The goal of this research was to create a microstructure graded glass-ceramic and investigate the resulting properties as a function of crystallization processing. The desired glass-ceramic was a lithium disilicate material that has a crystallization gradient across the sample, leading to functionally graded properties as a result of the microstructure gradient. Samples were prepared by melting and pouring glass at 1400°C, annealing at 400°C for 48 hours, and nucleating at 480°C for 2 hours. To ensure that crystallization would not occur homogeneously throughout the sample, a temperature gradient was imposed during crystallization. Samples were crystallized on a self-constructed resistance wire furnace that was open to air. Several crystallization processing parameters were tested, including high temperature for a short time and low temperature for a long time. Samples were ground and polished to 0.25 microns before characterization methods were performed. Scanning electron microscopy (SEM) showed the microstructure transition across the sample cross section, with crystals present on the crystalline side and only nuclei present on the glassy side. Raman spectroscopy showed a transformation of the characteristic spectra across the sample cross section, with defined, high-intensity peaks on the crystalline side and broad, low-intensity peaks on the glassy side. Microhardness showed a slight transition in hardness values across the sample cross section, however the variability was too great to draw any conclusions. The characterization methods showed that the desired material was created and the resulting properties were a function of the crystallization processing parameters. / Master of Science

Syfte Syftet med föreliggande studie var att undersöka böjhållfastheten hos IPS e.max CAD före och efter termocykling med 10 000 respektive 15 000 cykler. Material och metod Trettio provkroppar framställdes från fem stycken IPS e.max CAD LT-block. Provkropparna var indelade i två testgrupper (GT10 och GT15), och en kontrollgrupp (GK), á 10 provkroppar i varje. Provkropparna utformades enligt måtten L 17,9 ± 0,03 mm x B 2,5 ± 0,03 mm x H 2,5 ± 0,03 mm. Samtliga provkroppar kristalliserades och grupp GK förvarades i rumstemperatur, resterande två grupper, GT10 och GT15 termocyklades i 10 000 respektive 15 000 cykler.Därefter utfördes ett trepunkts böjhållfasthetstest. Resultaten analyserades med One-way ANOVA, Tukey’s test med signifikansnivån α= 0,05 i statistikprogrammet SPSS. Resultat Resultaten visade att det inte fanns någon signifikant skillnad mellan grupp GK och GT10 (p>0,05) respektive mellan grupp GT10 och GT15 (p>0,05). Grupp GT15 hade högst medelvärde (516 MPa) och grupp GK hade lägst medelvärde (450 MPa). Signifikant skillnad fanns mellan grupp GK och GT15 (p<0,05). Grupp GT15 hade en signifikant högre böjhållfasthet (~470-637 MPa) jämfört med grupp GK (~406-494 MPa). Slutsats Inom föreliggande studies begränsningar kan följande slutsatser dras: Termocykling med 10 000 cykler påverkar inte böjhållfastheten, däremot ger ökat antal cykler (15 000) högre böjhållfasthet. / Purpose  The purpose of the present study was to investigate the flexural strength of IPS e.max CAD beforeand after thermal cycling with 10,000 and 15,000 cycles, respectively.  Material and method  Thirty specimens were prepared from five IPS e.max CAD LT blocks, divided into two test groups (GT10 and GT15), and one control group (group GK) (n=10). The specimens were designed with the dimensions L 17.9 ± 0,03 mm x W 2.5 ± 0,03 mm x H 2.5 ± 0,03 mm. All specimens were crystallized and group GK was kept in room temperature, the remaining two groups, GT10 and GT15 were thermocycled with 10,000 and 15,000 cycles respectively. A three-point flexural strength test was performed. The results were analyzed with One-way ANOVA, Tukey's test with a significance level α = 0.05 in the statistical program SPSS.  Results  The results showed that there was no significant difference between groups GK and GT10 (p> 0.05), and between groups GT10 and GT15 (p> 0.05). It was also observed that group GT15 had the highest average (516 MPa) and group GK had the lowest average (450 MPa). There was a significant difference between groups GK and GT15 (p <0.05). Group GT15 had a significantly higher flexural strength (~ 470-637 MPa) compared to group GK (~406-494 MPa).  Conclusion  Within the limitations of the present study, the following conclusions can be drawn:Thermal cycling comprising 10,000 cycles do not affect the flexural strength, however, increasing the number of cycles (15,000) will give higher flexural strength.

Objective: The primary objective of this study was to evaluate the roughness of CAD/CAM blocks of lithium disilicate glass-ceramic (IPS e.max CAD, Ivoclar Vivadent®, Schaan, Liechtenstein), before and after surface treatment with hydrofluoridric acid 10% and after silane coating by Atomic Force Microscopy and Optical Microscopy. The average size of silane as well as its fit to the valleys after acid etching was also studied. Methods: Ten specimens of CAD/CAM blocks of lithium disilicate glass-ceramic were analyzed by Atomic Force Microscopy. Before surface treatment with hydrofluoridric acid 10%, the specimens were also analyzed by Atomic Force Microscopy. All specimens were also analyzed by Optical Microscopy after the application of a layer of silane. Free software Gwyddion version 2.51 was used on data processing. The 3D surface measurements were: root mean square roughness, average roughness, maximum peak height, maximum pit depth, maximum height, Skewness and Kurtosis of surface and profile roughnesses. Images provided by Optical Microscopy were used to calculate the size of the silane particle, also using the free software Gwyddion version 2.5.1. Non-parametric tests were done by the free software R version 3.5.1. Results: Surface roughness and profile roughness were numerically different, but both increased after acid etching. All the skewness measurements concentrated around zero, indicating a more symmetrical behavior after acid conditioning. Silane cross-sectional area measured from 0,0374m² to 0,424351m² and its radius ranged from 0,115m to 0,3675m and could fit in on about 77,5% of the conditioned surface valleys. Significance: Roughness surface and silane layer are important factors to the bond strength between ceramic and resin cements, ensuring the success of restorative treatment. / Objetivo: O principal objetivo deste estudo in vitro foi analisar a rugosidade de superfície de blocos de CAD/CAM de cerâmica de dissilicato de lítio, antes e depois do condicionamento com ácido fluorídrico a 10% durante 20 segundos e após a aplicação de uma camada de silano, usando a Microscopia de Força Atômica e Microscopia Óptica. A média do tamanho do silano e como eles se ajustam nos vales da superfície condicionada também foram estudados. Metodologia: 10 amostras confeccionadas por blocos para CAD/CAM de cerâmica de dissilicato de lítio foram analisadas por um microscópio de força atômica. Depois do tratamento de superfície com ácido fluorídrico a 10% durante 20 segundos, os espécimes foram novamente analisados por Microscopia de Força Atômica. Todas as amostras foram analisadas em microscópio óptico depois da aplicação de uma camada de silano. O software Gwyddion (versão 2.5.1) foi usado para o processamento de dados. As medidas obtidas para as imagens 3D das superfícies foram: raiz quadrada média da rugosidade, rugosidade média, altura do pico mais alto, profundidade do vale mais baixo, máxima altura, assimetria e curtose, tanto para a análise de superfície quanto para a análise do perfil. As imagens obtidas pela Microscopia Óptica foram usadas para calcular o tamanho da partícula de silano, também usando o software Gwyddion (versão 2.5.1.). Testes não-paramétricos foram calculados pelo software R (versão 3.5.1). Resultados: As rugosidades da superfície e do perfil foram numericamente diferentes, mas ambas aumentaram após o condicionamento ácido. A assimetria concentrou-se próxima a zero, indicando um comportamento mais simétrico após o condicionamento. A área da secção transversal do silano mede entre 0,0374m² a 0,424351m² e o seu raio mediu entre 0,115m a 0,3675m. Esse tamanho de partícula pode ser acomodado em 77,5% dos vales presentes nas superfícies condicionadas. Significância: A rugosidade e a camada de silano são fatores importantes para o aumento da união entre a cerâmica e o cimento resinoso, assegurando o sucesso do tratamento restaurador.