Swelling equilibrium of dentin adhesive polymers formed on the water–adhesive phase boundary: Experiments and micromechanical model

Misra, Anil; Ranganathan, Parthasarathy; Ye, Qiang; Singh, Viraj; Spencer, Paulette

doi:10.1016/j.actbio.2013.09.017

Cited by 21 publications

(28 citation statements)

References 90 publications

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“…Less water miscibility will cause phase separation when monomer resins are cured in the wet, oral environment [28] leading to polymerized adhesive with a range of compositions and mechanical characteristics [41]. This phase separation can inhibit the formation of a structurally integrated bond at the composite/adhesive/tooth interface[39, 40] .…”

Section: Discussionmentioning

confidence: 99%

Synthesis and evaluation of novel siloxane-methacrylate monomers used as dentin adhesives

Ge¹,

Ye²,

Song³

et al. 2014

Dental Materials

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Objectives The objectives of this study were to synthesize two new siloxane-methacrylate (SM) monomers for application in dentin adhesives and to investigate the influence of different functionality of the siloxane-containing monomers on the adhesive photopolymerization, water sorption, and mechanical properties. Materials and method Two siloxane-methacrylate monomers (SM1 and SM2) with four and eight methacrylate groups were synthesized. Dentin adhesives containing BisGMA, HEMA and the siloxane-methacrylate monomers were photo-polymerized. The experimental adhesives were compared with the control adhesive (HEMA/BisGMA 45/55 w/w) and characterized with regard to degree of conversion (DC), water miscibility of the liquid resin, water sorption and dynamic mechanical analysis (DMA). Results The experimental adhesives exhibited improved water miscibility as compared to the control. When cured in the presence of 12 wt % water to simulate the wet environment of the mouth, the SM-containing adhesives showed DC comparable to the control. The experimental adhesives showed higher rubbery modulus than the control under dry conditions. Under wet conditions, the mechanical properties of the formulations containing SM monomer with increased functionality were comparable with the control, even with more water sorption. Significance The concentration and functionality of the newly synthesized siloxane-methacrylate monomers affected the water miscibility, water sorption and mechanical properties of the adhesives. The experimental adhesives show improved water compatibility compared with the control. The mechanical properties were enhanced with an increase of the functionality of the siloxane-containing monomers. The results provide critical structure/property relationships and important information for future development of durable, versatile siloxane-containing dentin adhesives.

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Section: Discussionmentioning

confidence: 99%

Synthesis and evaluation of novel siloxane-methacrylate monomers used as dentin adhesives

Ge¹,

Ye²,

Song³

et al. 2014

Dental Materials

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“…The variation of the dissolved oxygen under in vitro and in vivo conditions may be a significant factor influencing the photopolymerization behavior of these samples. High degree of conversion of the hydrophilic-rich phase at the miscibility limit may still yield a degradable polymer or a polymer with very poor mechanical integrity due to the low cross-linking density (Misra et al 2014). Degradation of poorly polymerized hydrophilic-rich phases would result in leaching of HEMA and low-molecular-weight degradants into the surrounding tissues.…”

Section: Discussionmentioning

confidence: 99%

“…In the presence of excess moisture, dentin adhesives can undergo phase separation into hydrophobic and hydrophilic-rich phases, leading to limited infiltration of the cross-linker into the wet, demineralized dentin matrix (Spencer and Wang 2002;Toledano et al 2012). A ternary phase diagram of model dentin adhesive composed of hydrophobic bisphenol A glycerolate dimethacrylate (BisGMA), hydrophilic 2-hydroxyethyl methacrylate (HEMA), and water (Ye et al 2011) has been used to determine quantitatively water miscibility, solubility, and phase partitioning behavior of dentin adhesive (Ye et al 2013;Misra et al 2014). The composition of the model hydrophilic-rich phase was determined quantitatively, and the results indicated limited cross-linkable dimethacrylate monomer and photoinitiators in the hydrophilic-rich phase (Ye et al 2012).…”

Section: Introductionmentioning

confidence: 99%

Polymerization Behavior of Hydrophilic-Rich Phase of Dentin Adhesive

Abedin

Parthasarathy

et al. 2015

J Dent Res

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The 2-fold objectives of this study were 1) to understand whether model hydrophobic-and hydrophilic-rich phase mimics of dentin adhesive polymerize similarly and 2) to determine which factor, the dimethacrylate component, bisphenol A glycerolate dimethacrylate (BisGMA) or photoinitiator concentration, has greater influence on the polymerization of the hydrophilic-rich phase mimic. Current dentin adhesives are sensitive to moisture, as evidenced by nanoleakage in the hybrid layer and phase separation into hydrophobic-and hydrophilic-rich phases. Phase separation leads to limited availability of the cross-linkable dimethacrylate monomer and hydrophobic photoinitiators within the hydrophilic-rich phase. Model hydrophobic-rich phase was prepared as a single-phase solution by adding maximum wt% deuterium oxide (D 2 O) to HEMA/BisGMA neat resins containing 45 wt% 2-hydroxyethyl methacrylate (HEMA). Mimics of the hydrophilicrich phase were prepared similarly but using HEMA/BisGMA neat resins containing 95, 99, 99.5, and 100 wt% HEMA. The hydrophilic-rich mimics were prepared with standard or reduced photoinitiator content. The photoinitiator systems were camphorquinone (CQ)/ethyl 4-(dimethylamino)benzoate (EDMAB) with or without [3-(3, 4-dimethyl-9-oxo-9H-thioxanthen-2-yloxy)-2-hydroxypropyl]trimethylammonium chloride (QTX). The polymerization kinetics was monitored using a Fourier transform infrared spectrophotometer with a time-resolved collection mode. The hydrophobic-rich phase exhibited a significantly higher polymerization rate compared with the hydrophilic-rich phase. Postpolymerization resulting in the secondary rate maxima was observed for the hydrophilic-rich mimic. The hydrophilic-rich mimics with standard photoinitiator concentration but varying cross-linker (BisGMA) content showed postpolymerization and a substantial degree of conversion. In contrast, the corresponding formulations with reduced photoinitiator concentrations exhibited lower polymerization and inhibition/delay of postpolymerization within 2 h. Under conditions relevant to the wet, oral environment, photoinitiator content plays an important role in the polymerization of the hydrophilic-rich phase mimic. Since the hydrophilic-rich phase is primarily water and monomethacrylate monomer (e.g., HEMA as determined previously), substantial polymerization is important to limit the potential toxic response from HEMA leaching into the surrounding tissues.

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“…These ultrasonic experiments were performed for saturated samples at high frequencies (5–10 MHz). Under these high frequencies, a typically stiffer response is obtained for water‐saturated materials owing to the inability of unbound water to migrate under loading, leading to undrained conditions . Also, a dimensional analysis of their expression for elastic modulus appears to indicate some inconsistency.…”

Section: Discussionmentioning

confidence: 99%

“…Clearly, there are intrinsic merits to understanding how these components perform individually as these insights can be used to better engineer the a–d interface. In our previous study, we reported on the mechanical behavior of the dentin adhesive and the various phases it forms when polymerized in the presence of water under different loading conditions and moisture exposure . In this article, we focus upon the viscoelastic behavior of the collagen–adhesive composites, under conditions that simulate the wet functional environment found in the oral cavity.…”

Section: Introductionmentioning

confidence: 99%

Viscoelastic properties of collagen–adhesive composites under water‐saturated and dry conditions

Singh

Misra

Ranganathan

et al. 2014

J Biomedical Materials Res

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To investigate the time and rate dependent mechanical properties of collagen-adhesive composites, creep and monotonic experiments are performed under dry and wet conditions. The composites are prepared by infiltration of dentin adhesive into a demineralized bovine dentin. Experimental results show that for small stress level under dry conditions, both the composite and neat adhesive have similar behavior. On the other hand, in wet conditions, the composites are significantly soft and weak compared to the neat adhesives. The behavior in the wet condition is found to be affected by the hydrophilicity of both the adhesive and collagen. Since the adhesive-collagen composites area part of the complex construct that forms the adhesive-dentin interface, their presence will affect the overall performance of the restoration. We find that Kelvin-Voigt model with at least 4-elements is required to fit the creep compliance data, indicating that the adhesive-collagen composites are complex polymers with several characteristics time-scales whose mechanical behavior will be significantly affected by loading rates and frequencies. Such mechanical properties have not been investigated widely for these types of materials. The derived model provides an additional advantage that it can be exploited to extract other viscoelastic properties which are, generally, time consuming to obtain experimentally. The calibrated model is utilized to obtain stress relaxation function, frequency-dependent storage and loss modulus, and rate dependent elastic modulus.

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Swelling equilibrium of dentin adhesive polymers formed on the water–adhesive phase boundary: Experiments and micromechanical model

Cited by 21 publications

References 90 publications

Synthesis and evaluation of novel siloxane-methacrylate monomers used as dentin adhesives

Synthesis and evaluation of novel siloxane-methacrylate monomers used as dentin adhesives

Polymerization Behavior of Hydrophilic-Rich Phase of Dentin Adhesive

Viscoelastic properties of collagen–adhesive composites under water‐saturated and dry conditions

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