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Table of Contents   
ORIGINAL RESEARCH  
Year : 2015  |  Volume : 26  |  Issue : 2  |  Page : 170-175
Comparative evaluation of shear bond strength of nano-hydroxyapatite incorporated glass ionomer cement and conventional glass ionomer cement on dense synthetic hydroxyapatite disk: An in vitro study


Department of Pedodontic and Preventive Dentistry, JSS Dental College and Hospital, Mysore, Karnataka, India

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Date of Submission18-Nov-2014
Date of Decision17-Dec-2014
Date of Acceptance17-Apr-2015
Date of Web Publication22-Jun-2015
 

   Abstract 

Aim: The aim was to evaluate and compare the shear bond strength of nano-hydroxyapatite (Nano-HAp) incorporated and conventional glass ionomer cement (GIC).
Materials and Methods: Nano-HAp GIC was prepared by replacing 8 wt% of GIC powder with nano-HAp powder. Twenty-six HAp disks were used as substrate for bonding and divided into two equal groups. Before bonding the HAp disk was prepared by silicon carbide (no. 2500) followed by 10% polyacrylic acid conditioning. The standardized samples were prepared using split teflon mold on customized bonding jig so as to adhere testing materials to pretreated HAp disk. These samples were stored in distilled water for 24 h at 37°C before bond strength testing.
Results: The descriptive statistical analysis and independent samples t-test were used. The nano-HAp incorporated and conventional GIC had the mean shear bond strength of 3.28 ± 0.89 MPa and 5.25 ± 0.88 MPa, respectively. Nano-HAp incorporated GIC had lower shear bond strength with very high level of significance (P < 0.001). The nano-HAp incorporated GIC showed mainly mixed type of failure whereas conventional GIC showed mainly a cohesive failure.
Conclusion: The lower shear bond strength of nano-HAp incorporate GIC revealed that the addition of nano-HAp interfered with the bonding ability of GIC to the substrate interface, but the mixed type of failure in nano-HAp incorporated GIC suggests that it increases the strength of the matrix. However, the role of nano-size particles on the micro-size particles of GIC for the bonding mechanism and the ratio and proportions of nano-HAp to the GIC needs further elucidation.

Keywords: Hydroxyapatite disk, nano-hydroxyapatite incorporated glass ionomer cement, shear bond strength

How to cite this article:
Choudhary K, Nandlal B. Comparative evaluation of shear bond strength of nano-hydroxyapatite incorporated glass ionomer cement and conventional glass ionomer cement on dense synthetic hydroxyapatite disk: An in vitro study. Indian J Dent Res 2015;26:170-5

How to cite this URL:
Choudhary K, Nandlal B. Comparative evaluation of shear bond strength of nano-hydroxyapatite incorporated glass ionomer cement and conventional glass ionomer cement on dense synthetic hydroxyapatite disk: An in vitro study. Indian J Dent Res [serial online] 2015 [cited 2020 Oct 30];26:170-5. Available from: https://www.ijdr.in/text.asp?2015/26/2/170/159152
With the dawn of esthetic dentistry, esthetic restorative materials are the preferred choice for various applications. These novel restoratives have proved successful due to their ability to match the tooth color and withstand the dynamic oral environment.

Glass polyalkenoate cements are materials made of calcium or strontium alumina fluoro silicate glass powder (base) combined with a water-soluble polymer (acid). Kent called such materials "glass ionomer" cements, and that name has become part of the dental vernacular. Glass ionomers were invented in 1969 and reported by Wilson and Kent in the early 1970s. [1]

Glass ionomer cement (GIC) is favorable restorative materials due to their ease of use and unique biocompatibility among direct restoratives. However, brittleness limits their use in the load bearing posterior region. A low abrasion resistance and inferior strength, toughness, and fatigue performance currently contraindicates the application as a permanent class I or class II filling materials. Several attempts in improving their mechanical parameters are still underway, and some forecast a promising future for GIC as a dental filling material with extended indications.

Hydroxyapatite (HAp, Ca 10 [PO 4 ] 6 [OH] 2 ) is a typical biomineral that is abundant in organisms. It can be used as bone scaffolds and luminescence materials, and it also has many important applications in drug delivery and biomedical engineering based on its chemical and biological similarity with the mineral constituents of human bones and teeth. To date, various derivatives of HAp, such as carbonated HAp, strontium HAp, F-substituted HAp, and HAp-based nanocomposites, have been reported. [2]

Because of their limited strength and wear resistance, GIC are indicated generally for the restoration of low-stress areas where caries activity potential is of significant concern. Therefore, HAp materials were added to improve the consistency and compressive strength of GIC. GICs have the ability to adhere to HAp resulted in a variety of clinical application in dentistry.

Variations in research methodology and protocols suggest that, the reports from different researchers may be contradictory and comparison between studies may be difficult. Therefore, the standardization of testing parameters is being emphasized which includes standardization of substrate also. [3]

Human dental enamel has traditionally been used as substrate for various laboratory-based testing. However, the use of extracted teeth for research continues to have potential disadvantages like lack of consistency of crown surface contours, variations in mineralization patterns, presence of surface defects, and problems of appropriate disinfection and storage. [4],[5],[6]

Dense synthetic HAp is being investigated in an attempt to develop an artificial substrate, which is closer to enamel in terms of composition and surface features. [7],[8]

As GIC adheres to tooth structure, the present study has been designed to assess the effect of incorporation of nano-HAp on the bonding ability of conventional GIC in terms of shear bond strength using the dense synthetic HAp disk.

The results obtained from this study, if favorable, may positively enhance the role of nano-HAp incorporated GIC as a restorative material encompassing aesthetics, fluoride release, and strength into one.


   Materials and Methods Top


The present study was done at Department of Pedodontics and Preventive Dentistry, JSS Dental College and Hospital, Mysore. Shear bond strength were tested at Sundaram Polymers Division of Brakes India Limited, Nanjungud using "universal testing machine."

Conventional GIC was used in this study as the control and base material. The nano-HAp powder (Ca 10 [PO 4 ] 6 [OH] 2 ), used with 10-20 nm crystalline size (Granular) and 10 μm particle size. Eight weight percent (8% w/w) of the conventional GIC powder was replaced by nano-HAp as this proportion of HAp had led to the highest increase in flexural strength as was shown in an initial investigation by Arita et al. [9]

Twenty-six dense synthetic HAp disks were used in this study and were divided into two equal groups of 13 each. Each disk was embedded in self-cure acrylic resin (similar to study done by Li et al.) [10] using a customized jig of 35 mm × 40 mm × 2.5 mm dimension. The methodologies adopted during this study were the same as it were standardized during previous study (unpublished thesis by Roli Agrawal et al.; 2012 from JSS University; Mysore, titled "comparative evaluation of shear bond strength of HAp incorporated and conventional GIC on dense synthetic HAp disk-an in vitro study" adopted from the study by Li et al.) Metal jigs were painted with nail varnish, and the transparent adhesive tape was stuck over it to prevent leaching of metal ions from the jig during the entire procedure until strength testing.

Surface pretreatment of HAp disk was done using silicon carbide paper (no. 2500), then surface conditioning with 10% polyacrylic acid was done for 20 s. A metal bonding jig was prepared for stabilizing the HAp disk during the bonding procedure [Figure 1]. Holes of 3 mm diameter were punched in a teflon sheet of 2 mm thickness and hence that samples of the uniform dimension of 3 mm × 2 mm could be obtained. Teflon was then split exactly through the center so that it could be removed from prepared sample without applying undue force.
Figure 1: Customized bonding jig with split teflon mold

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The conditioned HAp disk assembly was seated in bonding jig and split teflon mold were secured in position exposing the bonding site. The teflon mold was filled with GIC using plastic filling instrument [Figure 2]. Varnish was applied on the exposed surface. After initial set, the screws were loosened and HAp disk with GIC was retrieved from the jig [Figure 3]. It was then stored in distilled water at 37°C for 24 h before bond strength testing.
Figure 2: Packing of cement

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Figure 3: Prepared samples

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Shear bond strength of prepared samples were measured on a universal testing machine. A semicircular chisel was mounted on the upper member of the testing machine to debond the sample from HAp disks. HAp disk assembly was attached to the testing jig mounted in the lower member. The cutting edge of the chisel was engaged at the HAp-GIC interface and force were applied parallel to it at the cross head speed of 1 mm/min [Figure 4]. The maximum force needed to debond the sample was recorded in Newtons (N).
Figure 4: Shear bond strength testing in universal testing

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Following statistical methods were applied to the present study:

  • Descriptive statistics
  • Independent samples t-test.



   Results Top


The shear bond strength ranged between 2.14 and 5.15 MPa for nano-HAp incorporated and 3.83-7.23 MPa for conventional GIC.

The mean shear bond strength observed for nano-HAp incorporated and conventional GIC were 3.28 ± 0.89 MPa and 5.25 ± 0.88 MPa, respectively with a mean difference of 1.97 [[Table 1] and Graph 1].
Table 1: Intergroup shear bond strength comparison of nano-hydroxyapatite incorporated and conventional GIC


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Statistical analysis revealed t-value of 5.664 with 24 degree of freedom. A very highly significant difference (P < 0.001) was found between the mean shear bond values of nano-HAp incorporated and conventional GIC.

The samples after bond strength testing were evaluated to determine the type of fracture. The types of fracture occurred were:

  • Adhesive (A): Failure at the GIC-HAp disk interface
  • Cohesive (C): Complete failure in GIC
  • Mixed (M): Combination of adhesive and cohesive failure.


In nano-HAp incorporated GIC group, the failure mode distribution among a total of 13 samples were observed as cohesive failure in 3 (23.1%) and mixed failure in remaining 10 (76.9%) samples, whereas for conventional GIC group showed cohesive failure for 10 (76.9%), mixed failure for 2 (15.4%), and adhesive failure for 1 (7.7%) [[Table 2] and Graph 2].
Table 2: Percentagewise distribution of failure modes at fracture sites of nano-hydroxyapatite incorporated and conventional GIC


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   Discussion Top


Glass ionomer cement is known for its ability to chemically bond to tooth substrate, so it is of great concern that the incorporated HAp should not interfere with the bonding ability of GIC.

Glass ionomer cement glass is mainly composed of SiO 2 , AlO 3 , CaF 2 , Na 3 AlF 6 , and AlPO 4 . However, strontium can be substituted for calcium with little change in the GIC structure in order to increase the capacity of GIC to X-rays, because strontium and calcium have similar ionic radii. Fuji IX (Lot No. 1309281, GC Corporation, Tokyo, Japan) was selected as the base GIC material because it is one of the strongest commercially available conventional restorative GIC, and is recommended for this reason by World Health Organization for atraumatic restorative atraumatic.

Fuji IX contains strontium instead of calcium. The presence of strontium and the absence of calcium were verified by energy dispersion X-ray spectrometry and X-ray photoelectron spectroscopy analysis. It is, therefore, advantageous to use Fuji IX for investigation. [9]

In the present study, HAp disks had been used as substrate for bonding, as it closely resembles enamel in terms of composition and surface characteristics. [7],[8] This was an attempt made to standardize the substrate for bond strength testings.

In general, two substrates have been reported in the literature for adhesion testing-human and bovine teeth. Causton stated that the best substrate would be living human dentin. Difficulty with in vivo bond strength studies, however, has led to the almost exclusive use of extracted teeth for in vitro testing. [4]

During sample preparation, it was observed that for nano-HAp incorporated GIC, the setting time taken by this new material was more compared to the conventional GIC.

According to the study done by Roche, the nano-HAp appears to have improved the strength, it seriously degraded the working properties of the cement so that consistency between samples was poor and some batches could not be mixed at all. Modified cements were prepared by dispersing nano-HAp in the liquid component of the cement prior to mixing the cement and maximum of 0.5 wt% of nano-HAp were added. It is clear that although the addition of nano-HAp can be beneficial, the preparation procedure needs to be improved to obtain reliable results, even with low quantities of nanoparticle addition. The high surface to mass ratio of the nanoparticles makes them difficult to disperse, resulting in inconsistent mixing of the cement. [11] However, the role of nano-HAp on the setting reaction and proportion of both the material needs further elucidation.

The present study showed that the shear bond strength of nano-HAp incorporated GIC had very highly significant lower value than conventional GIC bonded to HAp disk. The values obtained for nano-HAp incorporated and conventional GIC were 3.28 ± 0.89 MPa and 5.25 ± 0.88 MPa, respectively. The 24 h shear bond strength values obtained from previous studies for conventional GIC ranged between 3 MPa and 7 MPa, [12],[13],[14] which is in correlation with our study.

The mean shear bond strength values obtained for nano-HAp incorporated GIC bonded to HAp disk (3.28 ± 0.89 MPa) was lower to the value obtained from study by Moshaverinia et al. (6.0 MPa), but in their study the teeth (dentin) were used as a substrate and Fuji II GC was used as a base material, which could account for the difference. [15] Yoshida et al. analyzed the chemical interaction of a synthesized polyalkenoic acid with enamel and synthetic HAp and pointed out that carboxylic groups of the polyalkenoic acid replaces phosphate ion of the substrate and make ionic bonds with calcium ions of HAp. [16]

This suggests that the HAp is participating in chemical changes that are taking place during the initial setting of the cement. [17] The HAp is soluble in acidic solution and its solubility rate is rapidly increased with a pH below 2.05 upon contact with polyacrylic acid (pH 1.23), calcium ions may be liberated from the surface of the HAp. It is possible that calcium from the added HAp is available earlier than other metal ions from the glass surface, that is, calcium, aluminum, strontium to react with polyacrylic acid. [17] Therefore this extra calcium which is available for the cement formation, polysalt bridge formation and cross-linking, all of which reinforce the glass ionomer matrix may increase the bonding inside the matrix but may be affecting the bonding ability of the GIC to the HAp surface. However, the role of nano-size particles on the micro-size particles of GIC and the ratio and proportions of nano-HAp to the GIC needs further elucidation.

For the nano-HAp incorporated GIC, it seems likely that the strength of cement is influenced by the size of particles and the powder-liquid ratio, leading to the recommendation that particles should not be too fine or too large in order to achieve high strength. [9]

It is possible that the reaction of the component of nano-HAp occurs more slowly compared to the micro-size particles due to the extremely high crystallinity, low specific surface area, and low porosity. [9]

While chemical reactivity generally increases with decreasing particle size, surface coatings, and their modifications can have complicating effects, even reducing reactivity with decreasing particle size in some instances. The atoms situated at the surface have less neighbors than bulk atoms, resulting in lower binding energy per atom with decreasing particle size. [18] This could explain the reason of decreased bond strength of nano-HAp GIC.

In the present study, nano-HAp added GIC showed mainly mixed type of failure whereas conventional group showed mainly a cohesive failure.

The cohesive failure observed with the conventional group was in accordance with the study by Fruits et al. [19] It implies that the interfacial strength of the cement-tooth bond is higher than the inherent strength of the material which also implies that conventional glass ionomer has poor fracture strength. Ngo et al. reported that the bond between the cement matrix and dental hard tissues was stronger than that between the matrix and the glass particles. [20]

Barry et al in his studies regarding HAp demonstrated that the chemical reaction of polyacrylic acid with calcium in sintered HAp resulted in the precipitation of insoluble calcium polyacrylate which is the same compound responsible for the initial set of GIC. [21] The addition of nano-HAp might had resulted in a strengthened matrix, therefore there was no adhesive failure observed and mainly the mixed type of failure mode was observed. However, there was adhesive failure noted in the case of conventional GIC. More number of mixed failure and no adhesive failure suggests that the bonding inside the matrix is increased.

The previous studies have been conducted with teeth as substrate and the role of HAp disk to analyze the failure mode of a restorative material needs further evaluation. Imthiaz et al. concluded that HAp could be used as an alternative to enamel for comparative laboratory studies until a closer alternative is found. [22]

In this study, intra-oral variables such as normal masticatory stress, moisture, intra-pulpal pressure, and operator inconsistencies were not taken into consideration. Therefore, further studies are necessary to test the long-term stability of these bonding mechanisms.


   Conclusion Top


The lower shear bond strength of nano-HAp incorporate GIC revealed that the addition of nano-HAp interfered with the bonding ability of GIC to the substrate interface, but the mixed type of failure in nano-HAp incorporated GIC suggests that it increases the strength of the matrix. However, the role of nano-size particles on the micro-size particles of GIC for the bonding mechanism and the ratio and proportions of nano-HAp to the GIC needs further elucidation.

 
   References Top

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Williams VD, Svare CW. The effect of five-year storage prior to bonding on enamel/composite bond strength. J Dent Res 1985;64:151-4.  Back to cited text no. 5
    
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Baldassarri M, Margolis HC, Beniash E. Compositional determinants of mechanical properties of enamel. J Dent Res 2008;87:645-9.  Back to cited text no. 8
    
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Arita K, Yamamoto A, Shinonaga Y, Harada K, Abe Y, Nakagawa K, et al. Hydroxyapatite particle characteristics influence the enhancement of the mechanical and chemical properties of conventional restorative glass ionomer cement. Dent Mater J 2011;30:672-83.  Back to cited text no. 9
    
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Li J, Liu Y, Liu Y, Söremark R. Bonding strength of glass ionomers to dense synthetic hydroxyapatite and fluoroapatite ceramics. Acta Odontol Scand 1996;54:19-23.  Back to cited text no. 10
    
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Roche KJ. Improving mechanical properties of glass ionomer cements with fluorhydroxyapatite nanoparticles. Dublin City University. Available from: http://www4.dcu.ie/sites/default/files/conference_sbc/Kevin%20Roche_UCD.pdf [Last accessed on 2015 May 19].  Back to cited text no. 11
    
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McCarthy MF, Hondrum SO. Mechanical and bond strength properties of light-cured and chemically cured glass ionomer cements. Am J Orthod Dentofacial Orthop 1994;105:135-41.  Back to cited text no. 12
    
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Moshaverinia A, Ansari S, Moshaverinia M, Roohpour N, Darr JA, Rehman I. Effects of incorporation of hydroxyapatite and fluoroapatite nanobioceramics into conventional glass ionomer cements (GIC). Acta Biomater 2008;4:432-40.  Back to cited text no. 15
    
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Yoshida Y, Van Meerbeek B, Nakayama Y, Snauwaert J, Hellemans L, Lambrechts P, et al. Evidence of chemical bonding at biomaterial-hard tissue interfaces. J Dent Res 2000;79:709-14.  Back to cited text no. 16
    
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Fruits TJ, Duncanson MG Jr, Miller RC. Bond strengths of fluoride-releasing restorative materials. Am J Dent 1996;9:219-22.  Back to cited text no. 19
    
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Ngo H, Mount GJ, Peters MC. A study of glass-ionomer cement and its interface with enamel and dentin using a low-temperature, high-resolution scanning electron microscopic technique. Quintessence Int 1997;28:63-9.  Back to cited text no. 20
    
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Correspondence Address:
Dr. Kanupriya Choudhary
Department of Pedodontic and Preventive Dentistry, JSS Dental College and Hospital, Mysore, Karnataka
India
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Source of Support: None, Conflict of Interest: None


DOI: 10.4103/0970-9290.159152

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    Figures

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