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Mechanical characterization of resin cements used for luting ber posts by nanoindentation
Laura Ceballos a , Miguel Angel Garrido b , Victoria Fuentes a , Jesus Rodrguez b,
a b

Departamento de Ciencias de la Salud III, Universidad Rey Juan Carlos, C/Tulipan s/n, 28933 Mostoles, Madrid, Spain Departamento de Ciencia e Ingeniera de Materiales, Universidad Rey Juan Carlos, C/Tulipan s/n, 28933 Mostoles, Madrid, Spain

a r t i c l e
Article history:

i n f o

a b s t r a c t
Objectives. To evaluate the mechanical behavior of resin cements used for luting ber post. The inuence of the curing mode is analysed. Methods. Nanoindentation techniques have been applied to determine hardness and Youngs modulus of disc-shaped specimens of three types of cements: chemical- , photo- and dual-cured, provided by Ivoclar-Vivadent. Results obtained have been compared with mea-

Received 29 July 2005 Accepted 6 December 2005

Keywords: Resin cements Fiber posts Bonding Mechanical properties Nanoindentation

surements performed inside the postcementdentin system. Mechanical properties are evaluated together with scanning electron micrographs showing the postcement and dentincement interfaces. Results and Signicance. Differences have been detected between mechanical measurements performed inside the postcementdentin system and those carried out in laboratory discshaped specimens. The close presence of post and dentin boundaries has a lot of inuence on the cement behavior. The nanoindentation measurements indicate that the photo-cured cement exhibits a high hardness and stiffness, but with a more marked tendency to brittle failure. The chemically cured cement is the material with higher ability to bear deformation without damage, although its hardness and elastic modulus are signicantly lower. Dualcured cements present the best combination of properties. 2005 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

1.

Introduction

The use of ber posts to restore teeth with excessive loss of coronal structure due to caries, trauma or overaggressive endodontic procedures is gaining widespread acceptance with dental clinicians [13]. Several characteristics of these posts have contributed to their popularity. They have comparable elastic properties to dentin [4], inducing a stress eld similar to that of natural tooth [5]. This results in a reduction in the incidence of root fractures, demonstrated in both in vitro [6] and in clinical studies [2,7]. Moreover, the chemical nature of the posts allows them to be bonded to canal walls with adhesive systems in combination with resin cements [8], avoiding friction between dentin

walls and the post [4], and reinforcing the remaining tooth structure [9]. However, adhesive technique performance in root canals is a further challenge, due to the variable ability of bonding systems to demineralize and inltrate the dentin walls, the poor control of moisture, the inuence of different density and orientation of dentin tubules along the root canal, and the accessibility during handling of the materials [8,11]. Regarding resin cements, an adequate polymerization is utterly necessary to provide mechanical properties, such as modulus of elasticity and hardness, good enough to reinforce weakened roots [12] and clinically ensure retention of the post. According to the curing mode, three possible alternatives may

Corresponding author. Tel.: +34 914887159. E-mail address: jesus.rodriguez.perez@urjc.es (J. Rodrguez). 0109-5641/$ see front matter 2005 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.dental.2005.12.007

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be chosen: chemical-, photo- or dual-curing resin cements [10]. The use of chemically cured resin cements guarantees polymerization without the inuence of post space depth, but offers worse handling characteristics due to the absence of control of the setting reaction. Photo-curing resin cements allow sufcient time and control for proper seating of the post into the canal [12]. However, even when translucent ber posts are supposed to transmit the light into the post space [8,13], a reduction of resin cement hardness with depth has been determined [12,13]. Dual-curing resin cements are expected to combine favorable properties of both, auto- and photo-curing systems. The curing mode can also inuence the amount of shrinkage produced after polymerization. Shrinkage stresses of resin cements in root canals are especially relevant due to the unfavorable factor of conguration that restricts the ow of resin cement, which may affect the integrity of the adhesive interface [10]. Traditionally, the mechanical properties of dental materials on a small scale have been evaluated by means of microhardness tests. In recent years, the use of nanoindentation has become very popular in several elds, mainly for its possibilities in the characterization of very small quantities of material and, additionally, for providing simultaneous measures of hardness and elastic modulus [14]. In this work, the mechanical behavior of resin cements for luting ber posts has been evaluated by depth sensing indentation. Three types of resin cement were studied (chemical-, photo- and dual-curing) comparing the results obtained from laboratory disc-shaped specimens with those derived from actual restored teeth.

2.

Materials and methods

The materials evaluated in the present study are shown in Table 1. Disc-shaped specimens were prepared for each resin cement evaluated, Multilink, Variolink II Base and Variolink II Base plus Catalyst (Ivoclar-Vivadent Schaan, Liechenstein) using a metallic mold, 14 mm in diameter and 1 mm thick. The discs were placed over a glass plate and the materials were inserted into the discs. After insertion, the mold was covered with a mylar sheet and a glass microscope slide. Multilink resin cement was allowed to autocure, while Variolink II Base

Table 1 Materials used in the study

FRC Postec (Ivoclar-Vivadent) Multilink primer A and B (Ivoclar-Vivadent) Multilink resin cement (Ivoclar-Vivadent) Excite DSC (Ivoclar-Vivadent) Variolink II Base (Ivoclar-Vivadent) Variolink II Base plus Catalyst (Ivoclar-Vivadent) Glassber reinforced composite posts Self-etching adhesive Self-etching and self-curing resin cement Dual-curing adhesive Light-curing resin cement Dual-curing resin cement

and Variolink II Base plus Catalyst mixture were photopolymerized for 30 s (Astralis 10, program ESC; Ivoclar-Vivadent). After 20 min, specimens were removed from the molds and stored in darkness until evaluation. Additionally, teeth were restored with ber posts in order to compare the mechanical behavior of the luting resin cements in a situation similar to the clinical one. For this aim, singlerooted teeth, free of caries and extracted for periodontal reasons were selected. The crowns of the teeth were eliminated by cutting them 1 mm coronally to the cementumenamel junction with a diamond bur mounted on a high-speed handpiece under water cooling. Endodontic treatment was performed with stainless-steel K-les (Dentsply-Maillefer, Paris, France) in combination with 2.5% sodium hypochlorite irrigation. The canals were lled with laterally condensed guttapercha and TopSeal sealer (Dentsply De-Trey GmbH, Konstanz, Germany). The post space was prepared with the drills provided by the manufacturer of the posts (FRC Postec, Size 1; IvoclarVivadent), leaving 4 mm of guttapercha in the apical portion. The specimens were randomly allocated to three experimental groups according to the adhesive system and resin cement applied. In all cases, the glassber reinforced composite posts FRC Postec (Size 1: length 15 mm and a 0.8 mm diameter in the apical extreme; Ivoclar-Vivadent) were used. They were all cleaned with alcohol after try-in and silanized for 60 s (Monobond S, Ivoclar-Vivadent). In group 1, the specimens were treated with Multilink Primer A/B (Ivoclar-Vivadent) and the self-curing and selfetching cement Multilink (Ivoclar-Vivadent) according to manufacturers recommendations. Multilink Primer A and B were mixed and applied into the root canal walls by means of a microbrush. The excessive adhesive solution was removed with a paper point and after 15 s, it was dried but not lightcured. Multilink cement was mixed and the post was coated with it and inserted into the post space. In group 2, the posts were luted with the dual-curing adhesive Excite DSC (Ivoclar-Vivadent) and the light-curing cement Variolink II Base (Ivoclar-Vivadent). The root canal walls were etched with 35% phosphoric acid (Ultradent, South Jordan) for 15 s, water rinsed and then gently dried with paper points. This adhesive is offered in a single-dose vessel with an applicator indicated for root canals. Excessive adhesive was removed with a paper point. The adhesive was polymerized for 10 s (Astralis 10 using ADH program; Ivoclar-Vivadent). Then the posts were covered with Variolink II Base cement and seated into place. The cement was light polymerized through the post for 30 s (Astralis 10, program ESC; IvoclarVivadent). Finally, in group 3, the posts were also luted with Excite DSC adhesive (Ivoclar-Vivadent) and the dual-curing cement Variolink II (Ivoclar-Vivadent). The adhesive system was applied as previously described, but it was not light-cured. Variolink II, Base plus Catalyst, were mixed and applied covering the posts. Fiber posts were seated and the cement was polymerized also for 30 s (Astralis 10, program ESC; Ivoclar-Vivadent). Samples were included in resin blocks and after 24 h samples were sectioned perpendicular to their long axis (Accutom5, Struers, Copenhagen, Denmark), in order to obtain sections from the coronal and apical root areas. Surfaces were polished

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with alumina suspension slurry of 3 m and OP-A (Struers, Copenhagen, Denmark). Indentations were made on the disc-shaped specimens and in different regions of the resin cement used to lute the ber post. Youngs modulus and hardness of the cements were determined from the loaddisplacement curves following the OliverPharr methodology [15].

Table 2 Nanoindentation data from disc-shaped specimens Cements

Multilink (self-curing cement) Variolink II Base (light-curing cement) Variolink II Base plus Catalyst (dual-curing cement)

E (GPa)
4.9 (0.2) 8.8 (0.5) 7.4 (0.2)

H (GPa)
0.21 (0.01) 0.31 (0.03) 0.31 (0.01)

H/E
0.042 0.035 0.042

H2 /E (GPa)
0.009 0.011 0.013

2.1. Preparation of the samples for scanning electron microscopy observation

Selected specimens from each group with their corresponding posts were prepared for scanning electron microscope (SEM) observation. In order to observe hybrid layer formation, samples were longitudinally sectioned, demineralized with 35% phosphoric acid for 15 s, deproteinized with 2% sodium hypochlorite for 120 s and dehydrated with increasing concentrations of alcohol [8]. Other samples were immersed in a solution of 30% HCl for 24 h and in 2% sodium hypochlorite for 10 min in order to completely eliminate the dental tissues for better observation of resin tags formation [8]. Finally, samples were mounted on aluminum stubs with carbon cement and sputter coated with gold (Sputtercoater, Baltec, SCD005) and observed under a Philips XL 30 environmental scanning electron microscope (ESEM).

Average values and standard deviations are in parentheses.

3.
3.1.

Results and discussion

Nanoindentation tests

Fig. 1 shows an example of the loaddisplacement curves obtained from the nanoindenter for the disc-shaped specimens. As can be appreciated, the nanoindentation technique is quite sensitive to material behavior. Elaborate results are included in Table 2, where apart from hardness, H, and Youngs modulus, E, the ratios H/E and H2 /E are also included. The magnitude H/E can be considered as a measure of the materials ability to bear elastic deformation. In other words, H/E

is related to the deformation limit before permanent damage is caused. On the other hand, H2 /E can be understood as a measure of the materials ability to store elastic energy. Both magnitudes are signicant in the mechanical performance of the resin cement within the tooth restored with a ber post. According to the results obtained, the chemically cured cement, Multilink (Ivoclar-Vivadent), presents the lowest values of stiffness and hardness, although its ability to being deformed without damage is superior to other cements. Photo-cured cement, Variolink II Base (Ivoclar-Vivadent), is the stiffest and hardest, but its low value of H/E is a warning of brittle failure. Dual-cured cement, Variolink II Base plus Catalyst (Ivoclar-Vivadent) seems to posses the best combination of properties. It is almost as stiff and hard as the photo-cured version, but with a much higher ability to be reversibly deformed. One of the most valuable advantage of nanoindentation is the possibility of testing the cements in situ, i.e., inside the postresin cementdentin system. Obviously, the situation is clearly different from that in the disc-shaped specimens, mainly due to the inuence of viscosity, uncontrollable void formation, thickness, factor of conguration, etc. A very thin layer of cement does not have to behave as the bulk cement characterized from disc-shaped specimens. Table 3 summarized the results obtained in each type of resin cement, measured in different regions. These results provide appealing conclusions. Multilink (Ivoclar-Vivadent), the chemically cured cement, exhibited remarkable changes in the appar-

Fig. 1 Nanoindentation loaddisplacement curves from disc-shaped specimens.

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ent hardness and Youngs modulus. The values of H and E measured in situ increase by almost 100%. Interestingly, the ratio H/E is not so severely altered, remaining constant at the coronal region and exhibiting increases of 40% at the apical zone.

Fig. 3 ESEM micrographs showing: (a) resin tags at coronal and mid-zones for Multilink Primer and resin cement (1200); (b) resin tags for Variolink II Base (80); (c) resin tags at coronal and mid-zones for Variolink II Base plus Catalyst (500). Fig. 2 ESEM micrograhs showing: (a) gap at the interface obtained with Multilink Primer and resin cement (1000); (b) interface obtained with Excite DSC and Variolink II Base (800); (c) interface detected for Excite DSC and Variolink II Base plus Catalyst (800).

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Table 3 Nanoindentation data from in situ specimens Cement

Multilink (self-curing cement)

Region
Coronal Apical Coronal Apical Coronal Apical

E (GPa)
8.1 (0.4) 7.1 (0.3) 9.4 (0.6) 7.0 (0.3) 6.9 (0.3)

H (GPa)
0.38 (0.01) 0.43 (0.02) 0.29 (0.04) 0.38 (0.02) 0.31 (0.02)

H/E
0.047 0.062 0.030 0.054 0.045

H2 /E (GPa)
0.018 0.027 0.009 0.021 0.014

Variolink II Base (light-curing cement)

Variolink II Base plus Catalyst (dual-curing cement)

Average values and standard deviations are in parentheses.

Photo-cured Variolink II Base cement (Ivoclar-Vivadent) is virtually unaltered in all the properties measured. It is worthy of note to explain here, that an improper curing process makes it difcult to obtain consistent results in the apical region. The difculties of attaining complete photo-curing have previously been reported and it is one of the drawbacks of this type of cement, conrmed in this work. Finally, as is expected, the dual cement, Variolink II (IvoclarVivadent) brings together the best properties of the other cements. Its hardness and stiffness values are as high as those of the photo-cured cement, but with a deformation capability similar to that of the chemically cured cement. No appreciable differences are observed between coronal and apical regions in this case. It is clear that the boundary conditions are decisive when the thickness of the cement layer is quite low. The close proximity of the post and the dentin surfaces plays a displacement constraint role, leading to higher values of hardness and elastic modulus. It would be very signicant to analyse if cracks and discontinuities between resin cement and post or dentin are observed. The presence of this type of defect may partially cancel the shrinkage stresses caused by polymerization.

that the higher viscosity of this cement restricted its ow along the post space or that it was not properly polymerized due to the attenuation of light with depth (Fig. 3c). Posts bonded with Variolink II in dual-curing mode, were completely covered with the resin cement. When the dentincement interface was examined, the adhesive could not be clearly detected, probably because it was not photopolymerized before post luting. The thickness of the cement layer changed according to the different root canal morphologies. Some voids were observed in the three resin cements evaluated, probably due to their viscosity that restricts their placement inside the post space and the mixing procedure of the base and catalyst pastes.

Acknowledgements
Authors are indebted to the company Ivoclar-Vivadent for providing the materials used in this study. Thanks are also extended to the University Rey Juan Carlos for partially nancing this work.

3.2.

Scanning electron microscopy observations

references

The interface obtained when Multilink adhesive and resin cement were applied showed a discontinuous gap between the resin cement and the inltrated dentin, while this situation is not observed in the other cements (Fig. 2). Moreover, at this level, there were zones with no resin tags and others where they only plugged the tubules, probably due to the reduced density of tubules [16]. Also, many small and few bigger voids in the resin cement were visible. In the coronal and mid-zones, few areas were detected with long and numerous resin tags. Generally, resin tags were short and no adhesive lateral branches were observed (Fig. 3a). Unlike self-etching adhesive Multilink, the density of the resin tags was very high in coronal and mid-zones when Excite DSC was applied after acid etching, regardless of the resin cement used. Resin tags were also very long and numerous lateral branches were observed (Fig. 3b). Probably phosphoric acid is more effective in penetrating thick smear layers and demineralizing the underlying dentin [10,11]. When light-curing Variolink II was used, areas were the cement was detached from the post surface could be detected in its apical extreme, being visible only in small areas. Moreover, short resin tags were observed in these areas. It may be

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