BACKGROUND: Polymer-infiltrated zirconia ceramic, benefiting from the synergistic effect of the ceramic matrix providing strength and the polymer enhancing toughness, has the potential to mimic the structure of natural teeth in its optical and mechanical properties. OBJECTIVE: To determine the effect of additives and various sintering temperatures on the optical and mechanical properties of zirconia ceramic matrix composites. MATERIALS AND METHODS: Groups consisted of unmodified zirconia powder, and zirconia modified with porcelain and porogens to form the porous ceramic matrix. Three types of Tosoh zirconia powder, TZ-3YSB-E, Zpex, and Zpex Smile, were used to fabricate porous blocks. Zirconia powder and porcelain powder were ball-milled separately. Zirconia powder was dry pressed and then cold isostatic pressed. The blocks were sintered at 1000 and 1150 ºC and sectioned into discs (n=10). For zirconia with additives groups, 10% of Titankeramik and 5% of PEG8000 were mixed to zirconia powder using a high-speed mixer. The zirconia blocks were pressed and sintered at 1000, 1150, 1200 and 1300 ℃, and sectioned into discs (n=10). Porous discs were treated with a 10% wt solution of 10-MDP for 4 hours and then dried in a vacuum oven for 24 hours. TEGDMA-UDMA resin monomers were infiltrated into discs and cured at 90°C under pressure. Polymer-infiltrated ceramics specimens were polished to 1.5 mm in thickness. Optical properties were determined with an X-rite spectrophotometer. Biaxial flexural strength and Vickers indentation tests were performed using an Instron universal mechanical tester. Vickers hardness and indentation fracture toughness values were calculated by measuring the indent dimensions under FESEM, in addition to microstructure assessment. Statistical analyses were performed using computer software, Microsoft Excel 2016 and JMP Pro 15. RESULTS: This study revealed that the type of zirconia powder utilized for the fabrication of porous ceramics for polymer-infiltration structures did not significantly influence their optical properties. Mean values of fully sintered zirconia showed significantly higher biaxial flexural strength (628.5-1277.4 MPa) than polymer-infiltrated groups (105.4-433.6 MPa), with P-3Y1150 achieving the highest value. Higher pre-sintering temperature from 1000 ℃ to 1150 ℃ led to enhanced biaxial flexural strength for polymer-infiltrated pure zirconia specimens, with values rising from 126.5-158.2 MPa to 243.4-433.6 MPa. Adding porcelain and porogens did not significantly affect the optical or specific mechanical properties, such as biaxial flexural strength and Vickers hardness, despite increasing the sintering temperature to 1300 ℃. Nevertheless, a significant increase in indentation fracture toughness was noted with ZPTKPEG1200 (7.65±0.55 MPa·m1/2) and ZPTKPEG1300 (7.09±0.61 MPa·m1/2), values that were markedly higher than those in all control groups of fully sintered zirconia (p<0.001). Sintering temperature was found to be a key determinant in influencing the ceramic matrix's microstructure, porosity, and density, as well as the biaxial flexural strength, Vickers hardness, and indentation fracture toughness of polymer-infiltrated zirconia. While changes in temperature did not affect optical properties, and polymer infiltration did not enhance all attributes, it did substantially elevate the indentation fracture toughness in mixed zirconia samples with additives, offering a potential area for further research. CONCLUSION: The mechanical properties of polymer-infiltrated ceramics responded significantly to the sintering temperature and the type of zirconia powder utilized, most notably in the 3Y-TZSB-E group. A notable increased indentation fracture toughness was discernible when Zpex powder, mixed with additives, was subject to polymer infiltration and sintered at temperatures between 1200-1300 °C. Even though polymer infiltration and additive incorporation did not uniformly enhance all properties, a noticeable improvement in fracture toughness was observed. These findings open the door to future research, especially in potential applications of dental restorative materials that demand superior fracture toughness.

Submitted by Luciana Ferreira (lucgeral@gmail.com) on 2014-08-12T13:22:56Z No. of bitstreams: 1 dissertacao andreia assis carvalho.pdf: 1800077 bytes, checksum: 9621151283f1dec9c48115c5ac9df906 (MD5) / Made available in DSpace on 2014-08-12T13:22:56Z (GMT). No. of bitstreams: 1 dissertacao andreia assis carvalho.pdf: 1800077 bytes, checksum: 9621151283f1dec9c48115c5ac9df906 (MD5) Previous issue date: 2010-02-18 / The use of composite resin (CR) in dental restorations is a common practice, however, in the oral environment, these polymers are subject to hygroscopic and hydrolytic effects, and strength of occlusion and mastication. This study aimed to evaluate in vitro the influence of different light sources, energy densities and polymerization techniques on sorption, solubility and biaxial flexural strength (RFB) of an RC. 240 specimens were fabricated (2mm x 8 MMO) RC (Esthet-X), shade A2. Two groups were obtained, depending on the instrument used: halogen lamp and light emitting diodes (LED) and subdivided according to the energy density (16 J/cm2 and 20 J/cm2), polymerization (conventional pulse I stopped and interrupted pulse II) and type of permeant (water and ethanol 75%). The methodology for the development of sorption and solubility test was based on ISO 4049:2000. Then the specimens were tested for RFB (ASTM F 394-78). We used ANOVA and Tukey test for parametric data and Kruskal-Wallis and Mann-Whitney test for data nãoparamétricos (? = 0.05). It was observed that in general there was no statistically significant differences when comparing the sources of light and the polymerization techniques (p&gt; 0.05). Energy density of 16 J/cm2 and pulse interrupted technique II was possible to observe that the LED generated higher values of sorption and solubility of the halogen light and, in the conventional technique, lower RFB (p&gt; 0.05 ). The ethanol produced higher values of sorption and solubility, and lower RFB compared with water. In general, light sources, energy densities and polymerization techniques did not influence the values of sorption, solubility and RFB / O uso de resina composta (RC) em restaurações odontológicas são uma prática frequente, entretanto, no meio bucal, esses polímeros estão sujeitos a efeitos higroscópicos e hidrolíticos, além de forçaa da oclusão e mastigação. Este trabalho teve como objetivo avaliar, in vitro, a influência de diferentes fontes de luz, densidades de energia e técnicas de polimerização na sorção, solubilidade e resistência flexural biaxial (RFB) de uma RC. Foram confeccionados 240 espécimes (2mm x 8 mmØ) de RC (Esthet-X), cor A2. Dois grupos foram obtidos, em função do aparelho utilizado: lâmpada halógena e luz emitida por diodo (LED); e subdivididos de acordo com a densidade de energia (16 J/cm2 e 20 J/cm2), técnica de polimerização (convencional, pulso interrompido I e pulso interrompido II) e tipo de permeante (água deionizada e etanol 75%). A metodologia utilizada para o desenvolvimento do teste de sorção e solubilidade foi baseada na ISO 4049:2000. Em seguida, os espécimes foram testados quanto à RFB (ASTM F 394-78). Foram utilizados os testes ANOVA e Tukey para os dados paramâtricos e os testes Kruskal-Wallis e Mann-Whitney para os dados não paramétricos ( =0,05). Foi observado que, em geral, não houve diferenças estatisticamente significantes quando comparados as fontes de luz e as técnicas de polimerização (p&gt;0,05). Na densidade de energia de 16 J/cm2 e na técnica por pulso interrompido II foi possível observar que o LED gerou maiores valores de sorção e solubilidade do que a lâmpada halógena e, na técnica convencional, menores valores de RFB (p&gt;0,05). O etanol gerou maiores valores de sorção e solubilidade, e menores de RFB quando comparado com a água. Em geral, as fontes de luz, densidades de energia e técnicas de polimerização não influenciaram nos valores de soção, solubilidade e RFB

Syfte  Syftet med föreliggande studie var att undersöka hur böjhållfastheten på zirkonia påverkas av värmebehandling, ytbehandlingar vid re-cementering och långtidsförvaring i cirka två år. Material och metod I en tidigare studie av A.Cervenka och H. Ekdahl (7) designades 30 stycken zirkoniahättor, med måtten 6 mm i tjocklek och 14 mm i ⌀(Z-CAD, HTL, Metoxit), i ett CAD-program (3shape) och frästes (DATORN 5).  Zirkoniahättorna delades in i tre grupper med tio provkroppar i varje grupp, beroende på ytbehandling: kontrollgrupp (C), sandblästring med aluminiumoxid (A) och skrapning (S). Zirkoniahättorna cementerades på titandistanser. Grupp S och grupp A utsattes för värmebehandling, för att kunna lossa hättorna från titandistanserna. Överskottet av cement avlägsnades genom två olika ytbehandlingar innan recementering (A respektive S). Samtliga grupper termocyklades i 5000 cykler (5° till 55°) innan de utsattes för ett draghållfasthetstest. När föreliggande studie genomfördes hade zirkoniahättorna förvarats torrt i rumstemperatur i cirka två år. Zirkoniahättornas underdel slipades ner till 2,9 mm i tjocklek i en slipmaskin (Phoneix 4000) för att tillverka provkroppar lämpade för utförande av ett biaxialt böjhållfasthetstest. Resultaten analyserades med One-way ANOVA, Tukey’s test med en signifikansnivå på α =0,05.   Resultat Det biaxiala böjhållfasthetstestet påvisade att grupp C hade högst medelvärde och S hade lägst medelvärde. Det fanns inte någon signifikant skillnad mellan grupperna, p&gt;0,05.  Slutsats Inom ramen för föreliggande studie kan följande slutsats dras:  Böjhållfastheten på zirkoniahättor som har långtidsförvarats i cirka två år påverkas inte av tidigare genomförd värmebehandling och olika ytbehandlingar vid recementering / Purpose The purpose of the present study was to investigate how the flexural strength of zirconia is affected by heat treatment, various surface treatments during re-cementation, and long term storage for about two years. Material and method In a previous study by A.Cervenka and H. Ekdahl (7), 30 zirconia copings, measuring 6 mm in thickness and 14 mm in ⌀ (Z-CAD, HTL, Metoxit), were designed in a CAD-program (3shape) and milled (DATORN 5). Zirconia copings were divided into three groups with ten specimens in each group, depending on different surface treatment: control group (C), aluminum oxide abrasion group (A) and scraping (S). Zirconia copings were cemented on titanium abutments. Group S and group A were subjected to heat treatment in order to be able to detach the zirconia copings from titanium abutments. The excess cement was removed by two various surface treatments before the recementation (A respective S). All groups were thermocycled for 5000 cycles (5 ° to 55 °) before being subjected to a tensile strength test. At the time of the present study zirconia copings had been stored dry at room temperature for about two years. The lower part of the zirconia copings was reduced to 2.9 mm in thickness using a grinding machine (Phoneix 4000)in order to produce specimens suitable to performe a biaxial flexural strength test. The results were analyzed with One-way ANOVA, Tukey's test with a significance level of α = 0.05.. Results The biaxial flexural strength test showed that group C had the highest mean and S had the lowest mean. There was no significant difference between the groups, p&gt; 0.05.  Conclusion Within the limitations of this study, the following conclusion can be drawn: The flexural strength of zirconia copings that have been stored for about two years is not affected by previously heat treatment performed during recementation and various surface treatments during recementation.

Indiana University-Purdue University Indianapolis (IUPUI) / Background: Numerous studies have reported the use of hydrofluoric (HF) acid as one of the most effective methods for the achievement of a durable bond between glass-based ceramics and resin cements. Nevertheless, there is little information available regarding the potential deleterious effect on the ceramic mechanical strength. Objectives: (1) to investigate the effect of HF acid etching regimens on the biaxial flexural strength of a low-fusing nanofluorapatite glass-ceramic (IPS e.max ZirPress, Ivoclar Vivadent), (2) to study the ability of an unfilled resin (UR) to restore the initial (i.e., before etching) mechanical strength, and (3) to evaluate the effect of HF acid etching on the ceramic surface morphology before and after UR treatment via scanning electron microscopy (SEM). Methods: One hundred and forty-four disc-shaped (15 ± 1 mm in diameter and 0.8 ± 0.1 mm in thickness) IPS e.max ZirPress specimens were allocated into 12 groups, as follows: G1-control (no etching), G2-30 s, G3-60 s, G4-90 s, G5-120 s, G6- 60 + 60 s. Meanwhile, groups (G7- G12) were treated in the same fashion as G1-G6, but followed by silane and UR applications. Surface morphology evaluation of non-etched and etched IPS e.max ZirPress (G1-G12) was carried out by scanning electron microscopy (SEM). The flexural strength was determined by biaxial testing as described in ISO 6872. Statistics were performed using two-way ANOVA and the Sidak multiple comparisons (α = 0.05). In addition, the Weibull statistics were estimated. Results: A significant effect of etching time (p=0.0290) on biaxial flexural strength was observed. Indeed, G4 led to a significantly (p=0.0392) higher flexural strength than G1. Correspondingly, G10 revealed a considerably higher flexural strength than G7 (p=0.0392). Furthermore, biaxial flexural strength was significantly higher for G7 – G12 than for G1 – G6 (p<0.0001). For G1 – G6, G4 showed the highest Weibull characteristic strength while the lowest Weibull characteristic strength was seen in G6. In G7 – G12, the highest Weibull characteristic strength was presented in G10 whereas G7 had the lowest. Finally, the SEM data revealed that the HF acid etching affected the surface of IPS e.max ZirPress by generating pores and irregularities and more importantly that the UR was able to penetrate into the ceramic microstructure. Conclusion: Within the limitations of this study, HF acid etching time did not show a damaging effect on the biaxial flexural strength of the IPS e.max ZirPress ceramic. Moreover, the ceramic biaxial flexural strength could be enhanced after UR treatment.

Indiana University-Purdue University Indianapolis (IUPUI)

O presente estudo teve como objetivo avaliar as propriedades de dois compósitos convencionais [Charisma Diamond (CD) e Filtek Z250XT (FZ250XT)] e dois do tipo Bulk Fill [Aura Bulk Fill, (ABF) e Filtek Bulk Fill (FBF)] em função da profundidade de polimerização e modo de obtenção (O) dos espécimes submetidos ou não a tratamento térmico (TT, 170?C x 10 min)) e um protocolo de envelhecimento acelerado (C, 150000 ciclos, 14,7 N). Para a obtenção dos corpos de prova em forma de disco (10 mm diâmetro e 1 mm espessura) utilizou-se dois tipos de molde de poliéster (segmentado e não segmentado). Foram fotoativados (1000 mW/cm2 X 20 s) nas espessuras de 2 mm (convencionais) e 5 mm (Bulk Fill.). As propriedades avaliadas foram: Grau de conversão (GC), dureza (KHN) e resistência à flexão biaxial (RFB). A análise estatística do GC % para as resinas convencionais mostrou diferença no fator Condição (imediato 58,8 %, sem TT 24h 66,3 %, com TT 83,8 %), na interação Marca X Tratamento Térmico a CD com TT (88,1 %) > FZ250XT (79,6 %) mas nas outras condições foi semelhante. Quanto às resinas do tipo Bulk, a FBF (73,5 %) > ABF (71,8 %), o GC em função da profundidade diminuiu, os primeiros dois milímetros foram semelhantes 1 mm (77,0 %), 2 mm (77,4 %) > 3 mm ( 72,1 %) e 4 mm (70,8 %), semelhantes entre si, e o 5 mm obteve o menor GC (66,2 %). Comparado o 5 mm, a ABF (61,1 %) < FBF (71,4 %). No fator Condição o GC aumenta em 24 h (70,2 %) comparada com o imediato (61,7 %) e com o tratamento térmico aumenta ainda mais (86,2 %). Com o tratamento térmico, a FBF foi a que obteve o maior aumento (88,4 %), ABF (84,1 %), mas as duas sem tratamento térmico não apresentaram diferença significante ABF (69,9 %), FBF (70,5 %). Os valores de KHN tanto para as resinas convencionais como para as reinas do tipo Bulk Fill variaram em função da marca; resinas convencionais FZ250XT (64,8 KHN) > CD (50,8 KHN) e resinas do tipo Bulk Fill FBF (47,2 KHN) > ABF (33,1 KHN); em função da Forma de Obtenção, resinas convencionais Bloco-topo (61,7 KHN) < Fatia-topo (67,3 KHN), Bloco-base (54,0 KHN) > Fatia-base (48,2 KHN), e as resinas do tipo Bulk Fill Bloco-topo (44,5 KHN) < Fatia-topo (48,1 KHN), Bloco-base (38,0 KHN) > Fatia-base (29,9 KHN); e em função do Tratamento Térmico, resinas convencionais com TT (54,15 KHN) > sem TT (53,23 KHN) e resinas do tipo Bulk Fill com TT (44,4 KHN) > sem TT (35,9 KHN). Quanto à RFB, o fator Forma de Obtenção apresentou diferenças significativas para as quatro resinas; o Tratamento térmico aumentou à RFB nas 4 resinas estudadas, a porcentagem de aumento foi de 16,1 % para a resina CD, de 4,7 % para a FZ250XT, de 14,1 % para a ABF e de 28,3 % para a FBF. Com base nos resultados obtidos, pode-se concluir que: maior grau de conversão conduziu à maior resistência à flexão; O tratamento térmico conduziu a um aumento de todas as propriedades estudadas. A ciclagem mecânica, utilizada como protocolo de envelhecimento, permitiu a diferenciação dos materiais. / The aim of this study was to evaluate the properties of two conventional composites [Charisma Diamond (CD) e Filtek Z250XT (FZ250XT)] and two bulk fill composites Fill [Aura Bulk Fill, (ABF) e Filtek Bulk Fill (FBF)] regarding the depth of polymerization and the mode of acquisition (O) of the specimens which were submitted or not submitted to heat treatment (HT, 170 ?C x 10 min) and a protocol of accelerated aging (C, 150,000 cycles, 14.7 N). For the acquisition of the samples in disc format (10 mm in diameter and 1 mm in thickness) two different polyester molds were used (segmented and non-segmented). The samples were light cured in the thickness of 2 mm (conventional composites) and 5 mm (Bulk Fill composites). The properties evaluated were degree of conversion (DC %), hardness (KHN) and biaxial flexural strength (BFS). Statistical analyses of the DC % for the conventional composites showed differences for the factors Condition (immediate 58.8 % < without HT 24h 66.3 % < with HT 83.8 %), in the interaction Brand X Heat Treatment the group CD with HT (88.1 %) was higher than FZ250XT (79.6 %) but for all other conditions the results were similar. As for the Bulk Fill resins, the DC% for FBF (73.5 %) showed higher DC % when compared to ABF (71.8 %). The DC% in function of depth decreased: for the first two millimeters the results were similar: 1 mm (77.0 %) = 2 mm (77.4 %) > 3 mm (72.1 %) = 4 mm (70.8 %), and the 5 mm obtained the lowest DC % (66.2 %). Comparing the 5 mm level among brands, ABF (61.1 %) was lower than FBF (71.4 %). For the factor Condition the DC % increases in 24h (70.2 %) compared to immediate (61.7 %) and with the HT increases even more (86.2 %). With the HT FBF obtained the highest increase (88.4 %), ABF (84.1 %), but both without HT present no statistically significant difference: ABF (69.9 %), FBF (70.5 %). The KHN values for both the conventional composites and the bulk fill ones varied based on the brand; conventional composites: FZ250XT (64,8 KHN) > CD (50.8 KHN) and Bulk Fill resins: FBF (47,2 KHN) > ABF (33,1 KHN); for the mode of acquisition, conventional resins block-top (61.7 KHN) lower than slice-top (67.3KHN), block-base (54.0 KHN) higher than slice-base (48.2 KHN); the bulk fill resins presented the results block-top (44.5 KHN) lower than slice-top (48.1 KHN), block-base (38.0 KHN) higher than slice-base (29.9 KHN); and regarding the HT, conventional resins with HT (54.15 KHN) higher than no HT (53.23 KHN) and bulk fill resins with HT (44.4 KHN) higher than without HT (35.9 KHN). Regarding BFS the factor mean of acquisition presented statistically significant differences for the 4 composites; heat treatment increased the BFS for all resins tested. 16.1 % was the percentage of increase for the CD resin, 4.7 % for FZ250XT, 14.1 % for ABF and 28.3 % for FBF. Based on the results obtained it can be concluded that: the higher conversion rate led to higher flexural strength resistance; the heat treatment led to an increase of all properties evaluated. Mechanical cycling, used as aging protocol, permitted the differentiation of materials.

Fundação de Amparo a Pesquisa no Estado do Rio Grande do Sul / The aim of this study was to evaluate the effect of hard machining, thermal cycle for glazing and acid etching on the surface roughness and flexural strength of a leucite glass-ceramic. Additionally, it was investigated whether the roughness after machining would be influenced by the machining order and by the pair of burs employed. Six pair of burs were used to produce 144 discs by automated machining, which were divided into groups (n=24): 1) machining (M); 2) machining and heat treatment (MH); 3) machining and acid etching (MA); 4) machining, heat treatment and acid etching (MHA); 5) machining and polishing (MP); 6) machining, polishing and acid etching (MPA). The roughness after each treatment was measured using a contact profilometer. The discs were submitted to a piston-on-three ball flexure test (ISO 6872/2008). Weibull analysis was used to compare the characteristic strength (σ0) and Weibull modulus (m) of the groups. The effect of the treatments, machining order and pair of burs on the surface roughness of the specimens was analyzed. Machining reduced the σ0 when compared to polishing. The polishing protocol was able to eliminate the defects introduced by machining, which was observed by means of scanning electron microscopy. The heat treatment did not alter the roughness, but reduced the σ0 and created amorphous material on the ceramic surface, as shown by the x-ray diffraction. Acid etching increased roughness, without reduce σ0. The Weibull modulus did not differ significantly among the groups, which means that all the treatments resulted in similar defects distribution. Spearman s coefficient (rs) indicated strong and significant correlation between machining order and roughness (rsRa = -0,66; rsRz = -0,73). The roughness after machining differed significantly according to the pair of burs employed (p<0,05). Thus, hard machining and thermal cycle for glaze demonstrated a negative effect on the ceramic strength, as opposed to acid etching, which does not appear to affect the flexural strength of the material. Variability in the roughness data could be expected after machining, since the Ra and Rz values seem to be influenced by the machining order and the pair of burs employed. / O presente trabalho objetivou avaliar o efeito da usinagem de corte duro, do ciclo térmico de glazeamento e do condicionamento ácido na rugosidade superficial e na resistência flexural de uma cerâmica vítrea reforçada por leucita. Adicionalmente, buscou-se investigar se a rugosidade após usinagem seria influenciada pela ordem de usinagem e pelo par de brocas utilizado. Seis pares de brocas foram empregados na confecção de 144 discos por usinagem automatizada, os quais foram divididos nos grupos (n=24): 1) usinagem (U); 2) usinagem e tratamento térmico (UT); 3) usinagem e condicionamento ácido (UCA); 4) usinagem, tratamento térmico e condicionamento ácido (UTCA); 5) usinagem e polimento (UP); 6) usinagem, polimento e condicionamento ácido (UPCA). A rugosidade (Ra e Rz) após os tratamentos foi mensurada em perfilômetro de contato. Os discos foram submetidos ao ensaio de flexão biaxial piston-on-three ball (ISO 6872/2008). Análise de Weibull foi utilizada para comparar-se os grupos quanto à resistência característica (σ0) e ao módulo de Weibull (m). Os efeitos dos tratamentos, da ordem de usinagem e dos diferentes pares de brocas sobre a rugosidade superficial dos corpos de prova foi estudado. A usinagem reduziu a σ0, quando comparada ao grupo UP. O protocolo de polimento adotado foi capaz de eliminar os defeitos oriundos da usinagem, o que foi verificado por meio de imagens em microscopia eletrônica de varredura. O tratamento térmico não alterou a rugosidade, mas reduziu a σ0 e ocasionou a formação de material amorfo na superfície da cerâmica, como mostrado pela difração de raios-x. O condicionamento ácido aumentou a rugosidade, sem alterar a σ0. O valor de m não diferiu significativamente entre os grupos, o que significa dizer que os tratamentos aplicados na cerâmica resultaram em distribuição similar de defeitos. Coeficiente de Spearman (rs) indicou correlação forte e significativa entre ordem de usinagem e rugosidade (rsRa = -0,66; rsRz = -0,73), a qual diferiu significativamente conforme o par de broca empregado para a usinagem (p<0,05). Sendo assim, a usinagem de corte duro e o ciclo térmico usado no glazeamento demostraram efeito negativo na resistência da cerâmica, em oposição ao condicionamento ácido, o qual parece não afetar a resistência do material. Variabilidade dos dados de rugosidade pode ser esperada após usinagem, uma vez que os valores de Ra e Rz parecem ser influenciados pela ordem de usinagem e pelo par de brocas utilizado.