Thermal conductivity is an important thermophysical property needed for effectively predicting fuel performance. As part of the Next Generation Nuclear Plant (NGNP) program, the thermal conductivity of tri-isotropic (TRISO) fuel needs to be measured over a temperature range characteristic of its usage. The composite nature of TRISO fuel requires that measurement be performed over the entire length of the compact in a non-destructive manner. No existing measurement system is capable of performing such a measurement. A measurement system has been designed based on the steady-state, guarded-comparative-longitudinal heat flow technique. The system as currently designed is capable of measuring cylindrical samples with diameters ~12.3-mm (~0.5″) with lengths ~25-mm (~1″). The system is currently operable in a temperature range of 400 K to 1100 K for materials with thermal conductivities on the order of 10 W/m/K to 70 W/m/K. The system has been designed, built, and tested. An uncertainty analysis for the determinate errors of the system has been performed finding a result of 5.5%. Finite element modeling of the system measurement method has also been accomplished demonstrating optimal design, operating conditions, and associated bias error. Measurements have been performed on three calibration/validation materials: SS304, 99.95% pure iron, and inconel 625. In addition, NGNP graphite with ZrO2 particles and NGNP AGR-2 graphite matrix only, both in compact form, have been measured. Results from the SS304 sample show agreement of better than 3% for a 300–600°C temperature range. For iron between 100–600°C, the difference with published values is < 8% for all temperatures. The maximum difference from published data for inconel 625 is 5.8%, near 600°C. Both NGNP samples were measured from 100–800°C. All results are presented and discussed. Finally, a discussion of ongoing work is included as well as a brief discussion of implementation under other operating conditions, including higher temperatures and adaptation for use in a glovebox or hot cell.

Thermal conductivity is an important thermophysical property needed for effectively predicting nuclear fuel performance. As part of the Next Generation Nuclear Plant (NGNP) program, the thermal conductivity of tri-isotropic (TRISO) fuel needs to be measured over a temperature range characteristic of its usage. The composite nature of TRISO fuel requires that measurement be performed over the entire length of the compact in a non-destructive manner. No existing measurement system is capable of performing such a measurement. A measurement system has been designed based on the steady-state, guarded comparative-longitudinal heat flow technique. The system is capable of measuring cylindrical samples with diameters ∼12.3 mm (∼0.5 in.) with lengths ∼25 mm (∼1 in.). The system is currently operable in a temperature range of 100-700°C for materials with thermal conductivities on the order of 10-70 W*m-1*K-1. The system has been designed, built, and tested. An uncertainty analysis for the determinate errors of the system has been performed finding a result of 6%. Measurements have been performed on three calibration/validation materials: a certified glass ceramic reference material, 99.95% pure iron, and Inconel 625. The deviation of the validation samples is < 6-8% from the literature values. In addition, surrogate NGNP compacts and NGNP graphite matrix-only compacts have been measured. The results give an estimation of the thermal conductivity values that can be expected. All the results are presented and discussed. A Finite Element Analysis was done to compare the accuracy of multiple effective conductivity models. The study investigated the effects of packing structure, packing fraction, matrix thermal conductivity, and particle heat generation. The results show that the Maxwell and the Chiew & Glandt models provide the most accurate prediction of the effective thermal conductivity of the TRISO fuel compacts. Finally, a discussion of ongoing work is included as well as the possibility of correlating effective thermal properties of fuel compacts to their constituents with measurements of well-defined samples.

Temperature rise due to Joule heating of on-chip interconnects can severely affect performance and reliability of next generation microprocessors. Thermal predictions become difficult due to large number of features, and the impact of electron size effects on electrical and thermal transport. It is thus necessary to develop efficient numerical approaches, and accurate metal and dielectric thermal characterization techniques. In this research, analytical, numerical, and experimental techniques were developed to enable accurate and efficient predictions of interconnect temperature rise. A finite element based compact thermal model was developed to obtain temperature rise with fewer elements and acceptable accuracy. Temperature drop across the interconnect cross-section was ignored. The compact model performed better than standard finite element model in two and three-dimensional case studies, and the predictions for a real world structure agreed closely with experimentally measured temperature rise. A numerical solution was developed for electron transport based on the Boltzmann Transport Equation (BTE). This deterministic technique, based on the path integral solution of BTE within the relaxation time approximation, free electron model, and linear response, was applied to a constriction in a finite size thin metallic film. A correlation for effective conductance was obtained for different constriction sizes. The Atomic Force Microscope (AFM) based Scanning Joule Expansion Microscopy (SJEM) was used to develop a new technique to measure thermal conductivity of thin metallic films in the size effect regime. This technique does not require suspended metal structures, and thus preserves the original electron interface scattering characteristics. The thermal conductivities of 43 nm and 131 nm gold films were extracted to be 82 W/mK and 162 W/mK respectively. These measurements were close to Wiedemann-Franz Law predictions and are significantly smaller than the bulk value of 318 W/mK due to electron size effects. The technique can potentially be applied to interconnects in the sub-100 nm regime. A semi-analytical solution for the 3-omega method was derived to account for thermal conduction within the metallic heater. It is shown that significant errors can result when the previous solution is applied for anisotropic thermal conductivity measurements.

Este trabalho apresenta uma revisão de técnicas para medir propriedades térmicas de lmes, seguida de enfoque na termo-re etância transiente (TTR). Dentre as tecnologias existentes para medir propriedades térmicas, métodos ópticos são preferidos devido à sua natureza não-destrutiva, potencial de alta resolução temporal e espacial e calibração independente de contato físico. A implementação experimental deste método é apresentada, assim como a teoria da linha de transmissão utilizada para tratamento por Transformada de Laplace da equação de Fourier unidimensional do calor. Para facilitar o cálculo de invers ão desta Transformada, uma aproximação numérica, empregando o método Stehfest, foi usada. Experimentalmente, a evolução temporal da temperatura normalizada é mostrada para um lme de Au sobre Si e para lmes de Cu sobre substratos de vidro e Si, assim como foram utilizadas técnicas complementares de caracterização dos lmes (per lometria, elipsometria, microscopia de força atômica, eletrônica de varredura e de transmissão). Para o filme de ouro com espessura de 4:6µm, a teoria apresenta boa concordância com os resultados experimentais, já que o valor encontrado para a condutividade térmica do ouro está entre 230W/m.K e 280W/m.K, próximo e abaixo do valor da condutividade térmica do Au em volume (318W/m.K), indicando a validade do método implementado. Para lmes de cobre, porém, os resultados iniciais não apresentam a mesma concordância, e possíveis causas são discutidas. Futuramente, a TTR implementada poderá ser utilizada para determinação da condutividade térmica de lmes nos dielétricos ou semicondutores, e possivelmente na caracterização da componente transversal em filmes anisotrópicos. / This work presents a review of techniques to measure thermal properties off films, followed by a focused attention to the transient termo-re ectance (TTR). Amongst the existing technologies to measure thermal properties, optical methods are preferred due their nondestructive nature, high potential of spacial and temporal resolution, and independence from physical contact. The experimental implementation of this method is presented, as well as the theory of the transmission line theory used in the Laplace Transform treatment of the Fourier one-dimensional heat conduction equation. To facilitate the calculation of the Transform inversion, a numerical method, using the Stehfest method, was used. Experimentally, evolution of the normalized temperature is shown for a lm of Au on Si and for films of Cu on glass and Si substrates, whereas complementary techniques were used for film characterization (pro lometry, ellipsometry, atomic force microscopy, scanning and transmission eletron microscopy). For the Au film 4:6µm thick, the theory presents good agreement with the experimental results, and the value found for the thermal conductivity of the gold film is between 230W/m.K and 280W/m.K, near and below the bulk Au thermal conductivity (318W/m.K), indicating the validity of the method implementation. For Cu films, however, the initial results do not present the same agreement, and possible causes are discussed. In the future, the implemented TTR could be used for determination of the thermal conductivity of dielectric or semicondutors thin films, and possibly in the characterization of the transversal component in anisotropic films.

Este trabalho apresenta uma revisão de técnicas para medir propriedades térmicas de lmes, seguida de enfoque na termo-re etância transiente (TTR). Dentre as tecnologias existentes para medir propriedades térmicas, métodos ópticos são preferidos devido à sua natureza não-destrutiva, potencial de alta resolução temporal e espacial e calibração independente de contato físico. A implementação experimental deste método é apresentada, assim como a teoria da linha de transmissão utilizada para tratamento por Transformada de Laplace da equação de Fourier unidimensional do calor. Para facilitar o cálculo de invers ão desta Transformada, uma aproximação numérica, empregando o método Stehfest, foi usada. Experimentalmente, a evolução temporal da temperatura normalizada é mostrada para um lme de Au sobre Si e para lmes de Cu sobre substratos de vidro e Si, assim como foram utilizadas técnicas complementares de caracterização dos lmes (per lometria, elipsometria, microscopia de força atômica, eletrônica de varredura e de transmissão). Para o filme de ouro com espessura de 4:6µm, a teoria apresenta boa concordância com os resultados experimentais, já que o valor encontrado para a condutividade térmica do ouro está entre 230W/m.K e 280W/m.K, próximo e abaixo do valor da condutividade térmica do Au em volume (318W/m.K), indicando a validade do método implementado. Para lmes de cobre, porém, os resultados iniciais não apresentam a mesma concordância, e possíveis causas são discutidas. Futuramente, a TTR implementada poderá ser utilizada para determinação da condutividade térmica de lmes nos dielétricos ou semicondutores, e possivelmente na caracterização da componente transversal em filmes anisotrópicos. / This work presents a review of techniques to measure thermal properties off films, followed by a focused attention to the transient termo-re ectance (TTR). Amongst the existing technologies to measure thermal properties, optical methods are preferred due their nondestructive nature, high potential of spacial and temporal resolution, and independence from physical contact. The experimental implementation of this method is presented, as well as the theory of the transmission line theory used in the Laplace Transform treatment of the Fourier one-dimensional heat conduction equation. To facilitate the calculation of the Transform inversion, a numerical method, using the Stehfest method, was used. Experimentally, evolution of the normalized temperature is shown for a lm of Au on Si and for films of Cu on glass and Si substrates, whereas complementary techniques were used for film characterization (pro lometry, ellipsometry, atomic force microscopy, scanning and transmission eletron microscopy). For the Au film 4:6µm thick, the theory presents good agreement with the experimental results, and the value found for the thermal conductivity of the gold film is between 230W/m.K and 280W/m.K, near and below the bulk Au thermal conductivity (318W/m.K), indicating the validity of the method implementation. For Cu films, however, the initial results do not present the same agreement, and possible causes are discussed. In the future, the implemented TTR could be used for determination of the thermal conductivity of dielectric or semicondutors thin films, and possibly in the characterization of the transversal component in anisotropic films.

Este trabalho apresenta uma revisão de técnicas para medir propriedades térmicas de lmes, seguida de enfoque na termo-re etância transiente (TTR). Dentre as tecnologias existentes para medir propriedades térmicas, métodos ópticos são preferidos devido à sua natureza não-destrutiva, potencial de alta resolução temporal e espacial e calibração independente de contato físico. A implementação experimental deste método é apresentada, assim como a teoria da linha de transmissão utilizada para tratamento por Transformada de Laplace da equação de Fourier unidimensional do calor. Para facilitar o cálculo de invers ão desta Transformada, uma aproximação numérica, empregando o método Stehfest, foi usada. Experimentalmente, a evolução temporal da temperatura normalizada é mostrada para um lme de Au sobre Si e para lmes de Cu sobre substratos de vidro e Si, assim como foram utilizadas técnicas complementares de caracterização dos lmes (per lometria, elipsometria, microscopia de força atômica, eletrônica de varredura e de transmissão). Para o filme de ouro com espessura de 4:6µm, a teoria apresenta boa concordância com os resultados experimentais, já que o valor encontrado para a condutividade térmica do ouro está entre 230W/m.K e 280W/m.K, próximo e abaixo do valor da condutividade térmica do Au em volume (318W/m.K), indicando a validade do método implementado. Para lmes de cobre, porém, os resultados iniciais não apresentam a mesma concordância, e possíveis causas são discutidas. Futuramente, a TTR implementada poderá ser utilizada para determinação da condutividade térmica de lmes nos dielétricos ou semicondutores, e possivelmente na caracterização da componente transversal em filmes anisotrópicos. / This work presents a review of techniques to measure thermal properties off films, followed by a focused attention to the transient termo-re ectance (TTR). Amongst the existing technologies to measure thermal properties, optical methods are preferred due their nondestructive nature, high potential of spacial and temporal resolution, and independence from physical contact. The experimental implementation of this method is presented, as well as the theory of the transmission line theory used in the Laplace Transform treatment of the Fourier one-dimensional heat conduction equation. To facilitate the calculation of the Transform inversion, a numerical method, using the Stehfest method, was used. Experimentally, evolution of the normalized temperature is shown for a lm of Au on Si and for films of Cu on glass and Si substrates, whereas complementary techniques were used for film characterization (pro lometry, ellipsometry, atomic force microscopy, scanning and transmission eletron microscopy). For the Au film 4:6µm thick, the theory presents good agreement with the experimental results, and the value found for the thermal conductivity of the gold film is between 230W/m.K and 280W/m.K, near and below the bulk Au thermal conductivity (318W/m.K), indicating the validity of the method implementation. For Cu films, however, the initial results do not present the same agreement, and possible causes are discussed. In the future, the implemented TTR could be used for determination of the thermal conductivity of dielectric or semicondutors thin films, and possibly in the characterization of the transversal component in anisotropic films.

Thin film material properties and measurement characterisation techniques are crucial for the development of micro-electromechanical systems (MEMS) devices. Furthermore, as the technology scales down from microtechnology towards nanotechnology, nanoscale materials such as carbon nanotubes (CNTs) are required in electronic devices to overcome the limitations encountered by conventional materials at the nanoscale. The integration of CNTs into micro-electronics and material applications is expected to provide a wide range of new applications. The work presented in this thesis has contributed to the development of thin film material characterisation through research on the thermal conductivity measurement and the control of the residual stress of thin film materials used commonly in MEMS devices. In addition, the use of CNTs in micro-electronics and as filler reinforcement in composite materials applications have been investigated, leading to low resistivity CNTs interconnects and CNTs-Polyimide (PI) composites based resistive humidity sensors. In the first part of this thesis, the thermal conductivity of conductive thin films as well as the control of the residual stress arising from fabrication process in PI micro-cantilevers have been studied. A MEMS device has been developed for the thermal conductivity characterisation of conductive thin films showing good agreement with thermal conductivity of bulk material. Low energy Ar+ ion bombardment in a plasma has been used to control the residual stress present in PI cantilevers. Appropriate ion energy and exposure time have led to stress relaxation of the beams resulting in a straight PI cantilever beam. In the second part of this thesis, low resistivity CNTs interconnects have been developed using both dielectrophoresis (DEP) and Focused Ion Beam (FIB) techniques. An investigation of the effects of CNT concentration, applied voltage and frequency on the CNTs alignment between Al and Ti electrodes has resulted in the lowering of the CNTs’ resistance. The deposition of Pt contact using FIB at the CNTs-metal electrodes interface has been found to decrease the high contact resistances of the devices by four and two orders of magnitude for Al and Ti electrodes respectively. The last part of this thesis focuses on the preparation of CNTs-PI composite materials, its characterisation and its application as resistive humidity sensor. The integration of CNTs inside the PI matrix has resulted in enhancing significantly the electrical and mechanical properties of the composites. In particular, a DEP technique employed to induce CNTs alignment inside the PI matrix during curing has been attributed to play an important role in improving the composite properties and lowering the percolation threshold. In addition, the fabrication and testing of CNTs-PI resistive humidity sensors have been carried out. The sensing performance of the devices have shown to be dependent highly on the CNT concentration. Finally, the alignment of CNTs by DEP has improved the sensing properties of CNTs-PI humidity sensors and confirmed that the change of resistance in response to humidity is governed by the change of the CNTs’ resistances due to charge transfer from the water molecules to the CNTs.

Este trabalho apresenta o estudo, a implementação e a caracterização de transdutores compostos por uma estrutura formada por grades de Bragg (FBG, Fiber Bragg Gratings) e grades de período longo (LPG, Long Period Gratings) em fibra óptica com cobertura metálica autoaquecida para medição da condutividade térmica e da difusividade térmica de materiais baseado no método do fio quente (HWM, Hot-Wire Method) convencional. O autoaquecimento da fibra óptica do dispositivo desenvolvido neste trabalho é provocado pela luz de espectro infravermelho injetada por um laser de bombeamento, que é espalhada por uma LPG e absorvida por um filme fino metálico depositado na superfície da fibra. Os transdutores apresentados são compactos, simples, robustos e imunes a interferências eletromagnéticas. O arranjo experimental utilizando o dispositivo híbrido LPG-FBG foi capaz de medir as condutividades térmicas do ar atmosférico e da água comum com precisões de 27% e 14%, respectivamente. Foram identificados vários fatores que afetam a precisão e a exatidão das medidas realizadas, sendo propostas diversas formas de correções de modo a melhorar o desempenho do arranjo. Foi demonstrada com sucesso a viabilidade da aplicação original do arranjo experimental utilizando o dispositivo híbrido LPG-FBG em fibra óptica autoaquecida para a medição de propriedades térmicas de fluidos (ar e água). / This work presents the study, implementation, and characterization of transducers composed of a structure formed by Fiber Bragg Gratings (FBG) and Long Period Gratings (LPG) in optical fiber with self-heating coverage for measurement of thermal conductivity and thermal diffusivity of materials based on the Hot-Wire Method (HWM). The self-heating fiber optic device developed in this work is caused by the light of infrared spectrum injected by a pumping laser, which is spread by an LPG and absorbed by a thin metallic film deposited on the surface of the fiber. The transducers are compact, simple, robust and immune to electromagnetic interference. The experimental arrangement using the optical fiber sensor based on LPG-FBG hybrid structure was able to measure the thermal conductivity of atmospheric air and water with accuracies of 27% and 14%, respectively. Several factors were identified that affect the precision and the accuracy of the measures carried out, whereby various forms of corrections are being proposed to improve overall performance. The viability of the original application of the experimental arrangement using the LPG-FBG hybrid device in self-heating optical fiber for the measurement of thermal properties of fluids (air and water) has been successfully demonstrated.

Este trabalho apresenta o estudo, a implementação e a caracterização de transdutores compostos por uma estrutura formada por grades de Bragg (FBG, Fiber Bragg Gratings) e grades de período longo (LPG, Long Period Gratings) em fibra óptica com cobertura metálica autoaquecida para medição da condutividade térmica e da difusividade térmica de materiais baseado no método do fio quente (HWM, Hot-Wire Method) convencional. O autoaquecimento da fibra óptica do dispositivo desenvolvido neste trabalho é provocado pela luz de espectro infravermelho injetada por um laser de bombeamento, que é espalhada por uma LPG e absorvida por um filme fino metálico depositado na superfície da fibra. Os transdutores apresentados são compactos, simples, robustos e imunes a interferências eletromagnéticas. O arranjo experimental utilizando o dispositivo híbrido LPG-FBG foi capaz de medir as condutividades térmicas do ar atmosférico e da água comum com precisões de 27% e 14%, respectivamente. Foram identificados vários fatores que afetam a precisão e a exatidão das medidas realizadas, sendo propostas diversas formas de correções de modo a melhorar o desempenho do arranjo. Foi demonstrada com sucesso a viabilidade da aplicação original do arranjo experimental utilizando o dispositivo híbrido LPG-FBG em fibra óptica autoaquecida para a medição de propriedades térmicas de fluidos (ar e água). / This work presents the study, implementation, and characterization of transducers composed of a structure formed by Fiber Bragg Gratings (FBG) and Long Period Gratings (LPG) in optical fiber with self-heating coverage for measurement of thermal conductivity and thermal diffusivity of materials based on the Hot-Wire Method (HWM). The self-heating fiber optic device developed in this work is caused by the light of infrared spectrum injected by a pumping laser, which is spread by an LPG and absorbed by a thin metallic film deposited on the surface of the fiber. The transducers are compact, simple, robust and immune to electromagnetic interference. The experimental arrangement using the optical fiber sensor based on LPG-FBG hybrid structure was able to measure the thermal conductivity of atmospheric air and water with accuracies of 27% and 14%, respectively. Several factors were identified that affect the precision and the accuracy of the measures carried out, whereby various forms of corrections are being proposed to improve overall performance. The viability of the original application of the experimental arrangement using the LPG-FBG hybrid device in self-heating optical fiber for the measurement of thermal properties of fluids (air and water) has been successfully demonstrated.

<p>  We utilize thermoreflectance (TR) thermal imaging to experimentally study heat transport and reliability of micro to nano-scale devices. TR imaging provides 2D thermal maps with sub-micron spatial resolution. Fast thermal transients down to 50 ns resolution can be captured. In addition, finite element modeling is carried out to better understand the underlying physics of the experiment. We describe four main applications; 1) Development of a full-field thermoreflectance imaging setup with a variable optical (laser) heating source as a general characterization tool. We demonstrate the setup’s sensitivity to extract anisotropic<br> thermal conductivity of thin flms and evaluate its sensitivity for detecting buried (below the surface) defects in 3D integrated circuits. This method provides a low-cost noncontact alternative to destructive defect localization methods. It also doesn’t require any special sample<br> preparations. 2) Physics of localized electromigration-failures in metallic interconnects is investigated. One can distinguish two separate mechanisms responsible for electromigration depending on the current density and temperature gradient. 3) Thermal transport in silicon near sub-micron electrical heaters is studied. Quasiballistic and hydrodynamic (fluid-like) behavior is observed at room temperature for different device sizes and geometries. 4) Temperature-dependent thermoreflectance coefcient of phase-change materials is characterized. We focus on tungsten (W) doped VO₂ (W_0.02V_0.98O₂) compound, which experiences an insulator-to-metal transition (IMT) at ≈33 °C. Strong TR-signal non-linearity is observed at the IMT temperature. This non-linearity is used to localize the phase-change boundary with resolutions down to ≈0.2 µm. TR full-feld imaging enables a simple and fast characterization complementing near-feld microscopy techniques. <br>  </p>