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Article

Evaluation of Microleakage, Tensile Bond Strength, and Adhesive Interface of Bulk Fill, Ormocer, and Alkasite Against Conventional Composite in Caries-Affected Primary Molars

by
Nourah N. Shono
and
Fahad Alkhudhairy
*
Restorative Dental Sciences Department, College of Dentistry, King Saud University, Riyadh 11545, Saudi Arabia
*
Author to whom correspondence should be addressed.
Coatings 2025, 15(3), 321; https://doi.org/10.3390/coatings15030321
Submission received: 13 February 2025 / Revised: 3 March 2025 / Accepted: 7 March 2025 / Published: 10 March 2025
(This article belongs to the Special Issue Bioactive Coatings on Elements Used in the Oral Cavity Environment)
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Abstract

This study presents an evaluation of the microtensile bond strength (µTBS) and microleakage (ML) of a bulk-fill (BF) composite, Ormocer, and Alkasite in comparison to the conventional composite bonded to caries-affected dentin (CAD) in deciduous dentition. Eighty-four human primary molars displaying carious lesions involving the middle third of dentin were included. CAD was exposed, and the teeth were randomly assigned to four groups based on the type of restorative material used: Group 1 (conventional composite), Group 2 (BF composite), Group 3 (Alkasite), and Group 4 (Ormocer). Sample storage and artificial aging were performed. Dye penetration, a universal testing machine, and a stereomicroscope were used for microleakage, µTBS, and failure mode assessment. The interface was evaluated by scanning electron microscopy (SEM). µTBS and ML results were analyzed using a one-way analysis of variance (ANOVA) and Tukey’s post hoc tests (p < 0.05). Group 1 (conventional composite) exhibited the highest microleakage and lowest bond strength. The minimum ML and maximum μTBS values were demonstrated by Group 4 (Ormocer). Ormocer and Alkasite proved to be better alternatives to conventional composites in terms of ML and bond strength in deciduous dentition.

1. Introduction

Restorative dentistry combines scientific knowledge with artistic skills, encompassing various components [1]. Success in this area depends on achieving an optimal balance between function and aesthetics in dental procedures [2]. A significant concern is the worldwide prevalence of dental caries in primary teeth, which can reach up to 90% [3]. The minimally invasive dentistry (MID) approach aims to preserve caries-affected dentin (CAD) while removing infected tissues [4]. Previous research has shown that restoring CAD in both primary and permanent teeth leads to a substantial reduction in microtensile bond strength (µTBS) and increased microleakage (ML) compared to sound dentin [4].
There is no clear consensus in the dental literature regarding the optimal restorative material for primary teeth, necessitating further research and guidance in this area [5]. Resin-based composite (RBC) materials are commonly preferred for their aesthetic qualities in restorative procedures, owing to their ease of use, minimal tooth structure removal, and suitability for direct application [5,6,7]. However, a major disadvantage of these composites is the shrinkage that occurs during polymerization, potentially leading to compromised restoration edges and an elevated risk of secondary decay [8]. To combat these polymerization shrinkage issues, researchers are working on modifying traditional composites to enhance the durability and effectiveness of restoration.
Recently, bulk-fill (BF) resin-based composites have attracted considerable attention in the dental field. This material is characterized by its larger filler particle size, which can exceed 20 μm, and lower filler content compared to conventional composite resins [5]. These modifications enhance translucency and enable a more profound cure, reaching depths of up to 4 mm [9]. A laboratory study conducted by AlQhtani et al. demonstrated that the BF resin composite exhibited superior µTBS and reduced microleakage scores in primary molars compared with other tested groups [10]. Nevertheless, available information remains limited, necessitating further research on CAD surfaces.
Ormocer, an acronym for organically modified ceramics, has emerged as a promising dental material. This innovative composite resin was engineered to combat polymerization shrinkage, boost wear resistance, and improve edge adaptation, ultimately prolonging the lifespan of dental restorations [11]. Certain Ormocer-based products, such as Admira Fusion, have demonstrated superior flexural strength compared to bulk-fill composites [12]. Moreover, the incorporation of amide groups into ormocers increases their affinity for dental tissues, establishing them as a favored option for dental restoration treatment [13]. Nonetheless, further investigations are required to assess their suitability as restorative materials for primary CAD molars.
Alkasite, an advanced composite material, contains alkaline fillers that release fluoride, calcium, and hydroxide ions. A notable example of this type is Cention N®, which is characterized by its exceptional longevity, pleasing aesthetics, dual-curing functionality, and effectiveness in bulk-fill applications [14]. Contemporary research indicates that Alkasite demonstrates superior marginal sealing capabilities compared with alternative materials tested for permanent dental restorations [14,15]. In terms of shear bond strength (SBS), Alkasite outperforms glass ionomer cement (GIC). Moreover, it exhibits a higher immediate and delayed SBS than GIC [16]. Although Alkasite shows considerable potential, additional comprehensive long-term studies are essential to fully elucidate its performance across diverse clinical applications [16].
The present study was conducted based on the assumption that a notable significant difference would be observed in the ML of a BF composite, Ormocer, and Alkasite when compared with traditional composites bonded to CAD in primary molars. Additionally, it was expected that µTBS would be greater in various filler-modified composites than in the conventional control. Consequently, this laboratory investigation aimed to assess and compare the mechanical characteristics (ML, µTBS) and adhesive interface via scanning electron microscope (SEM) of a BF composite, Ormocer, and Alkasite against the conventional composite in primary teeth.

2. Materials and Methods

CAD Identification and Inclusion of Samples: This study included 84 primary human molars with carious lesions classified according to the International Caries Detection and Assessment System (ICDAS) 5, which extends into the middle third of dentin [17]. The number of samples was calculated using the WHO sample size calculator with a confidence level of 95%, an anticipated population proportion of 70%, and an effect size of 10% [4,17]. The penetration depth of CAD was verified by radiographic examination. Each specimen underwent a thorough sterilization process by being submerged in 1% thymol solution (Aladdin Industrial Co., Shanghai, China). All the attached debris was meticulously removed using an ultrasonic scaler. Dentin that displayed black staining, mushiness, and softness was identified as infected and was subsequently excised. Various techniques have been used to identify the presence of CAD, such as visual examination, an evaluation of surface hardness with a dental explorer, and the staining of dentin using 0.5% basic fuchsin. Dentin exhibiting both hardness and a pink hue following staining was classified as CAD [4,17].
Sample Preparation and Randomization: The samples were immersed in an auto-cure acrylic resin (Technovit 4004; Kulzer, Germany). The occlusal surface was flattened by placing a diamond bur (Edenta, Euadd, Edenia, GmbH, Switzerland, Eagle Dental, Kiryat Ata, Israel) perpendicular to the long axis of the tooth using a straight slow-speed handpiece (HAY-L-711484, Beijing, China). Sample preparation was performed by a single operator (NNS). The teeth were randomly assigned via a simple random sampling technique into four groups according to the type of restorative material used (n = 21) [4].
Group 1 (Conventional Resin Composite): A layer of one coat self-etching bond (OC) primer (Coltene Whaledent, Altstätten, Switzerland) was applied gently and allowed to stay for 20 s, followed by air thinning. The bonding agent was applied in the same manner as the primer and thinned with air for 10 s. The bonding agent was photopolymerized using LED light (3 M ESPE Elipar Deep Cure-L Light, Berlin, Germany) for 10 s. A translucent plastic mold tube with dimensions of 4 mm in height and 5 mm in diameter was used to build the composite resin (GrandioSO, Voco; GmbH, Germany shade A1) in 2 mm increments, followed by light curing for 40 s [1]. Group 2 (BF Resin Composite): The SE primer and bonding resin were applied in the same manner as in Group 1. The application of Tetric® N-Ceram BF composite (Ivoclar Vivadent Inc., NY, USA) was performed in a bulk increment of 4 mm, followed by a curing process lasting 40 secs. Group 3 (Alkasite): The CAD surface underwent thorough rinsing and was subsequently dried with a blotting paper strip. The bonding agent (Tetric N-Bond Ivoclar Vivadent) was meticulously applied and subjected to light curing for 15 secs. The cavity was subsequently restored using Alkasite-based material (Cention N) (Ivoclar Vivadent Inc., NY, USA, A2 shade). A ratio of 4.6 parts powder to 1 part liquid by weight was used to prepare the material. It was then photopolymerized for 20 s [18]. Group 4 (Ormocer): SE adhesive was applied in the same manner as in Group 1. A bulk-fill ORMOCER resin composite (Admira Fusion Xtra, VOCO GmbH) was placed into the mold in a single increment with a curing time of 40 s [19] (Table 1).
Sample Storage and Artificial Aging: The preservation of samples was performed in distilled water for 24 h at 37 °C. All samples underwent 10,000 temperature fluctuations in a thermocycler (Qiagen, Germantown, MD, USA) between 5 °C and 55 °C in a controlled water bath for 30 s in each bath with a transfer time of 5 s to stimulate oral conditions [20,21].
Dye Penetration Test for Microleakage Assessment: Through the use of nail paint, the entire surface of the 40 samples (n = 40) was coated, except for the 1 mm margin surrounding the restoration. After 24 h, each painted sample from each group was immersed in a separate reservoir containing 1% methylene blue dye solution. Subsequently, the remaining methylene blue was removed from the teeth using regular tap water. A microtome cutting machine (Perci, T201A, Paris, France) was used to longitudinally segment the samples to evaluate ML.
Protocol for µTBS Testing and Failure Mode Assessment: Six beams were cut from each sample (n = 10 in each group) using the same microtome machine to measure the bond strength. Beams were excluded if they had cracks or did not meet the requirements. At least five bonded beams measuring 1 mm wide and 8 mm long, with a bonding area of 1 mm2, were chosen from every tooth to assess the bond strength in all groups. Using cyanoacrylate adhesive (Zapit, Dental Ventures Inc., Ilinois, USA), the beams were attached to a universal testing machine (UTM) (Gester, Gester International Co., Beijing, China). A crosshead speed of 1 mm/min was used in the loading method to apply stress until a fracture point was reached. A stereomicroscope (Olympus SZX 16 Hachioji, Tokyo, Japan) with a magnification of 40× was used to identify the mode of failure after debonding, which was categorized as adhesive, cohesive, or admixed. Adhesive failure: failure between the adhesive and substrate (tooth or restorative material). Cohesive failure: failure occurring within the material. Mixed failure: combination of adhesive and cohesive failures
Interface Assessment using SEM (n = 1 for each group): The samples were sectioned in the same way as in the marginal leakage specimens. To reveal the resin tags, a 37% H3PO4 gel was applied to freshly sectioned teeth for 30 min, followed by air–water spray rinsing for 15 s. The specimens were then immersed in 2%NaOCl solution for 30 min. They were then rinsed thrice with distilled water. All specimens were affixed to aluminum stubs using carbon tape for gold sputtering (SPI Module Sputter Carbon/Gold Coater, EDEN instruments, Japan) and analyzed using SEM (JEOL, Ltd., Tokyo, Japan). Images were obtained at a magnification of 2000×, and the accelerating voltage was set to 30 kV.
Statistical Analysis: The normality of the data was assessed using the Kolmogorov–Smirnov Test. SPSS Version 23 (IBM, Chicago, IL, USA) was used for data analysis. The µTBS and microleakage results were analyzed using a one-way analysis of variance (ANOVA) and Tukey’s post hoc test (p < 0.05).

3. Results

ML assessment: Table 2 shows the ML of different restorations bonded to CAD in deciduous molars. The maximum values of ML were observed in Group 1 (conventional composite) (47.23 ± 0.10) samples. Nevertheless, the minimum ML was established by Group 4 (Ormocer) (13.22 ± 0.12) specimens. Comparison between different tested groups demonstrated that Group 3 (Alkasite) (15.24 ± 0.14) and Group 4 exhibited comparable scores of marginal sealing (p > 0.05). However, Group 2 (BF composite) (15.24 ± 0.14) presented significantly higher scores than Groups 3 and 4, yet lower scores than Group 1 (p < 0.05).
μTBS analysis: Table 3 displays the μTBS values of different restorations bonded to CAD in primary molars. The minimum values of bond strength were observed in Group 1 (conventional composite) (9.92 ± 0.53 MPa) samples. Nevertheless, the maximum μTBS was established in Group 4 (Ormocer) (13.42 ± 0.19 MPa). Comparison between different tested groups showed that Group 3 (Alkasite) (13.12 ± 0.16 MPa) and Group 4 exhibited comparable scores of bond integrity (p > 0.05). However, Group 2 (BF composite) (11.18 ± 0.22 MPa) presented significantly lower scores than Groups 3 and 4, yet higher scores than Group 1 (p < 0.05).
The failure mode analysis in Figure 1 presents the failure modes of the different investigated groups. Groups 3 and 4 predominantly presented cohesive fractures. However, admixed failures were mostly observed in Groups 1 and 2.
SEM Valuation: Figure 2: (A) SEM micrograph illustrates an occluded tubular dentin architecture exhibiting fissures. There exists inadequate adhesion at the junction between primary CAD and the conventional composite. (B) The SEM imagery reveals collapsed dentinal tubules alongside impaired resin tag development when CAD is rehabilitated using the bulk-fill composite. (C) The formation of pronounced resin tags with hybridization indicates a superior-quality adhesive interface when primary CAD is restored with Alkasite and (D) Ormocer.

4. Discussion

The present research was based on the hypothesis that there would be a significant difference in the marginal leakage of the BF composite, Ormocer, and Alkasite in comparison to conventional composites when bonded to CAD in primary molars. Additionally, it was expected that µTBS would be greater in various filler-modified composites than in the conventional control. Based on the outcomes obtained, it can be observed that the contemporary restorative materials displayed lower ML and higher bond integrity compared to the conventional composite used, thus allowing for both hypotheses to be accepted. To simulate oral conditions, the specimens were subjected to aging. Artificial aging techniques offer a predictive model for evaluating the durability of dental restorations, enabling more informed material choices in clinical settings [22].
The indexed literature suggests an inverse correlation between the ML score and µTBS. The results of this study demonstrated that Ormocer displayed the highest µTBS and minimal leakage scores, consistent with laboratory analyses conducted by Alla et al. [12], Ebaya et al. [23], and Dindaroğlu et al. [24]. The superior bonding capability of Ormocer compared to other tooth-colored restorative materials may be attributed to its reduced polymerization shrinkage stress, resulting from the inorganic–organic hybrid polymer that forms a siloxane network [12]. This innovative technology employs a three-dimensional polymerized structure with a decreased organic component compared to conventional resin composites, leading to diminished shrinkage and cytotoxicity while improving abrasion resistance and polishability [23].
Nevertheless, Alkasite’s bond strength and ML, which are comparable to those of Ormocer, align with the findings reported by Awad et al. [25]. This is mainly attributed to the bulk-fill characteristics resulting from compositional modifications. The powder component consists of various glass fillers, initiators, and pigments, while the liquid component contains di-methacrylates and initiators. Additionally, the incorporation of an isofiller enhances adhesion strength and reduces leakage [25,26]. The results of both groups can be further corroborated through SEM interface analysis, as they exhibited longer resin tags than the other tested groups
The BF composite demonstrated reduced ML and enhanced bond strength compared with traditional incrementally placed composites [27]. This can be attributed to its highly viscous nature, which results in less contraction during polymerization shrinkage. However, evidence regarding the mechanical properties of BF composites compared with CAD in primary teeth is inconclusive. Previous studies have shown that the marginal integrity of BF composite resin restorations in primary molars is not significantly different from that of incrementally placed conventional composite resins [27]. These findings align with the results of an in vitro study conducted by Eltoum et al. [28] Nevertheless, additional research is necessary to validate the findings of the current investigation.
Contrary to the existing literature, which generally reports similar outcomes for microleakage and bond strength between conventional and BF composite resins [29,30], the current study’s unexpected findings revealed that conventional composites had the lowest mechanical testing scores. This discrepancy may be attributed to excessive polymerization shrinkage [31]. Microleakage and sealing ability can be influenced by the physical properties of the composite, such as viscosity and filler content [32]. Furthermore, the inconsistency in findings across studies could be due to variations in methodological approaches, including thermal aging techniques, adhesive types, and restorative materials used [6,33].
Bond failure provides valuable information regarding the connection between restorative materials and dental structures [34]. When bonds between different materials break down, this is termed adhesive failure. In contrast, cohesive failure occurs when debonding occurs within a material [35]. Based on available evidence, cohesive failure can be attributed to several factors, including material defects, contamination, molecular interactions, and environmental conditions [36,37]. The bond scores obtained in the present study are supported by the presence of cohesive failure in Groups 3 and 4 and mixed failure in Groups 1 and 2.
This study has certain limitations. The artificial environment of the laboratory tests cannot fully replicate the actual conditions experienced during dental restorations in the mouth (i.e., mechanical stress, pH variations, masticatory forces, and cycling protocols), as it is nearly impossible to accurately simulate the oral cavity and its associated pressures. Evidence suggests that thermal cycling can effectively assess the durability of materials, but the results may not directly correlate with long-term clinical performance [38]. To validate the results obtained in this laboratory environment, future in vivo clinical trials should be conducted. Additionally, this study only examined the self-etch adhesive method for bonded restorations. Further investigation and analysis are required to evaluate other bonding techniques, such as total-etch and universal approaches, focusing on the formation of resin tags and measuring the depth of resin penetration. This should be followed by evaluations of the cell cytotoxicity of resin composites. Future investigations should employ atomic force microscopy (AFM) to assess surface changes after applying different adhesives to the CAD surface. Additional mechanical tests, including flexural strength, fatigue resistance, shear bond strength, and surface roughness measurements, should be conducted in subsequent studies to provide a more comprehensive evaluation of restorative materials.

5. Conclusions

Regarding marginal sealing and bond strength in primary dentition, Ormocer and Alkasite exhibited superior characteristics compared to conventional composite materials.

Author Contributions

Conceptualization, F.A. and N.N.S.; methodology, F.A. and N.N.S.; software, F.A. and N.N.S.; validation, F.A. and N.N.S.; formal analysis, F.A. and N.N.S.; investigation, F.A. and N.N.S.; resources, F.A. and N.N.S.; data curation, F.A. and N.N.S.; writing—original draft preparation, F.A. and N.N.S.; writing—review and editing, F.A. and N.N.S.; visualization, F.A. and N.N.S.; supervision, F.A.; project administration, F.A.; funding acquisition, N.N.S. All authors have read and agreed to the published version of the manuscript.

Funding

The authors are grateful to the Researchers Supporting Program (RSPD) at King Saud University for providing funding through project number (RSPD2025R815), Riyadh, Saudi Arabia.

Institutional Review Board Statement

The research experiments conducted in this article were approved by the Ethical Committee of King Saud University under CDRC number FC93-8623. The lab-based comparative study followed a checklist for reporting in vitro study (CRIS) guidelines.

Informed Consent Statement

Informed consent was obtained from all subjects involved in the study.

Data Availability Statement

The data can be made available on request.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. Percentage distribution of modes of failure.
Figure 1. Percentage distribution of modes of failure.
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Figure 2. (A) SEM micrograph depicts occluded tubular dentin structure with cracks (Arrows). Poor bonding at the interface between primary CAD to Conventional composite (×800). (B) SEM image depicts collapsed dentinal tubules with compromised resin tag formation when CAD is restored with Bulk fill composite (Arrows) (×800). (C) Prominent resin tags formation with hybridization demonstrating good quality adhesive interface when primary CAD restored with Alkasite (×750) and (D) Ormocer (Arrows) (×800).
Figure 2. (A) SEM micrograph depicts occluded tubular dentin structure with cracks (Arrows). Poor bonding at the interface between primary CAD to Conventional composite (×800). (B) SEM image depicts collapsed dentinal tubules with compromised resin tag formation when CAD is restored with Bulk fill composite (Arrows) (×800). (C) Prominent resin tags formation with hybridization demonstrating good quality adhesive interface when primary CAD restored with Alkasite (×750) and (D) Ormocer (Arrows) (×800).
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Table 1. Composition of Materials used in the study.
Table 1. Composition of Materials used in the study.
MaterialsComposition
Bulk-fill Composite GrandioSO, Voco; GmbH GermanyFiller 89% w/w: Glass Ceramic Filler; Functionalized Silicon Dioxide Nanoparticles; Iron Oxide; Titanium Oxide.Resin: BisGMa; TEGDMA
Camphorquinone Photocatalyst
Butylated Hydroxytoluene Stabilizer
BF composite Tetric® N-Ceram BF composite (Ivoclar Vivadent, NY, USA)Monomer Matrix: Mono-methacrylate and Di-methacrylate (28 wt.%) Fillers: Barium glass, Ytterbium trifluoride and Copolymers (71 wt.%). Additives, initiators, stabilizers and pigments are additional ingredients (<1.0 wt.%)
Alkasite (Cention N) (Ivoclar Vivadent Inc., NY, USA, A2 shade)Liquid consists of Methacrylate and initiators, while the Powder includes a mixture of glass fillers, initiators, and pigments
Ormocer (Admira Fusion xtra, VOCO GmbH)Pure silicate-based ORMOCER matrix, containing a high percentage of Nano-hybrid fillers (60% nano-particulate and 40% micro/macro-particulate). Free of traditional monomers like Bis-GMA or HEMA.
Table 2. Mean ± SD of ML scores among different restorative materials bonded to CAD in primary molars.
Table 2. Mean ± SD of ML scores among different restorative materials bonded to CAD in primary molars.
Experimental GroupsMean ± SDp-Value !
Group 1: Conventional Composite47.23 ± 0.10 c˂0.05
Group 2: BF Composite27.11 ± 0.11 b
Group 3: Alkasite15.24 ± 0.14 a
Group 4: Ormocer13.22 ± 0.12 a
! ANOVA. Bulk fill (BF). The different small superscript letters denote statistically significant differences (p < 0.05) (post hoc Tukey Multiple Comparison Test).
Table 3. Mean ± SD of µTBS scores among different restorative materials bonded to CAD in primary molars.
Table 3. Mean ± SD of µTBS scores among different restorative materials bonded to CAD in primary molars.
Experimental GroupsMean± SD (MPa)p-Value !
Group 1: Conventional Composite 9.92 ± 0.53 c˂0.05
Group 2: BF Composite11.18 ± 0.22 b
Group 3: Alkasite13.12 ± 0.16 a
Group 4: Ormocer13.42 ± 0.19 a
! ANOVA. Bulk fill (BF). The different superscript small letters denote statistically significant differences (p < 0.05) (post hoc Tukey Multiple Comparison Test).
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MDPI and ACS Style

Shono, N.N.; Alkhudhairy, F. Evaluation of Microleakage, Tensile Bond Strength, and Adhesive Interface of Bulk Fill, Ormocer, and Alkasite Against Conventional Composite in Caries-Affected Primary Molars. Coatings 2025, 15, 321. https://doi.org/10.3390/coatings15030321

AMA Style

Shono NN, Alkhudhairy F. Evaluation of Microleakage, Tensile Bond Strength, and Adhesive Interface of Bulk Fill, Ormocer, and Alkasite Against Conventional Composite in Caries-Affected Primary Molars. Coatings. 2025; 15(3):321. https://doi.org/10.3390/coatings15030321

Chicago/Turabian Style

Shono, Nourah N., and Fahad Alkhudhairy. 2025. "Evaluation of Microleakage, Tensile Bond Strength, and Adhesive Interface of Bulk Fill, Ormocer, and Alkasite Against Conventional Composite in Caries-Affected Primary Molars" Coatings 15, no. 3: 321. https://doi.org/10.3390/coatings15030321

APA Style

Shono, N. N., & Alkhudhairy, F. (2025). Evaluation of Microleakage, Tensile Bond Strength, and Adhesive Interface of Bulk Fill, Ormocer, and Alkasite Against Conventional Composite in Caries-Affected Primary Molars. Coatings, 15(3), 321. https://doi.org/10.3390/coatings15030321

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