Materiais híbridos, como poliedros oligoméricos silsesquioxanos (POSS), têm recebido especial atenção nos últimos anos pois são materiais que possuem uma combinação sinérgica de propriedades de materiais orgânicos e inorgânicos. Sua preparação necessita de elevados tempos de síntese e o uso de aquecimento dielétrico se apresenta promissor. Entretanto, reatores comerciais são caros e uma alternativa passa a ser a adaptação de fornos de uso domésticos. Neste contexto, este trabalho busca adaptar um forno de micro-ondas doméstico para a síntese de POSS, comparando materiais obtidos via aquecimento por microondas e convencional (banho em óleo). O POSS foi sintetizado através da condensação hidrolítica do viniltrietoxisilano (VTES) e da mistura VTES e tetraetil ortosilicato (TEOS). As amostras sintetizadas foram caracterizadas por FTIR, RMN de 1H, TGA, GPC, MEV, MET e DRX. O uso de micro-ondas possibilitou a obtenção de POSS com maior rendimento para os sistemas VTES e VTES/TEOS, apresentando taxas de reação respectivas de 47 e 59 vezes maior que a síntese convencional. Todas as amostras apresentaram bandas FTIR intensas em ~1090 e ~568 cm-1, ambas relacionadas a formação de gaiolas de silsesquixanos. Não foram observadas vibrações -O-CH2CH3 mostrando que a reação de hidrólise foi totalmente completa. A presença de deformações OH nas amostras VTES/TEOS indica a formação de estruturas não totalmente condensadas, confirmada pelos espectros de RMN de H1 onde é observada a presença de silanóis não condensados. Análises GPC para o POSS VTES apresentaram a maior fração (96,5%) de estruturas T8 via convencional, e (93,93%) via micro-ondas. A adição de TEOS reduziu a fração de estruturas T8 obtidas, (78,0%) via dielétrico e (33,0%) convencional. A análise TGA de todas as amostras mostraram uma única etapa de degradação, onde diferenças observadas no sistema VTES/TEOS são associadas ao tamanho da estrutura do POSS conforme a análise de GPC. Imagens de MEV mostraram a presença de estruturas cúbicas e esféricas em todas as amostras, e a adição de TEOS indicou uma tendência a redução de tamanho. Imagens por MET para o POSS VTES mostrou morfologia similar as observadas por MEV, e para VTES/TEOS, a presença de aglomerados esféricos regulares nanométricos. O DRX para o POSS VTES micro-ondas, convencional e VTES/TEOS micro-ondas, indicou a presença de uma rede cristalina de estrutura romboédrica, típica de POSS T8. O POSS VTES/TEOS via convencional apresentou um padrão de DRX de uma amostra amorfa. As nanopartículas híbridas de POSS VTES, via aquecimento convencional e dielétrico em refluxo, mostrou possuírem características químicas muito semelhantes, confirmadas pelas técnicas de análise realizadas. Entretanto, a mesma comparação entre o POSS obtido via mistura VTES/TEOS, a mesma semelhança não é observada. Isto se deve ao precursor VTES ser trifuncional e ao TEOS ser tetrafuncional, ou seja, possuem momentos dipolares diferentes, induzindo estruturas irregulares orientadas aleatoriamente e de diferentes tamanhos, principalmente no aquecimento convencional, onde a reação apresentada é mais lenta. / Submitted by Ana Guimarães Pereira (agpereir@ucs.br) on 2015-09-14T18:28:06Z No. of bitstreams: 1 Dissertacao Igor Luiz Penso.pdf: 3673859 bytes, checksum: f0f80b6c32267df60b2b04fa4df6d307 (MD5) / Made available in DSpace on 2015-09-14T18:28:06Z (GMT). No. of bitstreams: 1 Dissertacao Igor Luiz Penso.pdf: 3673859 bytes, checksum: f0f80b6c32267df60b2b04fa4df6d307 (MD5) / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior. / Hybrid materials, such as polyhedral oligomeric silsesquioxanes (POSS), nowadays have received special attention because they are materials that have a synergistic combination of organic and inorganic materials properties. Their preparation requires high time of synthesis and the use of dielectric heating appears promising. However, commercial reactors are expensive and the adaptation of domestic microwave ovens becomes an alternative. In this context, this work aims to adapt a domestic microwave oven for the synthesis of POSS, comparing materials obtained by microwave and conventional (oil bath) heating. The POSS was synthesized by the hydrolytic condensation of vinyltriethoxysilane (VTES) and tetraethyl orthosilicate (TEOS) in different proportions. The synthesized samples were characterized by FTIR, 1H-NMR, TGA, GPC, SEM, TEM and XRD. The use of microwaves enable the manufacture of POSS with increased yield for VTES and VTES/TEOS systems, respectively with rates of 47 to 59 times higher than conventional synthesis. All samples showed intense FTIR bands at ~ 1090 and ~ 568 cm-1, both related to formation of silsesquioxane cages. It was not observed -O-CH2CH3 vibrations showing the hydrolysis reaction has been fully completed. The presence of OH deformations in the VTES/TEOS samples indicate the formation of non-fully condensed structures, confirmed by 1H NMR spectra, where it is observed the presence of non-condensing silanol. GPC analysis for the POSS VTES exhibited a major fraction (96.5%) of T8 structures via conventional, and (93.9%) via microwave synthesis. The addition of TEOS decreased the fraction of T8 structures, (78.0%) via dielectric and (33.0%) for conventional synthesis. TGA analysis of all samples showed a single stage of degradation, differences between VTES/TEOS samples are associated with the size of the POSS structure according to GPC analysis. SEM images showed the presence of spherical and cubic structures in all samples, and the addition of TEOS indicated a tendency to increase the size of these structures. TEM images for POSS VTES showed similar morphology to those observed by SEM. The presence of nanometric regular spherical agglomerates was observed in VTES/TEOS samples. The XRD for POSS VTES microwave, conventional and VTES/TEOS microwave synthesis, indicated the presence of rhombohedral lattice structure, typical POSS T8. The POSS VTES/TEOS conventional route showed a XRD pattern of an amorphous sample. The hybrid nanoparticles of POSS VTES, prepared via conventional and dielectric heating using reflux system, showed a very similar chemical properties as confirmed by the analytical techniques performed. However, the same comparison between the POSS obtained via mixing of VTES/TEOS, the same behavior is not observed. This is due to the VTES precursors be trifunctional and TEOS tetrafunctional, i.e. have different dipole moments, inducing randomly oriented irregular structures and different sizes, especially in the conventional heating where reaction is slower.

Materiais híbridos, como poliedros oligoméricos silsesquioxanos (POSS), têm recebido especial atenção nos últimos anos pois são materiais que possuem uma combinação sinérgica de propriedades de materiais orgânicos e inorgânicos. Sua preparação necessita de elevados tempos de síntese e o uso de aquecimento dielétrico se apresenta promissor. Entretanto, reatores comerciais são caros e uma alternativa passa a ser a adaptação de fornos de uso domésticos. Neste contexto, este trabalho busca adaptar um forno de micro-ondas doméstico para a síntese de POSS, comparando materiais obtidos via aquecimento por microondas e convencional (banho em óleo). O POSS foi sintetizado através da condensação hidrolítica do viniltrietoxisilano (VTES) e da mistura VTES e tetraetil ortosilicato (TEOS). As amostras sintetizadas foram caracterizadas por FTIR, RMN de 1H, TGA, GPC, MEV, MET e DRX. O uso de micro-ondas possibilitou a obtenção de POSS com maior rendimento para os sistemas VTES e VTES/TEOS, apresentando taxas de reação respectivas de 47 e 59 vezes maior que a síntese convencional. Todas as amostras apresentaram bandas FTIR intensas em ~1090 e ~568 cm-1, ambas relacionadas a formação de gaiolas de silsesquixanos. Não foram observadas vibrações -O-CH2CH3 mostrando que a reação de hidrólise foi totalmente completa. A presença de deformações OH nas amostras VTES/TEOS indica a formação de estruturas não totalmente condensadas, confirmada pelos espectros de RMN de H1 onde é observada a presença de silanóis não condensados. Análises GPC para o POSS VTES apresentaram a maior fração (96,5%) de estruturas T8 via convencional, e (93,93%) via micro-ondas. A adição de TEOS reduziu a fração de estruturas T8 obtidas, (78,0%) via dielétrico e (33,0%) convencional. A análise TGA de todas as amostras mostraram uma única etapa de degradação, onde diferenças observadas no sistema VTES/TEOS são associadas ao tamanho da estrutura do POSS conforme a análise de GPC. Imagens de MEV mostraram a presença de estruturas cúbicas e esféricas em todas as amostras, e a adição de TEOS indicou uma tendência a redução de tamanho. Imagens por MET para o POSS VTES mostrou morfologia similar as observadas por MEV, e para VTES/TEOS, a presença de aglomerados esféricos regulares nanométricos. O DRX para o POSS VTES micro-ondas, convencional e VTES/TEOS micro-ondas, indicou a presença de uma rede cristalina de estrutura romboédrica, típica de POSS T8. O POSS VTES/TEOS via convencional apresentou um padrão de DRX de uma amostra amorfa. As nanopartículas híbridas de POSS VTES, via aquecimento convencional e dielétrico em refluxo, mostrou possuírem características químicas muito semelhantes, confirmadas pelas técnicas de análise realizadas. Entretanto, a mesma comparação entre o POSS obtido via mistura VTES/TEOS, a mesma semelhança não é observada. Isto se deve ao precursor VTES ser trifuncional e ao TEOS ser tetrafuncional, ou seja, possuem momentos dipolares diferentes, induzindo estruturas irregulares orientadas aleatoriamente e de diferentes tamanhos, principalmente no aquecimento convencional, onde a reação apresentada é mais lenta. / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior. / Hybrid materials, such as polyhedral oligomeric silsesquioxanes (POSS), nowadays have received special attention because they are materials that have a synergistic combination of organic and inorganic materials properties. Their preparation requires high time of synthesis and the use of dielectric heating appears promising. However, commercial reactors are expensive and the adaptation of domestic microwave ovens becomes an alternative. In this context, this work aims to adapt a domestic microwave oven for the synthesis of POSS, comparing materials obtained by microwave and conventional (oil bath) heating. The POSS was synthesized by the hydrolytic condensation of vinyltriethoxysilane (VTES) and tetraethyl orthosilicate (TEOS) in different proportions. The synthesized samples were characterized by FTIR, 1H-NMR, TGA, GPC, SEM, TEM and XRD. The use of microwaves enable the manufacture of POSS with increased yield for VTES and VTES/TEOS systems, respectively with rates of 47 to 59 times higher than conventional synthesis. All samples showed intense FTIR bands at ~ 1090 and ~ 568 cm-1, both related to formation of silsesquioxane cages. It was not observed -O-CH2CH3 vibrations showing the hydrolysis reaction has been fully completed. The presence of OH deformations in the VTES/TEOS samples indicate the formation of non-fully condensed structures, confirmed by 1H NMR spectra, where it is observed the presence of non-condensing silanol. GPC analysis for the POSS VTES exhibited a major fraction (96.5%) of T8 structures via conventional, and (93.9%) via microwave synthesis. The addition of TEOS decreased the fraction of T8 structures, (78.0%) via dielectric and (33.0%) for conventional synthesis. TGA analysis of all samples showed a single stage of degradation, differences between VTES/TEOS samples are associated with the size of the POSS structure according to GPC analysis. SEM images showed the presence of spherical and cubic structures in all samples, and the addition of TEOS indicated a tendency to increase the size of these structures. TEM images for POSS VTES showed similar morphology to those observed by SEM. The presence of nanometric regular spherical agglomerates was observed in VTES/TEOS samples. The XRD for POSS VTES microwave, conventional and VTES/TEOS microwave synthesis, indicated the presence of rhombohedral lattice structure, typical POSS T8. The POSS VTES/TEOS conventional route showed a XRD pattern of an amorphous sample. The hybrid nanoparticles of POSS VTES, prepared via conventional and dielectric heating using reflux system, showed a very similar chemical properties as confirmed by the analytical techniques performed. However, the same comparison between the POSS obtained via mixing of VTES/TEOS, the same behavior is not observed. This is due to the VTES precursors be trifunctional and TEOS tetrafunctional, i.e. have different dipole moments, inducing randomly oriented irregular structures and different sizes, especially in the conventional heating where reaction is slower.

A proliferation of choices available to consumers as they select a major cooking appliance necessitated the development of a Buyer’s Guide which will provide consumers with generic information by which they can compare range cooktops and microwave ovens. The microwave oven is included because it is often used in the place of a cooktop. The Buyer’s Guide for Range Cooktops and Microwave Ovens as an information resource is designed to be used by consumers to assist in making an informed purchase decision. The study was conducted in three phases: 1) identification of items included in the Buyer’s Guide; 2) establishment of test procedures; and 3) focus panel evaluation of the Buyer’s Guide. Phase 1 - Eleven items considered to be important in making purchase decisions were identified by members of the Virginia Retail Merchants Association and by Virginia home economics Extension agents. Items rated as important for inclusion were: purchase price, maintenance, life expectancy, operating costs, energy use, speed of heating, evenness of heating, heat retention, heat recovery, ease of cleaning, and ease of use. Phase 2 - Using standardized test procedures, data were obtained for the radiant coil electric smoothtop to allow the comparison of items found on the Buyer’s Guide with other types of range cooktops (conventional electric coil, gas burner, induction cooktop, smoothtop resistance coil, solid element) and the microwave oven. Phase 3 - Four focus panels were conducted to evaluate the Buyer’s Guide for Range Cooktops and Microwave Ovens for clarity of content, practicality of format, and its usefulness to consumers. The 26 focus panel participants recommended changes which were incorporated into the Buyer’s Guide for Cooktops and Microwave Ovens. They indicated a belief that the Buyer’s Guide would be useful for consumers seeking generic information by which to compare major cooking appliances. Further research is needed to evaluate the Buyer’s Guide for Range Cooktops and Microwave Ovens for its usefulness to consumers in the selection of a cooking appliance in the marketplace. / Ph. D.

The purpose of this study was to develop a framework for analysis and assessment of the cost of ownership and use of major cooking appliances. This involved an assessment of the monetary cost as well as the cost of human resources required to maintain and operate cooking systems. The goal was to provide information useful in making purchase decisions within a framework that can be used to organize information about cost beyond the initial purchase price. Five cooktops--conventional electric coil, induction, solid element with thermostatic control, solid element with thermal limiter, and gas--and a microwave oven were used to develop a decision-making matrix. Data were collected in the Virginia Polytechnic Institute and State University College of Human Resources household equipment laboratory. In addition, data were compiled from previous studies which included the same variables. One-way analysis of variance, Student-Newman-Keuls, and Tukey’s HDS techniques were used to analyze the data. Results were used to assign weights in the matrix used to develop a 10-point scale which represented the total cost of owning and using a cooking system in food preparation. The scale was then used to evaluate the appliances used in this study. Based on the matrix, the microwave oven received the highest score followed by gas, conventional electric coil, solid element with thermostatic control, solid element with thermal limiter, and induction cooktops. The cost of owning and using any of these appliances is not markedly different in terms of life expectancy, maintenance, energy, or cooking time. However, such factors as user interaction with the appliance, speed of heat-up, heat recover rate, retained heat, evenness of heating, cleaning time, and initial purchase price do vary and are likely to influence satisfaction with a cooking system. / Ph. D.

In recent years, advancements in the field of wireless communication have led to more innovative consumer products at reduced cost. Over the next 2 to 5 years, short-range wireless devices such as Bluetooth and Wireless Local Area Networks (WLANs) are expected to become widespread throughout hospital environments for various applications. Consequently the medical community views wireless applications as ineludible and necessary. However, currently there exist regulations on the use of wireless devices in hospitals, and with the ever increasing wireless personal applications, there will be more unconscious wireless devices entering and operating in hospitals. It is feared that these wireless devices may cause electromagnetic interference that could alter the operation of medical equipment and negatively impact patient care. Additionally, unintentional electromagnetic radiation from medical equipment may have a detrimental effect on the quality of service (QoS) of these short-range wireless devices. Unfortunately, little is known about the impact of these short-range wireless devices on medical equipment and in turn the interference caused to these wireless devices by the hospital environment. The objective of this research was to design and develop an automated software reconfigurable measurement system (PRISM) to characterize the electromagnetic environment (EME) in hospitals. The portable measurement system has the flexibility to characterize a wide range of non-contiguous frequency bands and can be monitored from a remote location via the internet. In this work electromagnetic interference (EMI) measurements in the 2.4 GHz ISM band were performed in two hospitals. These measurements are considered to be very first effort to analyze the 2.4 GHz ISM band in hospitals. Though the recorded EMI levels were well within the immunity level recommended by the FDA, it can be expected that Bluetooth devices will undergo a throughput reduction in the presence of major interferers such as WLANs and microwave ovens. A Bluetooth throughput simulator using semi-analytic results was developed as part of this work. PRISM and the Bluetooth simulator were used to predict the throughput for six Bluetooth Asynchronous Connectionless (ACL) transmissions as a function of piconet size and interferer distance. / Master of Science

This thesis investigates the interference potential of microwave ovens to Bluetooth data communication. Interference experiments are conducted in the CWT's Bluetooth lab, using CSR™ (Cambridge Silicone Radio) Bluetooth radios and a Tektronics™ Protocol Analyzer to record packet transmissions between the master and slave units. A novel, "quasi-real time" spectral measurement concept is developed to take radio frequency measurements. A LabView program enables a spectrum analyzer to download oven spectral data onto a computer via the instrument's serial port. From this data, three-dimensional plots of microwave radiated power levels versus ISM band frequencies over time periods are produced for different microwave ovens. These plots are compared with the results of interference experiments to explain Bluetooth packet errors. In addition to causing packet errors, emitted oven power levels at certain frequencies are sometimes strong enough to cause data packets to be lost (dropped) as they are transmitted over the air. This is a major problem since the Protocol Analyzer does not "see" these packets and cannot record the transmissions during an experiment. These lost packets can be accounted for if the frequency hopping scheme of the communicating Bluetooth devices is know prior to data transmission. Bluetooth's Frequency Hop Scheme is coded in Matlab for the purpose of predicting a data transmission's hopping sequence. The lost packets on each Bluetooth channel are counted by subtracting the Analyzer's recorded number of data transmissions per channel from the total number of transmissions per channel predicted by Matlab. A method is devised to calibrate the Bluetooth receiver and the spectrum analyzer is used to measure the received power level of Bluetooth signals on a particular frequency (channel). The number of packet errors on a channel is determined from the channel's C/I (carrier-to-interference ratio). If a channel's C/I level falls below the calculated C/I threshold at any instant of time due to oven operation, the packet transmitted at that instant is likely in error. A Matlab program estimates the number of packet errors per channel by counting the number of times the C/I of a channel falls below it's threshold value. The predicted number of packet errors is compared with the measured packet errors from experiments to yield extremely good results. Various oven-interference experiments are conducted in a small building, a large office environment and outdoors. For each experiment, the number of occurrences of transmitted data is plotted for each Bluetooth channel. Composite Excel bar graphs, created from this data, are compared with the oven spectral plots to describe an oven's effect on Bluetooth transmission. It is determined that different ovens cause packet errors on specifically different channels, in addition to channels 52-54 around the oven's 2450 MHz center operating frequency. The interference experiments suggest that placing an oven a radius of 10 m away from Class I (devices in a piconet will not affect data transmission). / Master of Science

Effects of container geometry and material on microwave cooking performance, as measured by evenness of cooking, firmness, and moisture content were compared. Three food items were heated in round, tube, loaf, and square containers made of clear glass, amber glass, thermoset polyester, and polysulfone. Unflavored gelatin, custard, and cakes were prepared three times in each of the 13 microwave containers. Evenness of cooking was determined by comparing meltdown and temperature in gelatin, temperature and separation/uncooked portions in custard, and index to volume in cakes. Firmness was measured in custard while moisture content was determined in cakes. In analysis of the data, ANOVA and Duncan's multiple range test were performed. Significant differences were found between shapes as food items heated more evenly in tube and round containers than in square containers. Food quality was affected more by shape than by material. Foods prepared in the, plastic materials were more evenly heated than in the glass materials. Statistically, shape and material interacted with each other for three measures of microwave appliance performance temperatures and separation/uncooked portions of custards, and index to volume in cakes. The interaction of shape and material was greater as the heating time increased. / Master of Science

As the demand for microprocessors is increasing with more and more consumers using integrated circuits in their daily life, the demand on the industry is increasing to ramp up production. In order to speed up the manufacturing processes, new and novel approaches are trying to change certain aspects of it. Microwaves have been tried as an alternative to conventional ovens in the curing of the polymers used as underfills and encapsulants in integrated circuits packages. Microwaves however being electromagnetic waves have non uniform energy distribution in different settings, causing burning or incomplete cure of polymers. In this study, we compare the two main types of microwaves proposed to perform the task of curing the polymers. To limit the study and obtain comparable results, both microwaves were limited to propagate in a single mode, TE10. The first is a closed microwave cavity using air as the propagation medium, and the second is an open microwave oven with a PTFE cavity that uses an evanescent field to provide energy. The open air cavity was studied with different orientations of a substrate placed inside it so as to find the best case scenario in the curing process. This scenario was then compared with the best case scenario found for a sample cured in an evanescent field. This comparison yielded results showing an advantage of the open microwave in maximum field present, thus leading to higher localized energy absorption and temperatures in the substrate, however this case also lead to a higher temperature gradient. The substrate cured in the closed microwave has a lower temperature gradient, but also a lower maximum field which leads to slower cure. In the TE10 mode therefore, a closed microwave has an overall advantage as the heating process is only slightly slower than that of an open cavity, but the temperature gradient in this case is significantly lower.

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Made available in DSpace on 2014-10-09T12:50:56Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:58:30Z (GMT). No. of bitstreams: 1 11106.pdf: 6970470 bytes, checksum: 75dd1652faa57785066487ced8605c9d (MD5) / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP