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< Vol. 13 Issue 4 | Oct-Dec 2015 | pp. e301 - e388

Roughness and microhardness of composites after different bleaching techniques

Abstract

Background

The aim of this study was to evaluate the roughness and microhardness of SonicFill™ (Kerr), and compare it with Filtek™ Supreme XTE (3M ESPE) after 2 bleaching regimens.

 Methods

Sixty cylindrical specimens (10 × 2 mm) of each of the 2 composites were prepared and divided into 6 groups (n = 20): groups 1, 2: no treatment; groups 3, 4: 10% carbamide peroxide (CP); and groups 5, 6: 35% hydrogen peroxide (HP) plus LED. After treatments, specimens were thermocycled (500 cycles, 5°C/55°C, dwell time 30 minutes). A mechanical roughness tester was employed to measure the surface roughness parameters and the Vickers test to measure microhardness. One-way ANOVA, Tukey and Bonferroni methods with a significance level of 5% were used for the statistical analysis.

 Results

For SonicFill™, there was no statistically significant difference in microhardness between the control group (no. 1) and the bleached groups (nos. 3, 5), but there was difference between CP and HP treatments; for Filtek™ Supreme XTE, there was no significant difference in microhardness among all groups. There was no significant difference in average roughness (Ra) and the root mean square of the roughness (Rq) among all groups. The mean roughness depth (Rz) parameter showed no statistically significant differences among all groups for SonicFill™, but in Filtek™ Supreme XTE, there was a significant increase between control and bleaching treatments; roughness skewness (Rsk) showed no statistically significant differences among all groups for SonicFill™ and Filtek™ Supreme XTE, except for nos. 2 and 4, where the Rsk increased with CP.

 Conclusions

The microhardness of Filtek™ Supreme XTE is less affected by bleaching than that of SonicFill™. Both bleaching treatments affect Rz in Filtek™ Supreme XTE in contrast to SonicFill™, but only the CP treatment affects the Rsk of Filtek™ Supreme XTE, with no significant effect of SonicFill™.

J Appl Biomater Funct Mater 2015; 13(4): e381 - e388

Article Type: ORIGINAL RESEARCH ARTICLE

DOI:10.5301/jabfm.5000239

OPEN ACCESS ARTICLE

Authors

Andreia Leal, Anabela Paula, Amílcar Ramalho, Miguel Esteves, Manuel Marques Ferreira, Eunice Carrilho

Article History

  • • Accepted on 30/04/2015
  • • Available online on 27/11/2015
  • • Published online on 18/12/2015

Disclosures

Financial support: No financial support was received for this study. The authors wish to thank 3M ESPE, KERR and Meodental, who provided material for this study.
Conflict of interest: The authors do not have any financial interest in the companies whose materials are included in this article.

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Introduction

The use of bleaching agents to improve the appearance of natural dentition has become a popular procedure since their introduction by Haywood and Heymann (1).

Currently, bleaching agents are based primarily on hydrogen peroxide (HP) or its compounds, such as carbamide peroxide (CP) (2-3-4-5). Bleaching agents provide bleaching of tooth structure through decomposition of peroxides into unstable free radicals (6, 7). These radicals further break down into large pigmented molecules through either an oxidation or a reduction reaction. The oxidation/reduction process changes the chemical structure of interacting organic substances of the tooth, which results in color change (8-9-10).

Tooth whitening treatment was classified by the American Dental Association into 4 categories: professionally applied (in the dental office), dentist-prescribed/dispensed (patient home use), consumer purchased/over-the-counter (applied by patients) and other nondental options (2).

In-office bleaching materials contain high HP concentrations (typically 15%-38%), while the HP content in at-home bleaching products usually ranges from 3% to 10% (2). In general, most in-office and dentist-prescribed at-home bleaching techniques have been shown to be effective, although results may vary depending on factors such as type of stain, age of patient, concentration of the active agent and treatment time and frequency (2). However, the application of bleaching agents can affect human teeth and restorative materials (3, 11, 12).

Many studies have examined the changes caused by bleaching in the properties of composite resins, a material commonly used for aesthetic dental treatments, such as color, surface hardness and roughness, staining susceptibility, microleakage and elution (11).

Hardness is defined as the resistance of a material to indentation or penetration (13). Surface hardness is one of the most important physical characteristics of dental materials (14, 15). Since hardness is related to a materials’ strength, proportional limit and ability to abrade or to be abraded by opposite dental structures/materials, any chemical softening resulting from bleaching may have implications for the clinical durability of restorations (16).

Furthermore, surface roughness is also considered an important property of dental materials (17-18-19) and an important factor in aesthetic appearance (15). Materials with roughened surfaces enhance bacterial adhesion, having a smaller free surface energy (18). In addition to promoting plaque adherence, roughened materials also suffer from increased staining (18).

Controversial results about the effects of bleaching on the surface roughness and microhardness of resin composite have been reported in the literature (3, 10, 12, 16, 18, 20-21-22-23-24-25-26-27-28-29-30-31-32-33-34-35-36-37-38-39-40-41-42-43).

The resin composite SonicFill™ (Kerr Corp., Orange, CA, USA) was recently introduced onto the market. It is indicated for use as bulk fill in posterior composite restorations and can be bulk filled in layers up to 5 mm in depth due to reduced polymerization shrinkage. SonicFill™ incorporates a highly filled proprietary resin with special modifiers that react to sonic energy. As sonic energy is applied through the handpiece, the modifier causes the viscosity to drop (up to 87%), increasing the flowability of the composite and enabling quick placement and precise adaptation to the cavity walls. When the sonic energy is stopped, the composite returns to a more viscous, nonslumping state that is perfect for carving and contouring (44).

The aim of the current study was to investigate the effect of 35% HP and 10% CP on the surface roughness and microhardness of this recent resin composite, SonicFill™, and compare it with a nanofilled composite, Filtek™ Supreme XTE (3M ESPE, St. Paul, MN, USA).

Method and materials

Specimen preparation

One hundred and twenty composite disks were prepared with 10 × 2 mm (diameter/thickness), using an acrylic mould (41). A color corresponding to shade A3 was used for each material. The resin composite (Tab. I) was inserted in only 1 increment. Each surface was covered with a glass slab to allow flushing of the excess material and to obtain a smooth upper surface of the sample (20, 23, 25, 32). Specimens were then photopolymerized with a halogen light polymerizing unit (Bluephase®; Ivoclar Vivadent AG, Schaan, Liechtenstein) with light intensity of 1,500 mW/cm2 ± 10% using 40 seconds for nanofilled composite and 20 seconds for nanohybrid, in accordance with the manufacturer’s instructions. The curing light intensity was verified with a radiometer (Bluephase® meter; Ivoclar Vivadent, Schaan, Liechtenstein). All specimens were stored in artificial saliva at 37°C for 24 hours to ensure complete polymerization (31).

Resin composites used in this study

Resin composite Nanofilled composite Nanohybrid composite
Data are from (45-47).
Product name, manufacturer Filtek™ Supreme XTE, 3M ESPE, St. Paul, MN, USA SonicFill™, Kerr Corp., Orange, CA, USA
Main composition Silane-treated ceramic, silane-treated silica, diurethane dimethacrylate (UDMA), bisphenol A polyethylene glycol diether dimethacrylate, bisphenol A diglycidyl ether dimethacrylate (BISGMA), silane-treated zirconia, polyethylene glycol dimethacrylate, triethylene glycol dimethacrylate (TEGDMA), 2,6-di-tert-butyl-p-cresol (BHT) Glass, oxide, chemicals, 3-trimethoxysilylpropyl methacrylate, silicon dioxide, ethoxylated bisphenol A dimethacrylate, bisphenol A bis (2-hydroxy-3-methacryloxypropyl) ether, triethyleneglycoldimethacrylate
Loads Size 4-20 nm Not available from manufacturer
% by weight 78.5% 83.5%
% by volume 63.3% Not available from manufacturer
Lot no. N422474; N443370; N339166 N440317; N422474; N443370; N337197

The composite disks were polished with polishing disks (Super-Snap Rainbow® Technique Kit; Shofu Inc., Kyoto, Japan) in descending order of granulation. Each polishing step was performed on a slow-speed handpiece in accordance with the manufacturer’s instructions. After polishing, the specimens were stored in artificial saliva at 37°C for 24 hours. The composition of the artificial saliva, used in this study, was potassium chloride 20.1 mmol/L; sodium hydrocarbonate 17.9 mmol/L; sodium dihydrogen phosphate 3.6 mmol/L; potassium thiocyanate 5.1 mmol/L; lactic acid 0.10 mmol/L and distilled water (48).

Exposure to the superficial treatment

The specimens were then randomly divided into 6 groups (n = 20), as shown in Table II. Groups 1 and 2: specimens were stored in artificial saliva at 37°C for 14 days and served as control. Saliva was changed daily. Groups 3 and 4: specimens were treated with CP at 10% for 8 hours per day during 14 days. Each day after the active treatment period, the specimens were rinsed with distilled water for 1 minute to remove the bleaching agent, and stored in artificial saliva. During the test period, the specimens were kept at 37°C. Groups 5 and 6: specimens were treated with HP at 35%, for 15 minutes, in a progressive program. First of all, PowerPrep+™ was applied for 3 minutes on the surface of specimens according to the manufacturer’s recommendations. After this period, specimens were rinsed with distilled water and dried with an air jet. The procedure followed was to apply HP at 35% on the surface of specimens. Bleaching agent was activated by a light-emitting diode (LED) lamp (White+™ lamp; Meodental, Prime Dental Manufacturing, Chicago, IL, USA). The bleaching treatment was conducted after 14 days of storage in artificial saliva at 37°C. After the active treatment period, the specimens were rinsed with distilled water for 1 minute to remove the bleaching agent and stored in artificial saliva at 37°C.

Summary of control and experimental groups: bleaching systems on tested resin composites

Bleaching system Composite
Nanohybrid composite Nanofilled composite
Control (artificial saliva) Group 1 n = 20 Group 2 n = 20
Opalescence® Group 3 n = 20 Group 4 n = 20
White+™ Group 5 n = 20 Group 6 n = 20

Twenty-four hours after the end of the treatments, specimens went through 500 cycles of thermocycling between 5°C and 55°C with a dwell time of 30 seconds. The compositions of the bleaching agents used are described in Table III.

Bleaching agents evaluated in this study

Bleaching agent Type Composition Manufacturer Lot no.
Opalescence® Home bleaching system 10% carbamide peroxide, glycerine, water, xylitol, carbomer, PEG-300, sodium hydroxide, potassium nitrate, EDTA, sodium fluoride. Ultradent, South Jordan, UT, USA 474339
White+™ Bleaching product Office bleaching system 35% hydrogen peroxide, water, polyethylene glycol, fumed silica, thickener, potassium nitrate, sodium fluoride, sodium hydroxide, dye, mineral Dead Sea salt. Meodental, Prime Dental Manufacturing, Chicago, IL, USA 2012-5786
PowerPrep+™ Distilled water, citric acid, potassium nitrate, fumed silica, pigments.

Surface roughness analysis

The specimens were taken from the artificial saliva 24 hours after the end of the treatments. These procedures having been followed, specimens were rinsed with distilled water, dried with an air jet and observed for directionality marks on the surface, a consequence of polishing, in an optical microscope.

Roughness measurements were performed according the DIN EN ISO 4288 standard. The roughness parameters evaluated were arithmetic mean roughness (Ra), root mean square roughness (Rq), mean roughness depth (Rz) and roughness skewness (Rsk). The analysis of roughness was linear. The measuring apparatus was a mechanical roughness tester (Mitutoyo Surftest- SJ-500/P Series 178; Mitutoyo).

In each sample, 5 measurements were performed, evenly distributed along the surface and perpendicular to the previous 1 to minimize the influence of directionality.

Microhardness surface analysis

The hardness measurements were performed after the roughness analysis for each sample specifically to eliminate the influence of the Vickers indentations.

The measuring apparatus was a Struers Duramin-2 microhardness tester, and the measurements were performed according to the Standard Test Method for Micro-indentation Hardness of Material (ASTM WK27978, 2010). For the surface microhardness measurements a load of 0.2 kilogram-force (kgf; or 1.962 N) was applied for 40 seconds.

All samples were subject to 7 measurements, uniformly distributed, mainly to assure low dispersion hardness values.

Analysis of variance

One-way analysis of variance (ANOVA; 1 factor) was applied to the recorded data for comparison purposes. Two methods were used, Tukey and Bonferroni, suited for multiple comparisons between same groups. In every analysis a confidence interval of 95% was considered.

Results

Figures 1 to 5 present the values of the roughness parameters evaluated, microhardness and standard deviation for all tested groups.

Arithmetic mean roughness (Ra).

Roughness measurements

When the data obtained from this study were subjected to statistical analysis, using 1-way ANOVA, Tukey and Bonferroni methods with a significance level of 5%, it was observed that there was no significant difference in Ra and Rq among all groups tested (p>0.05) (Figs. 1 and 2)

Root mean square roughness (Rq).

The Rz parameter showed no statistically significant differences among all groups for SonicFill™. However, for Filtek™ Supreme XTE, there was a significant increase between control and bleaching treatments (Fig. 3).

Mean roughness depth (RZ). *p<0.05.

The Rsk showed no statistically significant differences among all groups for SonicFill™. In the case of Filtek™ Supreme XTE, there was a statistically significant difference between the control group (group 2) and the group submitted to CP at 10% (group 4), where the Rskincreased with CP at 10% (Fig. 4).

Roughness skewness (Rsk). *p<0.05.

Microhardness measurements

For SonicFill™, there was no statistically significant difference in microhardness between the control group (group 1) and the bleached groups (groups 3 and 5), but there was a difference between CP and HP treatments. However, for Filtek™ Supreme XTE, there was no significant difference in microhardness among all groups (Fig. 5).

Mean Vickers hardness values. *p<0.05.

Discussion

Currently, dentistry is experiencing a trend of increasing demand from patients for superior aesthetic restorations (32). Very often in daily clinical practice, tooth colored restorations exist in teeth that are planned to be bleached (35). Therefore, it is important to understand the effects of bleaching agents on the physical properties of the restorative materials (32).

Various studies have been performed that deal with the effects of bleaching agents on composite resin. However, it is difficult to compare the results of those studies, due to the variety of restorative materials used (36).

Composite resins have been shown to be more prone to chemical alteration compared with inert metal or ceramic restorations, because of their organic matrix (49).

The purpose of this study was to compare the surface roughness and microhardness of a recent nanohybrid composite with a nanofilled composite after the submission of both to the action of 2 bleaching agents: 10% CP and 35% HP.

A power test was performed using Pillai’s trace method (α = 0.05). It was observed that the number of samples of all groups was sufficient to validate the study. In case of groups 1, 3 and 5, the observed power was 0.986; and for groups 2, 4 and 6, it was 1.

In this study, bleaching agents were applied with clinically relevant bleaching regimes, according to the manufacturers’ recommendations. Between each bleaching treatment, the specimens were stored in 37°C artificial saliva so that the specimens were not continuously exposed to bleaching products to simulate cumulative effects over time.

The impact of bleaching on surface microhardness of composites is described controversially in the literature. Increases (23, 24, 30) as well as decreases (10, 12, 21, 28, 30, 37-38-39-40-41) in surface microhardness induced by home bleaching have been found, whereas other studies revealed no significant alteration (3, 27, 32-33-34-35, 50). Regarding in-office tooth whiteners, some studies showed that they did not significantly affect microhardness of composite materials (5, 3, 16, 26, 35, 37), and other studies reported a decrease (39, 42, 43). The discrepancies between these studies may be explained by the differences in experimental methodologies, bleaching agents applied (25, 33) and restorative materials used (25, 51). The different frequencies with which bleaching agents were changed may also contribute to the disparity between the results of the studies (33, 36).

Based on the statistical results of this study, the bleaching products used did not affect the microhardness of the resin composites evaluated. This result is in accordance with the findings of various other studies (3, 5, 16, 26, 27, 32-33-34-35, 37, 50), which reported that the microhardness of composite resin was not significantly affected by the use of bleaching agents. Yap and Wattanapayungkul (16) reported that no significant difference was observed in microhardness levels between the control and bleached groups for all materials tested with in-office bleaching (CP at 35% and HP at 35%). Silva Costa et al (3) indicated that microhardness after bleaching (home bleaching and office bleaching) in the nanofilled composite was not perceptible or significant. A recent study by Mourouzis et al (15) showed that the bleaching procedure did not alter the microhardness of any of the composite resins tested. These resin composites had in their composition a high proportion and small size of fillers (15).

However, there was a statistically significant difference in microhardness between home bleaching (group 3) and in-office bleaching regimen (group 5) with SonicFill™, in contrast to Filtek™ Supreme XTE, where there was no difference among any of the groups. The group treated with HP at 35% (group 5) showed statistically higher microhardness than the group that received CP at 10% (group 3). Various studies have shown that composites which underwent a secondary heat treatment to increase the degree of polymerization showed higher hardness values than did composites that were light cured only (13). Therefore, considering that microhardness is related to the degree of polymerization (13), it is conceivable that an increase in microhardness may be due to an additional polymerization of residual monomers, with the LEDs used in in-office bleaching regimens.

As for microhardness, investigations on the surface roughness of resin composites after bleaching have shown contradictory results (51). Some researchers have reported that in-office bleaching adversely affected the surface roughness of composites (21-22-23-24). Conversely, other studies reported that it was not detrimental to the surface roughness of composites (18, 25, 26). Different results were also evident regarding the use of lower concentration home bleaching agents. Some studies reported that home bleaching increases surface roughness (27-28-29), and other studies showed that composites could be safely bleached without compromising their roughness (30, 31).

Specific roughness parameters were selected in this study, according to the targeted results desired and the ISO 4287-1997 standard, since the measurements were performed according to the DIN EN ISO 4288 standard (52).

The Ra and Rq present a fair representation of the typical surface profile for comparison reasons. Most studies only include the Ra parameter for characterizing surface roughness. However, that parameter alone may not be sufficient to distinguish different variations: for example, it does not make a distinction between peaks and valleys, it does not qualitatively evaluate the form of the peaks and valleys and, generally, it does not consider unusual peaks and valleys (53).

Therefore, it is necessary to include other parameters in the analysis to overcome limitations related to the use of Ra alone (53). The Rz and Rsk can contribute to the differentiation by characterizing the depth between peak and valley and the quantification of each one. Rskmay be used to quantify the symmetry of the surface as it may relate to various considerations such as particulate retention. A surface with predominantly deep valleys will tend to have a negative skew, whereas a surface comprising a disproportionate number of peaks will have a positive skew (54, 55). This parameter becomes quite relevant when considering that an area which features a predominance of depressions tends to accumulate a larger amount of material on its surface (54).

In this study, there was no significant difference in Ra and Rq among all groups tested (p>0.05). However, when the Rzparameter was analyzed, Filtek™ Supreme XTE showed a significant increase between control and bleaching treatments.

Because different compounds are present in both the organic and inorganic fractions of restorative materials, even in products that are similarly categorized, these materials can react differently to the same treatment (17, 56). This possibility was confirmed in this present study.

Filtek™ Supreme XTE, as a nanofilled composite, has an average particle size ranging from 4 to 20 nm, while a nanohybrid, such as SonicFill™, has an average particle size ranging from 0.03 to 3 µm (46, 57). These characteristics may explain the different profilometric postbleaching changes seen here. The filler load is directly related to the surface area that is taken up by filler particles versus resin matrix, as the surface smoothness is generally determined by the largest inorganic particles present within the composite (58). The total content of inorganic fillers in Filtek™ Supreme XTE (78.5% by weight) is lower than in SonicFill™ (83.5% by weight) and might be another reason that this material is more susceptible to alteration during bleaching procedures, as suggested by Polydorou et al (36, 46). Since it has been suggested that roughening is a result of erosion of the matrix, the consequent debonding of resin–filler interfaces would lead to dislodgment and also to elution of fillers (15, 17). Thus, any difference in surface roughness is expected to occur in composites with higher resin content (36). Aside from this, it has been pointed out that composite matrices composed of bisphenol A glycidyl methacrylate (Bis-GMA) and urethane dimethacrylate (UDMA) resin polymers, which are present in the composition of Filtek™ Supreme XTE, can be softened with similar solubility parameters (16, 36).

With regard to Rsk, the current study showed a statistically significant increase in Filtek™ Supreme XTE after being treated with CP at 10%. This phenomenon is explained by an increase in the predominance of peaks in their topography. Although each specimen was rinsed with distilled water to remove the bleaching agent completely, this result may be due to accumulation of residual components, present in CP, on superficial surface of specimens during 14 days of treatment, such as carbomer.

In future studies, it will be relevant to brush the specimens after the end of each application of bleaching agent to ensure that it is completely removed.

It is important to refer to the fact that in vitro studies are limited in their attempt to simulate clinical conditions (15). In this study, the bleaching agents were not diluted or buffered with any water content such as saliva or distilled water during bleaching treatments, as it was in other studies (16, 25, 30). Storage of composite specimens in artificial saliva between incubation with the bleaching material was done to simulate a clinical situation (3, 10, 54). The artificial saliva was renewed every day to minimize the effect on the monomers’ leaching of the composite materials on their surface (36). For the purpose of standardization, this intermittent storage was performed in the present study with artificial saliva instead of human saliva (10). Storage in natural saliva may modify or attenuate the effect of peroxides by formation of a surface protection salivary layer on the restorative material (12).

It must be emphasized that this study was in vitro, and specimens were stored in artificial saliva, without any influence of the bacterial flora present in clinical situations. An increase in surface roughness is not only associated with plaque retention, but also makes it difficult for it to be removed by mechanical procedures, which may lead to gingival inflammation and caries formation (25, 51, 54). It was reported by Mor et al that bleaching agents may affect adherence of certain cariogenic microorganisms to the outer surfaces of composite resin restorations (59). In this context, it should be mentioned that salivary proteins absorbed on the surface of composite materials decreased after bleaching with peroxide-containing agents, which is suggested to have an influence on bacterial adhesion of cariogenic bacteria such as Streptococcus sobrinus and Streptococcus mutans, but not of Actinomyces viscosus (12).

Therefore, considering that bleaching is widely applied in approaches to improving dental aesthetics (60), it will relevant to test the effects of microhardness and roughness of resin composites in clinical trials.

Conclusions

Within the limitations of this study, it can be concluded that:

The microhardness of Filtek™ Supreme XTE and SonicFill™ was not affected by bleaching treatments.

Both bleaching treatments evaluated increased the Rz parameter in the Filtek™ Supreme XTE groups, in contrast to in the SonicFill™ groups.

CP 10% treatment affected the Rsk in the Filtek™ Supreme XTE group, with no significant effect in the SonicFill™ group.

Disclosures

Financial support: No financial support was received for this study. The authors wish to thank 3M ESPE, KERR and Meodental, who provided material for this study.
Conflict of interest: The authors do not have any financial interest in the companies whose materials are included in this article.
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Authors

Affiliations

  • Faculty of Medicine, University of Coimbra, Coimbra - Portugal
  • Faculty of Sciences and Technology, University of Coimbra, Coimbra - Portugal

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