abstract: Increasing density of microelectronic packages, results in an increase in thermal and mechanical stresses within the various layers of the package. To accommodate the high-performance demands, the materials used in the electronic package would also require improvement. Specifically, the damage that often occurs in solders that function as die-attachment and thermal interfaces need to be addressed. This work evaluates and characterizes thermo-mechanical damage in two material systems – Electroplated Tin and Sintered Nano-Silver solder. Tin plated electrical contacts are prone to formation of single crystalline tin whiskers which can cause short circuiting. A mechanistic model of their formation, evolution and microstructural influence is still not fully understood. In this work, growth of mechanically induced tin whiskers/hillocks is studied using in situ Nano-indentation and Electron Backscatter Diffraction (EBSD). Electroplated tin was indented and monitored in vacuum to study growth of hillocks without the influence of atmosphere. Thermal aging was done to study the effect of intermetallic compounds. Grain orientation of the hillocks and the plastically deformed region surrounding the indent was studied using Focused Ion Beam (FIB) lift-out technique. In addition, micropillars were milled on the surface of electroplated Sn using FIB to evaluate the yield strength and its relation to Sn grain size. High operating temperature power electronics use wide band-gap semiconductor devices (Silicon Carbide/Gallium Nitride). The operating temperature of these devices can exceed 250oC, preventing use of traditional Sn-solders as Thermal Interface materials (TIM). At high temperature, the thermomechanical stresses can severely degrade the reliability and life of the device. In this light, new non-destructive approach is needed to understand the damage mechanism when subjected to reliability tests such as thermal cycling. In this work, sintered nano-Silver was identified as a promising high temperature TIM. Sintered nano-Silver samples were fabricated and their shear strength was evaluated. Thermal cycling tests were conducted and damage evolution was characterized using a lab scale 3D X-ray system to periodically assess changes in the microstructure such as cracks, voids, and porosity in the TIM layer. The evolution of microstructure and the effect of cycling temperature during thermal cycling are discussed. / Dissertation/Thesis / Doctoral Dissertation Materials Science and Engineering 2018

Submitted by LÍGIA TIAKI YAMAMOTO null (ligia_yamamoto@bol.com.br) on 2018-02-08T01:02:07Z No. of bitstreams: 1 TESE DOUTORADO LIGIA TIAKI YAMAMOTO.pdf: 7712416 bytes, checksum: 463070944b5e98b407008fb138aa9256 (MD5) / Approved for entry into archive by Silvana Alvarez null (silvana@ict.unesp.br) on 2018-02-08T12:56:09Z (GMT) No. of bitstreams: 1 yamamoto_lt_dr_sjc.pdf: 7712416 bytes, checksum: 463070944b5e98b407008fb138aa9256 (MD5) / Made available in DSpace on 2018-02-08T12:56:09Z (GMT). No. of bitstreams: 1 yamamoto_lt_dr_sjc.pdf: 7712416 bytes, checksum: 463070944b5e98b407008fb138aa9256 (MD5) Previous issue date: 2017-12-08 / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / O sucesso a longo prazo das restaurações dentárias é limitada pela sua durabilidade no meio bucal. Testes in vitro continuam sendo ferramentas indispensáveis para avaliação inicial dos materiais dentários. Ciclagem térmica é um dos procedimentos mais utilizados para simular o envelhecimento fisiológico no qual os biomateriais são submetidos na prática clínica. Os objetivos desse estudo foram determinar o efeito da variação da temperatura, isolando o efeito hidrolítico, na degradação de uma cerâmica feldspática e de um cimento resinoso por meio de comparação entre os métodos artificiais de envelhecimento: armazenamento em água destilada, termociclagem em água e termociclagem em óleo mineral seguido pelo ensaio de flexão de 3 pontos e mini-flexão. Blocos de CAD-CAM de cerâmica feldspática foram cortados e lixados para obter-se 100 barras, com dimensões de 14 x 4 x 1,2 mm. Foram confeccionadas 100 barras de cimento resinoso autoadesivo, com dimensões de 12 x 2 x 2 mm. As barras foram aleatoriamente divididas (n = 10) e envelhecidos por meio de termociclagem em água e óleo mineral por 500 (norma ISO 11405), 5000 e 10000 ciclos com banhos de 30 s a 5 oC e 55 oC e armazenados em água destilada em estufa a 37 oC pelo mesmo tempo que foi realizado a ciclagem (9 h, 4 dias e 8 dias), além de dois grupos controles, um de cerâmica feldspática e outro de cimento resinoso ambos sem envelhecimento, totalizando 20 grupos. Após o envelhecimento, as barras foram fraturadas por meio do ensaio de flexão de 3 pontos e mini-flexão e os dados foram submetidos à análise estatística. Amostras representativas de cada grupo foram submetidas ao teste de dureza Knoop (cimento resinoso) e Vickers (cerâmica feldspática). Algumas superfícies fraturadas foram analisadas em Microscópio eletrônico de varredura. Para cerâmica feldspática não houve diferença significativa entre os grupos, apontando que os envelhecimentos propostos pelo trabalho não degradaram as amostras, já para o cimento resinoso houve diminuição da resistência à flexão após 8 dias ou 10000 ciclos térmicos, sendo que a termociclagem degradou ainda mais a amostra quando comparada ao armazenamento em água por 8 dias. Para dureza Vickers na cerâmica houve decréscimo após 10000 ciclos térmicos em óleo mineral. Para dureza Knoop no cimento resinoso, os valores diminuíram conforme aumentou o número de ciclos para a termociclagem em óleo e aumentou no armazenamento em água e não houve diferença para a termociclagem em água. Dentre as limitações desse estudo concluiu-se que é necessário mais ciclos térmicos/tempo para degradar a cerâmica feldspática e que para o cimento resinoso 10000 ciclos térmicos são suficientes para apontar degradação desse material. / The long-term success of dental restorations is limited by their durability in oral environments. In vitro tests remain essential to evaluate dental materials. Thermocycling is one of the most commonly used test to simulate physiological aging, to which biomaterials are exposed in clinical practice. The aim of this study was to determine the effect of thermocycling, in non-aqueous surroundings, on feldspathic ceramic and resin cement degradation comparing 3-point bending flexural strength test and mini-flexural strength test respectively. CAD-CAM feldspathic ceramic blocks were cut and polished to obtain 100 bars (14 x 4 x1.2 mm). One hundred resin cement bars were fabricated (12 x 2 x 2 mm). The bars were randomly divided into groups (n = 10) and submitted to aging using thermocycling in water (ISO 11405) and in mineral oil for 500, 5000 and 100000 cycles from 5 °C to 55 °C, with 30 s dwell time and stored in distilled water in a dry oven at 37°C for the same time as cycling occurred (9 h, 4 days and 8 days) besides the two control groups, one feldspathic ceramic and one resin cement both without aging, totaling 20 groups. After aging, the bars were fractured using 3 point bending test and mini-flexural test and the data was subjected to statistical analysis. Representative samples of each group were subjected to Knoop (resin cement) and Vickers (feldspathic ceramic) hardness test. Some of the fractured surfaces were analyzed through scanning electron microscope. No significant difference was observed between the feldspathic ceramic groups, showing that aging processes suggested in the study did not degrade the samples. As for the resin cement, a decrease in flexural strength after 8 days or 10000 thermal cycles was observed, in which thermocycling degraded the sample further when compared to the water storage for 8 days. For Vickers hardness in the ceramic there was decrease after 10000 thermal cycles in mineral oil. For Knoop hardness in the resin cement, values decreased as the number of thermal cycles for increased in oil and values increased in water storage and there was no difference for thermocycling in water. Within the limitations of the study, it is concluded that more cycles/days are necessary to degrade feldspathic ceramic and that for resin cement degradation to become evident 10000 thermal cycles are sufficient. / FAPESP: 2016/08672-6

Made available in DSpace on 2015-05-08T14:57:19Z (GMT). No. of bitstreams: 1 arquivototal.pdf: 1298323 bytes, checksum: 6a19c3b38cf846b711c2c52ac67ab30a (MD5) Previous issue date: 2014-11-28 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / A thermoelectric generator is a solid-state temperature dependent device that provide power generation on thermoelectric conversion. For that, the thermoelectric modules needs a temperature difference to ensure the thermoelectric conversion process. However, being subject to temperature variations may compromise the thermoelectric generator lifetime. Thus, in order to evaluate the temperature variation (thermal cycling) that the thermoelectric generators are exposed, this work has proposed an experimental platform that submits the thermoelectric generators modules to thermal cycling. With the experimental platform proposed the parameters of the thermoelectric generators may be to investigate properly. To evaluate the degradation effects on TEG the parameters were evaluated before the thermal cycling and then the parameters were evaluated after the thermal cycling process. At the research end, the parameters are presented by a comparative table with parameters evaluation before the thermal cycling and parameters evaluation after thermal cycling which brings to the experimental platform reliability. / Objetivo: Os geradores termoelétricos são dispositivos de estado sólido que utilizam a diferença de temperatura para a conversão em energia elétrica. No entanto, submeter os geradores termoelétricos a variações de temperatura pode comprometer o tempo de vida desses dispositivos. Assim, com o objetivo de investigar a possível influência das variações de temperatura ciclos térmicos a que os módulos geradores termoelétricos (TEGs) estão expostos, este trabalho desenvolveu uma plataforma experimental capaz de submeter TEGs à influência de ciclos térmicos, permitindo assim que os TEGs possam ser avaliados. Para constatar os efeitos na degradação do TEG, alguns parâmetros foram avaliados antes da aplicação dos ciclos térmicos e após uma sequência de ciclos térmicos. Ao fim da pesquisa, as avaliações feitas nos parâmetros são apresentadas em uma tabela comparativa, em que são apresentados os valores obtidos antes da aplicação dos ciclos térmicos e os valores dos parâmetros após a aplicação dos ciclos térmicos.

O acelerado e freqüente desenvolvimento de novos materiais e técnicas restauradoras tornam necessárias avaliações rápidas que estimem seus desempenhos clínicos. Este estudo avaliou protocolos de envelhecimento acelerado, in vitro, capazes de simular o desempenho de restaurações adesivas frente aos desafios inerentes ao ambiente oral. Foram utilizados 36 molares hígidos, cortados ao meio e divididos aleatoriamente em 12 grupos. Em todos os grupos foi realizada a exposição da superfície dentinária, delimitação da área de adesão e condicionamento ácido da superfície, seguida a aplicação do Sistema Adesivo Scotchbond Multiuso, e colocação da resina composta Z100, em incrementos. Foram confeccionados 6 grupos em formato de palito e 6 grupos em formato de haltere: dois grupos não foram submetidos à ciclagem térmica e mecânica (STSM-P e STSM-H); outros dois foram submetidos à ciclagem térmica (1.000 ciclos; 5-55ºC; 1min em cada banho) e não a mecânica (CTSM-P e CTSM-H); dois ainda foram submetidos à ciclagem mecânica com dispositivo Nova Ética e não a térmica (STNE-P e STNE-H); dois foram submetido à ciclagem mecânica com dispositivo Nova Ética (500.000 ciclos), acrescido de ciclagem térmica (CTNE-P e CTNE-H); outros dois por fim, foram submetidos à ciclagem mecânica por Microrotação (105 ciclos, aproximadamente por 7 horas), e não a térmica (STMR-P e STMR-H); por fim os dois últimos grupos foram submetido à ciclagem mecânica por Microrotação acrescido de ciclagem térmica (CTMR-P e CTMR-H). Todos os grupos foram preparados para teste de microtração. Com as medidas de resistência de união dos palitos e halteres de cada dente foi realizada análise de variância e teste de Tukey. A interação tripla Formato -FORM- (Palito ou haltere) X Ciclagem Térmica- T- (Com e Sem) X Ciclagem Mecânica-M- (Nova Ética e Microrotação) não foi significante (p=0,698), bem como a interação 2 a 2 dos mesmos fatores: FORMxT (p=0,391); TxM (p=0,477); FORM x M (p=0,746). O fator Formato do espécime (Palito ou Haltere) teve diferença extremamente significante (p=0,000), sendo que os valores dos halteres foram maiores que os dos palitos. O fator Ciclagem Térmica (Com e Sem) não foi estatisticamente significante (p=0,2), bem como o fator Ciclagem Mecânica (Nova Ética e Microrotação) (p=0,587). Pode-se concluir que: a ciclagem térmica, bem como as ciclagens mecânicas sistema Nova Ética e Microrotação não foram capazes de reduzir significativamente os valores de resistência de união das interfaces adesivas, nem quando aplicadas isoladamente, nem quando associadas; os espécimes com formato de palito apresentaram valores de resistência de união menores do que os em formato de haltere; não foi possível estabelecer nenhum padrão de degradação entre os grupos através da microscopia eletrônica de varredura; os elementos finitos identificaram uma distribuição mais homogênea das tensões geradas na interface dos espécimes em formato de haltere. / The rapid and frequent development of new materials and restorative techniques necessitate rapid assessments to estimate their clinical outcomes. This study sought to evaluate protocols for accelerated aging, in vitro, capable of simulating the performance of adhesive restorations with challenges inherent to the oral environment. The study included 36 molars that were randomly divided into 12 groups. In all groups were exposed dentin surface, defining the area of adhesion and etching the surface, then the application of Scotchbond Multipurpose Adhesive System, and placement of composite resin Z100, in increments. Six groups were fabricated in the shape of sticks and six other groups in dumbbell shape: the first was not subjected to thermal cycling and mechanical (STSM-P and STSM-H), the second was subjected to thermal cycling (10,000 cycles, 5-55 ° C) and not the mechanics (CTSM-P and CTSM-H); the third was subjected to mechanical cycling device with new Ethics (500,000 cycles) and not thermal (STNE-P and STNE-H); the fourth was subjected to mechanical cycling device with new Ethics, plus thermal cycling (CTNE-P and CTNE-H); the fifth was submitted the mechanical cycling device for Microrotation (105 cycles), but not thermal (STMR-P and STMR-H) and finally the sixth was subjected to mechanical cycling device for Microrotation plus thermal cycling (CTMR-P and CTMR-H). All groups were prepared for microtensile bond-strength test. With the measures of bond strength of each tooth was performed statistical analysis (ANOVA and Tukey test). Random samples of specimens were evaluated by SEM. The triple interaction format (stick or dumbbell-shaped) X Thermal cycling (with and without) X Cycling Mechanics (New Ethics and Microrotation) was not significant (p = 0.698), as well as the interaction 2-2 of the same factors: FORMXT (p = 0.391); TXM (p = 0.477); FORMxM (p = 0.746). With regard to factor Format specimen is observed that the bond strength values obtained for the dumbbell-shaped are higher than those obtained for the sticks (p = 0.000). With regard to factor Thermal cycling was observed that the difference was not statistically significant (p = 0.2). As for factor Cycling Mechanics, the values of groups without cycling were very similar to those obtained in groups cycled through the system New Ethics, and the system by Microrotation, no significant difference between any of them (p = 0.587). The conclusions were that the stick-shaped specimens showed values of bond strength lower than the dumbbell-shaped; thermocycling and mechanical cycling were not able to significantly reduce the values of bond strength of adhesive interfaces, even when applied alone or when associated. It could not be establish any pattern of degradation among the groups by SEM; the finite element identified a more homogeneous distribution of stresses generated at the interface of dumbbell shaped specimens.

Today, Scania CV AB is facing challenging demands on functionality and performance within their vehicles. The electronics are increasing rapidly and to stay competitive on the market, concerns regarding reliability of electronic systems needs to be evaluated. Prognostics and health management (PHM) is a concept where reliability of, for example, electronic control units (ECUs) are assessed. It requires customized systems for each specific environment, due to different strains and stresses. One approach is to have canaries (components with reduced soldering mass) implemented into ECUs as an indication that something is about to happen. Another essential aspect is the continuous real-time data acquisition from sensors, that can be used for different algorithms and models, which could provide forecasts on remaining useful life (RUL) of the ECUs. An appliance is the big data acquisition, where a database will collect data from vehicles, which means that ECU data need be communicated differently than today. This is why this master thesis project investigated canaries on printed circuit boards (PCBs) when they were subjected to vibrations as well as thermal cycling (TC), which are common parameters within vehicles. The PCBs consisted of both lead (Sn-Pb) and lead-free (SAC305) soldering for material comparison, since a transition to lead-free electronics is happening. Several fatigue tests were performed to collect as much information as possible. For further advances towards a PHM implementation, thermal shock (TS) tests on ECUs were performed as well. The ECUs were shocked in a temperature cabinet while being in active state. The internal temperature sensor was communicated with via controller area network (CAN). Scania’s CAN program was used and the data was logged in a computer, which in turn was compared to the data from the surrounding thermocouples, placed in specific spots. The results that were achieved clearly showed that lead-free PCBs are much more sensitive to stresses (both vibrations and TC). It was also shown that canaries failed in a much higher extent than regular resistors. The real-time data acquisition from the ECU could successfully be managed, where continuous data was logged. Also, the TS tests showed how the correlation between sensors indifferent positions was. Finally, the results from these tasks were discussed for future work. One have to keep in mind that this is just the beginning of a many-years project within Scania. The results and progress within this master thesis project will hopefully be a step in the rightdirection.

Durability is the most important factor in the design of heat-exchangers to meet the specifications of the customers. To predict the durability, endurance tests are carried out. In this thesis, one of the endurance tests, thermal cycling is performed for three different internal coolant flows until failure which is known as Wöhler test. A tool is developed in MATLAB that could import data from all kinds of endurance tests and visualizes time histories of every channel of the test (test parameters such as temperature, pressure, flow). An algorithm is developed for Level Crossing counting method which works based on the Markov cycle counting method. This produces Level crossing curves (LCC) for all the channels of the test which says how well a test has been performed and the total number of cycles of the test. It was observed that the LCCs obtained from the tool gives accurate results when compared with those obtained from LMS software whose approach of producing LCCs is Rainflow cycle counting method. Strain measurements are performed for the same flowrates as that of the Wöhler tests. The results from strain measurements and Wöhler tests are used in the determination of Basquin’s coefficient of the Wöhler curve. It was observed that the optimal value of Basquin’s coefficient is 3.4.

The effect of thermal cycling on the state of stress in polymeric materials bonded to stiff elastic substrates was investigated using numerical techniques, including finite element methods. The work explored the relationship between a cyclic temperature environment, temperature-dependent viscoelastic behavior of polymers, and thermal stresses induced in a constrained system. Due to the complexity of developing a closed-form solution for a system with time, temperature, material properties, and boundary conditions all coupled, numerical techniques were used to acquire approximate solutions. Descriptions of attempted experimental verification are also included. The results of the numerical work indicate that residual stresses in an elastic-viscoelastic bimaterial system incrementally shift over time when subjected to thermal cycling. Tensile axial and peel stresses develop over a long period of time as a result of viscoelastic response to thermal stresses induced in the polymeric layer. The applied strain energy release rate at the crack tip of layered specimens is shown to similarly increase. The rate of change of the stress state is dependent upon the thermal cycling profile and the adhesive’s thermo-mechanical response. Discussion of the results focuses on the probability that the incrementing tensile residual stresses induced in an adhesive bond subjected by thermal cycling may lead to damage and debonding, thus reducing durability. / Master of Science

Currently, there are two major driving forces for considering alternative materials to lead- based products, specifically interconnections, in electronics applications, including the impending legislation or regulations which may tax, restrict, or eliminate the use of lead and the trend toward advanced interconnection technology, which may challenge the limits of present soldering technology. The reliability of solder joints is a concern because fracture failures in solder joints accounts for 70% of failures in electronic components. Lead-free solders are being investigated as replacements for lead solders currently used in electronics. Thermo-mechanical properties describe the stresses accumulated due to thermal fatigue as a result of CTE mismatch within the system. By understanding the failure mechanisms related to lead-free solders, the application of lead- free solders could be more strategically designed for specific applications. The objective of this thesis is to observe microstructural change in large-area solder joints caused by thermal cycling and relate these changes to reliability issues in large-area lead and lead-free solder constructed semiconductor power devices. This study focused on the microstructural changes within the solder alloy of a large-area solder joint under thermal cycling conditions. Two major primary observations were made from this research, they are: 1) due to a combination of testing conditions and material properties, the lead-free solders, Sn/3.5Ag and Sn/Ag/0.7Cu, sustained the most severe damage as compared to Sn/37Pb, and 2) due to elevated stresses at the solder/substrate interface in a simulated power semiconductor device sample damage was found to be most severe. / Master of Science

The aim and objective of this study was to determine the bond strength of a twostep and a single-step dentin bonding agent and to determine the effect of repeated thermal-cycling from 50C and 550C on the bond strength values of these dentin bonding agents.

<p>Thermal barrier coatings (TBC) are used for reduction of component temperatures in gas turbines. The service temperature for turbines can be as high as 1100ºC and the components are exposed to thermal cycling and gases that will cause the component to oxidize and corrode. The coatings are designed to protect the substrate material from this, but eventually it will lead to failure of the TBC. It is important to have knowledge about when this failure is expected, since it is detrimental for the gas turbine.</p><p>The scope of this thesis has been to see if an existing life model for thin TBC also is valid for thick TBC. In order to do so, a thermal cycling fatigue test, a tensile test and finite element calculation have been performed. The thermal cycling fatigue test and finite element calculation were done to find correlations between the damage due to thermal cycling, the number of thermal cycles and the energy release rate. The tensile test was preformed to find the amount accumulated strain until damage.</p><p>The thermal cycling lead to failure of the TBC at the bond coat/top coat interface. The measurment of damage, porosity and thickness of thermally grown oxide were unsatisfying due to problems with the specimen preparation. However, a tendency for the damage development were seen. The finite element calculations gave values for the energy release rate the stress intensity factors in mode~I and mode~II that can be used in the life model. The tensile test showed that the failure mechanism is dependent of the coating thickness and it gave a rough value of the maximum strain acceptable.</p>