Nanostructured Glass-Ceramic Materials from Glass Waste with Antimicrobial Activity.

Modern consumption patterns have led to a surge in waste glass accumulating in municipal landfills, contributing to environmental pollution, especially in countries that do not have well-established recycling standards. While glass itself is 100% recyclable, the logistics and handling involved present significant challenges. Flint and amber-colored glass, often found in high quantities in municipal waste, can serve as valuable sources of raw materials. We propose an affordable route that requires just a thermal treatment of glass waste to obtain glass-based antimicrobial materials. The thermal treatment induces crystallized nanoregions, which are the primary factor responsible for the bactericidal effect of waste glass. As a result, coarse particles of flint waste glass that undergo thermal treatment at 720 °C show superior antimicrobial activity than amber waste glass. Glass-ceramic materials from flint waste glass, obtained by thermal treatment at 720 °C during 2 h, show antimicrobial activity against Escherichia coli after just 30 min of contact time. Laser-induced breakdown spectroscopy (LIBS) was employed to monitor the elemental composition of the glass waste. The obtained glass-ceramic material was structurally characterized by transmission electron microscopy, enabling the confirmation of the presence of nanocrystals embedded within the glass matrix.

Effect of the use of bromelain associated with bioactive glass-ceramic on dentin/adhesive interface.

OBJECTIVES: To evaluate the effect of bromelain associated with Biosilicate on the bond strength (BS) of a universal adhesive system to sound (SD) and caries-affected dentin (CAD), and on the proteolytic activity. MATERIALS AND METHODS: Cavities were prepared in 360 molars, half submitted to cariogenic challenge. Teeth were separated into groups (n=20): Control-No treatment; CHX-0.12% chlorhexidine; NaOCl-5% sodium hypochlorite; Br5%-5% bromelain; Br10%-10% bromelain; Bio-10% Biosilicate; NaOClBio-NaOCl+Bio; Br5%Bio-Br5%+Bio; Br10%Bio-Br10%+Bio. Following treatments, the adhesive system was applied, and cavities were restored. Samples were sectioned into sticks and stored at 37 °C for 24 h, 6 months, and 1 year. Microtensile BS (2-way ANOVA, Bonferroni's test, α=0.05), fracture patterns (SEM), and adhesive interfaces (TEM) were evaluated. Bacterial collagenase assay and in situ zymography were performed. RESULTS: In CAD, Br10% presented higher BS (p=0.0208) than Br5%Bio. Br5% presented higher BS (p=0.0033) after 6 months than after 24 h; and association of treatments, higher BS (p<0.05) after aging than after 24 h. Mixed fractures were the most prevalent. Association of treatments promoted a more uniform hybrid layer with embedded Bio particles. Experimental groups presented lower (p<0.0001) relative fluorescence units than Control. Bromelain, associated or not with Bio, showed collagenolytic degradation. CONCLUSIONS: Bromelain associated with Biosilicate did not affect the BS to SD. In CAD, Br5%Bio decreased immediate BS but had no long-term influence. This association decreased the proteolytic activity. CLINICAL RELEVANCE: Bromelain and Biosilicate may enhance the longevity of adhesive restorations by inhibiting endogenous proteases.

Hydrofluoric acid concentration and etching time affect differently the microstructure and surface properties of pressed lithium disilicate glass ceramics.

OBJECTIVE: To evaluate the effect of different hydrofluoric acid concentrations and etching times on the surface, chemical composition and microstructure of lithium disilicate. MATERIAL AND METHODS: Ninety specimens of pressed lithium disilicate (LDS) were obtained (IPS e.max Press, Rosetta SP and LiSi Press). The specimens of each material were divided in two groups according to the hydrofluoric acid concentration: 5% and 10% (n = 15/group), and subdivided according to the etching time: 20, 40 and 60 s (n = 5/group). Crystalline evaluations and chemical composition were performed through x-ray diffraction (XRD) and energy-dispersive x-ray spectroscopy (EDS), respectively. Microstructural analyses were performed by scanning electron microscope (SEM), surface roughness (Ra), and material thickness removal evaluation. Thickness removal and Ra data were analyzed by ANOVA and Tukey test (p < 0.05). RESULTS: XRD demonstrated characteristic peaks of lithium disilicate crystals, lithium phosphate and of a vitreous phase for all materials. EDS identified different compositions and SEM confirmed different surface responses to acid etching protocols. Material and etching time influenced Ra and material thickness removal (p < 0.05). CONCLUSION: Hydrofluoric acid concentration and etching time affect the surface characteristics of LDS differently. LiSi Press presented higher resistance to hydrofluoric acid etching compared to e.max Press and Rosetta SP. CLINICAL SIGNIFICANCE: Applying the appropriate etching protocol is pivotal to avoid excessive material removal and to prevent jeopardize the mechanical and optical properties of the material.

Effects of glass-ceramic produced by the sol-gel route in macrophages recruitment and polarization into bone tissue regeneration.

Effective bone substitute biomaterials remain an important challenge in patients with large bone defects. Glass ceramics produced by different synthesis routes may result in changes in the material physicochemical properties and consequently affect the success or failure of the bone healing response. To investigate the differences in the orchestration of the inflammatory and healing process in bone grafting and repair using different glass-ceramic routes production. Thirty male Wistar rats underwent surgical unilateral parietal defects filled with silicate glass-ceramic produced by distinct routes: BS - particulate glass-ceramic produced via the fusion/solidification route, and BG - particulate glass-ceramic produced via the sol-gel route. After 7, 14, and 21 days from biomaterial grafting, parietal bones were removed to be analyzed under H&E and Massons' Trichome staining, and immunohistochemistry for CD206, iNOS, and TGF-ß. Our findings demonstrated that the density of lymphocytes and plasma cells was significantly higher in the BS group at 45, and 7 days compared to the BG group, respectively. Furthermore, a significant increase of foreign body giant cells (FBGCs) in the BG group at day 7, compared to BS was found, demonstrating early efficient recruitment of FBGCs against sol-gel-derived glass-ceramic particulate (BS group). According to macrophage profiles, CD206+ macrophages enhanced at the final periods of both groups, being significantly higher at 45 days of BS compared to the BG group. On the other hand, the density of transformation growth factor beta (TGF-ß) positive cells on 21 days were the highest in BG, and the lowest in the BS group, demonstrating a differential synergy among groups. Noteworthy, TGF-ß+ cells were significantly higher at 21 days of BG compared to the BS group. Glass-ceramic biomaterials can act differently in the biological process of bone remodeling due to their route production, being the sol-gel route more efficient to activate M2 macrophages and specific FBGCs compared to the traditional route. Altogether, these features lead to a better understanding of the effectiveness of inflammatory response for biomaterial degradation and provide new insights for further preclinical and clinical studies involved in bone healing.

Mechanical Behavior of Repaired Monolithic Crowns: A 3D Finite Element Analysis.

This study evaluated the mechanical behavior and risk of failure of three CAD-CAM crowns repaired with different resin composites through a three-dimensional (3D) finite element analysis. Three-dimensional models of different cusp-repaired (conventional nanohybrid, bulk-fill, and flowable resin composites) crowns made of zirconia, lithium disilicate, and CAD-CAM resin composite were designed, fixed at the cervical level, and loaded in 100 N at the working cusps, including the repaired one. The models were analyzed to determine the Maximum Principal and Maximum Shear stresses (MPa). Complementary, an in vitro shear bond strength test (n = 10) was performed to calculate the risk of failure for each experimental group. The stress distribution among the models was similar when considering the same restorative material. The crown material affected the stress concentration, which was higher for the ceramic models (±9 MPa for shear stress; ±3 MPa for tensile stress) than for the CAD-CAM composite (±7 MPa for shear stress; ±2 MPa for tensile stress). The shear bond strength was higher for the repaired CAD-CAM resin composite (±17 MPa) when compared to the ceramics (below 12 MPa for all groups), while the repair materials showed similar behavior for each substrate. The stress distribution is more homogenous for repaired resin composite crowns, and a flowable direct resin composite seems suitable to repair ceramic crowns with less risk of failure.

Effect of Biosilicate® Addition on Physical-Mechanical and Biological Properties of Dental Glass Ionomer Cements.

This study investigated the influence of incorporating Biosilicate® on the physico-mechanical and biological properties of glass ionomer cement (GIC). This bioactive glass ceramic (23.75% Na2O, 23.75% CaO, 48.5% SiO2, and 4% P2O5) was incorporated by weight (5%, 10%, or 15%) into commercially available GICs (Maxxion R and Fuji IX GP). Surface characterization was made by SEM (n = 3), EDS (n = 3), and FTIR (n = 1). The setting and working (S/W time) times (n = 3) and compressive strength (CS) were analyzed (n = 10) according to ISO 9917-1:2007. The ion release (n = 6) was determined and quantified by ICP OES and by UV-Vis for Ca, Na, Al, Si, P, and F. To verify cell cytotoxicity, stem cells from the apical papilla (SCAP) were exposed to eluates (n = 3, at a ratio of 1.8 cm2/mL) and analyzed 24 h post-exposure. Antimicrobial activity against Streptococcus mutans (ATCC 25175, NCTC 10449) was analyzed by direct contact for 2 h (n = 5). The data were submitted for normality and lognormality testing. One-way ANOVA and Tukey's test were applied for the working and setting time, compressive strength, and ion release data. Data from cytotoxicity and antimicrobial activity were submitted for Kruskal-Wallis' testing and Dunn's post hoc test (α = 0.05). Among all experimental groups, only those with 5% (wt) of Biosilicate® showed better surface quality. Only M5% showed a comparable W/S time to the original material (p = 0.7254 and p = 0.5912). CS was maintained for all Maxxion R groups (p > 0.0001) and declined for Fuji IX experimental groups (p < 0.0001). The Na, Si, P, and F ions released were significantly increased for all Maxxion R and Fuji IX groups (p < 0.0001). Cytotoxicity was increased only for Maxxion R with 5% and 10% of Biosilicate®. A higher inhibition of S. mutans growth was observed for Maxxion R with 5% of Biosilicate® (less than 100 CFU/mL), followed by Maxxion R with 10% of Biosilicate® (p = 0.0053) and Maxxion R without the glass ceramic (p = 0.0093). Maxxion R and Fuji IX presented different behaviors regarding Biosilicate® incorporation. The impacts on physico-mechanical and biological properties were different depending on the GIC, but therapeutic ion release was increased for both materials.

The effect of Phytosphingosine and bioactive glass-ceramics in preventing dental enamel erosion

Abstract This study evaluated the effect of phytosphingosine (PHS) and bioactive glass-ceramic (Biosilicate) on dental enamel in terms of color alteration (ΔE), microhardness, and surface roughness when submitted to erosive challenge (EC). Sixty specimens of bovine teeth (6×6×2mm) were obtained. Initial color (Easyshade, VITA), KHN (HMV-2, Shimadzu), and Ra (SJ-201P, Mitutoyo) measurements were performed. Specimens were separated into groups according to treatments: PHS, 10% Biosilicate, PHS+10% Biosilicate, and artificial saliva (control) and submitted to EC with Coca-Cola for 2 min. This cycle was repeated 4 times daily/15 days. Between cycles, specimens remained in artificial saliva (2 h/37°C). After daily cycles, they were also stored in artificial saliva at 37ºC. Final color, microhardness, and surface roughness measurements were done. Color and KHN data were analyzed by one-way ANOVA, Tukey's test; and Ra, by 2-way ANOVA, repeated measures, and Tukey's test (p<.05). The highest ΔE occurred in Saliva+EC (p<.05). Groups treated with PHS presented lower color change than Saliva+EC (p<.05). All the groups presented mean values above the 50:50% perceptibility (50:50%PT) and acceptability (50:50%AT) thresholds, except for control that showed mean value above 50:50%PT but below 50:50%AT. Biosilicate+EC showed higher relative microhardness than Saliva+EC (p<.05), but was similar to PHS+EC and PHS+Biosilicate+EC. Final enamel surface roughness increased for all the groups (p<.05), except for the control. The Biosilicate may prevent enamel mineral loss induced by erosion better than saliva. The PHS associated or not to Biosilicate demonstrated better color stability than saliva.

Resumo Este estudo avaliou o efeito da Fitoesfingosina (PHS) e da vitrocerâmica bioativa (Biosilicato) sobre o esmalte dental em termos de alteração de cor (ΔE), microdureza (KHN) e rugosidade superficial, quando submetido a desafio erosivo (DE). Sessenta espécimes de dentes bovinos (6×6×2mm) foram obtidos. Foram realizadas leituras de cor inicial (Easyshade, VITA), microdureza (HMV-2, Shimadzu) e rugosidade superfícial (SJ-201P, Mitutoyo). Os espécimes foram separados em grupos de acordo com os tratamentos: PHS, Biosilicato a 10%, PHS+Biosilicato a 10%, e saliva artificial (controle). Em seguida, foram submetidos a DE com Coca-Cola por 2 min. Esse ciclo foi repetido 4 vezes/dia por 15 dias. Entre os ciclos, as amostras foram mantidas em saliva artificial (2 h/37°C). Após os ciclos diários, os espécimes também foram armazenados em saliva artificial a 37ºC. Foram realizadas leituras finais de cor, microdureza e rugosidade superficial. Os dados de cor e microdureza foram analisados ​​por ANOVA de uma via, teste de Tukey; e dados de rugosidade superficial, por ANOVA de duas vias, teste de Tukey (p<.05). A maior ΔE ocorreu em Saliva+DE (p<.05). Grupos tratados com PHS apresentaram menor alteração de cor do que Saliva+DE (p<.05). Biosilicate+DE demonstrou valores intermediários, similar (p>.05) aos outros grupos, exceto Saliva+DE. Todos os grupos presentaram média acima dos limites 50:50% de perceptibilidade (50:50%LP) e aceitabilidade (50:50%LA) exceto o controle que demonstrou média acima do 50:50%LA mas abaixo do 50:50%LP. Biosilicate+DE mostrou maior microdureza realativa do que Saliva+DE (p<.05), mas similar a PHS+DE e PHS+Biosilicato+DE. A rugosidade de superfície do esmalte aumentou para todos os grupos, exceto para o controle que presentou a menor alteração (p<.05). O Biosilicato apode prevenir perda mineral do esmalte indizido pela erosão melhor que a saliva. O PHS associado ou não ao Biosilicato demonstrou melhor estabilidade de cor que a saliva.

Incorporation of bioactive glass-ceramic into coconut oil for remineralization of incipient carious lesions

Abstract This study evaluated the efficacy of incorporating different concentrations of bioactive glass-ceramic (Biosilicate) into coconut oil on the remineralizing potential and surface roughness of white spot lesions. Fragments (6 x 6 x 2mm) of bovine teeth were sectioned and initial microhardness (KHN) and surface roughness (Ra) readings were obtained. The samples were submitted to cariogenic challenge to form white spot lesions and were separated into six groups (n=13): 1) Artificial Saliva (AS); 2) Coconut Oil (CO); 3) CO+2% Biosilicate (CO+2%Bio); 4) CO+5% Biosilicate (CO+5%Bio); 5) 2% Biosilicate Suspension (2% Bio) and 6) 5% Biosilicate Suspension (5% Bio). The treatments for 1 cycle/day were: immersion into the treatments for 5 minutes, rinsing in distilled water, and storage in artificial saliva at 37ºC. After 14 days, KHN and Ra readings were taken. The surface roughness alteration ((Ra) was analyzed (Kruskal-Wallis, Dunn's post-test, p<0.05). CO+2%Bio had higher (p = 0.0013) (Ra followed by CO+5%Bio (p = 0.0244) than AS. The relative KHN and remineralization potential were analyzed (ANOVA, Tukey, p<0.05), and 5% Bio treatment presented a higher relative microhardness than all other groups (p>0.05). The remineralizing potential of all the treatments was similar (p > .05). When Biosilicate was added, the pH of the suspensions increased and the alkaline pH remained during the analysis. Biosilicate suspension is more efficient than the incorporation of particles into coconut oil at white spot lesion treatment. In addition to the benefits that coconut oil and Biosilicate present separately, their association can enhance the remineralizing potential of Biosilicate.

Resumo Este estudo avaliou a eficácia da incorporação de diferentes concentrações de vitrocerâmica bioativa (biosilicato) ao óleo de coco no potencial remineralizante e na rugosidade superficial de lesões de manchas brancas. Fragmentos (6 x 6 x 2mm) de dentes bovinos foram seccionados e as leituras iniciais de microdureza (KHN) e rugosidade superficial (Ra) foram obtidas. As amostras foram submetidas ao desafio cariogênico para formação de lesões de manchas brancas e foram separadas em seis grupos (n=13): 1) Saliva Artificial (AS); 2) Óleo de Coco (CO); 3) CO+2% Biosilicato (CO+2%Bio); 4) CO+5% Biosilicato (CO+5%Bio); 5) Suspensão de Biosilicato 2% (2% Bio) e 6) Suspensão de Biosilicato 5% (5% Bio). Os tratamentos de 1 ciclo/dia foram: imersão nos tratamentos por 5 minutos, enxágue em água destilada e armazenamento em saliva artificial a 37ºC. Após 14 dias, foram feitas as leituras de KHN e Ra. A alteração da rugosidade superficial ((Ra) foi analisada (Kruskal-Wallis, pós-teste de Dunn, p<0,05). CO+2%Bio apresentou maior (p = 0,0013) (Ra seguido de CO+5%Bio (p = 0,0244) do que AS. O KHN relativo e o potencial de remineralização foram analisados (ANOVA, Tukey, p<0,05), e o tratamento 5% Bio apresentou uma microdureza relativa maior do que todos os outros grupos (p>0,05). A suspensão de biosilicato é mais eficiente que a incorporação de partículas ao óleo de coco no tratamento de lesões de mancha branca. Além dos benefícios que o óleo de coco e o Biosilicato apresentam separadamente, sua associação pode amplificar o potencial remineralizante do Biosilicato.

Influence of surface treatment and ageing on the bond strength of resin cement to hybrid and glass-ceramic CAD/CAM materials.

The influence of different surface treatments and ageing on the shear bond strength (SBS) of computer-aided design/computer-aided manufacturing (CAD/CAM) materials is still contentious. Therefore, this study evaluated the effect of surface treatments and ageing on the SBS of resin cement to polymer-infiltrated ceramic network (PICN) and zirconia-reinforced lithium silicate (ZLS) CAD/CAM materials. Specimens of PICN (n=10) and ZLS (n=10) were submitted to four surface treatment groups: 1) 5% hydrofluoric acid etching (HF) + silanisation (SI); 2) Air abrasion (AB)+HF+SI; 3) HF + universal adhesive (UA); 4) AB+HF+SI+UA. The treated specimens were bonded with resin cement cylinders and tested in SBS after 24 h and one year of water storage. Data were assessed by "analysis of variance" (ANOVA) and Tukey test (α=0.05) and failure modes were classified. No significant differences were observed among treatments at each evaluation time (p>0.05). SBS decreased after one year of storage, except for PICN treated with HF+UA (p=0.068). Air-abraded groups displayed a lower SBS reduction for ZLS. PICN and ZLS exhibited predominantly adhesive and mixed failures, but at one year, PICN cohesive failures increased. In conclusion, HF+UA is an effective surface treatment for PICN, while the combination AB+HF+SI+UA was more appropriate for ZLS. The water storage for one year reduced the SBS for most groups.

Super Broadband at Telecom Wavelengths From RE3+-Doped SiO2-Ta2O5 Glass Ceramics Planar Waveguides.

This paper reports on the preparation of Er3+/Yb3+/Tm3+, Er3+/Yb3+/Nd3+, and Er3+/Tm3+/Nd3+ triply doped and Er3+-doped SiO2-Ta2O5 glass ceramic nanocomposites and active planar waveguides by the sol-gel process using the dip-coating technique as deposition method. The investigation of their structural, morphological, and luminescent properties using XRD, AFM, and photoluminescence analysis, are reported here. The XRD results showed the presence of L-Ta2O5 nanocrystals dispersed in the SiO2-based amorphous host for all the nanocomposites and films. The rare earth ion (RE3+) doping concentration affected both the crystallinity, and the crystallite sizes of the Ta2O5 dispersed into SiO2-Ta2O5 nanocomposites and waveguides. AFM characterization revealed crack free and smooth surface roughness and differences in viscoelasticity on the Er3+-doped SiO2-Ta2O5 films surface, which allows the identification of Ta2O5 nanocrystals on the SiO2 amorphous host. The Er3+ doped and triply doped SiO2-Ta2O5 nanocomposites displayed broad- and super broadband NIR emissions with a FWHM up to 173 nm achieved in the telecom wavelengths. The lifetime of the 4I13/2 emitting level of the Er3+-doped SiO2-Ta2O5 waveguides is strongly dependent on Er3+ concentration and an emission quenching was negligible up to 0.81 mol%. The structural and luminescent investigations indicated that RE3+-doped SiO2-Ta2O5 glass ceramics are promising candidates for photonic applications in optical devices operating in wide wavelengths at the telecom bands.

Dissolution, bioactivity behavior, and cytotoxicity of 19.58Li2 O·11.10ZrO2 ·69.32SiO2 glass-ceramic.

Glass and bioactive glass-ceramic can be used in several applications. In bone growth where good bone/biomaterial adhesion was required, bioactive coatings for implants can improve bone formation. The glass and glass-ceramics of the LZS (Li2 O-ZrO2 -SiO2 ) system are very interesting because of their mechanical, electrical, and thermal properties. Very recently, their biological response in contact with human osteoblast has been evaluated. However, despite several initiatives, there are still no studies that systematically assess this system's bioactivity, dissolution, and cytotoxicity in vitro. This work aims to investigate the dissolution, bioactivity behavior, and cytotoxicity of LZS glass-ceramic. LZS glass-ceramics were produced from SiO2 , Li2 CO3, and ZrSiO4 by melting followed by quenching. The obtained glass frits were milled and uniaxially pressed and heat-treated at 800 and 900°C and submitted to physical-chemical, structural and mechanical characterization. Their dissolution behavior was studied in Tris-HCl, while bioactivity was performed in simulated solution body fluid (SBF). The cytotoxicity test was performed using glass-ceramic in direct contact with mesenchymal stem/stromal cells (SC) isolated from human exfoliated deciduous teeth. Structural and microstructural analyzes confirmed bioactivity. The results show that it was possible to produce bioactive glass-ceramic from LZS, proven by the formation of new calcium phosphate structures such as hydroxyapatite on the surface of the samples after exposure to SBF. The SC viability test performed indicated that the materials were not cytotoxic at 0.25, 0.5, and 1.0 mg/ml. The glass-ceramic system under study is very promising for a medicinal application that requires bioactivity and/or biocompatibility for bone regeneration.

Efecto de los Tratamientos de Calcinación y Pirólisis sobre la Estructura de Aluminosilicatos de Litio Dopadas con CuO / Effect of the Treatments of Calcination and Pyrolysis on the Structure of Aluminosilicate of Lithium Doped with CuO / Efeito dos Tratamentos de Calcinação e Pirólise na Estrutura de Aluminosilicatos de Lítio Dopadas com CUO

Resumen Introducción: Este artículo reporta la síntesis y caracterización de polvos vitrocerámicos del sistema Li2OAl2O3SiO2 (LAS), dopados con 0.5% y 1 % p/p de óxido de cobre (CuO), como una primera etapa pensando en su posterior evaluación como material termoluminiscente (TL) y su posible aplicación como dosímetro TL. Objetivo: Evaluar el efecto de los tratamientos de calcinación y pirolisis de los geles secos de aluminosilicatos de litio dopados con CuO, obtenidos mediante síntesis Sol-Gel. Materiales y Métodos: Las matrices puras y dopadas con CuO se obtuvieron mediante la verificación de formiatos de aluminio y litio, en presencia de tetraetoxisilano y CuO. Los geles obtenidos se secaron a 120 °C y 2,5 h. La mitad de la cantidad obtenida se sometió a un tratamiento de calcinación (480 °C, 5 h) mientras que la otra mitad se sometió a un proceso de pirolisis (atmósfera de nitrógeno) a 480 °C por 5 h. Las muestras obtenidas se caracterizaron por microscopía electrónica de barrido (SEM), espectroscopia infrarroja (FTIR), potencial zeta y difracción de rayos X (DRX). Resultados: mediante el análisis SEM se confirmó el tamaño de partícula micrométrica, de los espectros se observan algunas bandas prominentes entre Si-O u Al-O, además se asume que los tratamientos térmicos fueron adecuados para la liberación de grupos remanentes orgánicos. Conclusiones: La síntesis implementada permitió la obtención de partículas micrométricas (φp < 25 μm). Los tratamientos térmicos tuvieron un efecto significativo sobre la funcionalización superficial de las partículas obtenidas, y la composición del material y se verificó que la temperatura empleada fue adecuada para la liberación de remanentes orgánicos, además con los espectros se observó los grupos remanentes funcionales que estaban presentes en el material.

Abstract Introduction. This article reports the synthesis and characterization of the glass-ceramic powders of the Li2OAl2O3SiO2 (LAS) system, doped with 0.5% and 1% w / w copper oxide (CuO), as a first stage thinking about its subsequent evaluation as a thermoluminescent material (TL) and its possible application as a TL dosimeter. Objective. To evaluate the effect of the calcination and pyrolysis treatments of the dry gels of lithium aluminosilicates doped with CuO, obtained by Sol - Gel synthesis. Materials and Methods. The pure and doped CuO LAS matrices were obtained by the gelation of lithium aluminum formats, in the presence of tetraethoxysilane and CuO. The gels obtained were dried at 120 ° C and 2.5 h. Half of the amount obtained was subjected to a calcination treatment (480 °C, 5 h) while the other half was subjected to a pyrolysis process (nitrogen atmosphere) at 480 °C for 5 h. The samples obtained were characterized by scanning electron microscopy (SEM), infrared spectroscopy (FTIR), zeta potential and X-ray diffraction (XRD). Results. By means of the SEM analysis the micrometric particle size was confirmed, from the spectra some prominent bands are observed between Si-O or Al-O, besides it is assumed that the thermal treatments were suitable for the release of organic rebasing groups. Conclusions. The synthesis implemented allowed the obtaining of micrometric particles (φp < 25 μm). The thermal treatments had a significant effect on the superficial functionalization of the particles obtained, and the composition of the material and it was verified that the temperature used was adequate for the release of organic reagents, in addition with the spectra we observed the functional rebar groups that were present in the material.

Resumo Introdução: Este artigo relata a síntese e caracterização dos pós vitrocerâmicos do sistema Li2OAl2O3SiO2 (LAS), dopado com 0,5% e 1% p / p de óxido de cobre (CuO), como uma primeira etapa, pensando em sua posterior avaliação como material termoluminescente (TL). e sua possível aplicação como um dosímetro TL. Objetivo: Avaliar o efeito dos tratamentos de calcinação e pirólise de géis secos de aluminosilicato. Materiais e Métodos: As matrizes CuO LAS puras e dopadas foram obtidas pela gelificação de formatos de alumínio e lítio, na presença de tetraetoxisilano e CuO. Os géis obtidos foram secos a 120 ° C e 2,5 h. Metade da quantidade obtida foi submetida a um tratamento de calcinação (480 °C, 5 h) enquanto a outra metade foi submetida a um processo de pirólise (atmosfera de nitrogênio) a 480 °C por 5 h. As amostras obtidas foram caracterizadas por microscopia eletrônica de varredura (MEV), espectroscopia na região do infravermelho (FTIR), potencial zeta e difração de raios X (DRX). Resultados. por meio da análise de MEV, foi confirmado o tamanho micrométrico das partículas, observando-se, a partir dos espectros, algumas bandas proeminentes entre Si-O ou Al-O, além de se considerar que os tratamentos térmicos foram adequados para a liberação de grupos orgânicos de rebasing. Conclusões: A síntese implementada permitiu a obtenção de partículas micrométricas (φp < 25 μm). Os tratamentos térmicos tiveram um efeito significativo sobre a funcionalização superficial das partículas obtidas, e a composição do material e verificou-se que a temperatura utilizada foi adequada para a liberação de reagentes orgânicos, além dos espectros observamos os grupos funcionais de vergalhões que estavam presentes no material.

Optimizing the microstructure of a new machinable bioactive glass-ceramic.

OBJECTIVES: This study aimed to optimize the crystallization process and the microstructure of a new bioactive glass-ceramic (GC) previously developed by our research group to obtain machinable glass-ceramics. METHODS: Differential scanning calorimetry (DSC) analyses were conducted to explore the characteristic temperatures and construct a semi-quantitative nucleation curve. The GC specimens were characterized by X-ray diffraction (XRD) and Rietveld refinement. Their brittleness index (B) and machinability were characterized and compared with IPS e.max-CAD®. Their Young's modulus, fracture toughness, and hardness were assessed. RESULTS: We found that the maximum crystal nucleation rate temperature of this GC is ~470 °C. Treatments were designed based on the 1st DSC peak onset (570 °C), 1st peak offset (650 °C), and 2nd peak offset (705 °C) crystallization temperatures of lithium metasilicate (LS, LiSi2O3) and lithium disilicate (LS2, Li2Si2O5). Rietveld refinement indicated an increase in LS2 and a reduction in LS and amorphous phase for increased temperatures and longer treatment times. Their B values indicate good machinability compared with that of the control group based on statistical analyses. As expected, lower levels of LS2 increase the machinability regardless of the rotation speed adopted, leading to a greater depth of cut and reduced Edge Chipping Damage Depth (ECDD). CONCLUSION: This bioactive GC with optimized microstructure presents high machinability. For treatment temperatures above 570 °C, the number of elongated LS2 crystals increases and decreases the amorphous phase content, which reduce the machinability of the GC, and should therefore be avoided. The best results were obtained using heat treatment at 570 °C, which produces LS crystals embedded in a glassy matrix (67%) with small contents of secondary phases.

Polifluoruro de amonio como alternativa de acondicionamiento para laminados ultradelgados de disilicato de litio. Reporte de caso / Ammonium polyfluoride as an alternative for the surface conditioning of ultrathin lithium disilicate veneers. A case report

RESUMEN: Los laminados vitrocerámicos ultradelgados constituyen una alternativa conservadora para la resolución de alteraciones estéticas. Sin embargo, su acondicionamiento con ácido fluorhídrico suele no estar exento de complicaciones, por lo que el uso de un sistema autograbante en base a polifluoruro de amonio (Monobond Etch&Prime, MEP) permite disminuir el riesgo de sobregrabado, simplificando la técnica. El presente reporte presenta el seguimiento a dieciocho meses de un caso clínico resuelto mediante laminados vitrocerámicos acondicionados únicamente con MEP. Caso. Paciente joven con alteraciones estéticas en el sector anterosuperior. Se realizaron preparaciones conservadoras para la confección de laminados ultradelgados en disilicato de litio (e.maxPress). Las vitrocerámicas fueron acondicionadas sólo con MEP y se cementaron con Variolink Esthetic LC. Al año y medio las restauraciones se observaron indemnes, manteniendo un buen ajuste marginal y ausencia de tinciones. Conclusiones. MEP aparece como una alternativa prometedora para reemplazar al ácido fluorhídrico en la cementación de laminados vitrocerámicos.

ABSTRACT: Ultrathin glass-ceramic veneers are a conservative approach for the restorative treatment of aesthetic disorders in the anterior region. However, surface conditioning with hydrofluoric acid of the thin structures can be usually a challenging step. Therefore, the use of a self-etching ceramic primer containing ammonium polyfluoride (Monobond Etch&Prime, MEP) offers a simplified technique with a reduced risk of overetching. Here we present an 18-month follow-up of ultrathin glass-ceramic veneers conditioned with MEP only. Case. Young female patient with an aesthetic disorder in the front region. The four upper incisors were conservatively prepared for ultrathin lithium disilicate (e.maxPress) veneers. Pre-treatment of the glass-ceramics consisted only of MEP application, followed by adhesive cementation with Variolink Esthetic LC. At the 1.5-year recall, the restorations appeared undamaged, with no marginal gap or staining. Conclusions. MEP constitutes a promising alternative to hydrofluoric acid for the adhesive cementation of glass-ceramic veneers.

New sol-gel-derived magnetic bioactive glass-ceramics containing superparamagnetic hematite nanocrystals for hyperthermia application.

Although the three main phases of iron oxide - hematite, maghemite, and magnetite - exhibit superparamagnetic properties at the nanoscale, only maghemite and magnetite phases have been explored in magnetic bioactive glass-ceramics aimed at applications in cancer treatment by hyperthermia. In this work, it is reported for the first time the superparamagnetic properties of hematite nanocrystals grown in a 58S bioactive glass matrix derived from sol-gel synthesis. The glass-ceramics are based on the (100-x)(58SiO2-33CaO-9P2O5)-xFe2O3 system (x = 10, 20 and 30 wt%). A thermal treatment leads to the growth of hematite (α-Fe2O3) nanocrystals, conferring superparamagnetic properties to the glass-ceramics, which is enough to produce heat under an external alternating magnetic field. Besides, the crystallization does not inhibit materials bioactivity, evidenced by the formation of calcium phosphate onto the glass-ceramic surface upon soaking in simulated body fluid. Moreover, their cytotoxicity is similar to other magnetic bioactive glass-ceramics reported in the literature. Finally, these results suggest that hematite nanocrystals' superparamagnetic properties may be explored in multifunctional glass-ceramics applied in bone cancer treatment by hyperthermia allied to bone regeneration.

Transparent Glasses and Glass-Ceramics in the Ternary System TeO2-Nb2O5-PbF2.

Transparent fluorotellurite glasses were prepared by melt-quenching in the ternary system TeO2-Nb2O5-PbF2. The synthesis conditions were adjusted to minimize fluorine loss monitored as HF release. It was found that 10 mol% of Nb2O5 is the optimum content for PbF2 incorporation up to 35 mol% in the tellurite matrix without loss of glass forming ability. Such glass compositions exhibit a wide optical window from 380 nm to about 6 µm. Crystallization properties were carefully investigated by thermal analysis and compositions with higher PbF2 contents exhibit preferential precipitation of lead oxyfluoride Pb2OF2 at lower temperatures. The lead oxyfluoride crystallization mechanism is also governed by a volume nucleation, barely reported in tellurite glasses. Eu3+ doping of these glass compositions also promotes a more efficient nucleation step under suitable heat-treatments, resulting in transparent Eu3+-doped glass-ceramics whereas undoped glass-ceramics are translucent. Finally, Eu3+ spectroscopy pointed out a progressive, more symmetric surrounding around the rare earth ions with increasing PbF2 contents as well as higher quantum efficiencies. These new fluorotellurite glass compositions are promising as luminescent hosts working in the middle infrared.

Bioglass-based scaffolds coated with silver nanoparticles: Synthesis, processing and antimicrobial activity.

Over the past few years, several tridimensional synthetic bone grafts, known as scaffolds, are being developed to overcome the autologous grafts limitations. Among the materials used on the production of scaffolds, the 45S5 bioglass stands out due to its capacity of bonding to hard and soft tissues. Silver nanoparticles are well-known for their antimicrobial properties and their incorporation on the scaffold may promote its antimicrobial response, avoiding microorganism proliferation on the materials surface. This study proposes a simple way to coat 45S5 bioglass-based scaffolds with silver nanoparticles. The scaffolds were obtained by the sponge replication technique and the silver nanoparticles were incorporated by soaking under ultrasonic stirring. The antimicrobial activity of the scaffolds was analyzed against three different microbial strains: S. aureus, P. aeruginosa, and C. albicans. Due to the heat treatment during the scaffold production, the bioglass crystalized mainly in a sodium calcium silicate phase, forming a glass-ceramic scaffold. The silver nanoparticles were coated in a well-distributed manner throughout the scaffold, while avoiding their aggregation. The coated scaffold inhibited the growth of all the analyzed microorganism. Therefore, the use of ultrasonic stirring to coat the bioglass scaffold with silver nanoparticles showed to be an efficient way to promote its antimicrobial response.

Effect of repeated firings and staining on the mechanical behavior and composition of lithium disilicate.

OBJECTIVE: To evaluate the composition, flexural strength and fatigue behaviour of lithium disilicate ceramic (LD) after repeated firings and different staining techniques. METHODS: LD discs were fabricated and divided according to number of firing cycles and staining technique: CO - control, discs were crystallized (850°C/10min); SC - single-step characterization - crystallization and staining (applied with a thin brush) were performed in a single step with one firing cycle (850°C/10min); and DC - double-step characterization - crystallization firing cycle was performed first (850°C/10min), followed by staining firing cycle (770°C/90s). Specimens were fired two, four or six times (one crystallization firing cycle and one, three or five staining firing cycles), resulting into 9 groups (n=30): COII, COIV, COVI, SCII, SCIV, SCVI, DCII, DCIV and DCVI. The composition of the specimens was investigated (EDS, XRD, Raman spectroscopy), and the biaxial flexural strength (n=10) and staircase tests (n=20, 5×104 cycles, 5Hz) were performed. Data were subjected to one-way ANOVA and Tukey's test (α=0.05). RESULTS: EDS and XRD revealed amorphous content for stained groups. Biaxial flexural strength was not affected by repeated firings in any group, but stained groups presented lower flexural strength than control groups (p=0.001). The fatigue limit results decreased in all groups compared to flexural strength. SC groups showed similar (SCII and SCIV) or even higher fatigue limits (SCVI) than the control groups, and DC showed the lowest fatigue limit values. SEM and Raman suggested that the interfaces between staining and the LD showed only an overlap for the DC groups, whereas for the SC it was suggested an interaction between the stain and the LD. SIGNIFICANCE: Repeated firings did not result in decreased lithium disilicate flexural strength.Staining affected flexural strength and also resulted in increased amorphous content in the characterized specimens. Single-step staining resulted in the highest fatigue limit.

Different bonding agents effect on adhesive bond strength: lithium disilicate glass ceramic / Efeito de diferentes agentes de união na cimentação adesiva em superfície cerâmica de dissilicato de lítio

Introduction: The silanization of the ceramic surface prior to applying the adhesive and/or resinous materials plays an important role in bond strength. Nowadays, a new family of adhesive systems has been introduced into the market, aiming to simplify the technique of adhesive procedures during cementation. Objective: To investigate the effectiveness of different bonding agents containing silane and primer on Lithium Disilicate Glass Ceramic (LD) surface by shear bond strength tests. Material and method: 130 LD ceramic blocks were included in acrylic resin, polished and washed in ultrasound for 10 minutes. The specimens were divided into 2 groups according to surface treatment: Polished Surface (PS); Hydrofluoric Acid 9.5% - 20s (HF). Each group was divided into 5 subgroups (n = 13) according to bonding agent type: metallic primer containing MDP (ZPrimePlus, Bisco Inc); two traditional silanes (MonobondPlus, IvoclarVivadent / Porcelain Prime, Bisco Inc.); mixture of silane and resin (Kerr Silane, Kerr); mixture of silane and universal adhesive (Single-bond Universal, 3M Espe). The specimens were mounted in a standard device for shear testing (UltradentBonding Assembly), cemented with dual resin cement (RelyX UltimateTM, 3M Espe.) and photo-polymerized for 20s. The samples were tested after 24 hours and 3 months of storage in distilled water at ±36 °C. The data were analyzed by 3-Way Anova and Tukey's test (α = 5%). Result: Shear bond strength (SBS) was significantly influenced by surface treatment, bonding agent used and storage (p <0.001). Conclusion: Adequate adhesive bond strength to Lithium Disilicate Glass Ceramic can be obtained with traditional silanes, combined with HF acid pretreatment surface.

Introdução: A silanização da superfície cerâmica antes da aplicação do adesivo e/ou materiais resinosos desempenha um papel importante na resistência adesiva. Atualmente, uma nova família de sistemas adesivos foi introduzida no mercado, visando simplificar a técnica dos procedimentos adesivos durante a cimentação. Objetivo: Investigar a eficácia de diferentes soluções contendo silano e primer na superfície de cerâmicas de Dissilicato de Lítio (DLT) por meio de testes de resistência adesiva por cisalhamento. Material e método: 130 blocos cerâmicos DLT foram incluídos em resina acrílica, polidos e lavados em ultra-som por 10 minutos. Os espécimes foram divididos em 2 grupos de acordo com tratamento de superfície: Superfície Polida (PS); Ácido Hidro-Fluorídrico 9,5% - 20s (HF). Cada grupo foi dividido em 5 sub-grupos (n = 13) de acordo com o tipo de primer/silano: primer metálico contendo MDP (ZprimePlus, Bisco Inc); dois silanos tradicionais (MonobondPlus, IvoclarVivadent / Porcelain Prime, Bisco Inc.); mistura de silano e resina (Kerr Silane, Kerr); mistura de silano e adesivo universal (Single-bond Universal, 3M Espe). Os espécimes foram montados em um dispositivo padrão (UltradentBonding Assembly) para teste de cisalhamento Bisco Shear Bond Tester), cimentados com cimento resinoso dual (RelyX UltimateTM, 3M Espe.) e foto-polimerizados por 20s. O teste foi realizado após o período de: 24 horas e 3 meses de armazenamento em água destilada à ±36 °C. Os dados foram analisados por 3-Way Anova e Teste de Tukey (α=5%). Resultado: A resistência adesiva ao cisalhamento (SBS) foi significativamente influenciada pelo tipo de tratamento da superfície, pelo tipo de agente de união utilizado e pelo armazenamento (p<0,001). Conclusão: Adequada resistência adesiva pode ser obtida com silanos tradicionais, combinados com o pré-tratamento de superfície com ácido HF.

The progressive wear and abrasiveness of novel graded glass/zirconia materials relative to their dental ceramic counterparts.

OBJECTIVE: To investigate the wear behavior of novel graded glass/zirconia materials and their abrasiveness to the antagonist relative to homogeneous zirconias (polished or glazed) and a glass-ceramic. METHODS: Graded glass/zirconia specimens were prepared by sintering with concurrent glass-infiltration of pre-sintered zirconia (3Y-TZP) with a polished or as-machined surface. Monolithic zirconia samples were sintered and their surfaces were polished or glazed (as-machined). Glass-ceramic samples were obtained and the surface polished. All specimens were subjected to chewing simulations with a steatite antagonist (r = 3 mm) and a cyclic load of 50 N. Quantitative measurements of wear and roughness were performed on ceramics and antagonists for prescribed number of cycles. Damage sustained in ceramics and antagonists was analyzed by SEM. RESULTS: The polished zirconia presented little to no variation in wear depth (2 µm) and roughness (0.06 µm). Graded and glazed zirconia experienced a rapid increase in wear depth while the superficial glass layer was present (until 1000 cycles), but showed little variations afterwards - at 450k cycles ∼15 µm for graded and 78 µm for glazed zirconia. The glass-ceramic presented the greatest wear depth (463 µm) and roughness (1.48 µm). Polished zirconia, polished graded zirconia and glazed zirconia yielded significantly lower volumetric wear (∼3 mm3) of the antagonist than as-machined graded zirconia and glass-ceramic (∼5 mm3). SIGNIFICANCE: Polished graded zirconia and polished zirconia presented little wear and roughness, as well as yielded reduced antagonist wear. Glassy materials are both more susceptible to wear and more abrasive to the antagonist relative to zirconia.