Nano-porous thermally sintered nano silica as novel fillers for dental composites

doi:10.1016/j.dental.2011.10.015

Dental Materials

Volume 28, Issue 2, February 2012, Pages 133-145

https://doi.org/10.1016/j.dental.2011.10.015 Get rights and content

Abstract

Objectives

The study evaluates properties of an experimental dental composite consisting of a porous thermally sintered nano-silica as filler. The properties are compared with those of an experimental composite containing micro fillers and a commercially available nano-composite, Filtek Supreme^® Translucent. Different models are used to predict the elastic modulus and strength of the composites.

Methods

Nano-silica with primary particles of 12 nm was thermally sintered to form nanoporous filer particles. The experimental composites were prepared by incorporating 70 wt.% of the fillers into a mixture of Bis-GMA and TEGDMA as matrix phase. Having added photoinitiator system the composites were inserted into the test molds and light-cured. The microfiller containing composites were also prepared using micron size glass fillers. Degree of conversion (DC%) of the composites was measured using FTIR spectroscopy. Diametral tensile strength (DTS), flexural strength, flexural modulus and fracture toughness were measured. SEM was utilized to study the cross section of the fractured specimens. The surface topography of the specimens was investigated using atomic force microscopy (AFM). The specific surface area of the sintered nano silica was measured using BET method. The data were analyzed and compared by ANOVA and Tukey HSD tests (significance level = 0.05).

Results

The results showed improvements in flexural modulus and fracture toughness of the composites containing sintered filler. AFM revealed a lower surface roughness for sintered silica containing composites. No significant difference was observed between DTS, DC%, and flexural strength of the sintered nanofiller composite and the Filtek Supreme^®. The results also showed that the modulus of the composite with sintered filler was higher than the model prediction.

Significance

The thermally sintered nano-porous silica fillers significantly enhanced the mechanical properties of dental composites introducing a new approach to develop materials with improved properties.

Introduction

Since the introduction of dental composites to dentistry, their properties have greatly been improved to overcome the shortcomings of the esthetically interesting materials. The developments in material point of view can be summarized in three categories: (i) improvement of filler phase [1], [2], [3], (ii) modification of resin monomers and/or introducing new monomer systems [4], [5], [6], [7], [8], (iii) improvement of initiator system to reach higher degree of polymerization and/or controlled curing kinetics [9], [10], [11], [12].

Developments in dental bonding agents [13], [14] and composite replacement techniques [15], [16] should also be added to the aforementioned attempts for achieved higher efficacy of the modern dental composites. Although, one may also consider some other aspects of new composites such as fluoride release capacity, radiopacity and translucency as influencing factors for clinical choices, they have little impact on the mechanical properties of the composites.

The particulate fillers which are incorporated into the resin matrix of dental composites cover a wide range of hard glassy particles from the ground quartz with the particle size of several microns to nanosized silica particles.

The incorporation of nanoparticles into the dental composites may improve some properties such as wear resistance, gloss retention [17], modulus [18], flexural strength and diametral tensile strength [19], and fracture toughness [20]. On the other hand, the large surface to volume ratio in the nanoparticles may result in the higher water uptake and resultant degradation of resin–matrix interface [21]. Other problems in the incorporation of nanoparticles into the high viscosity resin monomers are lack of good wetting of the particles and low filler loading. The problems arise from the high surface area of the nanoparticles which is in the range of several hundred m²/g. The surface charge of the nano-sized particles results in agglomerated structures which makes them very difficult to be thoroughly dispersed in the matrix phase. Lack of good dispersion of the particles leaves lots of weak points in the composite which may cause local stress concentration resulting in the failure of the restoration.

The main interaction mechanism between matrix resin and filler surface in the composites is suggested to be chemical bonding of the matrix monomers and methacrylate group of the silane coupling agent bonded onto the filler surface through condensation of the silanol functional groups of pre-hydrolyzed silane and the hydroxyl groups on the particle surface [22].

In this study, silica nanoparticles were thermally sintered in order to provide porous particles with lower surface area to increase loading capacity of the nano fillers. The surface porosity of the sintered particles also provides mechanical interlocking between the cured matrix and the filler particles. Physical and mechanical properties of the experimental composites containing the sintered nanoparticles were then compared with those of the composites prepared using conventional micron-sized glass fillers.

Section snippets

Materials

2,2′-Bis-[4-(methacryloxypropoxy)-phenyl]-propane (Bis-GMA) and triethyleneglycol dimethacrylate (TEGDMA) were supplied by Evonik (Germany). Camphorquinone (CQ), N-N′-dimethyl aminoethyl methacrylate (DMAEMA), and 3-(methacryloyloxy)propyl trimethoxy silane (γ-MPS) were obtained from Sigma–Aldrich (Germany). Amorphous fumed silica with the primary particle size of 12 nm in diameter and surface area of 200 m²/g (Aerosil^® 200) was obtained from Evonik (Germany). Glass filler (micro fillers) with

Results

Table 1 presents the composition of the experimental composites and Filtek Supreme^® Translucent (3 M, ESPE, USA). Table 2 tabulated the predicted and experimental elastic modulus of the composites applying different models.

Fig. 1 illustrates schematic representation of the sintering process of the nanosilica particles. Fig. 2 is the SEM micrographs of nano silica sintered at different temperatures. As it is seen at 1200 °C no fusion of the particles/aggregates is observed, at 1400 °C the particles

Discussion

Developing dental composites with improved physical and mechanical properties has been the goal of dental material scientists. Introducing dental composites with nano-sized fillers is believed to overcome some shortcomings of the composites. Wear resistance, gloss retention and flexural strength are among the properties which are reported to be improved using nano-technology [17]. The main problems in the composites utilizing nano-sized particles as filler are low filler loading and lack of

Conclusions

This study describes the preparation of new dental fillers with porous structure from silica nanoparticles through thermal sintering. It compares the properties of experimental composites containing this porous filler and conventional microfiller. The properties are also compared with those of a commercially available dental nanocomposite. The following conclusions are made according to the results.

A porous structure is obtained by sintering the nano silica particles at 1300 °C.

The experimental

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Nano-porous thermally sintered nano silica as novel fillers for dental composites

Abstract

Objectives

Methods

Results

Significance

Introduction

Section snippets

Materials

Results

Discussion

Conclusions

Dent Mater

Dent Mater

Acta Biomater

Dent Mater

Dent Mater

Biomaterials

Dent Mater

Dent Mater

Dent Mater

Dent Mater

Dent Mater

Dent Mater

Dent Mater

J Dent

J Am Dent Assoc

Dent Mater

Dent Mater

J Dent

Dent Mater

Compos B Eng

Int J Mech Sci

Polymer

Dent Mater