O objetivo deste estudo foi a Y-TZP odontológica submetida ao envelhecimento hidrotérmico acelerado (EH). Especificamente: a) determinar a curva cinética de transformação de fase tetragonal para monoclínica; b) calcular a velocidade de crescimento da frente da camada transformada durante o EH; c) avaliar a relação entre a porcentagem de fase monoclínica e profundidade da transformação de fase com a resistência à flexão biaxial (FB); d) avaliar o efeito da associação do EH e fadiga na resistência à FB. Discos sinterizados (YZ- Vita YZ, LP-Lava Plus) foram submetidos ao EH a 120°C, 130°C e 150°C e analisados por difração de raios X (DRX). Uma amostra por grupo foi analisada por microscopia eletrônica de varredura (MEV) e tomografia de coerência óptica (OCT) para calcular a profundidade de transformação de fase e a velocidade da frente de transformação. Grupos de (YZ, LP e LA-Lava) foram submetidos ao EH (150°C) por (n=10): 0, 5, 25, 70 e 140 horas. Após o EH os grupos de YZ foram novamente divididos (n=10): com e sem ciclagem mecânica, todas as cerâmicas foram submetidas ao teste de flexão biaxial (ISO 6872) e análise de variância 1 fator (ANOVA) (α=0,05) para comparar os resultados. Os resultados de DRX indicam que a Y-TZP apresenta um comportamento sigmoidal de transformação de fase devido à limitação da profundidade de penetração dos raios X (~6,3 μm). As análises de MEV e OCT confirmaram o crescimento linear da frente de envelhecimento em função do tempo para todas as temperaturas. O ANOVA 1-fator demonstrou redução de 10-19% da resistência à FB após 140 horas de envelhecimento (150°C) para todas as cerâmicas, havendo correlação negativa entre profundidade da camada transformada e resistência à FB. Extrapolando os resultados de profundidade para 37°C foi calculado que a frente de transformação de fase levaria 1053 e 2104 anos para atingir a profundidade de 62,67μm e 85,55μm responsáveis pela diminuição da resistência mecânica da YZ e LP, respectivamente. A associação do EH com a ciclagem mecânica não apresentou efeitos deletérios para a YZ. O OCT foi validado como método preciso, fácil e rápido para avaliação da camada transformada e estudos de cinética. / The aim of this study was to evaluate the aging behavior of a dental Y-TZP submitted to an accelerated hydrothermal aging (HA). Specifically: a) determine the kinetic curve of tetragonal to monoclinic phase transformation (t-m); b) calculate the speed of the front of phase transformation zone growth during the HA; c) evaluate the relationship between percentage of monoclinic phase and depth of phase transformation with the biaxial flexural strength (BF); d) evaluate the effect of the association of HA and fatigue at the BF. Sintered discs of dental Y-TZP (YZ- Vita YZ, LP- Lava Plus) were submitted to HA at 120°C, 130°C and 150°C and analyzed by X-ray diffraction analysis (XRD). One specimen of each group was submitted to scanning electron microscopy (SEM) and optical coherence tomography (OCT) to calculate the phase transformation depth and the speed of the front transformation zone. Groups (YZ, LP and LA-Lava) were divided according to the aging time (n=10): 0, 5, 25, 70 and 140 hours (150°C/3.01 bar). After the HA the YZ group was divided once again (n=10): with and without mechanical cycling, all ceramics were submitted to biaxial flexural strength test (ISO 6872) and one way analysis of variance (ANOVA) (α=0.05) to compare the results. XRD results indicated that YTZP presented a sigmoidal behavior due to the limited depth of XRD penetration (~6.3 μm). SEM and OCT analysis confirmed a linear growth of the front as function of the time to all temperatures One way ANOVA showed a decrease in mechanical strength (10-19%) after 140 hours of HA (150°C) for all ceramics. Extrapolating the depth of the transformed zone results to 37°C it was calculated that the front of the transformed zone would take around 1053 and 2104 years to reach 62.67μm and 85.55μm, depth that decreased the mechanical strength of the YZ and LP, respectively. The association of HA and mechanical cycling did not present a deleterious effect for the YZ. The OCT was validated as a precise, easy and fast method to evaluate the depth of the transformed zone and for kinetics studies.

O objetivo deste estudo foi a Y-TZP odontológica submetida ao envelhecimento hidrotérmico acelerado (EH). Especificamente: a) determinar a curva cinética de transformação de fase tetragonal para monoclínica; b) calcular a velocidade de crescimento da frente da camada transformada durante o EH; c) avaliar a relação entre a porcentagem de fase monoclínica e profundidade da transformação de fase com a resistência à flexão biaxial (FB); d) avaliar o efeito da associação do EH e fadiga na resistência à FB. Discos sinterizados (YZ- Vita YZ, LP-Lava Plus) foram submetidos ao EH a 120°C, 130°C e 150°C e analisados por difração de raios X (DRX). Uma amostra por grupo foi analisada por microscopia eletrônica de varredura (MEV) e tomografia de coerência óptica (OCT) para calcular a profundidade de transformação de fase e a velocidade da frente de transformação. Grupos de (YZ, LP e LA-Lava) foram submetidos ao EH (150°C) por (n=10): 0, 5, 25, 70 e 140 horas. Após o EH os grupos de YZ foram novamente divididos (n=10): com e sem ciclagem mecânica, todas as cerâmicas foram submetidas ao teste de flexão biaxial (ISO 6872) e análise de variância 1 fator (ANOVA) (α=0,05) para comparar os resultados. Os resultados de DRX indicam que a Y-TZP apresenta um comportamento sigmoidal de transformação de fase devido à limitação da profundidade de penetração dos raios X (~6,3 μm). As análises de MEV e OCT confirmaram o crescimento linear da frente de envelhecimento em função do tempo para todas as temperaturas. O ANOVA 1-fator demonstrou redução de 10-19% da resistência à FB após 140 horas de envelhecimento (150°C) para todas as cerâmicas, havendo correlação negativa entre profundidade da camada transformada e resistência à FB. Extrapolando os resultados de profundidade para 37°C foi calculado que a frente de transformação de fase levaria 1053 e 2104 anos para atingir a profundidade de 62,67μm e 85,55μm responsáveis pela diminuição da resistência mecânica da YZ e LP, respectivamente. A associação do EH com a ciclagem mecânica não apresentou efeitos deletérios para a YZ. O OCT foi validado como método preciso, fácil e rápido para avaliação da camada transformada e estudos de cinética. / The aim of this study was to evaluate the aging behavior of a dental Y-TZP submitted to an accelerated hydrothermal aging (HA). Specifically: a) determine the kinetic curve of tetragonal to monoclinic phase transformation (t-m); b) calculate the speed of the front of phase transformation zone growth during the HA; c) evaluate the relationship between percentage of monoclinic phase and depth of phase transformation with the biaxial flexural strength (BF); d) evaluate the effect of the association of HA and fatigue at the BF. Sintered discs of dental Y-TZP (YZ- Vita YZ, LP- Lava Plus) were submitted to HA at 120°C, 130°C and 150°C and analyzed by X-ray diffraction analysis (XRD). One specimen of each group was submitted to scanning electron microscopy (SEM) and optical coherence tomography (OCT) to calculate the phase transformation depth and the speed of the front transformation zone. Groups (YZ, LP and LA-Lava) were divided according to the aging time (n=10): 0, 5, 25, 70 and 140 hours (150°C/3.01 bar). After the HA the YZ group was divided once again (n=10): with and without mechanical cycling, all ceramics were submitted to biaxial flexural strength test (ISO 6872) and one way analysis of variance (ANOVA) (α=0.05) to compare the results. XRD results indicated that YTZP presented a sigmoidal behavior due to the limited depth of XRD penetration (~6.3 μm). SEM and OCT analysis confirmed a linear growth of the front as function of the time to all temperatures One way ANOVA showed a decrease in mechanical strength (10-19%) after 140 hours of HA (150°C) for all ceramics. Extrapolating the depth of the transformed zone results to 37°C it was calculated that the front of the transformed zone would take around 1053 and 2104 years to reach 62.67μm and 85.55μm, depth that decreased the mechanical strength of the YZ and LP, respectively. The association of HA and mechanical cycling did not present a deleterious effect for the YZ. The OCT was validated as a precise, easy and fast method to evaluate the depth of the transformed zone and for kinetics studies.

Miljöpåverkan från konventionella förbränningsmotorer har bidragit till en övergång till elmotorer. I denna övergång spelar litiumjonbatterier en viktig roll som energilagringssystem, men på grund av sin reaktiva kemi kan de utgöra en säkerhetsrisk. I likhet med civilsamhället står Försvarsmakten inför ett skifte där förbränningsmotorer ska bytas ut mot el- och hybridmotorer. För en säker militär tillämpning är det därför viktigt att förstå hur litiumjonbatterier beter sig vid åldrande och bortom ramen för normal användning. Detta projekt syftar till att identifiera batteriparametrar (impedans, resistans, kapacitet och yttemperatur) att använda för bedömning av batteriets hälsotillstånd. Vidare syftar projektet till att värdera de identifierade batteriparametrarnas lämplighet för militära applikationer. Som en del av syftet undersöker detta projekt omgivningstemperaturens effekt på batteriparametrarna, samt använder batteriparametrarna för att uppskatta när ett batteri kan klassas som förbrukat. Kommersiella NMC/grafit-litiumjonbatterier åldrades genom full upp- och urladdning. Varje batteri utsattes för maximalt 250 upp- och urladdningscykler vid laddningsströmmar om 4 A och urladdningsströmmar om 10 A. Åldrandet övervakades genom regelbunden mätning av impedans, resistans, kapacitet och yttemperatur. Batterierna cyklades vid antingen 52 ± 3 °C, 21 ± 3 °C eller −15 ± 3 °C för att studera omgivningstemperaturens effekt på de undersökta batteriparametrarna. Impedansmätningar vid 980 Hz var stabilast med avseende på variationer i omgivningstemperatur samt batteriets laddningsnivå, och ansågs därför vara den lämpligaste batteriparametern att använda för uppskattning av batteriets hälsotillstånd när tillämpningen kräver stor flexibilitet. Förändringar i resistans och kapacitet vid givna omgivningstemperaturer ansågs å andra sidan bättre återspegla batteriets åldringsgrad. Därför ansågs resistans och kapacitet vara de lämpligaste batteriparametrarna för uppskattning av batteriets hälsotillstånd med avseende på precision. Mätning av yttemperatur gav otillräcklig information för att uppskatta batteriernas hälsotillstånd med precision. En sänkning av omgivningstemperaturen från 21 °C till −15 °C hade en stor påverkan på resistans och kapacitet; resistansen ökade medan kapaciteten minskade, vilket motsvarar en reducerad batteriprestanda. Med avseende på kapacitetsförlust så förbrukades inget av batterierna som förvarades i 21 °C under cyklingen. Batterier som förvarades i 52 °C och −15 °C var förbrukade efter 150–200 cyklingar. Med avseende på resistansökning var ett av batterierna som förvarades vid 21 °C förbrukat efter 200 cyklingar. Samtliga batterier förvarade vid 52 °C var förbrukade efter 150–200 cyklingar, medan batterier förvarade vid −15 °C var förbrukade efter 200–250 cyklingar. Slutligen, med avseende på impedansmätning vid 980 Hz så tog det 200 cyklingar tills dess att ett av batterierna som förvarades i 21 °C var förbrukat. Ett av batterierna som förvarades i 52 °C var förbrukat efter 150 cyklingar. Batterier förvarade vid −15 °C var förbrukade efter 200–250 cyklingar. / Environmental concerns associated with greenhouse gas emissions from conventional combustion engines have contributed to a transition towards electric mobility. In this transition, lithium-ion (Li-ion) batteries play an important part as an energy storage system. However, Li-ion batteries can pose a safety risk due to their reactive chemistry. The Swedish Armed Forces are approaching a transition towards electric mobility, therefore, understanding Li-ion battery behavior with regard to non-normal use and ageing is critical for safe military applications. This project aimed to identify and evaluate battery parameters (impedance, resistance, capacity and surface temperature) suitable for State of Health (SOH) estimation of Li-ion batteries in military applications. Furthermore, this project aimed to investigate the ambient temperature’s effect on battery parameters, and identify the battery’s end of life (EOL) based on battery parameter tracking. Commercial NMC/graphite Li-ion batteries were exposed to ageing through repeated charge and discharge cycles. A critical application was mimicked, where the batteries operated at 1C charge rate (4 A) and 2.5C discharge rate (10 A) between 100 % and 0 % state of charge, for up to 250 charge/discharge cycles. The ageing process was tracked through regular measurements of impedance, resistance, capacity and surface temperature. In order to investigate the ambient temperature’s effect on the investigated battery parameters, the batteries were aged at either 52 ± 3 °C, 21 ± 3 °C or −15 ± 3 °C. Impedance measured at 980 Hz was the most stable battery parameter with respect to variations in state of charge and temperature, and was therefore regarded as the most suitable parameter for SOH estimation with respect to flexibility. Measurements of resistance and capacity at given temperatures were likely reflecting electrochemical ageing phenomena more accurately, hence the most suitable battery parameters for SOH estimation with respect to accuracy. Tracking of surface temperature provided insufficient information for accurate estimation of the batteries SOH. Decreasing the ambient temperature from 21 °C to −15 °C had a major effect on capacity and resistance; the resistance increased and the capacity decreased, corresponding to a decrease in battery performance. With respect to capacity fade, neither of the batteries aged at 21 °C reached their EOL within 250 cycles, while batteries aged at 52 °C or −15 °C reached their EOL after 150–200 cycles. With respect to resistance, one battery kept at 21 °C reached their EOL after 200 cycles, all batteries kept at 52 °C reached their EOL after 150–200 cycles, and batteries kept at −15 °C reached their EOL between 200–250 cycles. Finally, with respect to impedance measured at 980 Hz, one battery kept at 21 °C reached their EOL after 200 cycles, one battery kept at 52 °C reached their EOL after 150 cycles, and batteries kept at −15 °C reached their EOL between 200–250 cycles.