The impact of delayed placement and resin matrix composition on adhesion between layers of resin composites

Authors

  • Suvi Vallittu Department of Biomaterials Science and Turku Clinical Biomaterial Center –TCBC, Institute of Dentistry, University of Turku, Turku, Finland
  • Sufyan Garoushi Department of Biomaterials Science and Turku Clinical Biomaterial Center –TCBC, Institute of Dentistry, University of Turku, Turku, Finland
  • Lippo Lassila Department of Biomaterials Science and Turku Clinical Biomaterial Center –TCBC, Institute of Dentistry, University of Turku, Turku, Finland
  • Pekka K. Vallittu Department of Biomaterials Science and Turku Clinical Biomaterial Center –TCBC, Institute of Dentistry, University of Turku, Turku, Finland; The Wellbeing Services County of Southwest Finland, Turku, Finland

DOI:

https://doi.org/10.2340/biid.v13.46529

Keywords:

Composite–composite interface, delayed placement, interlayer adhesion, shear bond strength, oxygen inhibition layer

Abstract

Objective: To investigate the effect of delay time in resin composite placement and resin matrix composition on interlayer adhesion between two successive composite layers.

Materials and methods: Three experimental resin composites were prepared by mixing 79 wt.% particulate filler with 21 wt.% dimethacrylate-based resin matrices (urethane dimethacrylate/​
triethylene glycol dimethacrylate [UDMA/TEGDMA]; ethoxylated bisphenol-A-dimethacrylate/urethane dimethacrylate/​triethylene glycol dimethacrylate [Bis-EMA/UDMA/TEGDMA]; bisphenol A-glycidyl methacrylate/triethylene glycol dimethacrylate [Bis-GMA/TEGDMA]). Fifteen groups of specimens were prepared (n = 6/group), consisting of a cured composite substructure onto which a successive surface layer was applied at different time intervals following light-initiated polymerization (0, 10 minutes, 1, 24, and 72 hours). After 2 days of dry storage at 37°C, interlayer adhesion was evaluated by measuring shear bond strength (SBS) using a universal testing machine. Failure modes were visually assessed. In addition, oxygen inhibition layer (OIL) thickness was measured microscopically, and Vickers hardness and viscosity were determined. Data were analyzed using two-way and one-way analysis of variance followed by Tukey Tukey’s Honestly Significant Difference (HSD) tests (α = 0.05).

Results: SBS values ranged from 10.3 ±2.4 to 24.5 ±3.0 MPa. Both placement delay time and resin matrix composition significantly affected SBS (p < 0.05). SBS decreased significantly when the application of the second successive layer was delayed beyond 1 hour, with the lowest values observed after 72 hours, particularly in Bis-GMA-based composites. The highest SBS was observed in the UDMA/TEGDMA group at 1 hour. Cohesive failure within the substructure was seen in all specimens. The UDMA/TEGDMA group exhibited the lowest OIL thickness (29.35 ± 0.69 µm).

Conclusion: Both incremental application timing and resin matrix composition significantly influenced composite interlayer adhesion. Short delays (10–60 minutes) enhanced interlayer adhesion, whereas prolonged delays (24–72 hours) resulted in a reduction in interlayer adhesion.

Downloads

Download data is not yet available.

References

Ferracane JL. A historical perspective on dental composite restorative materials. J Funct Biomater. 2024;15(7):173. DOI: https://doi.org/10.3390/jfb15070173

German MJ. Developments in resin-based composites. Br Dent J. 2022;232(9):638–43. DOI: https://doi.org/10.1038/s41415-022-4240-8

Gonçalves F, Kawano Y, Pfeifer C, Stansbury JW, Braga RR. Influence of BisGMA, TEGDMA, and BisEMA contents on viscosity, conversion, and flexural strength of experimental resins and composites. Eur J Oral Sci. 2009;117(4):442–6. DOI: https://doi.org/10.1111/j.1600-0722.2009.00636.x

Garoushi S, Vallittu P, Shinya A, Lassila L. Influence of increment thickness on light transmission, degree of conversion and micro hardness of bulk fill composites. Odontology. 2016;104(3):291–7. DOI: https://doi.org/10.1007/s10266-015-0227-0

Omran TA, Garoushi S, Abdulmajeed AA, Lassila LV, Vallittu PK. Influence of increment thickness on dentin bond strength and light transmission of composite base materials. Clin Oral Investig. 2017;21(5):1717–24. DOI: https://doi.org/10.1007/s00784-016-1953-6

Omran TA, Garoushi S, Lassila L, Shinya A, Vallittu PK. Bonding interface affects the loadbearing capacity of bilayered composites. Dent Mater J. 2019;38(6):1002–11. DOI: https://doi.org/10.4012/dmj.2018-304

Leprince JG, Lamblin G, Devaux J, Dewaele M, Mestdagh M, Palin WM, et al. Irradiation modes’ impact on radical entrapment in photoactive resins. J Dent Res. 2010;89(12):1494–8. DOI: https://doi.org/10.1177/0022034510384624

Tezvergil-Mutluay A, Lassila LV, Vallittu PK. Incremental layers bonding of silorane composite: the initial bonding properties. J Dent. 2008;36(7):560–3. DOI: https://doi.org/10.1016/j.jdent.2008.03.008

Shawkat ES, Shortall AC, Addison O, Palin WM. Oxygen inhibition and incremental layer bond strengths of resin composites. Dent Mater. 2009;25(11):1338–46. DOI: https://doi.org/10.1016/j.dental.2009.06.003

Bijelic-Donova J, Garoushi S, Lassila LV, Vallittu PK. Oxygen inhibition layer of composite resins: effects of layer thickness and surface layer treatment on the interlayer bond strength. Eur J Oral Sci. 2015;123(1):53–60. DOI: https://doi.org/10.1111/eos.12167

Kim JS, Choi YH, Cho BH, Son HH, Lee IB, Um CM, et al. Effect of light-cure time of adhesive resin on the thickness of the oxygen-inhibited layer and the microtensile bond strength to dentin. J Biomed Mater Res B Appl Biomater. 2006;78(1):115–23. DOI: https://doi.org/10.1002/jbm.b.30463

Truffier-Boutry D, Place E, Devaux J, Leloup G. Interfacial layer characterization in dental composite. J Oral Rehabil. 2003;30(1):74–7. DOI: https://doi.org/10.1046/j.1365-2842.2003.01008.x

Suh BI. Oxygen-inhibited layer in adhesion dentistry. J Esthet Restor Dent. 2004;16(5):316–23. DOI: https://doi.org/10.1111/j.1708-8240.2004.tb00060.x

Dall’Oca S, Papacchini F, Goracci C, Cury AH, Suh BI, Tay FR, et al. Effect of oxygen inhibition on composite repair strength over time. J Biomed Mater Res B Appl Biomater. 2007;81(2):493–8. DOI: https://doi.org/10.1002/jbm.b.30689

Özcan M, Pekkan G. Effect of different adhesion strategies on bond strength of resin composite to composite-dentin complex. Oper Dent. 2013;38(1):63–72. DOI: https://doi.org/10.2341/11-482-L

Ömeroğlu MK, Çam M, Doğruer I, Kaynar ZB. The effect of different surface treatments and adhesive systems on shear bond strength in universal nanohybrid composite resin repair. BMC Oral Health. 2025;25(1):459. DOI: https://doi.org/10.1186/s12903-025-05807-8

de Medeiros TC, de Lima MR, Bessa SC, de Araújo DF, Galvão MR. Repair bond strength of bulk fill composites after different adhesion protocols. J Clin Exp Dent. 2019;11(11):e1000–5. DOI: https://doi.org/10.4317/jced.56129

Kallio TT, Lastumäki TM, Vallittu PK. Bonding of restorative and veneering composite resin to some polymeric composites. Dent Mater. 2001;17(1):80–6. DOI: https://doi.org/10.1016/S0109-5641(00)00064-6

Bijelic-Donova J, Flett A, Lassila LVJ, Vallittu PK. Immediate repair bond strength of fiber-reinforced composite after saliva or water contamination. J Adhes Dent. 2018;20(3):205–12.

Sengupta A, Naka O, Mehta SB. The clinical performance of bulk-fill versus the incremental layered application of direct resin composite restorations: a systematic review. Evid Based Dent 2023;24:143. DOI: https://doi.org/10.1038/s41432-023-00905-4

Rueggeberg FA, Margeson DH. The effect of oxygen inhibition on an unfilled/filled composite system. J Dent Res. 1990;69(10):1652–8. DOI: https://doi.org/10.1177/00220345900690100501

Kamath U, Sheth H, Vigneshwar. Role of delayed light polymerization of a dual-cured composite base on marginal adaptation of class II posterior composite open-sandwich restoration. Indian J Dent Res. 2012;23(2):296. DOI: https://doi.org/10.4103/0970-9290.100462

Burtscher P. Stability of radicals in cured composite materials. Dent Mater. 1993;9(4):218–21. DOI: https://doi.org/10.1016/0109-5641(93)90064-W

Gauthier MA, Stangel I, Ellis TH, Zhu XX. Oxygen inhibition in dental resins. J Dent Res. 2005;84(8):725–9. DOI: https://doi.org/10.1177/154405910508400808

Eliades GC, Caputo AA. The strength of layering technique in visible light-cured composites. J Prosthet Dent. 1989;61(1):31–8. DOI: https://doi.org/10.1016/0022-3913(89)90104-2

Dietschi D, Monasevic M, Krejci I, Davidson C. Marginal and internal adaptation of class II restorations after immediate or delayed composite placement. J Dent. 2002;30(5):259–69. DOI: https://doi.org/10.1016/S0300-5712(02)00041-6

Asaka Y, Miyazaki M, Takamizawa T, Tsubota K, Moore BK. Influence of delayed placement of composites over cured adhesives on dentin bond strength of single-application self-etch systems. Oper Dent. 2006;31(1):18–24. DOI: https://doi.org/10.2341/04-157

Furuse AY, Mondelli J, Watts DC. Network structures of Bis-GMA/TEGDMA resins differ in DC, shrinkage-strain, hardness and optical properties as a function of reducing agent. Dent Mater. 2011;27(5):497–506. DOI: https://doi.org/10.1016/j.dental.2011.02.007

Papakonstantinou AE, Eliades T, Cellesi F, Watts DC, Silikas N. Evaluation of UDMA’s potential as a substitute for Bis-GMA in orthodontic adhesives. Dent Mater. 2013;29(8):898–905. DOI: https://doi.org/10.1016/j.dental.2013.05.007

Leyva Del Rio D, Seghi RR. Influence of the resin matrix phase on the fatigue resistance of model dental composite resins. Polymers (Basel). 2025;17(23):3118. DOI: https://doi.org/10.3390/polym17233118

He J, Liu F, Vallittu PK, Lassila LV. Synthesis and characterization of new dimethacrylate monomer and its application in dental resin. J Biomater Sci Polym Ed. 2013;24(4):417–30. DOI: https://doi.org/10.1080/09205063.2012.690283

Pereira LDE, Couto Neto MP, Pereira RG, Schneider LFJ. Influence of resin matrix on the rheology, translucency, and curing potential of experimental flowable composites for bulk-fill applications. Dent Mater. 2021;37(6):1046–53. DOI: https://doi.org/10.1016/j.dental.2021.03.003

Finger WJ, Lee KS, Podszun W. Monomers with low oxygen inhibition as enamel/dentin adhesives. Dent Mater. 1996;12(4):256–61. DOI: https://doi.org/10.1016/S0109-5641(96)80032-7

Aromaa MK, Vallittu PK. Delayed post-curing stage and oxygen inhibition of free-radical polymerization of dimethacrylate resin. Dent Mater. 2018;34(9):1247–52. DOI: https://doi.org/10.1016/j.dental.2018.06.019

Lastumäki TM, Kallio TT, Vallittu PK. The bond strength of light-curing composite resin to finally polymerized and aged glass fiber-reinforced composite substrate. Biomaterials. 2002;23(23):4533–9. DOI: https://doi.org/10.1016/S0142-9612(02)00197-7

Kallio TT, Lastumäki TM, Vallittu PK. Effect of resin application time on bond strength of polymer substrate repaired with particulate filler composite. J Mater Sci Mater Med. 2003;14(11):999–1004. DOI: https://doi.org/10.1023/A:1026311001967

Basavarajappa S, Perea-Lowery L, Alshehri AM, Al-Kheraif AAA, Matinlinna JP, Vallittu PK. Surface dissolution and transesterification of thermoset dimethacrylate polymer by dimethacrylate adhesive resin and organic catalyst-alcohol solution. Dent Mater. 2020;36(5):698–709. DOI: https://doi.org/10.1016/j.dental.2020.03.005

Khan AA, Al-Kheraif AA, Mohamed BA, Perea-Lowery L, Säilynoja E, Vallittu PK. Influence of primers on the properties of the adhesive interface between resin composite luting cement and fiber-reinforced composite. J Mech Behav Biomed Mater. 2018;88:281–7. DOI: https://doi.org/10.1016/j.jmbbm.2018.08.050

Säilynoja E, Garoushi S, Vallittu PK, Lassila L. Characterization of experimental short-fiber-reinforced dual-cure core build-up resin composites. Polymers (Basel). 2021;13(14):2281. DOI: https://doi.org/10.3390/polym13142281

Lovell LG, Newman SM, Bowman CN. The effects of light intensity, temperature, and comonomer composition on the polymerization behavior of dimethacrylate dental resins. J Dent Res. 1999;78(8):1469–76. DOI: https://doi.org/10.1177/00220345990780081301

Published

2026-07-16

How to Cite

Vallittu, S., Garoushi, S., Lassila, L., & Vallittu, P. K. (2026). The impact of delayed placement and resin matrix composition on adhesion between layers of resin composites. Biomaterial Investigations in Dentistry, 13(1), 593–600. https://doi.org/10.2340/biid.v13.46529