Dental materials : official publication of the Academy of Dental Materials · 2025
Evaluation of the physicochemical and adhesive properties of an etch-and-rinse adhesive system incorporated with magnesium whitlockite nanoparticles.
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Silvestre Francisbênia Alves, Andrade Neto Davino Machado, Araújo Áldrison Canafístula Rêgo, Ferreira Marcos Antonio de Albuquerque, Oliveira Diego Lomonaco Vasconcelos de, Marciano Sara Jessica, Mattos Adriano Lincoln Albuquerque, Moreira Madiana Magalhães, Feitosa Victor Pinheiro, Peixoto Raniel Fernandes
Аннотация
OBJECTIVE: To synthesize and characterize magnesium whitlockite nanoparticles (nMg-WH) to evaluate the physicochemical and adhesive properties of a conventional adhesive incorporating different concentrations of nMg-WH.
METHOD: nMg-WH were synthesized using a hydrothermal method and characterized using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and transmission electron microscopy (TEM). Six groups of adhesive systems were prepared with different concentrations of nMg-WH (wt%: 0 % [Control], 0.1 %, 0.2 %, 0.5 %, 1 %, and 2 %) to evaluate the degree of conversion (DC, %), viscosity (cP), water sorption (WS, µg/mm³), and solubility (SL, µg/mm³). Forty-eight molars (n = 8) were sectioned and randomized between groups and evaluated for contact angle (in degrees) and microshear bond strength (µSBS), before and after thermocycling (TC) involving 10,000 cycles with a 30-s immersion time at temperatures of 5 °C and 55 °C. Statistical analysis was performed using one-way ANOVA (DC, cP, WS and SL) or mixed ANOVA (µSBS), followed by Tukey's test for multiple comparisons (α = 0.05).
RESULTS: Regarding the physicochemical properties, the 0.2 % (51.3 ± 0.3), 0.5 % (49.0 ± 1.4), and 1 % (49.2 ± 1.9) nMg-WH groups showed significantly higher DC compared to the control (41.0 ± 0.2). The 0.2 % group presented the lowest contact angle (16.24 ± 7.79), indicating enhanced wettability. Viscosity increased proportionally with concentration, although 0.1 % (28.91 ± 0.75) remained comparable (p > 0.05) to the control (31.00 ± 1.08). WS and SL were not significantly affected at higher concentrations (0.5 %, 1 %, and 2 %). Before TC, the 0.1 % (32.1 ± 4.0) and 0.2 % (30.9 ± 2.1) nMg-WH groups demonstrated statistically higher (p < 0.05) µSBS values than the control (18.0 ± 5.2). After TC, concentrations of 0.2-2 % exhibited higher μSBS compared to the control, with the 0.5 % nMg-WH group showing the highest value (31.8 ± 1.0).
SIGNIFICANCE: nMg-WH improved the physicochemical properties of the adhesive system and increased adhesion to dentin, particularly at concentrations ranging from 0.2 % to 1 %.
METHOD: nMg-WH were synthesized using a hydrothermal method and characterized using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and transmission electron microscopy (TEM). Six groups of adhesive systems were prepared with different concentrations of nMg-WH (wt%: 0 % [Control], 0.1 %, 0.2 %, 0.5 %, 1 %, and 2 %) to evaluate the degree of conversion (DC, %), viscosity (cP), water sorption (WS, µg/mm³), and solubility (SL, µg/mm³). Forty-eight molars (n = 8) were sectioned and randomized between groups and evaluated for contact angle (in degrees) and microshear bond strength (µSBS), before and after thermocycling (TC) involving 10,000 cycles with a 30-s immersion time at temperatures of 5 °C and 55 °C. Statistical analysis was performed using one-way ANOVA (DC, cP, WS and SL) or mixed ANOVA (µSBS), followed by Tukey's test for multiple comparisons (α = 0.05).
RESULTS: Regarding the physicochemical properties, the 0.2 % (51.3 ± 0.3), 0.5 % (49.0 ± 1.4), and 1 % (49.2 ± 1.9) nMg-WH groups showed significantly higher DC compared to the control (41.0 ± 0.2). The 0.2 % group presented the lowest contact angle (16.24 ± 7.79), indicating enhanced wettability. Viscosity increased proportionally with concentration, although 0.1 % (28.91 ± 0.75) remained comparable (p > 0.05) to the control (31.00 ± 1.08). WS and SL were not significantly affected at higher concentrations (0.5 %, 1 %, and 2 %). Before TC, the 0.1 % (32.1 ± 4.0) and 0.2 % (30.9 ± 2.1) nMg-WH groups demonstrated statistically higher (p < 0.05) µSBS values than the control (18.0 ± 5.2). After TC, concentrations of 0.2-2 % exhibited higher μSBS compared to the control, with the 0.5 % nMg-WH group showing the highest value (31.8 ± 1.0).
SIGNIFICANCE: nMg-WH improved the physicochemical properties of the adhesive system and increased adhesion to dentin, particularly at concentrations ranging from 0.2 % to 1 %.