1. Introduction
Complete dentures are removable prostheses designed to fit the upper and lower jaws with oral mucosa support in cases where all teeth have been lost due to various causes such as caries, bone resorption, or trauma [
1]. The denture base materials used in complete dentures play a fundamental role in meeting the functional, aesthetic, and phonetic needs of edentulous patients. These materials must ensure biocompatible adaptation to the oral tissues, resistance to masticatory forces, and long-term dimensional stability. A denture base material with inadequate physical or mechanical properties may negatively affect the retention and stability of the prosthesis, potentially leading to clinical problems such as tissue irritation, prosthesis fractures, and decreased patient satisfaction [
2].
Various methods have been employed in the fabrication of complete dentures using polymethyl methacrylate (PMMA) resin [
3,
4]. The most commonly used technique for producing complete denture bases is the conventional compression molding method. While this method offers advantages such as ease of application and low cost, it may also present drawbacks such as polymerization shrinkage and porosity [
2].
Another method is subtractive manufacturing (milling) using computer-aided design and computer-aided manufacturing (CAD/CAM). With the increasing adoption of CAD/CAM technology in dentistry, complete denture bases can now be fabricated through subtractive manufacturing. In this technique, pre-polymerized industrial PMMA blocks are milled using machines to match the digitally designed denture form. The CAD/CAM method provides significant advantages, including high dimensional accuracy, a porosity-free structure, homogeneous polymerization, and enhanced mechanical strength. Additionally, digital archiving facilitates the easy reproduction of dentures and reduces the risk of cross-contamination. However, this method also has certain limitations, such as material waste and restricted ability to reproduce fine details [
5].
While the CAD/CAM denture base fabricated by the subtractive method consists of DCL-filled PMMA, in this method the denture base is digitally designed, and the UDMA-based 3D denture base is produced by layer-by-layer photopolymerization of resins using light” [
6].
In parallel with subtractive methods, advancements in additive manufacturing have further expanded the possibilities for denture base fabrication. In this method, the denture base is digitally designed and produced by layer-by-layer polymerization of photopolymer resins using light [
7]. Dentures manufactured through 3D printing offer advantages such as high surface detail, reduced production time, and the potential for customization. However, the biological and mechanical adequacy of the resins used in the printing process remains an ongoing subject of research, and long-term clinical data are still limited [
8].
While these manufacturing methods enhance prosthetic fabrication, the prolonged use of removable dentures continues to present biological and clinical challenges. One of the most critical issues is residual ridge resorption, which occurs with long-term denture use. This condition leads to pain, instability, and eventual prosthesis failure. In such situations, patients face two options: either complete replacement of the prosthesis or restoration with a relining material [
9].
Replacement of prostheses is a difficult, costly procedure that requires several appointments for both the patient and the clinician [
10]. Therefore, it is very important to maintain patients’ existing prostheses. It is usually preferred to restore the patient’s prosthesis with a relining material [
11].
The bonding between the removable prostheses and the reline materials is of great importance during the procedure [
12]. Many studies have been conducted on the bonding properties between denture reline materials and denture base polymers [
13]. Tensile bond strength testing is frequently employed to evaluate the adhesion between denture base and reline materials as removable dentures are not only subjected to compressive masticatory forces but also to tensile stresses during insertion, removal, and functional vacuum effects in the oral cavity [
9].
The bond strength is determined by a number of factors, including the type of denture base resin, the composition of the denture liner, and the bonding agent. In addition, different surface treatments applied to the prosthesis base affect the connection of the prosthesis. Mechanical surface treatments, including milling, airborne-particle abrasion, and lasers, have also been proposed to increase the contact area between the prosthesis and the reline material [
14].
Denture liners are available in two types: silicone-based and acrylic-based resins, which can be further divided into heat-polymerizing or autopolymerizing categories [
1]. Adhesives or primers are not required for denture liners made of acrylic resin because their chemical makeup is similar to that of the acrylic resins used in denture bases [
13]. However, because debonding from the denture bases will be expected more frequently, adhesives would be necessary for silicone-based resilient denture liners because they have different fundamental chemical structures [
15].
In the literature, while there are numerous studies on the restoration of conventionally fabricated denture bases with relining materials, there is a notable lack of data regarding the restoration of denture bases produced by CAD-CAM milling and 3D printing methods. Recent studies have highlighted the challenges of achieving durable bonding in 3D-printed denture bases and emphasized that additional surface or chemical modifications may be required to improve adhesion with relining materials [
16]. The aim of this study is to investigate the bond strengths of three different types of bases by applying two different roughening processes and bonding them with two different relining materials.
The first null hypothesis is that the surface-treated base materials are no different from those of the control group. The second null hypothesis is that there is no difference in bond strength between the different base materials.
2. Materials and Methods
In this in vitro study, complete denture base specimens were prepared using three different manufacturing methods: conventional heat polymerization (HP), CAD/CAM milling (ML), and 3D printing (3D). The specimens in each manufacturing group were randomly divided into three subgroups based on the surface treatment method applied: control (C), airborne-particle abrasion (A), and laser surface treatment (L). The specimens were assigned to these subgroups using simple randomization with a computer-based random number generator (Microsoft Excel, RAND function). Two different relining materials were used: Tokuyama Rebase II (hard, acrylic-based; H) and Mucopren Soft (soft, silicone-based; S). Consequently, a total of 18 experimental groups were formed according to the 3 (manufacturing) × 3 (surface treatment) × 2 (reline material) design. The experimental groups are illustrated in
Figure 1.
The methods, material compositions, and manufacturer information used in this study are presented in
Table 1.
The sample size was determined using GPower (GPower 3.1 software; Heinrich Heine University, Düsseldorf, Germany) with a 5% margin of error, an effect size of 0.4, and a test power of 85%.
Each test specimen consisted of two base segments bonded together with the relining material and was subjected to a tensile test. To obtain six specimens (n = 6) per experimental group, twelve base segments were used. A total of 36 bar-shaped specimens were produced for each group by preparing 72 base segments. Accordingly, 108 bar-shaped test specimens were prepared for the entire study by combining 216 base segments in pairs using the reline materials.
The specimens were designed in STL (Standard Triangle Language) format using CAD-CAM software SolidWorks (Dassault Systèmes SolidWorks Corp., Waltham, MA, USA, Solidworks 2021),with the dimensions of 10 × 10 × 20 mm [
17,
18] and these files were used during the milling or 3D printing processes.
Specimens that were fabricated in accordance with the standardized dimensions (10 × 10 × 20 mm) and exhibited no defects during production were included in the study. Specimens presenting insufficiently roughened surfaces, sudden fracture during tensile testing, visible deformation, or incomplete bonding with the relining material were excluded from the analysis and subsequently remanufactured.
For the HP group, wax replicas were milled from CAD/CAM wax blocks (Bilkim, İzmir, Türkiye) using a milling machine (Coritec 350i, imes-icore, Eiterfeld, Germany). These wax patterns were invested in dental stone and placed into metal flasks (MD-135, Meta Dental, Ankara, Turkey). After wax elimination, the cavities were filled with a mixture of 14 mL liquid and 35 g powder of heat-polymerized acrylic resin (Integra, Birleşik Grup Dental, Ankara, Turkey) and prepared in accordance with the manufacturer’s instructions. Polymerization was carried out in boiling water at 100 °C for 30 min. This process was used to fabricate the denture base specimens for the conventional group.
For the milling group (M), IvoBase CAD PMMA discs (IvoBase CAD, Ivoclar Vivadent, Liechtenstein) were milled into 10 × 10 × 20 mm base specimens using a milling machine (Coritec 350i, imes-icore, Eiterfeld, Germany).
For the 3D printing group (3D), specimens measuring 10 × 10 × 20 mm were fabricated using a 3D denture base resin (Saremco Print Denturetec) with a 3D printer (Asiga MAX UV 3D), in accordance with the manufacturer’s instructions. Upon completion of the printing process, the specimens underwent a two-step cleaning protocol in 96% isopropyl alcohol. The first wash was conducted for 5 min, followed by a second wash in fresh solution for 3 min. After washing, the specimens were air-dried to ensure no solvent residues remained on the surface.
Subsequently, the specimens were subjected to a post-curing process for 20 min in an inert atmosphere (nitrogen gas) using a light source with a wavelength of 385 nm (Otoflash G171), as recommended by the manufacturer.
All specimens were stored in a water bath at 37 ± 1 °C (Nüve Incubator, Istanbul, Turkey) for 30 ± 2 days following fabrication. Afterwards, they were subjected to thermocycling for 5000 cycles between 5 °C and 55 °C, with a 60 s dwell time and a 30 s transfer time between baths [
19].
The specimens in each manufacturing group were divided into three subgroups according to the surface treatment applied. In the control group (C), no surface treatment was performed. In the airborne-particle abrasion group (A), the specimens were sandblasted with 100 µm aluminum oxide (Al
2O
3) particles at a pressure of 2 bar, from a distance of 10 mm for 10 s (Basic Quattro, Renfert, Germany). After the procedure, the surfaces were cleaned with oil-free compressed air [
14].
In the laser group (L), the bonding surfaces of the specimens were treated with an Er/YAG laser (LightWalker AT, Fotona, Slovenia) with a wavelength of 2940 nm, an energy of 150 mJ, and a power output of 1.5 W. The laser was applied with a pulse duration of 700 µs and a frequency of 10 Hz, using a 4 mm spot diameter from a 10 mm distance for 20 s.
Following the surface treatments, the specimen blocks were positioned facing each other with a 3 mm space between them (
Figure 2a). Custom-designed boxes that could hold the denture base blocks were created in STL format and fabricated (
Figure 2b). Using these boxes, the specimens were appropriately bonded with the designated reline materials (
Figure 2c).
Tokuyama Rebase II was applied in accordance with the manufacturer’s instructions. First, an adhesive was applied to the bonding surfaces of the denture base materials. Then, two doses from the dropper of Tokuyama Rebase II liquid were mixed with approximately one dose of Tokuyama Rebase II powder in the measuring cup. To minimize air bubbles, the powder was added into the liquid. The mixture was gently stirred with a spatula for about 5–10 s. Then, the reline material was applied to the specimen surfaces within 20 to 60 s (at room temperature). For complete polymerization of the reline material, one dose of Tokuyama Resin Hardener II was dissolved in 200 mL of water at a temperature of 40–60 °C (104–140 °F) in a beaker, and the bonded specimen was immersed in this solution for 3 min.
Mucopren Soft was applied in accordance with the manufacturer’s instructions. First, a single layer of adhesive was applied to the bonding surfaces of the denture base materials and left to dry for 90 s, followed by a second adhesive layer. Then, Mucopren® Soft was mixed evenly using a dispensing gun and used to bond the two specimens together. The 3D-printed and milled specimens were kept in a warm water bath (30 °C/86 °F–35 °C/95 °F) for 2 h. Mucopren® Soft (Kettenbach GmbH & Co. KG, Eschenburg, Germany) was applied in accordance with the manufacturer’s instructions.
One hour after the application of the reline materials, the bonded specimens were immersed in a water bath (Nüve Incubator, Istanbul, Turkey) at (37 ± 1) °C for (23 ± 1) hours [
17,
20].
The specimens were then placed in a Universal Testing Machine (Devotrans, D.V.T. GPE 5 KN YBS, İstanbul, Turkey) for tensile testing, and the schematic representation of the test setup is shown in
Figure 3.
The denture specimens were subjected to tensile force at a crosshead speed of 5 mm/min using a universal testing machine (Devotrans, D.V.T. GPE 5 KN YBS, Turkey) until failure occurred. The maximum tensile load prior to fracture was recorded in Newtons (N). The tensile bond strength values (in MPa) were calculated by dividing the maximum load (N) by the cross-sectional bonding area in mm2. The bonding area was taken as 100 mm2 (10 × 10 mm) for all denture base specimens.
To observe the effects of the surface treatments on the denture base materials, one specimen from each subgroup was randomly selected. The surfaces of these specimens were examined at various magnifications (500× to 10,000×) using a scanning electron microscope (Hitachi VP-SEM SU1510, Tokyo, Japan).
4. Discussion
In this study, the bond strength between denture base materials fabricated using different manufacturing methods and a reline material was evaluated following various surface treatment protocols. The findings revealed that bonding performance was significantly influenced by the type of material used, surface preparation, and relining technique; therefore, both null hypotheses were rejected.
The material type had a statistically significant effect on bond strength, with the highest values observed in the CAD-CAM milled group (
p < 0.001). These results are consistent with previous studies reporting that CAD-CAM milled materials exhibit higher mechanical strength and bonding capacity due to their high density and low porosity [
21].
In conventionally processed and CAD-CAM fabricated denture base materials, solvents or monomers are often applied to the base surface to promote chemical bonding with reline materials. This process induces swelling of the PMMA surface, facilitating monomer diffusion and enabling the formation of an interpenetrating polymer network (IPN) upon polymerization. The thickness of the IPN—and consequently the bond strength—is directly related to the degree of swelling of the PMMA [
21]. Solvents such as acetone, chloroform, and dichloromethane enhance this swelling, thereby improving bond strength. The presence of acetone in the monomer content of Tokuyama Rebase II may have contributed to the high bond strength observed in both the CAD-CAM (12.229 ± 0.78 MPa) and conventional (11.465 ± 0.773 MPa) groups [
22].
While polymerization in conventionally processed PMMA occurs through linear chain formation, 3D-printed resins typically incorporate multifunctional monomers such as bisphenol-A dimethacrylate (Bis-GMA) and urethane dimethacrylate (UDMA), resulting in highly cross-linked networks. These structures exhibit lower permeability and swelling in response to solvents, which restricts monomer diffusion and limits IPN formation. As a result, chemical bonding with hard reline materials may be adversely affected in 3D-printed denture base materials [
21].
This may explain the lower bond strength observed in the 3D-printed denture base group. According to the literature, DLP resins containing UDMA exhibit high chemical stability against solvents and show no significant changes in surface morphology [
21]. In line with the findings of the present study, previous research has also reported that bonding of hard reline materials to 3D-printed resin bases is less effective compared to conventionally processed bases [
23,
24].
SEM analysis results revealed that surface morphology was significantly affected by both the manufacturing method and the applied surface treatment. The smoother and more homogeneous surfaces observed in the CAD-CAM milled specimens support the higher bond strength found in this group [
17]. This finding is consistent with studies reporting that CAD-CAM materials, due to their lower porosity and denser structure, offer improved chemical and mechanical bonding with reline materials [
21].
Conversely, the pronounced microporosities observed in the control group of the 3D-printed specimens indicate a more heterogeneous surface structure, which may have reduced the interpenetration capacity and subsequently lowered bond strength [
24].
Surface treatment methods also significantly affected bond strength (
p < 0.001). Both sandblasting (6.76 MPa) and laser surface modification (6.2 MPa) significantly improved bonding compared to the untreated control group (4.49 MPa). The increase in surface roughness enhances mechanical interlocking, thereby contributing to improved bond strength [
14,
25]. Sandblasting not only removes surface contaminants but also increases surface roughness and the bonding area, which in turn enhances mechanical adhesion [
18,
22]. Following Al
2O
3 sandblasting, a high degree of surface roughness—particularly in the 3D-printed group—was observed due to intense particle embedding; while this improved mechanical retention, it also highlighted that chemical structure and monomer compatibility are critical determinants of bonding success [
13].
Although laser treatment produced microporous and irregular surface morphologies in some groups, the increase in surface area did not contribute to bond strength as effectively as sandblasting. In the conventional group, in particular, the fibrous cracks observed after laser treatment (
Figure 5i) suggest potential weak points for bonding [
14,
26]. However, a contrasting result was reported in a similar study by Korkmaz et al. (2013), where the control group exhibited higher bond strength than the specimens sandblasted with 50 µm Al
2O
3, which is inconsistent with the findings of the present study [
27]. This discrepancy may be attributed to the particle size of the Al
2O
3 used for sandblasting. In our study, Li et al. (2024), who used a similar particle size of 110 μm Al
2O
3, reported a significant increase in bond strength following surface roughening, supporting our findings [
18]. SEM analysis also confirmed that sandblasted surfaces exhibited greater roughness, further validating these results. Additionally, the presence of residual Al
2O
3 particles on the surface may negatively influence chemical bonding. Overall, the findings align with the existing literature, which supports the enhancement of bond strength through surface roughening techniques [
28].
The Er/YAG laser has the capacity to modify surface morphology by inducing controlled ablation on substrates such as dentin, acrylic, and similar materials. During laser application, rapid water evaporation and volumetric expansion cause micro-ablation on the surface, thereby increasing the surface area and creating microscopic irregularities. The resulting roughness and elevated surface energy expand the adhesive material’s contact area, reduce the contact angle, and facilitate the penetration of especially viscous reline materials [
14,
26,
27]. In line with these mechanisms, Moussa et al. (2024) reported that laser-treated denture base materials exhibited increased surface roughness and enhanced bond strength [
23]. Similarly, in the present study, laser surface treatment resulted in higher bond strength compared to the untreated control group, supporting the beneficial effects of laser-induced surface modification.
In the results regarding Mukopren bond strength, sandblasting was found to be more effective than laser surface treatment. A review of the literature reveals mixed findings: while laser treatment has been reported to either enhance or have no significant effect on the bonding of soft liner materials, sandblasting has often been found to have little or even detrimental effect [
25,
29,
30]. Consistent with our findings, Nakhaei et al. (2016) reported that air abrasion with 110 µm alumina particles created surface irregularities on the denture base, thereby increasing mechanical retention and improving bond strength [
28]. In contrast, Gundogdu et al. (2014) found that Er/YAG laser treatment using 150 mJ energy and 100 µs pulse duration did not enhance the bond strength of PMMA resin to autopolymerized silicone-based soft liners [
30]. One possible explanation for the lower bond strength observed with laser treatment could be the non-uniform surface irregularities caused by sweeping laser motions. These irregularities may have created voids that the soft liner material could not adequately flow into or adapt to, thereby reducing the effectiveness of bonding compared to the more consistent micro-retentive pattern achieved by sandblasting [
31].
The choice of the relining material was one of the most influential factors affecting bond strength (
p = 0.001). Bond strength values were significantly higher when Tokuyama Rebase II was used, with an average of 10.917 MPa, whereas this value was only 0.911 MPa with Mucopren Soft. In a study by Awad et al. (2023), similar trends were reported: the lowest bond strengths were observed with chairside soft reline materials, while the highest were achieved with hard laboratory-processed reline materials [
17]. Autopolymerizing silicone-based soft liners are structurally classified as polysiloxanes and generally exhibit low bonding affinity to denture base resins. This is because their adhesion is not directly to the base surface but occurs through limited infiltration, often mediated by a primer or adhesive layer applied during surface treatment [
21,
24,
30]. According to Craig and Gibbons (1961), a bond strength of 0.45 MPa is considered clinically acceptable for soft reline materials [
32]. Although no statistically significant difference in bond strength was found between different base material fabrication methods for the soft liner, all groups in our study exceeded this clinically acceptable threshold [
32].
In their in vitro study, Janyaprasert et al. (2024) compared the bond strength of denture base materials fabricated using heat polymerization, CAD/CAM milling, and 3D printing techniques after thermocycling, using various relining materials [
33]. Higher bond strength values were observed in the heat-polymerized and milled groups, whereas the 3D-printed group exhibited the lowest values. This outcome can be attributed to the lower cross-linking density and oligomer-based composition of 3D-printed materials, which make them more susceptible to thermal stress. The repeated thermal fluctuations induced by thermocycling may cause microscopic degradation in these materials, weakening the interfacial bond. Conversely, the high bond strength values observed in the milled groups with certain relining materials suggest that these materials are more stable under thermal stress and may therefore be more suitable for clinical use [
33].
The limitations of this study include the inability to fully replicate the complex dynamics of the intraoral environment, such as saliva, thermal fluctuations, and masticatory forces. This limits the direct clinical applicability and generalizability of the obtained bond strength results. Only two types of relining materials (hard and soft) and three different denture base materials were evaluated. Considering the broader range of materials available in the literature, the generalization of the findings to all clinical scenarios is constrained. Additionally, the bonding surface area in the specimens was standardized at 100 mm2. However, in actual prostheses, anatomical and morphological variations may significantly influence bonding behavior, which should be taken into account when interpreting the results.
In future studies, the variety of the denture base and relining materials should be expanded. Products from different manufacturers should be compared, with particular focus on the performance of advanced materials such as next-generation hybrid structures and nano-composite-based systems. The bonding characteristics and biomechanical behavior of these innovative materials, when compared to conventional systems, could provide valuable insights to guide clinical applications. Moreover, surface treatment should not be limited to mechanical methods alone. The integration of chemical agents—such as monomers, solvents, and silane-based modifiers—with mechanical surface treatments should be explored to evaluate potential synergistic effects. Such combination strategies may offer significant improvements, especially for 3D-printed resins, which tend to exhibit lower bond strength