The ofcial journal of the Australian Dental Association

Australian Dental Journal

Australian Dental Journal 2013; 58: 448453 doi: 10.1111/adj.12122

Effect of G-Coat Plus on the mechanical properties of glass-ionomer cements

R Bagheri,* NA Taha, MR Azar,* MF Burrow
*Department of Dental Materials, Biomaterial Research Centre, Faculty of Dentistry, Shiraz University of Medical Sciences, Shiraz, Iran. Department of Conservative Dentistry, Faculty of Dentistry, Jordan University of Science and Technology, Irbid, Jordan. Oral Diagnosis and Polyclinics, Faculty of Dentistry, The University of Hong Kong, Prince Philip Dental Hospital, Hong Kong SAR.

ABSTRACT
Background: Although various mechanical properties of tooth-coloured materials have been described, little data have been published on the effect of ageing and G-Coat Plus on the hardness and strength of the glass-ionomer cements (GICs). Methods: Specimens were prepared from one polyacid-modied resin composite (PAMRC; Freedom, SDI), one resinmodied glass-ionomer cement; (RM-GIC; Fuji II LC, GC), and one conventional glass-ionomer cement; (GIC; Fuji IX, GC). GIC and RM-GIC were tested both with and without applying G-Coat Plus (GC). Specimens were conditioned in 37 C distilled water for either 24 hours, four and eight weeks. Half the specimens were subjected to a shear punch test using a universal testing machine; the remaining half was subjected to Vickers Hardness test. Results: Data analysis showed that the hardness and shear punch values were material dependent. The hardness and shear punch of the PAMRC was the highest and GIC the lowest. Applying the G-Coat Plus was associated with a signicant decrease in the hardness of the materials but increase in the shear punch strength after four and eight weeks. Conclusions: The mechanical properties of the restorative materials were affected by applying G-Coat Plus and distilled water immersion over time. The PAMRC was signicantly stronger and harder than the RM-GIC or GIC.
Keywords: G-Coat Plus, glass-ionomer cements, mechanical properties. Abbreviations and acronyms: ANOVA = analysis of variance; GIC = glass-ionomer cement; PAMRC = polyacid-modied resin composite; RM-GIC = resin-modied glass-ionomer cement; VHN = Vickers Hardness Number. (Accepted for publication 5 March 2013.)

INTRODUCTION Conventional glass-ionomer cements (GICs) are formed by an acid-base neutralization reaction between an aqueous polyalkenoic acid and an aluminosilicate glass powder, which results in a relatively brittle material compared to resin composite. Since the end of the 1980s, more developed GICs such as resin-modied glass-ionomer cements (RM-GICs) have become available. Stronger and less brittle hybrid materials have been produced by the addition of water-soluble polymers to create a light-curing GIC formulation.1 The aim of introducing RM-GIC was to maintain the desirable properties of GIC and overcome the disadvantages such as moisture sensitivity and poor early mechanical strength.2 In their simple form, RM-GICs are water-hardening cements with the addition of a hydrophilic monomer, 2-hydroxyethyl methacrylate (HEMA).3 A recently introduced tooth-coloured restorative material that claimed to have the benets of the GICs
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and resin composite lling materials is the polyacidmodied resin composite (PAMRC), commonly called compomer. PAMRCs were introduced in approximately 1994.4 Commercially, the term compomer (composite-ionomer) is widely used to reect its resin composite and glass-ionomer derivation. PAMRCs combine glass polyalkenoic components with polymerizable resin constituents such as dimethacrylates. PAMRCs do not have an auto-setting acid-base reaction as in GICs but rely on resin polymerization to create a set functional restorative material.2 When selecting a material to restore teeth, one of the main considerations is its mechanical properties. A restorative material used to replace missing tooth structure needs to be strong enough to withstand the forces associated with mastication and other possible loading. Hardness and shear punch strength are two tests that can be used to evaluate the mechanical properties of a lling material. The material hardness can be dened as its resistance to surface indentation.5,6 The Vickers Hardness test is a method used
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Mechanical properties of restorative materials for brittle materials6 in which a pyramidal indentation is made using a specied load and application time, the resultant hardness number being independent of the applied load.7 The shear punch test has been used to determine properties of clinical signicance such as occlusal or incisal forces that occur during mastication.8 It has been used as a simple, reliable technique for assessing the mechanical properties of resin-based materials.9 Both hardness and shear punch strength of tooth-coloured materials have been evaluated to predict their durability, and a relationship between these mechanical properties to material ller content, ller size and silane coupling agent has also been demonstrated.10,11 The objectives of the present study were to place GIC, RM-GIC and PAMRC in distilled water for up to eight weeks at 37 C and determine: (1) the resultant surface hardness and shear punch strength; (2) the effect of ageing on the surface hardness and shear punch strength; and (3) the effect of a recently introduced resin surface coating (G-Coat Plus) on the hardness and shear punch strength of the GIC and RM-GIC. The null hypotheses are that there is no difference among the materials; that the ageing does not affect mechanical properties; and that the surface coating does not affect the mechanical properties of GICs. MATERIALS AND METHODS Specimen preparation The materials used in the study are listed in Table 1. For Freedom a total of 9 and for the GIC and RM-GIC, a total of 36 disc-shaped specimens for hardness testing (10.0 mm diameter 9 1.5 mm thick) were prepared. For shear punch testing, 18 and 72 disc-shaped specimens (10.0 mm diameter 9 0.7 mm thick) were prepared for Freedom, and the GIC and RM-GIC respectively (n = 6). All materials were placed in the appropriate plastic mould and pressed between two plastic matrix strips and glass slabs under hand pressure to extrude excess material. The glass slabs were removed and the light-cured materials Table 3. Mean Vickers Hardness Number (VHN; MPa) and standard deviations () of the materials following times interval (n = 3 discs 3 5 indentation = 15)
Materials Freedom Fuji II LC Fuji II LC+ Fuji IX Fuji IX+
aA bA cB dA dA

were cured according to the manufacturers instructions on each side using an LED curing light with a wavelength range of 440480 nm at an output of 1500 mW/cm2 (Radii plus LED, SDI, Bayswater, VIC, Australia). Specimens were removed from the mould and excess material around the mould was removed by manual gentle wet grinding both sides of the specimens in a circular motion with a sequence of 1000-, 1500-, 2000-grit silicon carbide papers. Each specimen was washed in an ultrasonic bath between each grinding. Specimens were randomly divided into ve groups for each test (Tables 2 and 3); each group was Table 2. Mean shear punch strength (MPa) and standard deviations () of the materials following times interval (n = 6)
Materials Freedom Fuji II LC Fuji II LC+ Fuji IX Fuji IX+
aA aA

24 hours 47.8 45.5 aA 40.0 bA 31.7 cA 25.0 (4.0) (7.5) (6.6) (2.3) (1.1)
aA aA

4 weeks 47.2 40.3 cC 59.3 bA 35.9 aA 42.56 (2.2) (2.3) (7.6) (3.8) (3.0)
aB bB

8 weeks 111.6 80.6 cB 95.2 dB 59.9 bB 76.2 (5.1) (6.5) (5.0) (6.2) (3.4)

Determines control group (not coated by G-Coat Plus). +Determines treatment group (coated by G-Coat Plus). Means with the same upper-case letter in each row are not signicantly different (p > 0.05). Means with the same lower-case letter in each column are not signicantly different (p > 0.05).

24 hours 87.6 49.3 27.8 15.5 15.4 (3.5) (2.4) (1.5) (0.5) (0.5)
aB bB

4 weeks 66.3 40.4 bA 43 cB 11.8 cB 7.3 (3.5) (4.7) (1.7) (0.7) (0.3)
aB aA

8 weeks 77.4 49.1 bB 28.4 cA 13.2 cB 8.2 (6.1) (2.4) (1.0) (1.7) (1.8)

Determines control group (not coated by G-Coat Plus). +Determines treatment group (coated by G-Coat Plus). Means with the same upper-case letter in each row are not signicantly different (p > 0.05). Means with the same lower-case letter in each column are not signicantly different (p > 0.05).

Table 1. Materials
Name Freedom Fuji II LC Fuji IX G-Coat Plus Manufacturer SDI, Vic, Australia GC Corporation, Tokyo, Japan GC Corporation, Tokyo, Japan GC Corporation, Tokyo, Japan Material type Polyacid-modied resin composite Resin-modied glass-ionomer cement Self-cure (conventional) glass-ionomer cement Nanolled self- adhesive light- cured protective coating Filler/resin type strontium uoroaluminium silicate/urethane dimethacrylate based Aluminium-uoro-silicateglass/Poly-HEMA Aluminium-uoro-silicate glass Batch# 121314 1202221 1110191

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R Bagheri et al. subdivided to three groups and conditioned in distilled water at 37 C for 24 hours, four and eight weeks. G-Coat Plus was applied on the specimens in the coated group by placing a thin coat of G-Coat Plus on the top surface of the specimen with a microbrush, then gently air blown for 5 seconds and lightcured for 20 seconds according to the manufacturers recommendation. Specimens were stored, and tested after 24 hours, four and eight weeks immersion in distilled water at 37 C. The water was changed weekly for each of the time periods. Measurements of Vickers Hardness and shear punch strength were carried out as described below. Shear punch strength The thickness of each specimen was measured with a digital micrometer, positioned in the shear punch jig (Fig. 1) and held in place by gently tightening the restraining screw. The shear punch jig was aligned to the loading axis of the universal testing machine (Zwick/Roll Z020, Zwick GmbH & Co, Germany). A at-ended 3.2-mm diameter stainless steel rod was used to punch out a disc through the centre of each specimen at a crosshead speed of 1 mm/min, and the maximum load recorded. Shear punch strength (MPa) was calculated using the following formula: load (N) punch circumference (mm) specimen thickness (mm)

Vickers Hardness Each disc was subjected to ve indentations with 35 lm apart across the specimen surface by applying a load of 300 g for 15 seconds using a Digital Hardness Tester (Buehler, Chicago, USA) (n = 3 discs 9 5 indentation = 15). The Vickers Hardness Number (VHN) was determined by dividing the load (kgf) by the surface area (mm2), and the resulting value converted to MPa multiply by 9.807 (MPa = Kgf 9 9.8/m2 9 106). Data analysis To evaluate the interaction between material and immersion time as well as the effect of G-Coat Plus in each of the two tests, two-way analysis variance (ANOVA) was carried out. To determine inter-material differences for each test, data were analysed using one-way ANOVA and Tukeys test at a signicance level of 0.05. A Pearson Correlation test was also conducted to determine if a relationship could be observed between hardness and shear punch strength. RESULTS Shear punch strength The means and standard deviations are shown in Table 2 and Fig. 2. The base line strength for the PAMRC was slightly greater than the RM-GIC, but signicantly greater than the GIC (p < 0.05). All materials showed a signicantly higher shear punch value after eight weeks immersion in distilled water. G-Coat Plus coated specimens showed an increase in

120 100 80 60 40 20 0 Freedom

24 hours

4 weeks

8 weeks

Shear Punch Strength (MPa)

Fuji II LC -

Fuji II LC +

Fuji IX -

Fuji IX +

Fig. 1 A schematic representation of the shear punch jig.

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Fig. 2 Shear punch strength (MPa) versus time interval for all materials in distilled water.
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Mechanical properties of restorative materials shear punch strength for the RM-GIC and GIC (p < 0.05) after four and eight weeks immersion respectively compared to the non-coated specimens. The Pearson Correlation test showed over each test period (24 hours, four and eight weeks) no correlation could be determined between shear punch strength and hardness. The correlations were 0.297, 0.175 and 0.23 for each of the time periods respectively. Irrespective of time, the correlation was calculated at 0.052. Vickers Hardness The means and standard deviations are shown in Table 3 and Fig. 3. With respect to the material tested, regardless of time, the hardness of the PAMRC was the highest and GIC the lowest. There was a signicant difference between all materials at baseline VHN (p < 0.05). Ageing in distilled water for most of the materials showed signicantly lower VHN after four weeks but then an increase after eight weeks that remained lower than at baseline. Tukeys test showed G-Coat Plus exhibited a signicant decrease in the VHN of the RM-GIC after 24 hours and eight weeks (p < 0.05), while it showed signicant increase after four weeks immersion compared to that of 24 hours. DISCUSSION Roydhouse8 introduced the shear punch test as a practical and reliable test for comparing dental cements. The shear punch test was conrmed by Nomoto et al.,11 as a suitable method for standard specication testing across a broad range of restorative materials. Although exural, compressive and diametral tests are the most commonly used, differences in specimen quality and stress concentration during loading are common problems when comparing inter-laboratory test results. In contrast to exural, diametral and compression testing, the shear punch test is not particularly technique sensitive in terms of the quality of the circumference edges of the disc. Therefore, simplicity of specimen preparation has been mentioned as the main advantage of the shear punch test over the other tests.11,12 In the current study, specimens were polished to obtain at surfaces for uniform stress distribution around the punch circumference. The modied shear punch test jig (Fig. 1) introduced by Nomoto et al.11 was used in the present study. In this method, the specimen was restrained during shear punch testing by a screw clamp over the top of the specimen, which has been advocated for the prevention of specimen exure during application of the force from the punch.11 In this study, in contrast to the effect of ageing on the hardness of the tested materials, storage in distilled water was associated with an increase in shear punch strength (Fig. 2). A statistically signicant increase in shear punch strength was observed for all materials as the time interval increased with the greatest increase observed after eight weeks immersion in distilled water (Table 2). The shear punch value for the specimens with the coating agent was more than the uncoated group. Coated specimens showed a signicant increase after four weeks immersion in distilled water and even more after eight weeks. It is a possibility that the coating agent exerted some local control on the setting of the materials after four and eight weeks or reduced the effect of surface porosity and crack propagation. The rank order of increasing shear punch strength in this study (GIC<RMGIC<PAMRC) is supported by outcomes from previous studies.12,13 A variation in results for some materials, particularly in the shear punch test of uncoated Fuji II LC and in the microhardness of coated Fuji II LC, at different time intervals was observed. These results may be related to the complexity of the stress distribution in a specimen during loading by the punch,8 as well as the possibility of voids existing within the material that could not be detected prior to testing. The existence of undetectable voids will cause differences in the strengths observed. The observed variation may also show a complex intrinsic change occurring within the materials as they continue to mature but also change due to absorption of water. Further study is needed to clarify and better understand what may be occurring in some of these materials. In the present study, the PAMRC had a signicantly greater hardness than RM-GIC and conventional GIC after 24 hours immersion in distilled water (Table 3). This outcome can be attributed to the type of inorganic llers in the PAMRC and resin matrix. A positive correlation between the hardness and inorganic ller has been previously shown;14 resin-based materials that contain barium glass llers showed
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90 80 Vickers hardness Number (MPa) 70 60 50 40 30 20 10 0 Freedom

24 hours

4 weeks

8 weeks

Fuji II LC -

Fuji II LC +

Fuji IX -

Fuji IX +

Fig. 3 Vickers Hardness Number (MPa) versus time interval for all materials in distilled water.
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R Bagheri et al. signicantly lower surface hardness than composites containing zirconia/silica ller particles. The hardness after 24 hours immersion in distilled water showed a signicantly greater value for the RM-GIC, approximately twice that of the GIC. Conventional GICs are formed by an acid-base reaction between an aqueous polyacrylic acid and an aluminosilicate glass powder, which results in a relatively brittle material in comparison to RM-GICs. Higher hardness values for the RM-GIC can probably be attributed to the polymerized resin component, polyHEMA,15 which may reinforce or stiffen the whole cement by creating a polymer structure throughout the set cement. Regarding the effect of storage in distilled water on the PAMRC and GIC, the hardness of all groups decreased as the time interval increased with the greatest decrease observed after four weeks (Fig. 3). This result is in agreement with the results of several other studies.16,17 The reduction of hardness in the PAMRC due to ageing could be attributed to many factors, including water sorption by the resin component causing plasticization. Since hardness is a surface property, it is affected by water sorption.18,19 Water sorption is a complex phenomenon and is dependent on the matrix resin, the ller, and the properties of the interface between the matrix and the ller.20 A decreased ller loading has been shown to result in greater water sorption.21 As water is a poor solvent of dental composites,22 the water sorption is a process of slow diffusion. Therefore, it would be expected that the storage time will have an inuence upon water sorption and consequently mechanical properties.23 It has been shown considerable time is needed for resin composite to become completely saturated by the water which may lead to a stabilization in hardness changes. Therefore, in order to compare the effect of water on the hardness of these materials more objectively, further longterm studies are needed. Both the GICs and RM-GIC showed a signicantly lower hardness after applying G-Coat Plus compared to the uncoated groups. The results of our previous study,24 the effect of coating on the fracture toughness (KIc) of GICs, revealed that coating with G-Coat Plus increased the KIc of GIC signicantly while it did not affect that of RM-GIC. A recent study25 also reported a similar nding. This study25 investigated the effect of G-Coat Plus on the fracture resistance of Fuji IX GP Extra after 14 days storage in distilled water. The highest reported fracture strength, 26.1 MPa, was for the GIC coated before water contamination in comparison with uncoated GIC and GIC coated after water contamination.25 According to the ndings of Bonifacio et al.,26 Fuji IX GP Extra showed signicant improvement in wear resistance and exural strength
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when G-Coat Plus was applied. They observed micromechanical interlocking between the G-Coat Plus and the GIC under SEM. The authors speculated that G-Coat Plus is advantageous if used with Fuji IX GP Extra to decrease the early wear and increase its fracture strength.26 Hardness is a surface phenomenon, while fracture toughness is an intrinsic characteristic of a material related to energy needed for cracks to propagate and how crack propagation may be prevented. Based on the manufacturers claim, inltration of G-Coat Plus gives internal protection against crack initiation and lls porosities, both of which may increase fracture toughness and thus reinforcing and strengthening the GIC and RM-GIC. The self-adhesive coating bonds to GIC and provides a lamination effect that has been shown to increase the fracture toughness.24 Its protective effect from extrinsic water may also allow complete maturation of the GIC reaction with delayed water exposure, thus possibly creating a stronger material while it may not reinforce the surface of the material. A recent clinical study trialled the use of the EQUIA system (GC Corp, Japan) in posterior teeth on occlusal and approximal restorations up to 24 months.27 The EQUIA system is Fuji IX GP Extra with G-Coat Plus. Their study concluded this system may be suitable for long-term temporary and small permanent restorations. However, the median age of the restorations was only 24 months and they failed to use a comparison material. The results of the present study in the context of clinical usage show that all the GICs gain strength some time after the initial set. In addition, the use of G-Coat Plus seems to provide some benet after the initial set (>24 hours), i.e. enhancing the initial strength. Hence, the longer term strength results lend some support to the clinical study that GIC could possibly be used in small load bearing restorations. It would also seem that the RM-GIC tested is approaching strengths of the PAMRC used. This is an interesting result that may indicate the placement of coated RM-GIC restorations could be as successful as PAMRC for small restorations not exposed to a high degree of load, e.g. anterior approximal or small occlusal restorations and deciduous teeth. However, further work is needed to determine if the loss of this surface coating due to occlusal wear will affect clinical survival. CONCLUSIONS Within the limitations of this study, the following conclusions were drawn and the three hypotheses were rejected. Ageing in distilled water affected the hardness and/or shear punch strength of all materials
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Mechanical properties of restorative materials to varying degrees. The effect of time and G-Coat Plus was material dependent. In general, most of the materials showed an increase in the shear punch strength and decrease in the VHN after immersion in distilled water, in comparison with the baseline. For both test results, the ranking was consistent with the clinical recommendation for the materials; the PAMRC was signicantly stronger and harder than the RM-GIC, which in turn was signicantly stronger and harder than the conventional GIC. In this study, surface coating of GIC and RM-GIC using G-Coat Plus was not found to be effective in increasing the Vickers Hardness of the materials. However, it was effective on the shear punch strength of those materials. Coated Fuji II LC and Fuji IX showed signicantly higher shear punch strength than uncoated groups after four and eight weeks immersion in distilled water while the coated specimens of the 24-hour group exhibited lower values than the uncoated groups. It must be emphasized that the results of the present study are valid for the laboratory conditions used. Laboratory data may provide an insight into clinical performance; however, a direct relationship between laboratory and clinical performance cannot always be assumed. REFERENCES
1. Wilson AD. Developments in glass-ionomer cements. Int J Prosthodont 1989;2:438446. 2. Sidhu SK, Watson TF. Resin-modied glass ionomer materials. A status report. Am J Dent 1995;8:5967. 3. Wilson AD. Resin-modied glass-ionomer cements. Int J Prosthodont 1990;3:425429. 4. McLean JW, Nicholson JW, Wilson AD. Proposed nomenclature for glass-ionomer dental cements and related materials. Quintessence Int 1994;25:587589. 5. Craig RG, Powers JM, Wataha JC. Dental materials properties and manipulation. St. Louis: Mosby, 2000. 6. Anusavice KJ. Phillips Science of Dental Materials. St. Louis: Mosby, 2003. 7. Wassell RW, McCabe JF, Walls AW. Subsurface deformation associated with hardness measurements of composites. Dent Mater 1992;8:218223. 8. Roydhouse RH. Punch-shear test for dental purposes. J Dent Res 1970;49:131136. 9. Ikejima I, Nomoto R, McCabe JF. Shear punch strength and exural strength of model composites with varying ller volume fraction, particle size and silanation. Dent Mater 2003;19:206 211. 10. McCabe JF, Wassell RW. Hardness of model dental composites: the effect of ller volume fraction and silanation. J Mater Sci Mater Med 1999;10:291294. 11. Nomoto R, Carrick TE, McCabe JF. Suitability of a shear punch test for dental restorative materials. Dent Mater 2001;17:415421. 12. Mount GJ, Makinson OF, Peters MC. The strength of autocured and light-cured materials: the shear punch test. Aust Dent J 1996;41:118223. 13. Bagheri R, Burrow MF, Tyas MJ. Comparison of the effect of storage media on hardness and shear punch strength of toothcolored restorative materials. Am J Dent 2007;20:329334. 14. Say EC, Civelek A, Nobecourt A, Ersoy M, Guleryuz C. Wear and microhardness of different resin composite materials. Oper Dent 2003;28:628634. 15. Kovarik RE, Muncy MV. Fracture toughness of resin-modied glass ionomers. Am J Dent 1995;8:145148. 16. Ferracane JL, Berge HX, Condon JR. In vitro aging of dental composites in water. Effect of degree of conversion, ller volume, and ller/matrix coupling. J Biomed Mater Res 1998;42:465472. 17. Ravindranath V, Gosz M, De Santiago E, Drummond JL, Mostovoy S. Effect of cyclic loading and environmental aging on the fracture toughness of dental resin composite. J Biomed Mater Res Part B Appl Biomater 2007;80:226235. 18. Momoi Y, McCabe JF. Hygroscopic expansion of resin based composites during 6 months of water storage. Br Dent J 1994;176:9196. 19. Sarrett DC, Ray S. The effect of water on polymer matrix and composite wear. Dent Mater 1994;10:510. 20. Beatty MW, Swartz ML, Moore BK, et al. Effect of microller fraction and silane treatment on resin composite properties. J Biomed Mater Res 1998;40:1223. 21. Kim KH, Ong JL, Okuno O. The effect of ller loading and morphology on the mechanical properties of contemporary composites. J Prosthet Dent 2002;87:642649. 22. Mante F, Saleh N, Mante M. Softening patterns of post-cure heat-treated dental composites. Dent Mater 1993;9:325331. 23. Ortengren U, Andersson F, Elgh U, Terselius B, Karlsson S. Inuence of pH and storage time on the sorption and solubility behavior of three composite resin materials. J Dent 2001;29:3541. 24. Bagheri R, Azar MR, Burrow MF, Tyas MJ. The effect of aging on the fracture toughness of aesthetic restorative materials. Am J Dent 2010;23:142146. 25. Lohbauer U, Kramer N, Siedschlag G, et al. Strength and wear resistance of a dental glass-ionomer cement with a novel nanolled resin coating. Am J Dent 2011;24:124128. 26. Bonifacio CC, Werner A, Kleverlaan CJ. Coating glass-ionomer cements with a nanolled resin. Acta Odontol Scand 2012;70:471477. 27. Friedl K, Hiller K-A, Friedl K-H. Clinical performance of a new glass ionomer based restoration system: a retrospective study. Dent Mater 2011;27:10311037.

Address for correspondence: Rafat Bagheri Ghasrodasht, Ghomabad Street Department of Dental Materials Faculty of Dentistry Shiraz University of Medical Sciences Shiraz Iran Email: bagherir@unimelb.edu.au

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