahedral ones are Gecupied. In the regular spinel (AB,O,), such a2 MAIO, the AI” gre in Oe wetahedral sites and the Ma” are in the tetrahedeal ones, EXPERIMENTAL FROCEDURE ‘The general experimental design was 2 type, based on previous experience [Aguilar J. Gonzalez M. ahd Géinez 1, 1997] the chosen variables were corapact load, applied power and exposed mass. For producing the calcium zirconate de values were (and 1300 Kiem” forthe load, 1000 and 2000 W for the applied power and a exposed mass of 8 and 1 For obtaining the magnesia-shurnina spine! the samples were compacted by a load of 1500 Kefem?, the power levels were 1500 and 2000 W and the masses were 7 and 14 gr. The mixture Tatios wer: stoichiometty |:| with & graphite bed of 0.5 gf becanse it is necessary te take the reactives to 2 temperature where they besome microwave absorbents; The materials enptoged and their characteristics are presented in the Table L The samples hae a disc shape with the dimensions that are presemed im Table IL 5Table 1, Particle size of the employed materials Table il. Dineensions ofthe samples te be processed ano, [Caos Mi ALO; ‘The perovskite BaTiO) and the spinel ZnALO were produced at a single power of 1500 AW with rmaxses of 9 and 16 gr. respectively froen the materials that were described in Table ‘After an analysis of the interaction of a high alumina crocible with the sample i was decided to keep i¢as a container for the prapblic aad the sample. the whole system was insulated wath cccamic fiber for decceasing tic heat losses. The average characteristice of the crucible were: Weight = 195 gr volume of the crucible: 41,8 ¢¢; density: 2,78 gree; capacity: 26 9 ev. ‘The generator was-a 3 KW variable power magnetron at 2.45 GHz, the waveguide was a WR2%4 (ype and the cavity: was: 425 em X 25.4 om X 25.4 cm made of stainless steet. Several data such 24 temperatuce. forward and reflceted power were recorded during the rest It wan decided to use optical Pyrometry for taking the teraperature, there js an ceror involved in this technique duc to the uncertainty in the emussivity factor, however we were adjusting ths value against a reference temperature, Other aspect is chat the cavity had a scxcen ‘as adoor, which is acally one of the walls of the cavity and ix interfering with the temperature measurement. Further tests with and without the seteen during cvaling (without the microwave field) allow to determine that the real temperature (compared against thermocouples) is aetually about 200°C above the one given by the optical pyrometer, An analysis of the cavity shows where the maximum arc Focal, tis was abo confimed by moving the sample and by burning 2 polymer inside the cavity [A. Garcia, 1957} so thot the sample wag sat in these places, The tuning was achicved with four screw tanec in suck a way that the reflected power was minimized, having, in this case: the maxinmum absorption. The samples were analyzed by means ox ray diffraction and electronic micrascopy. The absorbed energy ‘was estimated from both, the forward and reflected power RESULTS AND DISCUSSION Calcwum ziccomate: Although one of the most important results is the achieved reaction degree. Table Ill shows the rmaximmurn achiewe temperature in the experiments. Am analysis of normal probability shows thatthe applicd power i the mos: important factor, although this scem obvious, it was convenient to review the ffect ofthe rest ofthe variables, and the possible interaction between them. Further analysis sows that the compact variable does not have 8 significant effect over the achieved temperature, Figure | where it gan be seen the probable sintering protest as is described in the literature [Kingery W., 1976]Figure 1, SEM images of CaZrO; obtained by means of microwaves at 1500 W from non compact raw materials. Magnesia-alumina spinel The results of the MgAI,O, tests are summarized in Table IV. Reaction degree was higher than the encountered in previous works [Aguilar J., Gonzalez M. and Gémez 1, 1997]. The grain size of the spinel is appreciated in figure 2. while figure 3 shows lines that are very common in this kind of materials when they are processed rapidly. BaTiO; porovskite ‘The maximum temperature was 1800°C, but it was observed a strong iteration with the container, thus the results in this case are better apply to the system rather than the BaTiO; ZnALO, spinel ‘The maximum temperature was 2016°C. In this case there is a sudden temperature increase at about 800°C, which would correspond to an increase in the imaginary part of the permittivity as a temperature function. This increase has ‘been reported by some researches (Dadon and Gershon, 1997], although the temperatures are quit high the full reaction ‘was not achieved, but the partial reaction that took place exhibits the familiar structure of the spinel, Figure 2. SEM image of MgAl:0, spinel processed at Figure 3. Sample of MgAlO, showing the 1500 W for 5 min, (Sample B3) structure (SEM).Table 1V. Results ofthe experiments conducted for obtaining MgAlO, Exp. | Power(W) | mass (gr.) | comp. | Exposition time and | Tra(°C) | ‘Time (minutes) for @ 1500 power achieving Tax (C.) Keim? Bi 2000 6 0 ¥@2000W 214 256" 3°@800w 2'@ 1500W BD 2000 68 eS 255" 1196 235" BS, 1500. 13.7, no if 2127 507" Bez | 2000 i es 30 2142 ear" Be3 | _ 2000 738 es x 1931 TO FINAL COMMENTS One idea of this work was to verify iftwo materials with the same lattice have the same behavior under a microwave field, The results show that it was possible to produce CaZ10s however, the comparisons with the other two substances (BaTiO; and ZnAl,O.) showed that even whe le to produce these ones they respond in a different way to the compact and applied power, meaning that the heating mechanism is more related to the species rather than the lattice, altough it will neccesary to perform more test in a waveguide insetad of a cavity. ACKNOWLEDGMENTS The authors express their gratitude to CONACYT (Mexican Council for Science and Technology) and to the University of Nuevo Leén for their support. REFERENCES [1] Aguilar J, Gonzalez M., Gémez I. 1997. Microwaves as an energy source for producing magnesia-alumina spinel, J. Microwave Power and Electrom Energy 2 (32), 74-79 [2] Binner J. The potential of microwave processing of ceramics, Materials World 1, (3), 152 [3] Dadon D., Gershon D. Observation of an electromagnetically driven temperature wave in porous zinc oxide during microwave heating, Microwave Processing of Materials V, MRS 1996, vol 430. [4] Gareia A. Irradiacién de termoplasticos mediante microondas y su efecto sobre la adhesion en materiales compuesto. Thesis of Master of Science, Universidad Autnoma de Nuevo Leén, 1997. [5] Kingery W. Introduction to ceramics, John Wiley & Sons, 1976.DENSITY-INDEPENDENT PERMITTIVITY FUNCTIONS FOR MOISTURE SENSING IN FOODS AND AGRICULTURAL PRODUCTS SAMIR TRABELSI, ANDRZEJ W. KRASZEWSKI, AND STUART O, NELSON U.S. Department of Agriculture, Agricultural Research Service, Richard B. Russell Agricultural Research Center, Athens, GA 30604-5677, US.A. strabelsi@qaruars.usda.gov ABSTRACT Permittivity-based calibration functions for microwve moisture content determination in granular materials independent of density are a suitable solution for design and implementation of cost-effective on-line sensing devices. ‘Two of these functions are tested for corn and wheat at a microwave frequency of 11.3 GHz.and 24 °C. INTRODUCTION Moisture content is an important parameter often used in quality control and in defining optimum conditions for processing many food and agricultural products. Conventional methods for moisture determination rely on off-line oven drying of a few samples at a specific temperature for several hours or on batch type electrical moisture meters calibrated to oven standards, ‘These methods are time consuming and their representative character may be questionable when large quantities are considered. Also, they do not fulfill the needs of highly automated industrial processes for which moisture content has 10 be determined continuously on-line. For this purpose sensors based on permittivity ‘measurements at radio and microwave frequencies have been developed and successfully used for nondestructive testing of a wide variety of materials in different industries [Nyfors and Vainikainen, 1989]. Ata given frequency and a given temperature, the complex permittivity is dependent on the physical properties ofthe material under consideration. Many food and agricultural products are granular. Therefore, in addition to moisture content, bulk density and other factors such as geometry and dimensions of the granular particles affect the complex permittivity. To extract moisture content from permittivity measurements one should minimize effects generated by these factors or account for them in the final calibration equation. For moving or flowing grains, bulk density fluctuations are among the most troublesome. It is possible to reduce these fluctuations by mechanical means by keeping the layer thickness constant or by using a configuration that maintains an average density. This still produces unpredictable errors in moisture content determination. Another way is to determine bulk density by a separate measurement (gamma-ray attenuation or weighing) and compensate for its effect. A separate density measurement is always an additional cost with more technical complications in the design and implementation of the measuring system, A better alternative is to identify empirically or define theoretically density-independent functions of permittivity exclusively dependent on moisture content. From an industrial perspe-tive, these functions should be easy to manipulate for moisture content computation and tolerate instabilities produced by the measuring system and the immediate environment. Effectiveness of such functions for moisture prediction has been reported recently [Trabelsi and Nelson, 1998; Kraszewski etal, 1998]. These studies showed that a standard error of performance of about 0.3% moisture content or less is achievable. In this paper, results are shown for two permittivity-based density-independent functions for wheat and com at microwave frequencies. PERMITTIVITY-BASED DENSITY-INDEPENDENT FUNCTIONS ‘The intrinsic nature of the complex permittivity makes it the best entity to describe the wave-material interaction. However, because moist granular substances are mixtures of components exhibiting different dielectric behaviors, it is rather difficult to use the measured complex permittivity directly for moisture prediction. Fig. 1 and Fig. 2 show variations of the dielectric constant, ¢', and the dielectric loss factor, e", of wheat and shelled com with moisture content at 11.3 GHz and 24 4C. The scatter of data points at each moisture level is mainly caused by bulk density fluctuation, It is obvious that moisture content cannot be reliably extracted from these data. The essence of the definition of a density- independent function is based on the elimination of such effects and its exclusive dependence on water content. Historically, the first density-independent permittivity function was based on empirical observations [Kraszewski et al, 1977; Meyer and Schilz, 1981] and is expressed analytically as: 9Seo a In fact, the concept of a density-independent permittivity function is also expected to reflect a physical principle where the bulk density is no longer a variable. The energy distribution between stored and dissipated energy within the dielectric can be considered es such a principle for lossy materials. For this to be done the electric field inside the material has to be defined. This is rather difficult for complex media such as granular materials. One way to solve this problem is to consider the ratio of the two forms of energy, in which case the electric field cancels out and the ratio simplifies to the loss tangent, and = e"Ve'. This along with observations in the ¢*-c' complex plane [Trabelsi et al., 1997; Trabelsi et al, 1998a; Trabelsi et al, 1998b] constitute the essence of the density-independent function defined as: We eqee . rere ay fs constant ata ven feaneny. Fig. 3 and Fig. 4 show variations of yy and 2 vs. moisture content in wheat and com at 11.3 GHz and 24 °C. For both functions, the scatter of the data points is significantly reduced, and a linear relationship exist between each fanction and the moisture content. For the function 4), an individual relationship can be identified for each material: rwtear = wheat M+ wear ® Di,com = Qi,com M + bi,com @) where M is the moisture content in percent and a and b are slope and intercept constants. Therefore, two different calibration equations are needed to predict moisture content in wheat and cor, respectively, from measurements of the ‘complex permittivity when y, is used. For y, although com and wheat have pronounced differences in kernel dimensions and shape, bulk density, and composition, data points for a given frequency are nearly superimposed . Consequently, data can be fitted by the same equation: th=qMt+h, 6 resulting in a single calibration equation for both materials: a © This simplifies considerably the calibration procedure and the design of a moisture meter for moisture determination independent of density and independent of the material. The calibration constants for both calibration functions y, and Wp along with the standard errors of calibration, are given in Table 1. ‘The standard error of calibration for moisture content predicted with Eq. (6), for both wheat and com has a value between those for wheat and com determined with ve CONCLUSIONS Permittivity-based density-independent calibration functions for indirect nondestructive determination of moisture content in granular materials provide an adequate solution for the design and implementation of on-line microwave moisture sensors. Because they are fully defined in terms of the complex permittivity, these functions can be applied regardless of the measurement technique. Therefore, the accuracy with which moisture content can be determined is exclusively dependent on the accuracy with which the complex permittivity can be measured. The second function, Y, provides a unified calibration for wheat and com in which case a single calibration equation suffices for moisture ‘content determination in the granular materials regardless of the grain type. This constitutes an important step toward the design of a "universal" cost-effective moisture meter and the standardization of dielectric methods for reliable nondestructive and continuous determination of moisture content. 10REFERENCES Kraszewski, A. W., Kulinski, S., and Stosio, Z. 1977. A preliminary study on microwave monitoring of moisture content i ‘wheat. J. Microwave Power, 12 (3): 241-252. Kraszewski, A. W., Trabelsi, S. and Nelson, S. 0. 1998. Comparison of density-independent expressions for moisture content determination in wheat at microwave frequencies. J. Agric. Eng. Res. 71: 227-237. Meyer, W., and Schilz, W. M. 1981. Feasibility study of density-independent moisture measurement with microwaves. TEE] Trans. Microwave Theory Techn. 29 (7): 732-739. ‘Nyfors, E., and Vainikainen, P. 1989. industrial Microwave Sensors, Artech House, Norwood, MA. Trabelsi, S., and Nelson, S. 0. 1998. Density-independent functions for on-line microwave moisture meters: a general discussion. Meas. Sci, and Technol. 9 (4): 570-578, Trabelsi, S., Kraszewski, A. W., and Nelson, S. O. 1997. Simultaneous determination of density and water content of particulate materials by microwave sensors. Electronics Letters, 33 (1): 874-876. Trabelsi, S., Kraszewski, A. W., and Nelson, S. 0. 1998a. New density-independent calibration function for moisture sensing in particulate materials. IEEE Trans. Instrum. Meas. 47 (3): 613-622. Trabelsi, S., Kraszewski, A. W., and Nelson, S. 0. 1998b. Nondestructive microwave characterization for bulk density and moisture content determination in shelled com. Meas. Sci, Technol. 9: 1548-1556. ‘Table 1. Linear regression statistics and standard errors for calibration functions y) and yy for wheat and com at 11.3 GHzand 24°C, a ve ‘Statistic | wheat | com | wheat and com Slope, | 00193 | 00247 | _ 0.0183 Tntereeps, b | -0.0832 | -0.1089 | 0.0392 e 0.9876 | 0.9600 | 0.9619 SEC, % | 023 _| OAT 039 *Percent moisture content ptsncaa 2 ieee eae Baal ‘ bes, 8 a0 Bos 2 3 8 2s 5 Lae d 3 gos 2 r oa 10 12 1“ 16 © 20 4 “4 16 18 20 ‘MOISTURE CONTENT, % Fig. 1 Dependence of dielectric constant on moisture content in wheat and corn at 11.3 GHz and 24 °C. 040 [MOISTURE CONTENT, % Fig. 2 Dependence of dielectric loss factor on moisture content in wheat and com at 11.3 GHz and 24 °C. 0.95 020 020 018 010. er a i a er) MOISTURE CONTENT. Fig. 3 Dependence of yi on moisture content in wheat and shelled corn at 11.3 GHz and 24 °C. 12 . © 2 « 6 18 2 MOISTURE CONTENT, % Fig. 4 Dependence of y2 on moisture content in wheat and shelled com at 11.3 GHz and 24°C,DIELECTRIC CONSTANT OF LENTIL AND DRY PEAS Kailash Prasad Thakur and Wayne S. Holmes ‘The authors are affiliated with Imaging and Sensing Team, Industrial Research Limited, 24 Balfour Road, PO Box 2225, Pamell, Auckland, New Zealand, Email: k thakur@ir.cri.nz ABSTRACT ‘The dielectric constant of lentil and dry peas has been measured as functions temperature (20 C to 90 C) in the frequency range of 2.6GHz to 4GHz using a waveguide cell and a new dielectric mixture equation. Both real and imaginary components of the relative permittivity increase with temperature. Regression equations for the variation of permittivity ‘with temperature have been developed. INTRODUCTION Methods for measuring permittivity of materials using a waveguide cell are well known and described extensively {[Kraszewski and Nelson, 1996, Green 1997]. For granular materials in a waveguide cell, one is forced to measure the permittivity of mixture formed usually with air in the void space. The value of the dielectric constant must be extracted from the measured value for the mixture with air. This paper presents a technique for the measurement of dielectric constant of granular materials using a partially filled waveguide cell and a new mixture equation [Thakur et.al, 1999}, METHOD Methods for measuring the permittivity of granular materials using the waveguide cell has been reported recently (Thakur, 1999] that uses a realistic mixture equation [Thakur et. al., 1999] ef" aye +(1-ve™ a where vis the volume fraction of granular material in the mixture with air, €), &2 and &q are the dielectric constants of ‘granular material, air and the mixture, c is a constant, ‘The values of dielectric constant of mixture is measured for different values of vi and the result is extrapolated to generate €: corresponding to vi = 1. The results for pea and lentil are shown in Figures | and 2, respectively. ‘The values of dielectric constants obtained for pea and lentil are 5.673 and 4.905 respectively. Figures 1 and 2 also show a good agreement between the experimental and model results. We have also studied the effect of temperature upon the permittivity of lentil as shown in Figures 3 and 4. The abrupt behaviour of permittivity versus temperature curves in figures 3 and 4 at @ low value of moisture content is attributed to the nature of binding of water molecules and its coordination number. When the moisture content is very high (> 54%), water molecules form bond with its neighbouring hydrogen with coordination number ranging fom 4, 5 or even 6, The value of coordination number decreases as the moisture content is reduced, which gives rise to the behaviour shown in Figures 3 and 4. The regression equation for the dielectric constant of lentil is shown in Figure 3 as « quadratic function of temperature (°C). 132.6 GHz ve a Ss Dielectric Constant = a Ss 1.0 SS ae Oh." 04. 02 “03°04 ° 05. 06 Volume fraction of Pea Figure 1: Model values and the experimental values of dielectric constant of dry pea and air mixture as a function of volume fraction of peas. The model values are for c= ~0.361 and tua = 5.673 Dielectric Constant 0 01 02 03 04 08 06 Volume Fraction of Lentil Figure 2: Model values and the experimental values of dielectric constant of dry lentil and air mixture as a function of volume fraction of lentil. The model values are for = -0.361 and eugu = 4.9, mc 8% a3 ge 2721997810 + ocomngte7 “T+ 821780E-8*PT (at 268 GH) | = 2600401500 ooneazase T+ TEMGEEE TT (ata85 Gr) 200 300 «400500 0700 Temperature °C Figure 3: Variation of dielectric constant for the lentil (packing fraction 0.65, Moisture content 8 %) as a function of temperature 140.45, 0 2.68GH: 0.401 = 3.95GHe —— Regression 0.35 Regression 0.30 0.25 ea 0.20 20.0 40.0 600 800 ‘Temperature °C Figure 4: Variation of dielectric loss factor for the lentil (packing fraction 0.65, Moisture = 8 %) as a funetion of temperature ‘The regression analysis of dielectric loss factor for lentil as a function of temperature generated the straight lines e” = 0.1886 + 0.002533 * T; with R? = 0.996 at 2.66 GHz @ and e" = 0.1677 + 0.002255 * T; with R? = 0.999 at 3.95 GHz @) THREE PHASE MIXTURE EQUATION We have further caried out some measurements on the three phase system consisting of lentil, pea and air. The ‘mixture equation for two phases recently proposed on the basis of Pade approximant (Thakur, et al, 1999) is given by ‘equation (1). Now let us consider a system (mixture) of three components have volume fractions v, vz, and vs and the dielectric constants €,, ¢, and ¢, respectively in the mixture, If we consider that the component 1 is fixed and ony the ‘components 2 and 3 are changing the mixture equation for phases 2 and 3 is given by v, y, en 2 ot 4 V3 pits va + v5 v, +3 ® ixture equation for two phases having dielectric constants ¢, and 3, and volume Now we need to set up the fraction in mixture v; and V2+ evn ave +(v, +, )e% © From equations () and (5), we have em =e" +v,e7 + ye" o 15If there is no chemical reaction among the individual components, we have vtwtwel a Table 1 presents the results of comparison between the three phase model with experimental data for lentil, pea and sir mixture, where the NID contribution is defined in an earlier paper [Thakur, et. a, 1999]. Table J: Comparison of mixture model (ct = -0,361) for three phases (6) with experimental results Material Volume Dielectric | NID contribution Fraction Constant Pea 0.32881 5.673 0.04177 Lentil 0.33986 4.905 0.05785 Air 0.33633 1,000 0.23441 Mixture (Model, eq 6) | 7.00000 3.037 0.33403, Mixture (Experiment) | 1.00000 3.037 at 2.61 GHz Mixture (Experiment) | 1.00000 3.016 at 3.94 GHz CONCLUSION ‘This paper presents the results of the measurement of the dielectric constant of lentil and pea. Effect of temperature upon the permittivity of lentil is atributed to the binding of water molecules with grains and its coordination number. ‘The mixture model has the capability to work for a three phases mixture as well. ACKNOWLEDGMENT ‘The authors thank the Foundation for Research Science and Technology, New Zealand for funding this research through their contract CO8606. REFERENCES Green, A.1997. Measurements of the dielectric properties of cheddar cheese. J. Microwave Power and Electromagnetic Energy 32 (1): 16-27, ‘Thakur, K. P. 1999, Modelling the dielectric constant of rice grains, Collection of Papers presented at the Third Workshop on Electromagnetic Wave Interaction with water and moist substances, Sponsored by U. S. Department of Agriculture, Agriculrure Research Service, Athens, April 1999, pp. 239-243. ‘Thakur, K. P., Cresswell, K., Bogosanovich, M and Holmes, W. 1999. Modelling the permittivity of liquid mixtures, J. Microwave Power and Electromagnetic Energy 1999: in press Kraszewski, A. W. and Nelson, S. 0. 1996. Moisture content determination in single kernels and seeds with microwave resonance sensors. In Microwave Aquametry - Electromagnetic Wave Interaction with Water-Containing Materials, “edited by A. W. Kraszewski”, New York, The Intsitute of Electrical and Electronic Engineers, 1996, pp. 177-203. 16USE OF CEREAL GRAIN PERMITTIVITY FOR SENSING MOISTURE CONTENT STUART O. NELSON, ANDRZEI W. KRASZEWSKI, KURT C. LAWRENCE AND SAMIR TRABELSI U.S. Department of Agriculture, Agricultural Research Service, Richard B, Russell Agricultural Research Center, Athens, GA 30604-5677, U.S.A. sonelson@qaru.ars.usda gov ABSTRACT Findings of recent research on sensing moisture content through dielectric properties of cereal grains by radio frequency (RF) and microwave measurements are summarized. Results are described that provide the basis for reliable sensing of grain moisture content, including techniques explored for sensing moisture content independent of bulk Gensity fluctuation and which, therefore, have applicability to on-line moisture measurements necessary for monitoring moisture in lowing grain. INTRODUCTION Because the moisture content of cereal grains is the most important factor determining safe storage potential, and. because it is important in determining market value, suitability for processing, and the quality of processed products, much effort has been devoted to development of rapid methods for moisture content determination. The electrical properties of grain are highly correlated with moisture content and have, therefore, provided the most practical means for sensing moisture with electrical instruments in the grain trade for more than seventy years. Early instruments were based on measurements of the de conductivity of grain as it passed between crushing rollers, but for at least the past 50 years, electronic instruments that sense the permittivity, or dielectric properties, of grain have been the dominant type ‘of moisture meters used at the grain elevators and grading stations in the United States and many other countries [Nelson, 1977] For moisture sensing in grains, it is important to understand the dependence of the dielectric properties of the grain on moisture content and other factors as well [Nelson, 1981; Nelson, 1991]. The dielectric constant always increases with increasing moisture content, and the dielectric loss factor generally does also. Knowledge of the ‘Variation of the dielectric properties with frequency is important in selecting the frequency range to use for moisture sensing. Instrument designers have a wide range of frequencies to consider in building grain moisture meters. Often the frequency selection is based on tradition, familiarity with design in certain frequency ranges, and on component costs. Dielectric properties also vary with the temperature of the grain [Nelson, 1979; Lawrence et al, 1990; Kraszewski et al., 1996; Trabelsi et al., 1997a]. Both the dielectric constant and loss factor generally increase with increasing temperature In addition to frequency, moisture content, and temperature, the density of the: grain is an important factor influencing the dielectric properties. As the bulk density of a grain sample is increased, additional mass is present to react with the electric fields, and the permittivity (dielectric constant and loss factor) will increase. Thus, all of these factors must be taken into consideration in designing and calibrating instruments for measuring grain moisture content. GRAIN PERMITTIVITY MEASUREMENTS ‘The first method for measuring the dielectric properties of grain (1 to 50 MHz) and resulting data were published forty-six years ago [Nelson et al., 1953]. Since then, measurement techniques were developed for other frequency ranges, and additional data became available on several types of grain [Knipper, 1956; Nelson, 1965; Nelsom and Stetson, 1976; Ban and Suzuki, 1977; Jones et al., 1978; Nelson, 1979}. Dielectric properties data measured ont ‘many kinds of grain have been collected and made available for use in grain moisture meter design and other applications [Nelson, 1991; ASAE, 1998}. Because moisture determination by dielectric methods depends on the dielectric properties of grain and the dependence of those properties on moisture content and other factors, some techniques of measurement were adapted for more efficient reliable measurements of the dielectric properties. One method involved the use of a shielded open- circuit, coaxial sample holder for grain [Jones et al., 1978], measurements with computer controlled impedance analyzers, and use of the invariance-of-the-cross-ratio technique, to cover the frequency range from 100 kHz to 1 GHz v7[Lawrence et al., 1989]. This system was used to obtain temperature-dependent permittivity data for wheat [Lawrence al, 1990]. Another method was developed with a coaxial sample holder designed for full two-port S-parameter ‘measurements and calibrated to provide permittivity measurements on grain samples from 1 to 350 MHz [Lawrence et al, 1998} For determining the dielectric properties at microwave frequencies, free-space permittivity measurement techniques have been used to obtain dielectric constants and loss factors of wheat and corn as functions of moisture content, temperature, and bulk density in the range from 10 to 18 GHz [Kraszewski et al., 1996; Trabelsi et al., 1997}. Grain samples were held in polyethylene or Styrofoam containers between a transmitting horn and a receiving horn connected to a microwave network analyzer, and the dielectric properties were determined from attenuation and phase shift measurements as the microwaves traversed the grain layer. Horn/lens antennas, which provided a focused ‘microwave beam, permitted measurcments on wheat samples of reasonable size at 4.8 to 12.3 GHz. without concern for diffraction at the edges of samples or the interference of reflected energy from surroundings [Trabelsi et al., 19984. DENSITY-INDEPENDENT GRAIN MOISTURE DETERMINATION Because an increase in bulk density of a grain sample produces the same increase in permittivity as an increase in moisture content of a certain amount, the influence of bulk density must be accounted for if accurate moisture contents are to be determined by dielectric-type moisture meters. In conventional moisture meters, which test static grain samples, the effects of bulk density. or test weight, are taken into account in various ways. These include corrections in calibrations determined empirically, special electrode configurations designed to compensate for density Variation due to packing of grain samples, and weighing of samples and provisions for obtaining uniform filling of sample holders. However, considerable effort has been devoted to development of techniques that permit moisture determination from the dielectric properties alone and that are independent of bulk density variation in the grain, For measurements on flowing grain, bulk density fluctuations are much greater than for static samples, and the need for density-independent moisture sensing is even greater than itis for batch sample moisture testers. ‘Studies on multiple-frequency impedance measurements, in the range from 1 to 350 MHz, on static samples in parallel-plate and coaxial-line sample holders designed for eventual moisture sensing in flowing grain, revealed potential for density-independent moisture sensing in wheat with standard errors of performance between 0.3 and 0.5% ‘moisture content (Lawrence and Nelson, 1993; Lawrence et al., 1998]. An improved shielded parallel-plate sensor, tested with a wide range of corn samples provided a standard error of performance of 0.28% moisture content. The key to reliable broad-frequency-range measurements was proper design of sample holders to limit impedance mismatches and data analyses involving spectral data processing and principle component analysis. Density-independent functions of the permittivity components were used in some of this research. ‘The density-independent functions had their origin in studies on moisture sensing with microwave ‘measurements [Kraszewski and Kulinski, 1976; Kraszewski et al., 1977; Jacobsen et al., 1980; Meyer and Shilz, 1980, 1981; Kent and Kress-Rogers, 1986]. A number of these density-independent functions of the dielectric constant and loss factor were developed and studied recently, applying them to data obtained on wheat and com with free-space microwave measurements [Trabelsi and Nelson, 1998; Kraszewski et al., 1998]. These data were obtained over wide ranges of bulk density, temperature and moisture content at frequencies between 11 and 18 GHz. Those den: independent functions providing the best performance yielded standard errors of about 0.2% moisture content. In addition to providing density-independent moisture content with good accuracies, the microwave ‘measurements of attenuation and phase shift, at a single frequency, can simultaneously provide a determination of the bulk density of the grain at the time of measurement (Kraszewski et al., 1997; Trabelsi et al., 1997: Kraszewski et a., 1999]. The accuracy of bulk density determination has been on the order of 3% in studies with wheat. ‘The newest of the density-independent functions permits the expression of both moisture content and density in terms of the permittivity components measured by any desired means [Trabelsi et al., 1997, Trabelsi et al., 1998a, 1998, 1998c |. The expressions involve two constants which are dependent on the type of grain, Onc is the dielectric constant divided by density, e'/p = k, for that grain at zero moisture content, or for grain of any moisture content at very low temperature (Fig. 1). The other is a constant at a given frequency, which represents the slope of the straight line resulting from the plot of ¢/o vs.

1000 V), and a low voltage MOS transistor (Q2), connected between the “SOURCE” terminal of QJ and earth via the RI current feedback resistor. pMas0 nay em Bae Fen x spy MAGNETRON a Ae Puss 29‘The regulator QI is used as a constant current source: on the control input (Gate) there is a constant voltage that depends on the peak current required in the magnetron. Whereas the regulator Q2 is used digitally to control or block Ql, by tuming its earth connection ON or OFF. This system makes it possible to achieve particularly high speeds: Figure 4 shows the anode curent in the ‘magnetron on plot 1 and the “PULSE” input control of the power supply on plot 2. As may be scen at 50 kHz ~and service factor lower than 1/3- the wave shape i stil sufficiently square. Figure 4 The zener DZ diodes protect QI in the event of a sudden voltage surge, as may occur if there is any shortcircuiting in the jg} | ‘magnetron. The resistor RI, a small value in [$0 ys ‘ohms, decreases the peak current on DZ in the | 19.6.0 event of short-circuiting The resistor R2 circulates a current of approximately 3 mA even when OFF in onder to make the system indifferent to the magnetron loss current. The reference signal applied to the appliance (0-10 V) fixes the mean value of the output anode current. The “PULSE” digital 50 ys ny signal controls or blocks the passage of | 8.50KV current in the magnetron. Ifthe power supply is used as a continuous, not pulsed, generator, the “PULSE” signal becomes an “enabling” signal. In this case the power supply delivers freq) 21.9578 ke er 7 Preg(D) 49.9831 ke direct current with extremely low ripple. eae wee past) 2.849 50 ps 1.09 — E : : z| igure 5 When PM4S0 is used in pulsed mode, it is possible to use an extremely low load factor so as to obtain currents ‘with a high peak but moderate mean value. i And r Figure 5 shows the current in the a) EI I | ‘magnetron at 2 kHz on plot 2, with duty- factor 0.5 and mean current 400 mA. Plot | 1 represents the current inthe primary ‘winding of TI, and plot 4 the voltage V2. | 1 ieev |f Las 8.50Kv Freq 21.9316 kte Fea?) 2.00318 kie Pkpk (3) 0.6.0 ras) 8.78. 30Figure 6 Figure 6 shows the current in the magnetron at 10 KHz on plot 2, with 7 al uty-factor 0.3 and mean current 450 re Io, mA: the peak current is 15 A. sas | | ile 1.00 ore an | t= eet freq) 21.8131 hie Frog) 10.4478 hie poh) eau ms) aay PM450 is controlled by a powerful micro-controller that makes it easy to program the various set points with the graphic display on the front panel, and which also performs the function of a pulse generator. The user can therefore ‘easily aocess the machine's internal parameters and likewise control the work mode and acquire system diagnestic data. Any firmware upgrades can be made via the serial communications link equipping the CPU, which ‘permit future implementation of industrial communications protocols. CONCLUSION Availability of fast speed and high power transistors has led to manufacture a powerful unit with very good pulsed capability: the modular design, as well as the latest microcontroller technology, will allow to easy upgrade the unit to reach higher power for the growing demands of the plasma applications market. 31MICROWAVE-ACCELERATED SOLVENT-FREE CHEMICAL TRANSFORMATIONS RAJENDER S. VARMA,” DALIP KUMAR, KANNAN P. NAICKER Department of Chemistry and Texas Research Institute for Environmental Studies (TRIES), ‘Sam Houston State University, Huntsville, Texas 77341-2117, USA ABSTRACT A solvent-free approach to expeditious synthetic organic transformation is described that utilizes neat Teactants and microwave (MW) activation. The salient features of this solventless strategy such as solvent conservation and the ease of manipulation will be highlighted in solid-state oxidation of dihydropyridines to pyridines, direct synthesis of amides from esters and amines and preparation of thio analogues of ketones, flavonoids, amides, lactones and esters using Lawesson’s reagent. INTRODUCTION The functional group transformations are integral part of organic synthesis. In view of the environmental Constraints and because of their important role in synthetic chemistry, the development of environmentally benign synthetic methodologies continue to attract the attention of chemists in search for newer, selective and eco-friendly methods.’ Our ongoing research program targeted to accomplish efficient chemical conversions have introduced several practical solventless methods namely deprotection !4-k condensation,1-q oxidation," and reduction! reactions under microwave irradiation conditions using neat reactants on benign mineral mineral supports that can be recycled. SYNTHESIS OF THIOKETONES, THIOFLAVONES, THIOISOFLAVONES, THIOLACTONES, THIOAMIDES AND THIOESTERS USING LAWESSON’S REAGENT The synthesis of thio analogues of ketones, flavones, isoflavones, lactones, amides, and esters has received considerable attention due to the biological importance of these molecules,? their rich photochemistry? and their usefulness as precursors for the synthesis of a variety of organic compounds. These transformations have been effected by variety of reagents namely, phosphorous pentasulfide,>4> hydrogen sulfide in presence of acid, bis(tricyclohexyltin) sulfide with boron trifluoride,24 bis (trimethylsilyl) sulfide5? with CoCla. HO and the Lawesson’s reagent [2,4-bis(p-methoxy pheny!)-1,3-dithiaphosphetane-24- disulphide}°"8 Most of these lengthy procedures, however, require the excess of reagents and involve the use of aromatic hydrocarbon solvents namely toluene, xylene, benzene, triethylamine or pyridine under dry conditions and affording only moderate yields of products. Initially introduced in 1986, the chemical applications of microwaves have now become an area of interest for the synthesis of a wide variety of compounds and efficient functional group transformations under solvent-free conditions.1_ The advantages of microwave irradiation are cleaner reactions, shorter reaction fimes and the ease of manipulation. In continuation of our efforts towards environmently benign organic synthesis herein, we wish to report the synthesis of thioketones, thioflavones, thioisoflavones, thiolactones, thioamides and thionoesters using the Lawesson's reagent (L,) in the solid state. 32The syntheses of thioketones, thioflavones, thioisoflavones, thiolactones, thioamidess and thionoesters has been accomplished by this simple process which in its entirity involves mixing the substrates with the Lawesson's reagent followed by exposure to microwave irradiation under solventless conditions. ‘The reaction is very general as is apparent froma wide range of substituents accomodated (Scheme 1). Earlier procedures needed excess of the reagent in lengthy reactions which led to the poor yield of the product due to significant side reactions. The present solvent-free protocol avoids the use of dry benzene, toluene, triethyl amine and carbondisulfide. In case of amides, 0.5 equivalent of Lawesson’s reagent (LR} is sufficient for the completion of reaction but thionoesters require 1.0 equivalent of the reagent. This is ir. contrast to 0.6 -3.0 equivalent of the reagent used by existing protocols with extended period of time (3-25h)- A range of aliphatic, aromatic and cyclic analogs of thio compounds are preparedin high yields and in a much shorter reaction time. Our solid state microwave irradiation protocol affords thioflavones and thioisoflavones in almost quantitative yields by admixing flavones or isoflavones with the Lawesson's reagent (Scheme 1). A variety of substituents on aryl ring are well tolerated and the reaction lead to completion in all the cases. LR. MW, 3-4 min os 86.97% z R R Re ee i LR., MW, 3 min 7 \ i L.R,MW Sex’ 23 min X= 0, NH, OR (Scheme 1) OXIDATION OF 1,4-DIHYDROPYRINES TO PYRIDINES Hantzsch 14-dihydropyridines are the most widely studied class of calcium channel blockers and some of them have been utilized for the treatment of coronary diseases or hypertension. The oxidative conversion of 14-dihydropyridines to the corresponding pyridine derivatives occurs initially during the first pass metabolism in the liver which is then further metabolized leading to the cleavage of the ester groups.” Since the relevance of this oxidative event to the biological NADH redox process and the metabolic studies that require the reference standards, this transformation has attracted the attention of several research groups. 10 Although many reagents have been utilized for this oxidative conversion,?-11-16 there is still need to develop a general approach that precludes the dealkylation at 4-psition in case of secondary alkyl and benzyl substituents. Herein, we report a convenient process for the oxidation of dihydropyridines to pyridines undex solvent-free conditions using microwave (MW) irradiation, that utilizes either phenyliodine(III) bis(trifluoroacetate) (PIFA) at room temperature or elemental sulfur under microwave irradiation conditions (Geheme 2) 33" ts H5C,0.C. CO;CHs HZCO.C. A260, 6yH5 W502. A 00,65 foresee fate fon os aa Hy NO es psi Hy NL CEG, Hy N~ CH; la-i da 2b-i (Scheme 2) The utility of inexpensive elemental sulfur under solvent-free conditions make this protocol more economical and environment friendly. SOLVENT-FREE SYNTHESIS OF AMIDES FROM CARBOXYLIC ESTERS AND AMINES USING MICROWAVE IRRADIATION ‘The amide functionality is an important unit among the organic molecules, naturally occurring or synthetic1718 Several protocals have been devised for the amide bond formation the notable being the solid- phase assembly of peptides. Although the direct transformation of carboxylic esters to amides is a potentially important synthetic operation, the eco-friendly practical pathways are rather limited for a number of reasons.!7.18 Ester aminolysis, in general, occurs under harsh conditions that require higher temperature and extended reaction periods,!9 or the use of strong alkali metal catalysts under conditions that are not amenable to molecules bearing sensitive functional groups 20 Our simple procedure entails the addition of solid potassium tert-butoxide (tBuOK) to a premixed mixture of ester (1 mmol) and amine (1 mmol) and exposing the reaction mixture to microwave irradiation in an unmodified household MW oven. : +BuOK, MW RCO;X + R'NH) ae: RCONHR' X = Me, Et; R = Cos, CqHS; R’ = Cols, p CICGHy, Coy (Scheme 3) The results for a variety of substrates are summarized in the Scheme 3. Relatively, the aryl amines undergo reaction at a slower rate when compared to alkyl amines but the reaction is sluggish with secondary amines. Among the esters, the reaction is slower for ethyl-2-thiophenecarboxylate when compared to methylbenzoate. REFERENCES 1. __ For an overview of solvent-free reactions accelerated by exposure to microwave irradiation see: (a) ‘Varma, R.S. “Microwave-Assisted Reactions under Solvent-Free ‘Dry’ Conditions” in Microwaves: Theory and Application in Material Processing IV Clark, D.; Sutton, W.; Lewis, D., Eds., American Ceramic Society, Ceramic Transactions 1997, 80, pp 357-365. (b) Varma, RS. Green Chemistry 1999, pp 43-55. (c) Varma, RS. Clean Products and Processes 1999, in press. For cleavage-deprotection reactions see: (d) Varma, R. S.; Chatterjee, A. K;; Varma, M. Tetrahedron Lett. 1993, 34, 3207. (e) Varma, R. S.; Chatterjee, A. K.; Varma, M. Tetrahedron Lett. 1993, 34, 4603. (f) Varma, R.S; Varma, M,; Chatterjee, A. K. J. Chem. Soc., Perkin Trans. 1 1993, 999. (g) Varma, R. S.; Lamture, J.B; Varma, M. Tetrahedron Lett. 1993, 34, 3029. (h) Varma, R. S.; Saini, R. K. Tetrahedron Let. 1997, 38, 2623. 34Beene 1. 1B. 4. 16. 16. Vv. 18, 9. 20. () Varma, R. S Meshram, H. M. Tetrahedron Lett, 1997, 38, 5427. () Varma, R. S.; Meshram, H. M. Tetrahedron Lett. 1997, 38, 7973. (k) Varma, R. S.; Dahiya, R.; Saini, R.K. Tetrahetiron Lett. 1997,, 38, 8819. For condensation-cyclization reactions see: (1) Varma, R. S,; Dahiya, R.; Kumar, S, Tetrahedron Lett. 1997, 38, 2039. (m) Varma, RS Dahiya, R. Synlett 1997, 1245. (n) Varma, R. S.; Dahiya, R; Kumar, S. Tetrahedron Lett. 1997, 38, 5131. (0) Varma, R. S.; Saini, R. K. Synlett 1997, 857. (p) Varma, R. S.; Dahiya, R. J. Org. Chem. 1998, 63, 8038. (q) Varma, R. $.; Kumar, D.; Liesen, P. J. J. Chem. Soc. Perkin Trans. 1, 1998, 4093. For oxidation reactions see: (t) Varma, R. S.; Dahiya, R. Tetrahedron Lett, 1997, 38, 2043. (s) Varma, R. $. Saini, R. K; Meshram, H. M. Tetrahedron Lett, 1997, 38, 6525. (t) Varma, R. S.; Dahiya, R; Saini, RK. Tetrahedron Lett. 1997, 38, 7029. (u) Varma, R. S.; Saini, R. K; Dahiya, R. Tetrahedron Lett, 1997, 38, 7823. (v) Varma, R. S,; Dahiya, R. Tetrahedron Lett. 1998, 39, 1307. Varma, R. S,; Saini, R. K. Tetrahedron Lett. 1998, 39, 1481. (w) Varma, RS; Kumar, D.; Dahiya, R. J. Chem. Res. (5) 1998, 324 For reduction reactions see: (x) Varma, R. S.; Saini, R. K. Tetrahedron Lett. 1997, 38, 4337. (y) Varma, R. S.; Dahiya, R. Tetrahedron 1998, 54, 6293. (z) Varma, RS.; Naicker, KP.; Liesen, P.J. Tetrahedron Lett. 1998, 39, 8437, Peters, R. H.; Crowe, D. F; Avery, M. A.; Chong, W. K.M.; Tanabe, M. J. Med. Chem. 1988, 32, 1642. de Mayo, P; Sydnes, L. K; Wenska, G. J. Org. Chem. 1980, 45, 1549, and references therein. (@) Reynaud, P.; El Hamad, Y.; Davrinche, C.; Nguyen-Tri-Xuong, E.; Tran, G.; Rinjard, P. J. Heterocyct. ‘Chem. 1992, 29, 991. (©) Kraemer, 1; Schunack, W. Arch. Pharm. (Weinheim, Ger.) 1986, 319, 1091 (©) Bhattacharya, B. K.; Singh, H. H.; Yadav, L. D. S.; Hoomaert, G. Acta, Chim. Acad. Sci. Hung. 1982, 110, 133. (@) Mes, G. F. ; Rizeardo, E, Le, T. P. T.; Chen, Y. Makromol. Chem. 1992, 193, 369. (a) Scheeren, J. W.; Ooms, P. Hi J Nivard, R. J. F, Synthesis 1973, 149. (b) Dash, B.; Dora, E. K; Panda, C. S. Heterocycles 1982, 19, 2098. (©) Staudinger, H.; Freundenberger, H. Chem. Ber. 1928, 61, 1576. (@) Steliou, K; Mrani, M. J. Am. Chem. Soc. 1982, 104, 3104, (©) Capperucci, A.; Degl'Innocenti, A.; Ricci, A.; Mordini, A.; Reginato, G. J. Org. Chem. 1991, 56, 7323. ( Cava, M. P,; Levinson, M. I. Tetrahedrn 1985, 41, 5061 (g) Jones, B. A.; Bradshaw, J. S. Chem, Rev. 1984, 84, 17. Flaim, S. F, Zelis, R. Fed. Proc. 1981, £0, 2877. Bocker,R. H.; Guengerich, E. P. J. Med. Chem.1986, 29, 1596. Stout, D. M.; Meyers, A. I. Chem. Rev., 1982, 82, 223. Wei, X. Y; Rutledge, A.; Triggle, D. J. J. Mol. Pharmacol. 1989, 35, 541 Kill, R.J, Widdowson, D. A. In Biorganic Chemistry; Van Tamelen, E. E. Ed. Academic Press (NY) Vol. 4, 1978, 238 Delgado, F.; Alvarez, C.; Garcia, O; Penieres, G.; Marquez, C. Synth. Commun, 1991, 21, 2137. Vanden Eynde, }}.; D'orazio, R.; Yves Van, H. Tetrahedron, 1994, 50, 2479. Maquestiau, A.; Mayence, A.; Vanden Eynde, J-]. Tetraitedron, 1992, 48, 463. Pfister, J. R. Synthesis, 1990, 689. Balogh, M.; Hermecz, I; Meszaros , Z.; Laszlo, P. Helv. Chim. Acta. 1984, 64, 2270. Mashraqui , S. H.; Karnik, M. A. Synthesis, 1998, 713 and references therein. North, M. Contemp. Org. Synth. 1994, 1, 475. (a) Beckwith, A. L.J. In The Chemistry of Amides: Synthesis of Amides; Zabicky, J. ed.; Interscience: New York, 1970, p 96. (b) Hudson, D. J. Org. Chem, 1988, 53, 617. March, J. "Advanced Organic Chemistry” 3rd Edition, J. Wiley and Sons, NewYork, 1985, 375. Basha, A Lipton, M.; Weinreb, S. M. Tetrahedron Lett.1977, 171 35RATE ENHANCEMENT OF REACTIONS BY MICROWAVES. ARE NON-THERMAL EFFECTS INVOLVED? RICHARD N. GEDYE Department of Chemistry & Biochemistry, Laurentian University, Sudbury, ON, Canada. P3E 2C6 ABSTRACT There is evidence that some reactions occur faster tinder microwave heating than under conventional heating at the same temperature. These rate enhancements are observed mainly in reactions carried out under heterogeneous conditions, but have also been reported in reactions of polar compounds in solvents of low polarity . Reactions of the latter type have been investigated in this study. The possibility of the involvement of non-thermal effects in the rate enhancement of these reactions will be discussed. INTRODUCTION Recently, there has been a renewed interest in “specific” or “non-thermal” microwave effects. This is largely due to observations that microwave heating of ceramic materials results in enhanced diffusion and solid-state reaction rates compared with conventional heating at the same temperature [1,2]. Although these results have been regarded as controversial because of difficulties in accurate temperature measurements, recent more reliable methods of temperature measurement in solid-state systems indicate that non-thermal effects are in fact involved [1]. As far as organic reactions are concemed, most reports of substantial microwave rate enhancements other than those in closed (increased pressure) systems, are for reactions of polymers 3.4] and reactions under heterogeneous conditions [5,6]. Although homogeneous reactions in the presence of polar solvents show little or no rate increases in open systems [7] there have been a few recent reports of microwave enhancements of homogeneous reactions of polar reactants in non-polar solvents [8,9]. In the latter case it was suggested that non-thermal effects were involved in these rate increases [8]. RESULTS AND DISCUSSION A number of homogeneous reactions previously reported to show substantial rate enhancements under microwave irradiation compared with conventional heating at similar temperatures have been re-examined. In some cases it was found that the reactions occurred at the same rate and in other cases small rate enhancements were observed [7]. These small rate increases can be explained by superheating of the solvent to a few degrees above its normal boiling point. It has been reported that a series of 1,5-aryldiazepin-2-ones can be synthesized in high yield by the condensation of o-B-arylendiamines with B-ketoesters in xylene under microwave heating in open vessels [8]. Yields of over 80% were obtained in most cases after heating for 10 minutes with a final reaction temperature of 136-139°. In contrast, when the reactions were carried out under conventional (oil-bath) heating for 10 min. at the same temperature, no products were obtained These results were of particular interest because of the dramatic rate enhancements and it was considered possible that specific, or non-thermal effects, claimed in this report, might be involved. It is to be noted that the reaction involved polar reactants in a solvent of low polarity. In the present study, the reaction of o-phenylenediamine with ethyl acetoacetate in xylene was repeated using the same quantities of reactants and solvent used previously [8]. 36CH Ni CH N= ‘NH oO: x Et 01 Seas Care was taken to carry out the microwave and conventionally heated reactions in the same vessels and as close as possible to the same temperature. After carrying out a number of runs, both microwave and conventionally heated, for 10 minutes, it was found that there was virtually no difference in the yields obtained by the two heating methods. Hence there was no evidence for specific microwave effects in this reaction. In fact, the reaction is qute rapid at the boiling point of xylene and there is little advantage in using microwave heating in this case. ‘There appears to be some evidence that microwave enhancements are greater for slower reactions than faster reactions [5]. Observations in this laboratory that the slow Knoevenagel reaction of acetophenone with ethyl cyanoacetate shows a rate enhancement of 2.5 times under microwave irradiation in an open system, supports this hypothesis. Pho COE Ph _CN PhCOCH; + NCCH;CO,Et ———> Deak i = Hy ‘CN CHy CO2Et Investigations are currently underway on the effect of microwaves on slower reactions of polar reactants in solvents of low polarity. CONCLUSION Although recent research supports the involvement of non-thermal effects in microwave assisted reactions in the solid state, there is currently little evidence for non-thermal effects in homogeneous organic reactions. ‘The present investigation does not support claims that specific or non-thermal effects are involved in homogeneous reactions of polar compounds in solvents of low polarity. REFERENCES 1. JH. Booske, RF. Cooper, S.A. Freeman, K.J. Rybakov and V.E. Semenov, “Microwave ponderomotive forces in solid-state ionic plasmas.” Physics of Plasmas, 5, 1664 (1998) and references cited therein. 2. S.A. Freeman, JH. Booske and RF. Cooper, “Novel method for measuring intense microwave radiation effects on ionic transport in ceramic materials.” Rev. Sci. Instrum., 66, 3606 (1995). 3. D.A. Lewis, J.D. Summers, T.C. Ward and JE. McGrath, “Accelerated Imidization Reactions using Microwave Radiation.” J. Polym. Sci. Part A: Polymer Chem., 30, 1647 (1992). 4. J.B. Wei, Z. Fathi and M.C. Hawley, “Non-thermal effects during microwave processing of materials.” Proc. 30" Microwave Power Symposium. Denver, Colarado. (1995) p. 11. 7A. Loupy, P. Pigeon and M. Ramdani, “Synthesis of long chain aromatic esters in a solvent- free procedure under microwaves.” Tetrahedron, 52, 6705 (1996). C. Shibata, T. Kashima and K. Ohuchi, “Non-thermal influence of microwave power on chemical reactions.” Jpn. J. Appl. Phys., 35, 316 (1996). RN. Gedye and J.B. Wei, “Rate enhancement of organic reactions by microwaves at atmospheric pressure.” Can, J. Chem., 76, 525 (1998). K. Bougrin, A-K. Bennani, S.F. Tétouani and M. Soufiaoui, “An easy route to synthesize 1,5- aryldiazepin-2-ones.” Tetrahedron Lett. 35, 8373 (1994). ACS. Reddy, P.S. Rao and R.V. Venkataratnam, “Fluoro Organics: A facile and exclusive synthesis of novel 2-or 4-trifluoromethyl (1H,5) aryldiazepines.” Tetrahedron Lett. 37, 2845 (1996). 38ANALYSIS OF THE ELECTROMAGNETIC FIELDS IN MICROWAVE CAVITIES AND THE TEMPERATURE FIELDS IN LOADS USING FINITE-DIFFERENCE TIME DOMAIN METHOD S.H. CHO, Y.M.LEE, H.J.KIM, H.J.KANG ‘MIW Application team, Home Appliance Research Laboratory, LG Electronics Inc. 327-23, Gasan-Dong, Keumchen-Gu, Seoul, 153-023, Korea ABSTRACT The computation of the fields inside three dimensional microwave cavities are performed using Finite- Difference Time-Domain(FDTD) method. The temperature field in 2 dielectric load obtained from the heat conduction equation is compared with the infrared picture, The cavities with various types of waveguide aperture and various load are tested numerically and the change of the electromagnetic field and the resulting temperature field on a load was examined. INTRODUCTION ‘The microwave heating techniques have been used in industrial and food processes. To understand the heating mechanism and the electromagnetic field distribution in the microwave oven cavity, much research based on FEM(Finite Element Method) has been performed. However, due to the complexity of the numerical algorithm and high computational cost of FEM, the researchers have been in search of a better numerical method. Recently the FDID method, as first proposed by Yee( 1966), has been widely used in electromagnetic problems in the areas of antennas and microwave devices, scattering from random surfaces, non-construction evaluation problems. At first, Yee’s FDTD method did not receive much interest due to the limitation in applying the open boundary condition. However, after the PML(Perfectly Matched Layer), in which all the incoming waves were absorbed perfectly, was developed by Berenger(1994), the research using FDTD method increased exponentially, In this paper, three dimensional FDTD method is employed to analyze the electromagnetic field in a loaded rectangular cavity with various types of waveguide aperture and various load. In addition, the present work is included the heat analysis of the load in a cavity. To design an effective microwave cavity, in which the load is heated rmly, we have studied numerically the electromagnetic field in various microwave cavi NUMERICAL DETAILS It is well known that the governing equations for the electromagnetic field in a microwave oven cavity are the ‘Maxwell's equations, which are constituted from six coupled time-dependent partial differential equations, as follows. oH, a, 6, * ) oH, |= -o'H,|, a ay " &, oH, oH, ) e, ~oE, |, a x @ a ‘To calculate these equations, which are integrated explicitly with time, we developed a Maxwell's equations solver ‘based on the algorithm developed by Yee(1966). Because the E and H fields are coupled to each other, all of the E and H vector variables are located in 1/2 staggered position in time and space. The equations are used in a leap-frog scheme to incrementally march the E and H field forward in time. To maintain stability, the electromagnetic waves are allowed to propagate through no more than one cell per a time step. Because of numerical dispersion error, the ‘numerical grid size is decided to be smaller than 2/10, where 1. is the wavelength. 39‘The PML(erfectly Matched Layer), known to be very robust among various formulations of the open ‘boundary condition, is adopted at the open boundary as an absorbing boundary condition. All of the waves are absorbed perfectly in PML layer. The wall is assumed to be a perfect conductor, on which the normal magnetic field and the tangential electric feld should disappear. To model an input source, we need the frequency and the magnitude of the input source. The frequency is determined from the resonance frequency of a magnetron and the magnitude from the given input power and the specific resistance of the magnetron’s antenna. If the magnitude of the input source is uniform along time, the convergence performance would be bad. Therefore we used the tangent hyperbolic function for the magnitude of the input source until 20 periods. As integrating the Maxwell’s equations with time, the converged periodic solution can be obtained. After this time, we could analyze the time-averaged field from this periodic motion of electromagnetic field The governing equation for the temperature field in a load are the heat conduction equation, in which the heat source(Q) is calculated from the electric power and the loss factor of the dielectric load as follows. We assumed that the dielectric constant is uniform within a load and that is not the function of load temperature. = = PCr Se Vo(KVT)+Q where Q= waerE> RESULTS AND DISCUSSIONS The code, which is developed by FDTD method, is validated with the infrared picture by experiment. To analyze the electric power distribution in a microwave cavity, we examine a simple cavity of 200 X 280 X 280mm and waveguide 59.4 X 119 X 150mm. The load of 20x240x240mm is located 20mm upper position from cavity bottom wall, which is made of a wood, whose dielectric constant is €=2.3-j0.25. The source is excited sinusoidally in a waveguide for a frequency 2.45GHz. Figure 1 compares the time-averaged dissipated electric power( o |E*|) distribution by simulation and the temperature distribution by the infrared picture of a wood plate. We found that the temperature field is similar to the dissipated electric power of the load, therefore the temperature field in a load can be ‘guessed from the dissipated electric power distribution by simulation reasonably. (@) the simulation on the upper side © (@) the infrared picture on the lower side Figurel. Comparison of the electric power distribution by simulation and the temperature distribution by the infrared picture of the wood plate 40The simulations of the microwave cavities with the various waveguide apertures, which have three opening types(bottom opening, top opening, twin opening), are performed. From Figure2, we found that the different waveguide openings gave the different heating patterns of the load and the simulation result of the twin opening showed more complex heating pattern than others. We think that these simulations can help the design process of the ‘waveguide opening for uniform heating performance. | (@) bottom open (b) top open (b) twin open igure2. Comparison of the electric power distribution by computation and the temperature distribution by infrared picture Figure 3 represents the time-averaged dissipated electric power distribution by simulation and the temperature distribution by the infrared picture of a glass plate(10x240x240mm), which is located 20mm upper position from cavity bottom wall, whose dielectric constant is e~5.80.6. It was shown that the simulation result is virtually the same as that of infrared picture. As compared with the wood plate in Figure 1, this simulation result of the electric power distribution show more complex heating pattem because of the high dielectric constant of glass. @ the simulation (b) the infrared picture Figure3. Comparison of the electric power distribution by simulation and the temperature distribution by infrared picture of the glass plate The computations of the microwave cavities with a real waveguide aperture and a magnetron’s antenna and a Toad(20x240x240mm), which is located 20mm above the bottom cavity wall, are performed. The load is made of a ‘wood, whose dielectric constant is ¢=2.3-j0.25. The simulation result is the nearly same as that of the infrared picture in Figure 4. From this result, we confirmed that the modeling of the magnetron’s antenna and the input source is correct. ay@) the simulation (b) the infrared picture Figured. Comparison of the electric power distribution by simulation and the temperature di infrared picture of the glass plate Figure 5 represents the temperature distribution by simulation and infrared picture of a glass box(30x70x70mm), which is located 20mm upper position from cavity bottom wall, whose dielectric constant is e=5.8-j0.6. After 2 minutes heating, the maximum temperature in the load by simulation and infrared picture rose to about 45 degree. From this result, we are convinced of the modeling of the heat source. From the parametric studies using this simulation program and an optimal design program, we can design a new cavity for uniform heating performance. (@) the simulation Figure 5. The temperature field by simulation and by infrared picture ofa glass box (b) the infrared picture REFERENCE IP.Berenger, “A Perfectly Matched Layer for the Absorption of Electromagnetic Waves”, Journal of Computational Physies, Vol. 114, pp. 185-200, 1994 K S.Lee, “Numerical Solution of Initial Boundary Problems Involving Maxwell's Equations in Isotropic media”, IEEE Transactions on Antennas and Propagation, Vol. 14, pp.302-307, 1966 42HF ASSISTED CURING OF EPOXY-GLASS COMPOSITE FOR THE CAR INDUSTRY. Roussy, G.*, Parizot,G.*, Bastard,S.** * Laboratoire de Spectroscopie et des Techniques Microondes, Université Nancy I, BP 239, 54506 Vandoeuvre les Nancy, France. ** Renault SA, Direction de la Recherche, 78288 Guyancourt, France. The car industry is increasing its demand for parts epoxy-glass composite. HF techniques are well appreciated for manufacturing them and assisting epoxy curing. A teal industrial press machine was built for obtaining a robust model of HF curing, it was fully instrumented for measuring, continuously and during the process ~ the temperature at eight places inside the material sample ~ all the electric variables : the electric field which is applied to the material, the absorbed power and the complex permittivity of the material. Three V-I sensors, located in front of the applicator, in front of the matching box and inside the applicator are used as figure 1 shows. ‘Temperature measurement *“ | Computer V-I sensor V-I sensor Generator 10kW Matching box Material Optic fiber Figure 1 : Prototype HF set-up. 43Experiments were performed by step on-off field. Typical results are given figures 2, 3 and 4. These curves have been described many times, by many authors. The absorbed power varies although the HF field is constant because of the viscosity, which changes the permittivity of the material, before it cures. The temperature increases because the curing reaction is exothermic. —fibre optique 1 fibre optique 2 — fibre optique 3 —fibre optique 4 — positionxt0 (mm) P incidente 0 100 200 300 400 500 600 700 0 100 200 300 400 500 600 700 Figures 2 and 3 : Typical temperature distribution. 44“Modeling of the curing process. The main idea was to start to model the instantancous temperature distribution from the knowledge of the total instantaneous absorbed power Pa(t) measurements. We introduced the local instantaneous degree of cure : &. As usually, o =0 and =1 correspond respectivelly to the uncured and cured resin. We solved the heat equation by sampling the volume of the material, we took into account on the thermal contact of the material with the walls of the electrodes and we described the rate of cure with a parametric equation which introduced a single activation energy de eu (@- a)83 (100 - 0) exp -$$ The measured instantaneous absorbed power was distributed in the volume of the material by supposing that the complex permittivity of the material followed the Looyenga mixture law. ‘This interpretation gave a first determination of the thermal, kinetic, and dielectric parameters. ‘Then, the dependences of the imaginary part of the complex permittivity (when a = 0 and 1), on the temperature and on the degree of cure, are redetermined by fitting Pa(t) values with the obtained a(t) values. Finally, all experimental data are fitted again, so that the model ‘reproduced satisfactorily all the experimental results. Teo) Teo) 200 {— 200 4 150 2 10 100} rma, 100} sol Bs °° 200400 ~«g00 =O ~=«DOO Ks) 100 fh ] Ta! EE al 200400 ~~S~CwOSCHSC«CO KS) Teo), 200 es ‘s0| 100 Ps rT) eo : * oo ‘he A fi cm “ Pel of ee a eT TO ee rT TO) Figure 4 : Typical temperature deviation between the experimental and the calculed values. Conclusion By interpretating carefully the experimental responses (temperature and absorbed power) obtained by on-off step electric field, it was possible to model the HF assisted curing process. The model is robust. Although the chemical reaction should be complex, the curing reaction is described by a single activation energy value. 45ISOTHERMAL DRYING OF POROUS CERAMIC MICROSPHERES IN A MICROWAVE FLUIDISED BED G.D. SIZGEK AND E. SIZGEK ‘The authors are affiliated with Australian Nuclear Science and Technology Organisation PMB 1, Menai, NSW, 2234 A. ABSTRACT Drying characteristics of both water and salt solution impregnated ceramic microspheres in a pilot-scale, batch fluidised bed drier combined with microwave energy was studied under isothermal conditions. Drying curves were represented by ‘an empirical mass transfer model. The model tested with the experimental data shows good agreement and enables predictions to be made with respect to the microwave power requirements for selected drying rates. INTRODUCTION This study corresponds to first phase of the development of a suitable technology for impregnation and drying of the ‘ceramic microspheres. Preliminary, small scale experiments (Sizgek, 1997) in a variable power microwave oven revealed that microwave drying of salt solution (a mixture of nitrate salts) impregnated microspheres produced a homogenous distribution of the salt species and drying rates were nearly ten times quicker compared to the convection drying. In the present study impregnation and isothermal drying of the ceramic precursor powders were conducted in a custom designed and made microwave-heated fluidised bed system on 10-kg scale. The aim of this study was to simulate isothermal batch drying curves of microspheres by means of empirical equation to represent the influence of certain process variables effecting moisture transfer. EXPERIMENTAL ‘The fluidisation chamber was made of cylindrical borosilicate glass (300 mm in diameter) to allow microwave radiation to penetrate through the chamber wall into the precursor powder. The use of a glass fluidisation chamber also ‘enabled visual inspection of the fluidised bed during processing. The glass chamber was contained in a rectangular microwave cavity, which was manufactured from aluminium frame and mild steel perforated plates. A stainless-steel porous plate with a pore size of 10 micron was placed at the bottom of the glass chamber for fluidisation gas distribution Six thermocouples were attached to distributor plate to measure the powder bed temperature during processing. The ‘upper ends of the thermocouple shields were weld-sealed to protect the tips of the thermocouples from microwave field to prevent arcing. A stainless steel disengagement section was fitted with a candle type porous stainless steel metal filter assembly with a pore size of 20 micron to prevent particle carry over. The inlet temperature of the entering fluidisation gas was measured with a thermocouple placed in the gas line just before the entry port. The humidity and the temperature of the outlet gas/vapour stream were measured by a humidity sensor and transmitter system. Differential pressure through the bed was measured by means of a pressure sensor. A volumetric flow meter was used for measuring the flow rate of the fluidising gas. A microwave power source with a variable power generator providing continuous adjustment from 0 to 6 kW power at 2.45 GHz was used (Figure 1). A three-stub tuner has been utilised for matching the microwave generator to the load within the fluidised bed to maximise the energy to be absorbed by the powder bed. Isothermal drying experiments of wet microspheres were conducted at various powder bed temperatures, fluidising gas velocity and initial moisture contents. The moisture content of wet powder was defined by the ratio of the mass of ‘moisture to the mass of dry solid, For salt solution impregnated powders the increasing mass of dry powder, due to salt accumulation during drying, was taken into account in the moisture content calculations. The powder was fluidised with entering gas stream at ambient temperature and with a relative humidity of 0%. In these experiments the gas stream was not used as a heat source for liquid evaporation, Dielectric heating provided the evaporative energy. The main duty of the gas stream was to prevent condensation, carry away moisture and fluidise powder. In all experiments start-up microwave power level was $ kW. As soon as the powder bed reached to the desired operation temperature, variable energy input 46‘was applied by step-down reduction of microwave power level to maintain the bed at a given isothermal condition. During drying it was possible to achieve control over the bed temperature within the + 0.5 °C of the desired operation temperature, The temperature, the pressure drop and the change of moisture content of the bed were continuously monitored and recorded. Magnetron Circulator Three stub tuner Waye guide 1 1 S E Eaupely FORWARD and REFLECTED Water load IN OUT power sensor cavity eS oo lo] Glass section oo Forward Reflected Power supply system u Power meter Figure 1 Schematic illustration of the microwave generation and delivery system DRYING RATE EQUATION An attempt has been made to describe the moisture transfer within the microspheres using an empirical equation. The following equation (Strumillo and Kudra, 1986) was found to be the best fitted to the experimental data, eee Dene exp(-kt”") a where X is the material moisture content, X, is the equilibrium moisture content, k and n are the model parameters. The moisture ratio (#) is dependent and the time (t) is independent variables. The aim of the fiting procedure isto find those values of the parameters which best describe the data, The standard way of defining best fit is to choose the parameters so thatthe sum of squares ofthe deviations of the theoretical curve ffom the experimental points i at its minimum. In the case of one independent and one dependent variable the mean standard deviation, 77, can be expressed as: 2 Eu, (0, — £6 skin @ ‘where N is the number of degrees of freedom, and iis the number of observation. The quantities w, represent the weights of each experimental point. In order to estimate the best model parameters, the non-linear method of Levenberg- Marquard (Seber and Wild, 1989) was utilised. Fitting results showed that n value did not change significantly and the common value was found to be 1.65. The mean standard deviation for each individual experiment ranged from 2x10° to 1.2x10°. The influence of process variables can be represented by expressing parameter k in terms of those variables. ur analysis showed that parameter k was related to the microwave intensity (P, kW/kg moisture), the velocity of the fluidising gas (F, m/s), and the initial moisture content (Xo, kg moisture/kg dry powder). The effect of salt solution was 47also incorporated in to the model in terms of weight percentage of oxide equivalent of salt species (H, wt %) in the final product. Microwave intensity was calculated from total cumulative energy consumption for each run to keep bed at a required temperature, For the experiments the most relevant expression for the correlation sought, was found to be in the following form: K=C,+C, PHC QF +C, Xp+ CH 8 In this expression, the empitical coefficients C,, C,, C2, Cs and C, were estimated by fitting the variables with k values using multiple regression analysis. The final empirical equation which best fits the data is $= exp{-[-1.8 10% +3.94 10° P-8.1 107 F +14 10 Xp -1.20107H] t'} @ RESULTS AND DISCUSSIONS ‘The effect of bed temperature, fluidising gas velocity, initial moisture content and presence of salts on the drying kinetics ‘of microspheres was examined. The empirical model under consideration was applied to experimental data. Predicted values of moisture ratio were found to fit o the experimental data reasonably well. The drying results compared with the predicted curves are given below The drying curves for various gas velocities are given in Figure 2 at a constant bed temperature of 70 °C and initial moisture content of 0.15. It was observed that by inereasing gas velocity from 0.034 to 0.04 m/s (~18% increase) reduced the drying time about 20%. This inerease in drying rates is due to slight enhancement in mass transfer at the evaporating surface. However, further increase in gas velocity to 0.057 nvs did not practically change the total drying time. In fact the fluidising gas entering at ambient temperature cools the material so that some of the absorbed electromagnetic energy is consumed to heat the gas. Increase in total microwave energy consumption to maintain the bed at a given temperature with increasing gas velocity confirmed this point. Figure 3 shows drying curves of microspheres for constant bed temperatures of 60, 70 and 80 °C, which correspond to microwave intensity of 0.75, 1.45 and 2.04 kW/kg moisture, respectively. For a given gas velocity and initial moisture content, it is evident that higher bed temperatures would lead to higher moisture diffusivity and higher convective mass transfer driving force atthe surface ofthe particles resulting in faster drying, An inrease in temperature from 60 to 70°C decreased the drying time almost 45%. Further 10 °C increase to 80 "C resulted in additional 12% faster drying. However, the total microwave energy consumption for the various bed temperatures was found to be practically the same, 10 Mj, for the given gas velocity and initial moisture content. The results suggest that for the same level of energy ‘consumption it is possible to achieve faster drying operation by using higher microwave intensity. In Figure 4 at a given constant bed temperature and gas velocity, drying time increased with increasing initial moisture content. However, an increase in the average drying rate (kg moisture per second) was observed with increasing initial moisture content for the range investigated in this study. For example, increasing the intial moisture from 0.093 to (0.20 increased the average drying rate about 30%. Total microwave energy consumption to maintain the bed at a given temperature also increased with increasing initial moisture content of the microspheres. But the average consumed ‘microwave energy per kilogram of water decreased, suggesting that the microwave energy is more efficiently absorbed at higher moisture levels. Figure 5 illustrates drying rate curves for salt solution impregnated microspheres for successive salt solution impregnation steps (3.0 wt % to 9 wt % oxide equivalent of salt species). The amount of salt solution impregnated for ‘each consecutive step was kept the same. For comparison, drying curve of water impregnated microspheres was also shown for the same initial moisture content. As can be seen from Figure 5, for a given temperature and initial moisture content, drying time for water impregnated sample is shorter than salt impregnated samples and drying gets slower as the salt accumulation increases for each consecutive step. During drying of salt-impregnated microspheres, blockage of micropores occurs by crystallised nitrate salts. The mean pore size increases with increasing salt loading, while the surface area and the pore volume decreases (Sizgek, 1997). The decrease in drying in the presence of salts is mainly due to decrease in effective diffusivity as a result of change in structural properties of salt solution impregnated ‘microspheres, 48os + exorinectl 09 + experinnit _ 08 me oo ste gor gor bos bos 208 205 eos fos bos eos 02 02 Ret ae 92 : 3 f = oa A000 oon oan 4000” 00000 0000 Tine Tie Figure 2 Drying curves as function of gas velocity Figure 3 Drying curves as function of fluid bed temperature Fe0ctme + expermenat {4 moisture ratio 0 2000 4000 6000 Time (e) ° 2000 ‘4000 000 Tims (s) Figure 4 Drying curves as function of initial moisture Figure 5 Drying curves as function of salt loading content CONCLUSIONS Drying kinetics of porous ceramic microspheres have been represented with an empisical model that comprises influence of process variables. The empirical model tested with the experiments describes the results with a reasonable accuracy. It enables predictions to be made with respect to the microwave power requirements for selected drying rates. Microwave intensity mainly controls the process. For the conditions studied, the fluidising gas velocity does not show any appreciable effect on the total drying time. Increase in the initial moisture content influences the drying rate in a positive way. This is attributed to more efficient absorption of microwaves with increasing moisture loading up to a certain level at which the maximum matching between the load and the microwave field obtained. On the other hand the presence of salts slows down the drying rate, REFERENCES Seber, G. A. F.and Wild, C.1., 1989, Non-linear Regression, John Wiley & Sons, NY. Sizgek, G. D. and Sizgck, E., 1997, Microwave drying characteristics of impregnated Synroc ceramic microspheres, J. Microwave Power, 32(3), 171-179, Strumillo, C. and Kudra, T., 1986, Drying: Principles, Applications and Design, Gordon and Breach Science Publishers. 49REGENERATION OF A DIESEL ENGINE PARTICULATE FILTER USING MICROWAVE HEATING GENE A. DANKO, RICHARD SILBERGLITT*, A. CARL McDONALD** AND THOMAS M. YONUSHONIS** 4FM Technologies, Inc., 10529-B Braddock Road, Fairfax, VA 22032-2236 **Cummins Engine Company, Inc., 1900 McKinley Avenue, Columbus, IN 47202-3005 ABSTRACT. A ceramic wall-flow particulate filter contained in a stainless steel canister and surrounded with intumescent insulation was installed in the exhaust stream of a diesel engine and loaded with particulate emissions in an cngine test cell at the Cummins Engine Company Technical Center. The particulate-loaded canned filter was installed in atest stand at FM Technologies’ laboratory and heated with a custom-designed microwave system to 600°C in approximately 10-minutes. An exotherm was observed and visual inspection ofthe (take-apart) filter after heating verified regeneration (ie., removal of the soot). Additional heatings of the canned filter gave sigmoidal heating curves without exotherms, typical of clean filters. INTRODUCTION Since 1988, the amount of particulate matter (PM) emitted by diese! engines has decreased dramatically, from a level of 0.60 g/Bhp-hr (grams per brake horsepower-hour) to 0.1 g/Bhp-hr, a level in compliance with 1994 EPA requirements. The reduced level was reached using a combination of approaches, including: advanced fue! injection systems, combustion and air handling technology and exhaust aftertreatment methods such as catalysts. Reductions in the allowed level of nitrogen oxides (NO) have also been legislated at the same time as the PM emissions reductions, ‘hich has limited the flexibility of diesel engine manufacturers to respond with in-cylinder technologies, since PM and NO, levels typically move in opposite directions when combustion conditions are varied. Recently, work on aftertreatment technologies has accelerated as a result of projected further reductions in both PM and NO, emissions requirements, such as the 2002 EPA NO, reduction from 6 to 2 g/Bhp-hr and the proposed (2005) Euro IV reduction of PM to0.015 g/Bhp-hr. This paper describes results of recent work to reduce PM emissions through the use of a ceramic fibrous filter to collect the PM and microwave heating to combust the collected PM, and thus “regenerate” the filter for continued use ‘THE MICROWAVE REGENERATED PARTICULATE FILTER The filter used in this work [Cummins Engine Company, 1995] is a ceramic wall-low filter constructed of an alumina-based paper that is corrugated or pleated and then spiral wound into a cylinder approximately 6” in diameter and 6” Jong with channels running along the exhaust flow path. The opposite ends of neighboring channels are sealed 0 that the exhaust flow must pass through at least one wall between channels before exiting the filter. PM is thus collected in the filter walls. In order to enable the use of microwave enerey for regeneration, the filter materia is coated with SiC, which is applied using a chemical vapor infiltration process. ‘The filter is then wrapped with an {ntumescent insulation, and sealed into a stainless steel can which is installed in the exhaust system of a diesel engine. Microwave heating for regeneration of the filter is accomplished through a proprietary feed system that is connected to the stainless steel can containing the filter. LOADING OF THE PARTICULATE FILTER ‘The canned particulate filter was installed in a test cell at the Cummins Technical Center behind a 1994 215 hp B 45.9 liter diesel engine. Particulate lading was accomplished using the Federal Test Procedure (FTP) Transient Cycle. ‘The FIP Transient Cycle simulates driving heavy duty vehicles (Gross Vehicle Weight Rating > 8500 Ibs) in urban American cities and is used to determine emission levels. The cycle lasts 1200 seconds and is repeated with the engine warm, Once loaded, the canned filter was sent to FM Technologies to evaluate the microwave regeneration system. 50REGENERATION OF THE LOADED PARTICULATE FILTER ‘The loaded canned particulate filter was connected to a microwave heating system operating at 2.45 GHz. Microwaves were transported to the can containing the filter from wave launcher via WR284 waveguide, Reflected ‘power was minimized via three-stub tuner, and microwave components isolated from the exhaust gases via ceramic window. The temperature of the filter during heating was measured using a shiclded Type K thermocouple that was inserted axially into a filter channel. The temperature vs. time profile during filter heating, as well as reflected power and magnetron temperature, were digitally recorded. During the initial heating cycle, the filter was heated to regeneration temperature (600°C) in approximately 10 minutes, Moreover, the heating curve displayed a peak suggestive of the carbon exotherm anticipated during regeneration of a soot-laden filter. Following this intial heating, the filter was heated many times and the peaked temperature profile was never again observed. lll subsequent hheatings produced the sigmoidal curve that has been typical of heating for unloaded filters (McDonald etal, 1997}, providing further support for the conclusion that this filter was successfully regenerated, The axial temperature gradient in the filter was examined during the additional heatings, and it was found that the peak temperature ranged from approximately 790°C near the inlet end of the filter to approximately 650°C near the outlet end of the filter. During the experiments, there was a positive air flow from an air filtration system hood just above the outlet, which may have accounted for some of the cooling at the outlet end. Figure 1 shows the initial heating curve, and a typical subsequent heating curve obtained for this canned filter. Before and after microwave heating, the can containing the loaded particulate filter was disassembled and the fitter ‘was photographed, Figures 2 and 3 are photographis taken before and after the initial heating, respectively. They indicate that a significant amount of soot was removed from the filter during the initial heating. Note that the insulation on the outside of the filter and the inner core (which was not coated with SiC) were not heated and thus the soot remains in those places 1200 1000 - g 3 Initial Heating o@ 8004 ca § 6004 § Typical Subsequent Heating e 400 4 ie 200 5 cepa I screen see negro eee coer epee EET 0 10 20 30 40 50 60 70 Time, minutes Figure 1, Microwave heating profiles for loaded particulate filter 51Figure 3. Loaded particulate filter after microwave heating REFERENCES ‘The Cummins Engine Company, Inc., “Microwave Regenerated Particulate Trap for Diesel Engines,” California Energy Commission Consultant Report, Contract 500-92-047 (1995). ‘A.C. McDonald, Jr., T. M. Yonushonis, W. C. Haberkamp, F. Mako, L. K. Len, R. Silberglitt and 1. Ahmad, “Microwave Regenerated Particulate Trap,” Proceedings of the 1997 Diesel Engine Emissions Reduction Workshop, ULS. Department of Energy Office of Transportation Technologies Report No. CONF - 970799 (1997). 52WELDING PVDF-PIPES WITH MICROWAVES RUDOLF EMMERICH*, MICHAEL JAUSS*, VOLKER BRAUTIGAM** AND PETER ELSNER* Fraunhofer Institute Chemical Technology, Joseph-von-Fraunhofer-Str.7, D-76317 Pfinztal, Germany **Institute for Polymer Testing and Science, University of Stuttgart, P.O.Box 801140, D-70S11 Statwgart, Germany ABSTRACT ‘A new welding process using microwaves to heat up PVDF-pipes is presented. The main part of the welding machine is a microwave applicator, which consists of a non-rediating antenna system. High clectrical field strength which. occurs near the antennas is used to melt the joining zones of the pipes. When these zones are molten the pipes are Durt-welded INTRODUCTION Polyvinylidenfluoride (PVDF) is a highly polar polymer. It has high mechanical strength and good chemical resistance. Therefore this polymer is used in chemical applications for example for pipe systems in the semicomudetor industry. The pipes are welded with heated tool or with infrared joining machines. In case of the heated tool welding the joining zones of the pipes are in contact with the heated tool. The infrared-welding is a contactless process. The Joining zones of the pipes are fixed close in front of an infrared radiator. The convection of heat near the joining zones of pipes lead to an inhomogenous temperature distribution in this zone. The energy consumption ofthis process is very high. For both processes itis necessary to preheat the heated tool or the infrared radiator which result in long processing times and retooling times. The heated tool and the infrared radiator is not thermally isolated, so heat losses occur. A new contactless welding process is developed to overcome the disadvantages of the conventional processes. This new process uses microwaves of a frequency 2.45 GHz to heat the joining zones. MICROWAVE WELDING MACHINE ‘The experimental set-up of the microwave welding machine is shown in Fig. 1. The machine consists of microwave generator, 2 magnetron, a microwave applicator and a fixing device for the pipes. The maximum power of the rmagnetrons ate 1.2 KW. The microwave applicator and the fixing device is shown in detail in Fig. 2. The fixing device is taken from a standard heated tool welding machine. The joining zone of the two pipes are put in the microwave applicator. When the joining zone of the pipes are molten the microwave applicator is removed and the pipes arc butt- welded, ‘The main part of the microwave welding machine is the microwave applicator (1,2). In Fig. 3 is shown a schematic

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