Strategies for potential toughening of acrylic denture bases polymerized with microwave energy

Abstract Thiourethane additives have been shown to improve properties in several dental polymer applications. The aim of this study was to verify the effect of the addition of thiourethane oligomers and acrylamide or isobornyl-based plasticizers on the physical properties of the denture base acrylic resin polymerized with microwaves. Thiourethane oligomer (TU) was synthetized and added to microwaved acrylic resin in proportions varying between 3 and 14 wt%. Separate experimental groups included the addition of dimethyl acrylamide (DMAM) and isobornyl methacrylate as plasticizers, at concentrations varying from 5 to 20 wt%. Samples were polymerized using microwave energy at 500 Watts for 3 min, deflasked at room temperature, stored in water at 37 °C for 24 h, and evaluated for: linear dimensional change, gloss, Knoop hardness, surface roughness, impact strength, yield strength, elastic modulus, toughness, yield strength, viscosity, glass transition temperature and network heterogeneity, and water sorption/solubility. Data were analyzed with ANOVA/Tukey's post-hoc test (a=5%). The addition of TU led to properties that were similar or worse than the materials to which it was not added, except for dimensional stability. The impact on properties was statistically significant for all materials above 20% addition of TU. The addition of DMAM at 5 wt% or isobornyl methacrylate at 10 wt% improved yield strength and modulus, but increased water sorption and solubility. Except for dimensional stability, the addition of thiourethane oligomers to acrylic denture base materials compromised most tested properties. The use of DMAM and isobornyl methacrylate improved properties for selected compositions.

Resumo Aditivos de tiouretano demonstraram melhorar propriedades de polímeros em diversas aplicações. O objetivo deste estudo foi verificar o efeito da adição de oligômeros de tiouretano, monômeros de acrilamida ou baseados em funcionalidade isobornil na propriedades físicas de bases de dentadura de acrílico polimerizadas em micro-ondas. O oligômero de tiouretano (TU) foi sintetizado e adicionado à resina acrílica em proporções variando de 3 a 14% em peso. Dimetil acrilamida (DMAM) e isobornil metacrilato (IBMA) foram adicionados em formulações separadas como plastificantes em concentrações variando de 5 a 20% em peso. As amostras foram polimerizadas usando energia de micro-ondas (500 Watts oor 3 min), desincluídas da mufla a temperature ambiente, armazenadas em água a 37°C por 24 h, e submetidas aos testes de: alteração dimensional linear, brilho, dureza Knoop, rugosidade superficial, resistência ao impacto, tensão normal de escoamento, módulo de elasticidade, tenacidade, viscosidade, temperatura de transição vítrea e heterogeneidade da rede polimérica, além de sorção de água e solubilidade. Os dados foram analisados com ANOVA e teste de Tukey (a=5%). A adição de TU não afetou ou diminuiu todas as propriedades, exceto pela estabilidade dimensional. O impacto nas propriedades foi estatisticamente significante para todos os materiais em concentrações acima de 20% de TU. Isso pode ser explicado por um encurtamento das cadeias e diminuição do empacotamento das cadeias lineares do PMMA. A adição de 5% de DMAM ou 10% de isobornil metacrilato melhoraram a tensão de escoamento e o módulo, mas aumentaram a sorção de água e solubilidade. Exceto pela estabilidade dimensional, a adição de oligômeros de tiouretano à bases de dentatura compostas por resina acrílica prejudicou todas a propriedades testadas. O uso de DMAM e isobornil metacrilato melhorou as propriedades para composições selecionadas.

Influence of the incorporation of triclosan methacrylate on the physical properties and antibacterial activity of resin composite

Abstract The incorporation of antimicrobials in the composites as an attempt to reduce bacterial adhesion without jeopardizing mechanical properties is a challenge for Dentistry. Objective: To evaluate the bacterial adhesion and physical properties of a composite containing the methacrylate triclosan- derivative monomer (TM). Methodology: TM was synthesized and added to an experimental composite. Samples were divided into two groups: Control and TM (13.4 wt%). Antibacterial Activity: Three specimens of each material were prepared and placed on bacterial suspensions of Streptococcus mutans for 1, 5 and 10 days. After these periods the counting of the colonies (log10) was performed. Assays was performed in triplicate. Physical Properties: Three-body Abrasion (TBA): Ten specimens of each material were prepared and stored at 37°C/24 h. The surface roughness (Ra) and hardness (KHN) were analyzed. Next, the specimens were submitted to abrasive wear (30,000 cycles) and re-evaluated for Ra and KHN; Sorption/solubility (SS): cylindrical specimens (n=10) were prepared and weighted. The specimens were immersed in deionized water for 7 days at 37°C and then their weight was verified again. SS were calculated using accepted formulas; Diametral tensile strength (DTS): specimens (n=10) underwent test performed in an Instron universal testing machine at a crosshead speed of 1 mm/min. Data were submitted to appropriate statistical tests according to data distribution and assay (p<0.05). Results: Bacterial Adhesion: TM showed a significant reduction on biofilm accumulation in the evaluated periods: 1 day (1.537±0.146); 5 days (2.183±0.138) and 10 days (4.469±0.155) when compared with Control: 1 day (4.954±0.249); 5 days (5.498±0.257) and 10 days (6.306±0.287). Physical Properties: For TBA, SS and DTS no significant difference was found between groups Control and TM. The incorporation of methacrylate triclosan-based monomer in the experimental composite reduce bacterial adhesion of S. mutans and did not affect important polymer properties.

Doxycycline-containing glass ionomer cement for arresting residual caries: an in vitro study and a pilot trial

Abstract In a previous study, we demonstrated that the incorporation of doxycycline hyclate (DOX) into resin-modified glass ionomer cement (RMGIC) inhibited important cariogenic microorganisms, without modifying its biological and mechanical characteristics. In this study, we keep focused on the effect of that experimental material as a potential therapy for arresting residual caries by analyzing other in vitro properties and conducting a pilot clinical trial assessing the in vivo effect of DOX-containing RMGIC on residual mutans streptococci after partial carious removal in primary molars. Specimens of the groups RMGIC (control); RMGIC + 1.5% DOX; RMGIC + 3% DOX; and RMGIC + 4.5% DOX were made to evaluate the effect of DOX incorporation on surface microhardness and fluoride release of RMGIC and against biofilm of Streptococcus mutans. Clinical intervention consisted of partial caries removal comparing RMGIC and RMGIC + 4.5% DOX as lining materials. After 3 months, clinical and microbiologic evaluations were performed. Data were submitted to ANOVA/Tukey or Wilcoxon/Mann-Whitney set as α=0.05. Fluoride release and surface microhardness was not influenced by the incorporation of DOX (p>0.05). There was a significant reduction of S. mutans biofilm over the material surface with the increase of DOX concentration. After clinical trial, the remaining dentin was hard and dry. Additionally, mutans streptococci were completely eliminated after 3 months of treatment with RMGIC + 4.5% DOX. The incorporation of DOX provided better antibiofilm effect, without jeopardizing fluoride release and surface microhardness of RMGIC. This combination also improved the in vivo shortterm microbiological effect of RMGIC after partial caries removal.

Biological and mechanical degradation affecting the surface properties of aesthetic restorative

To evaluate the roughness (Ra), Knoop hardness (KHN) and change of color (ΔE) of esthetic restorative materials (Filtek Z350-composite nanoparticle; Empress Direct-composite nanohybrid and IPS e.Max-ceramic) subjected to contact with the Streptococcus mutans biofilm (biological degradation) associated with abrasion generated by tooth brushing (mechanical degradation). Methods: Ten specimens of each material were prepared, and the surface properties initial were evaluated. All specimens were exposed to Streptococcus mutans inoculum; after 7 days, surface properties were evaluated. The specimens were submitted to a 30,000 toothbrushing cycles, using a toothpaste slurry, then, surface properties were evaluated again. Data were analyzed by Proc-Mixed, One-way ANOVA, Tukey-Kramer and Tukey's tests (α = 0.05). Results: At the baseline, ceramic showed the highest Ra and KHN values; after the biological degradation the composites showed increased Ra, but KHN did not change; after the mechanical degradation, Empress showed decreased Ra and Z350 showed similar Ra, the KHN increased to both composites, and all materials had increased lightness after the mechanical degradation. Conclusions: The results suggest that, when exposed to Streptococcus mutans biofilm and toothbrush abrasion, the ceramics undergoes minimal degradation and the composites exhibited variable degradation, depending on the composition of the material (AU)

Effect of Metal Primers on Bond Strength of a Composite Resin to Nickel-Chrome Metal Alloy

Abstract This study evaluated the effects of three metal primers and one multi-mode adhesive system on the shear bond strength (SBS) of a flowable composite resin to nickel-chrome metal alloy (Ni-Cr). Ninety plates were cast from Ni-Cr and divided in nine groups (n=10). The surfaces were sandblasted with Al2O3 and primed with three adhesive primers: Alloy Primer (AP), Universal Primer (TP) and RelyX Ceramic Primer (CP), and a multi-mode adhesive (Scotchbond Universal, SU). The Adper Single Bond Plus (SB) and SU adhesives were also combined with adhesive primers. Control group did not have any surface treatment. The groups were: AP, AP+SB, AP+SU, TP+SB, TP+SU, CP+SB, CP+SU and SU. Composite cylinders were built on alloy surface. After 24 h, half the specimens were subjected to SBS and the other half to thermal cycling before testing. Data were analyzed by two-way ANOVA and Tukey’s test (a=0.05). Failure modes were assessed by SEM observation. Higher SBS were obtained with AP and TP combined with adhesives at 24 h and the lowest one for control group. Thermocycling reduced SBS for AP, CP+SU and SU. Combination between TP and SU resulted in the highest SBS after the thermocycling. TP groups showed all types of failures and high incidence of mixed failures. The use of AP and UP metal primers before application of SU and SB adhesive systems increased the SBS of composite to Ni-Cr. These combinations between metal primers and adhesives had the highest SBS after thermocycling.

Resumo Este estudo avaliou os efeitos de três primers para metais e um sistema adesivo multi-mode na resistência da união por cisalhamento (SBS) de um compósito resinoso de baixa viscosidade a uma liga niquel-cromo (Ni-Cr). Noventa placas Ni-Cr foram divididas em 9 grupos (n=10). As superfícies foram jateadas com Al2O3 e condicionadas com três primers adesivos: Alloy Primer (AP), Universal Primer (TP) e Rely X Ceramic Primer (CP) e um adesivo multi-mode (Scotchbond Universal, SU). Os adesivos Adper Single Bond Plus (SB) e SU foram combinados com os primers para metais. O grupo controle não recebeu nenhum tipo de tratamento superficial. Os grupos foram: AP, AP+SB, AP+SU, TP+SB, TP+SU, CP+SB, CP+SU e SU. Cilindros de resina foram construídos na superfície da liga. Após 24 h, metade dos espécimes foi submetido ao SBS, a outra metade foi termociclada previamente. Os dados foram analisados pelos testes ANOVA dois fatores e Tukey (a=0.05). Os tipos de fraturas foram determinados utilizando microscopia eletrônica de varredura (MEV). Os maiores valores de SBS foram obtidos com AP e TP combinados com adesivos após 24 h e o menor valor foi obtido no grupo controle. A ciclagem térmica reduziu a SBS para AP, CP+SU e SU. Combinação entre TP e SU resultou em altos valores de SBS após termociclagem. Os grupos TP apresentaram todos os modos de fratura e alta incidência de fraturas mistas. O uso dos primers AP e UP para metais antes da aplicação dos sistemas adesivos SU e SB aumentou a SBS entre o Ni-Cr e a resina composta. Essa combinação entre primers e adesivos mostrou os maiores valores de SBS após a termociclagem.

Influence of chemical degradation and abrasion on surface properties of nanorestorative materials

Aim: The aim of this in vitro study was to investigate the synergistic effect of chemical degradation (erosion) and three-body abrasion (mechanical degradation) on the surface roughness (Ra) and hardness (KHN) of two nanorestorative materials and two conventional materials. Methods:Disc-shaped specimens (5 mm in diameter, 2 mm thick) of Filtek Z350TM and TPH SpectrumTM composites and Ketac NanoTM and VitremerTM light-curing glass ionomer cements, nanomaterials and conventional materials were prepared according to the manufacturer's instructions. After 24 h, polishing procedures were performed and initial measurements of Ra and KHN were taken in all specimens. The specimens were divided into 12 groups (n = 10) according to material and storage media: artificial saliva, orange juice, and Coca-Cola(r). After 30 days of storage, the specimens were submitted to mechanical degradation and re-evaluated for Ra and KHN. Data were tested for significant differences by repeated-measure three-way ANOVA and Tukey's tests (p<0.05). Results:Erosion and abrasion wear significantly decreased hardness of all materials. Only Filtek Z350 roughness, however, was not affected by erosion and abrasion. All materials showed a significant increase in surface roughness after erosion and abrasion, except for Filtek Z350. After chemical and mechanical degradation, the KHN of all samples had decreased significantly. After mechanical degradation, the acidic drinks (Coca-Cola(r) and orange juice) were more aggressive than artificial saliva to all materials. Conclusions:A synergistic effect was observed by the increase in roughness for all materials, except for Filtek Z350; hardness values decrease for all materials, regardless of whether they were nanofilled or not. The RMGICs were more susceptible to degradation than the composites, considering both hardness and roughness surface parameters.

Microtensile bond strength of indirect composite restorations using different combinations of resin-coating technique / Resistência da união por microtração de restaurações indiretas de resina, usando diferentes combinações na técnica de Resin-Coating

The aim of this study was to evaluate microtensile bond strength (μ-TBS) and failure mode of indirect composite restorations bonded to dentin using different combinations of Resin-Coating (RC) after thermal and load cycling. Thirty five extracted third molars were used in the study. Two box-like Class II cavities were prepared in each tooth (mesial and distal surface). The 70 cavities were distributed in 7 groups according to the coating materials: G1:Etch-rinse 2steps (SB2); G2:Etch-rinse 2steps/Hydrophobic-monomer (SB2/B); G3:Etch-rinse 2steps/Flowable composite resin (SB2/FL); G4:Self-etch 1step (CS3); G5:Self-etch 1step/Hydrophobic monomer (CS3/B); G6:Self-etch1step/Flowable composite resin liner (CS3/PL), G7:Self-etch 2step/Flowable composite resin liner (CSEB/PL). The cavities were molded with a vinyl polysiloxane impression material and the molds were poured with a stone plaster. The fillings were confectioned using the Sinfony composite system (3M/ESPE) and were cemented with resin luting cement (Rely X ARC system). After 24 hours, the teeth were submitted to thermocycling (2,000C/5-55°C) and load cycling (250,000C/30N). After, the restored teeth were sectioned in to beams and μ-TBS were measured. The data were analyzed with ANOVA and Tukey test (p<0.05). In addition failure mode pattern was determined by scanning electrical microscopy. Bond strength were significantly higher in the groups CSEB/PL and CS3/B (p<0.05). In the groups in which was not used a liner, the failure mode exhibited dentin exposure. The groups CSEB/PL and CS3/B showed the highest values of bond strength and the failure mode reveal CSEB/PL exhibited better performance since doesn’t present any fracture kind A.

O objetivo deste estudo foi avaliar a resistência da união, por microtração (μ-TBS), e o modo de fratura de restaurações indiretas de resina aderidas à dentina por diferentes combinações na técnica de Resin-Coating (RC), após ciclagem térmica e mecânica. Neste trabalho foram utilizados trinta e cinco terceiros molares extraídos. Em cada dente foram preparadas duas caixas Classe II (nas faces mesial e distal). As 70 cavidades foram divididas em 7 grupos, de acordo com os materiais de cobertura: G1: adesivo convencional de 2 passos (SB2); G2: adesivo convencional de 2 passos/monômero hidrófobo (SB2/B); G3: adesivo convencional de 2 passos /resina composta flow (SB2/FL); G4:adesivo auto-condicionante de 1 passo (CS3); G5: adesivo auto-condicionante de 1 passo/monômero hidrófobo (CS3/B); G6: adesivo auto-condicionante de 1 passo/resina composta flow forradora (CS3/PL), G7: adesivo auto-condicionante de 2 passos/resina composta flow forradora (CSEB/PL). As cavidades foram moldadas por materiais à base de polivinilsiloxano e os modelos foram obtidos em gesso pedra especial. As restaurações foram confeccionadas usando o sistema Sinfony de compósitos (3M/ESPE); e foram cimentadas com cimento resinoso (Rely X ARC system). Após 24 h, os dentes foram submetidos a ciclagem térmica (2.000C/ 5-55oC) e mecânica (250.000/30N). Foram então seccionadas em palitos para medidas de μ-TBS. Os dados foram analisados por ANOVA e teste Tukey (p<0,05). Além disso, os padrões de fratura foram determinados por meio de microscopia eletrônica de varredura. A resistência da união foi significativamente mais alta nos grupos CSEB/PL e CS3/B (p<0.05). Nos grupos onde não foi usado um agente forrador, os padrões de fratura exibiram exposição de dentina. Os grupos CSEB/PL and CS3/Bos maiores valores de resistência de união e o modo de fratura revelou que CSEB/PL exibiu melhor performance, considerando o fato de não apresentarem nenhuma fratura Tipo A.

Marginal adaptation of indirect restorations using different resin coating protocols

This study evaluated the influence of material combinations used in the resin coating technique (RCT) on the marginal adaptation of indirect restorations with gingival margins in enamel (EM) and cement (CM). Eighty third-molars were used. Two cavities were prepared in each tooth. The cavities were distributed into 16 groups. Cavities with EM were filled with the following material combinations: G1: Single-Bond 2 (Sb2), G2: Sb2 + Bond/Scotchbond-Multipurpose (Sb2B), G3: Sb2 + Filtek-Flow Z350 (Sb2Fl), G4: Scotchbond-Multipurpose (SBMP), G5: Clearfil-S3 (CS3), G6: CS3 + Bond/Clearfil-SE Bond (CSE3B), G7: CS3 + Protect Liner F (CS3PL) and G8: Clearfil SE Bond + Protect Liner F (CSEBPL). The same combinations were applied to the cavities in CM: G9, G10, G11, G12, G13, G14, G15, G16, respectively. The fillings were performed with the Sinfony-System (3M/ESPE). After 24 h, the teeth were submitted to thermocycling (2,000 cycles, 5° to 55°C) and load-cycling (50,000 cycles, 50 N). Next, the Caries-Detector (Kuraray) was applied to the restoration margins. Images from the proximal margin were evaluated using the Image-Tool 3.0 software. The results were submitted to ANOVA and Tukey's test (α=0.05). The mean values (%) for the groups were: EM: G1=46.68, G2=15.53, G3=19.83, G4=27.53; G5=59.49, G6=25.13, G7=34.37, G8=15.20; CM: G9=38.38, G10=23.25, G11=26.97, G12=25.85, G13=37.81, G14=30.62, G15=29.17, G16=20.31. The highest percentages of marginal gap on EM or CM were found in the groups that did not use a liner. It can be concluded that the most appropriate RCT combinations were the groups that used a liner.

Este estudo avaliou a influência de diferentes combinações de materiais usados na técnica de selamento dentinário (TSD) sobre a adaptação marginal de restaurações indiretas, cujas margens gengivais localizam-se em esmalte (ME) ou cemento (MC). Oitenta terceiros molares foram selecionados e duas cavidades foram preparadas em cada dente, as quais foram distribuídas em 16 grupos. As cavidades com margem em esmalte foram forradas pelas seguintes combinações de materiais: G1: Single-Bond2 (Sb2), G2: Sb2 + Bond/Scotchbond-Multipurpose (Sb2B), G3: Sb2 + Filtek-Flow Z350 (Sb2Fl), G4: Scotchbond-Multipurpose (SBMP), G5: Clearfil-S3 (CS3), G6: CS3 + Bond/Clearfil-SE Bond (CSE3B), G7: CS3 + Protect Liner F (CS3PL), G8: Clearfil SE Bond + Protect Liner F (CSEBPL). As mesmas combinações foram aplicadas às cavidades com margens em cemento: G9, G10, G11, G12, G13, G14, G15, G16, respectivamente. As restaurações foram confeccionadas usando o sistema Sinfony (3M/ESPE). Após 24 h, os dentes restaurados foram submetidos à ciclagem térmica (2.000 ciclos - 5° a 55° C) e mecânica (50.000 ciclos, 50 N). Em seguida, Carie-Detector (Kuraray) foi aplicado sobre as margens das restaurações. As imagens obtidas da margem proximal foram avaliadas pelo software Image-Tool 3.0. Os resultados foram submetidos aos testes estatísticos ANOVA e Tukey (p<0,05). As médias (%) observadas para os grupos foram: ME: G1=46,68, G2=15,53, G3=19,83, G4=27,53; G5=59,49, G6=25,13, G7=34,37 e G8=15,20; MC: G9=38,38, G10=23,25, G11=26,97, G12=25,85, G13=37,81, G14=30,62, G15=29,17, G16=20,31. Os maiores valores de desadaptação marginal encontrados em ME e MC foram encontrados nos grupos que não utilizaram um "liner". Desta forma, pôde-se concluir que a combinação mais apropriada para a TSD é aquela que faz uso do "liner".

Effect of thickness of indirect restoration and distance from the light-curing unit tip on the hardness of a dual-cured resin cement

This study evaluated the Knoop hardness and polymerization depth of a dual-cured resin cement, light-activated at different distances through different thicknesses of composite resin. One bovine incisor was embedded in resin and its buccal surface was flattened. Dentin was covered with PVC film where a mold (0.8-mm-thick and 5 mm diameter) was filled with cement and covered with another PVC film. Light curing (40 s) was carried out through resin discs (2, 3, 4 or 5 mm) with a halogen light positioned 0, 1, 2 or 3 mm from the resin surface. After storage, specimens were sectioned for hardness measurements (top, center, and bottom). Data were subjected to split-plot ANOVA and Tukey's test (a=0.05). The increase in resin disc thickness decreased cement hardness. The increase in the distance of the light-curing tip decreased hardness at the top region. Specimens showed the lowest hardness values at the bottom, and the highest at the center. Resin cement hardness was influenced by the thickness of the indirect restoration and by the distance between the light-curing unit tip and the resin cement surface.

O estudo avaliou a profundidade de polimerização de um cimento resinoso dual, através da dureza Knoop (KHN), ativado em diferentes distâncias e espessuras de compósito resinoso. A dentina bovina foi planificada e embutida em resina, coberta com filme de PVC, onde um molde (0,8 mm x 5 mm) sobreposto foi preenchido com cimento e coberto com outro filme de PVC. A fotoativação (40 s) foi realizada através de discos de compósito (2, 3, 4 ou 5 mm-espessura) com a luz a 0, 1, 2 ou 3 mm de distância da superfície do compósito. Após armazenagem, os espécimes foram seccionados e a KHN medida (superfície, centro e base). Os dados foram submetidos à ANOVA com parcelas subdivididas e teste de Tukey (a=0.05). A espessura do compósito diminuiu a dureza do cimento. O aumento da distância de fotoativação diminuiu a dureza na superfície do cimento. Espécimes mostraram menores valores de dureza na região de base e os maiores valores no centro. A dureza do cimento resinoso foi influenciada pela espessura da restauração indireta e pela distância entre a ponta da unidade fotoativadora e a superfície do cimento resinoso.