Enhancing Near-Infrared Photothermal Efficiency of Biocompatible Flame-Synthesized Carbon Nano-Onions with Metal Dopants and Silica Coating.

As an alternative to eliminating cancer cells with minimal impacts on the nearby tissues, biocompatible nanoparticles based on silica-coated carbon nano-onions, with outstanding photothermal efficiency, are presented. Metal-doped carbon nano-onion@SiO2 materials are produced using flame synthesis. Metal complexes are injected in the flame to tune the carbon organization levels, which results in materials with excellent photostability and total photothermal conversion efficiency, regarding the incident light input, as higher as 48% for 785 nm laser. It was found that the metal dopant, even at a very low content, plays an interesting role in photothermal efficiency. We tested the effect of thin silica layers on the carbon nanosphere, first as a way to improve biocompatibility and provide a more reactive surface toward the modifications process to add vectorizing agents. Despite the primary goal of the silica shell, a notable increase in photothermal efficiency was observed. In vivo studies of the biological response to the materials as probed by the zebrafish model found that the as-prepared carbon nanospheres and the SiO2-coated particles are highly biocompatible. The SiO2-coated samples were found to be more suitable for photothermal application, due to the higher colloidal stability and higher photothermal efficiency.

Silica coating followed by heat-treatment of MDP-primer for resin bond stability to yttria-stabilized zirconia polycrystals.

This study evaluated the influence of silica coating, primer type and its heat treatment on bond strength durability between resin cement and an yttrium-stabilized polycrystalline tetragonal zirconia (Y-TZP). Eighty (80) Y-TZP blocks were allocated into 16 groups considering four factors: silica coating (without and with); type of primer (RelyX Ceramic Primer, a silane-based primer; Single Bond Universal, a universal MDP-based primer); heat treatment of the primer (without and with); aging (without and with). After zirconia treatments, resin cement cylinders (RelyX ARC) (n = 20; N = 320) were built. Half of the samples were tested after 24 h, and another half were subjected to aging (thermocycling 5-55°C/5.000, and storage in water for 6 months). Shear bond strength test and failure analysis were performed. Bond strength data were submitted to four-way ANOVA and Tukey test (p = 0.05). All factors were statistically significant (p < 0.001) for bond strength (MPa): silica coating (7.3 ± 5.9) > no-treatment (3.6 ± 4.3); universal primer (6.7 ± 4.8) > silane (4.2 ± 5.8); heat-treatment (6.5 ± 6.3) > no-heating (4.4 ± 4.3); no-aging (8.2 ± 5) > aging (2.7 ± 4.4). Tukey test revealed that the association of silica coating + universal primer + heat-treatment promoted higher and stable resin bond strength. Silica coating, universal adhesive application and heat treatment improve/increase durability and bond strength of zirconia. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 107B: 104-111, 2019.

Can the application of multi-mode adhesive be a substitute to silicatized/silanized y-tzp ceramics?

Abstract This study evaluated the effectiveness of a multi-mode adhesive (SBU-Scotch Bond Universal/3M) as a substitute for silica coating and silane application on the bonding of zirconia ceramics to resin cement. One-hundred and twenty sintered zirconia ceramic blocks (5 x 5 x 5 mm) were obtained, finished by grounding with silicon carbide paper (#600, #800, #1000 and #1200) and randomly divided into 12 groups (n=10) in accordance with the factors "surface treatment" (ScSi - silicatization + silanization; ScSBU - silicatization + SBU; SBU - SBU without photoactivation and SBUp - SBU photoactivated) and "ceramic" (Lava / 3M ESPE, Ceramill Zirconia / Amann Girrbach and Zirkonzahn / Zirkonzahn). Dual resin cement cylinders (RelyX Ultimate/3M ESPE) were subsequently produced in the center of each block using a silicon matrix (Ø=2 mm, h=5 mm) and photoactivated for 40 s (1200 mW/cm2). The samples were stored for 30 days in distilled water (37ºC) and submitted to shear bond strength test (1 mm/min, 100 KgF). Data (MPa) were analyzed under ANOVA (2 levels) and Tukey test (5%). Complementary analyzes were also performed. ANOVA revealed that only the factor "surface treatment" was significant (p=0.0001). The ScSi treatment (14.28A) promoted statistically higher bond strength values than the other ScSBU (9.03B), SBU (8.47B) and SBUp (7.82B), which were similar to each other (Tukey). Failure analysis revealed that 100% of the failures were mixed. The silica coating followed by the silanization promoted higher bond strength values of resin cement and ceramic, regardless of the zirconia ceramic or SBU.

Resumo Este estudo avaliou a efetividade de um adesivo "multi-mode" (Single Bond Universal/3M) como um substituto para a silicatização e aplicação do silano na resistência de união das cerâmicas de zircônia e um cimento resinoso. Para isso, 120 blocos cerâmicos sinterizados de zircônia nas dimensões de (5 x 5 x 5 mm) foram obtidos, lixados com lixas de granulação decrescente (#600, #800, #1000 e #1200) e divididos aleatoriamente em 12 grupos (n = 10), de acordo com os fatores "tratamento de superfície" (ScSi - silicatização + silanização; ScSBU - silicatização + Single Bond; SBU - SBU sem fotoativação e SBUp - SBU com fotoativação) e "cerâmica" (Lava/3M ESPE, Ceramill Zircônia/ Amann Girrbach e Zirkonzahn/Zirkonzahn). Posteriormente, cilindros de cimento resinoso dual (RelyX Ultimate/3M ESPE) foram confeccionados no centro de cada bloco com auxílio de uma matriz de silicone (Ø=2 mm; h=5 mm) e fotopolimerizados por 40 s (1200 mW/ cm²). Em seguida, as amostras foram armazenadas durante trinta dias em água destilada (37 °C) e submetidas ao ensaio de resistência de união ao cisalhamento (1 mm/min, 100 kgF). Os dados (MPa) foram analisados sob ANOVA (2 fatores) e teste de Tukey (5%). Análises complementares também foram realizadas. ANOVA revelou que apenas o fator "tratamento de superfície" foi significativo (p=0,0001). O tratamento ScSi (14.28A) promoveu valores de adesão estatisticamente superiores aos demais ScSBU (9.03B), SBU (8.47B) e SBUp (7.82B), os quais foram semelhantes entre si (Tukey). A Análise de falhas revelou que 100% da falhas que ocorreram foram mistas. A silicatização seguida da silanização promoveu a melhor resistência de união entre cimento resinoso e a cerâmica, independentemente do tipo da cerâmica ou do SBU.

Mono or polycrystalline alumina-modified hybrid ceramics.

OBJECTIVES: This study evaluated the effect of addition of alumina particles (polycrystalline or monocrystalline), with or without silica coating, on the optical and mechanical properties of a porcelain. METHODS: Groups tested were: control (C), polycrystalline alumina (PA), polycrystalline alumina-silica (PAS), monocrystalline alumina (MA), monocrystalline alumina-silica (MAS). Polycrystalline alumina powder was synthesized using a polymeric precursor method; a commercially available monocrystalline alumina powder (sapphire) was acquired. Silica coating was obtained by immersing alumina powders in a tetraethylorthosilicate solution, followed by heat-treatment. Electrostatic stable suspension method was used to ensure homogenous dispersion of the alumina particles within the porcelain powder. The ceramic specimens were obtained by heat-pressing. Microstructure, translucency parameter, contrast ratio, opalescence index, porosity, biaxial flexural strength, roughness, and elastic constants were characterized. RESULTS: A better interaction between glass matrix and silica coated crystalline particles is suggested in some analyses, yet further investigation is needed to confirm it. The materials did not present significant differences in biaxial flexural strength, due to the presence of higher porosity in the groups with alumina addition. Elastic modulus was higher for MA and MAS groups. Also, these were the groups with optical qualities and roughness closer to control. The PA and PAS groups were considerably more opaque as well as rougher. SIGNIFICANCE: Porcelains with addition of monocrystalline particles presented superior esthetic qualities compared to those with polycrystalline particles. In order to eliminate the porosity in the ceramic materials investigated herein, processing parameters need to be optimized as well as different glass frites should be tested.

A critical evaluation of bond strength tests for the assessment of bonding to Y-TZP.

OBJECTIVES: To compare three different designs for measuring the bond strength between Y-TZP ceramic and a composite material, before and after ceramic surface treatment, evaluating the influence of the size of the adhesive interface for each design. METHODS: 'Macro' tensile, microtensile, 'macro' shear, microshear, 'macro' push-out, and micropush-out tests were carried out. Two Y-TZP surface treatments were evaluated: silanization (sil) and tribochemical silica coating (30µm silica-modified Al2O3 particles+silanization) (TBS). Failure mode analysis of tested samples was also performed. RESULTS: Both the surface treatment and the size of the bonded interface significantly affected the results (p=0.00). Regardless of the type of surface treatment, the microtensile and microshear tests had higher values than their equivalent "macro" tests. However, the push-out test showed the highest values for the "macro" test. The tensile tests showed the greatest variability in results. The tribochemical silica coating method significantly increased bond strength for all tests. SIGNIFICANCE: Different test designs can change the outcome for Y-TZP/cement interfaces, in terms of mean values and reliability (variability). The 'micro' tests expressed higher bond strengths than their equivalent 'macro' tests, with the exception of the push-out test (macro>micro).

Methacrylate bonding to zirconia by in situ silica nanoparticle surface deposition.

OBJECTIVE: This study introduces an innovative method to enhance adhesion of methacrylate-based cements to yttria-stabilized zirconia (Y-TZP) by means of a silica-nanoparticle deposition process. METHODS: Two alkoxide organic precursors, tetraethyl-orthosilicate (TEOS) and zirconium tert-butoxide (ZTB) were diluted in hexane at different concentrations in order to obtain several experimental materials to enhance deposition of a SiO(x) reactive layer to Y-TZP. This deposition was attained via sintering alkoxide precursors directly on pre-sintered zirconia (infiltration method­INF) or application on the surface of fully sintered zirconia (coating method­COA). Untreated specimens and a commercial tribochemical silica coating were also tested as controls and all the treated Y-TZP specimens were analyzed using SEM-EDX. Specimens were bonded using silane, adhesive and dual-cure luting cement and submitted to shear bond strength test after different water storage periods (24 h, 3-, 6- and 12-months). RESULTS: SEM-EDX revealed Y-TZP surface covered by silica nanoclusters. The morphology of silica-covered Y-TZP surfaces was influenced by sintering method, employed to deposit nanoclusters. High bond strength (MPa) was observed when using COA method; highest TEOS percentage achieved the greatest bond strengths to Y-TZP surface (36.7±6.3 at 24 h). However, bonds stability was dependent on ZTB presence (32.9±9.7 at 3 months; 32.3±7.1 at 6 months). Regarding INF method, the highest and more stable resin-zirconia bond strength was attained when using experimental solutions containing TEOS and no ZTB. Both sintering methods tested in this study were able to achieve a bonding performance similar to that of classic tribochemical strategies. SIGNIFICANCE: This study demonstrates that it is possible to achieve a reliable and long-lasting bonding between yttria-stabilized zirconia ceramic and methacrylate-based cements when using this novel, simple, and cost-effective bonding approach.

Air-particle abrasion on zirconia ceramic using different protocols: effects on biaxial flexural strength after cyclic loading, phase transformation and surface topography.

This study evaluated the effect of different air-particle abrasion protocols on the biaxial flexural strength and structural stability of zirconia ceramics. Zirconia ceramic specimens (ISO 6872) (Lava, 3M ESPE) were obtained (N=336). The specimens (N=118, n=20 per group) were randomly assigned to one of the air-abrasion protocols: Gr1: Control (as-sintered); Gr2: 50 µm Al2O3 (2.5 bar); Gr3: 50 µm Al2O3 (3.5 bar); Gr4: 110 µm Al2O3(2.5 bar); Gr5: 110 µm Al2O3 (3.5 bar); Gr6: 30 µm SiO2 (2.5 bar) (CoJet); Gr7: 30 µm SiO2(3.5 bar); Gr8: 110 µm SiO2 (2.5 bar) (Rocatec Plus); and Gr9: 110 µm SiO2 (3.5 bar) (duration: 20 s, distance: 10 mm). While half of the specimens were tested immediately, the other half was subjected to cyclic loading in water (100,000 cycles; 50 N, 4 Hz, 37 °°C) prior to biaxial flexural strength test (ISO 6872). Phase transformation (t→m), relative amount of transformed monoclinic zirconia (FM), transformed zone depth (TZD) and surface roughness were measured. Particle type (p=0.2746), pressure (p=0.5084) and cyclic loading (p=0.1610) did not influence the flexural strength. Except for the air-abraded group with 110 µm Al2O3 at 3.5 bar, all air-abrasion protocols increased the biaxial flexural strength (MPa) (Controlnon-aged: 1,030 ± 153, Controlaged: 1,138 ± 138; Experimentalnon-aged: 1,307 ± 184-1,554 ± 124; Experimentalaged: 1,308 ± 118-1,451 ± 135) in both non-aged and aged conditions, respectively. Surface roughness (Ra) was the highest with 110 µm Al2O3(0.84 µm. FM values ranged from 0% to 27.21%, higher value for the Rocatec Plus (110 µm SiO2) and 110 µm Al2O3 groups at 3.5 bar pressure. TZD ranged between 0 and 1.43 µm, with the highest values for Rocatec Plus and 110 µm Al2O3 groups at 3.5 bar pressure.

Effect of surface treatments on the bond strength of a resin cement to commercially pure titanium

Investigation of the effectiveness of surface treatments that promote a strong bond strength of resin cements to metals can contribute significantly to the longevity of metal-ceramic restorations. This study evaluated the effect of surface treatments on the shear bond strength (SBS) of a resin cement to commercially pure titanium (CP Ti). Ninety cast CP Ti discs were divided into 3 groups (n=30), which received one of the following airborne-particle abrasion conditions: (1) 50 ?m Al2O3 particles; (2) 30 ?m silica-modified Al2O3 particles (Cojet Sand); (3) 110 ?m silica-modified Al2O3 particles (Rocatec). For each airborne-particle abrasion condition, the following post-airborne-particle abrasion treatments were used (n=10): (1) none; (2) adhesive Adper Single Bond 2; (3) silane RelyX Ceramic Primer. RelyX ARC resin cement was bonded to CP Ti surfaces. All specimens were thermally cycled before being tested in shear mode. Failure mode was determined. The best association was Rocatec plus silane. All groups showed 100 percent adhesive failure. There were combinations that promote higher SBS than the protocol recommended by the manufacturer of RelyX ARC.

A investigação da eficácia de tratamentos de superfície que promovem uma forte resistência de união de cimentos resinosos aos metais pode contribuir significantemente para a longevidade das restaurações metalocerâmicas. Este estudo avaliou o efeito de tratamentos de superfície na resistência ao cisalhamento da união de um cimento resinoso ao titânio comercialmente puro (Ti cp). Noventa discos foram fundidos em Ti cp e divididos em 3 grupos (n=30), os quais receberam uma das seguintes condições de jateamento: (1) partículas de Al2O3 de 50 ?m; (2) partículas de Al2O3 modificadas por sílica de 30 ?m (Cojet Sand); (3) partículas de Al2O3 modificadas por sílica de 110 ?m (Rocatec). Para cada condição de jateamento, os seguintes tratamentos pós-jateamento foram utilizados (n=10): (1) nenhum; (2) adesivo Adper Single Bond 2; (3) silano RelyX Ceramic Primer. O cimento resinoso RelyX ARC foi aplicado à superfície do Ti cp. Todos os espécimes foram termociclados antes do ensaio de cisalhamento. O modo de fratura também foi determinado. A melhor associação foi o Rocatec mais silano. Todos os grupos apresentaram 100 por cento de falha adesiva. Houve combinações que promoveram maior resistência ao cisalhamento da união que aquela recomendada pelo fabricante do RelyX ARC.

Tratamento superficial de cerâmicas reforçadas in-ceram previamente aos procedimentos de cimentação adesiva: revisão de literatura / Superficial treatment of the reinforced in ceram ceramic before the luting procedures: literature review

Desde o início do emprego das cerâmicas em restaurações indiretas, a odontologia passou a viver uma nova realidade. Na busca pelo aperfeiçoamento desses materiais surgiram as coroas protéticas de cerâmicas reforçadas por vidro, que possuem maior resistência à fratura, porém apresentam dificuldades no condicionamento superficial prévio aos procedimentos cimentadores. Objetivando apontar um protocolo de condicionamento superficial e de cimentação adesiva deste tipo de material, o presente trabalho traz uma revisão de literatura acerca das diferentes técnicas de tratamento de superfície interna de coroas protéticas de cerâmicas reforçadas por vidro. Os principais métodos empregados e que merecem ser discutidos são os jateamentos com óxido de alumínio e partículas de sílica, bem como a palicação de ácido fluorídrico e a silanização. Atualmente, as pesquisas têm apontado para a silicatização como o meio mais eficiente para prover a retenção entre este tipo de material e o remanescente dentário, quando procedimentos de cimentação adesiva são empregados. Os cimentos que possuem monômeros fosfatados também apresentam evidências de serem mais efetivos neste tipo de cimentação e têm sido indicados com sucesso.