Effect of different setting times of calcium silicate cements on the bond strength to paediatric restorative materials: an in vitro study

Background: This study aimed to evaluate the effect of cement maturation time on shear bond strength (SBS) between three calcium silicate-based cements and paediatric restorative materials. Methods: A total of 405 three-dimensional (3D)-printed resin blocks with standardised cavities (4 mm diameter, 2 mm depth) were filled with Biodentine, NeoMTA 2, or NeoPUTTY. A two-step self-etch adhesive system (Clearfil SE Bond 2) was then applied to the calcium silicate cement surfaces, and Dyract XP, Filtek Z550, or ACTIVA Kids BioACTIVE Restorative was placed after 3 min, 15 min, or 24 h using a Tygon tube with a 2-mm internal diameter to standardise the bonding area. Shear bond strength was measured after 24 h of storage at 37 ℃ and 100% humidity with a crosshead speed of 1 mm/min. Failure modes were examined stereomicroscopically, and selected interfaces were analysed by scanning electron microscopy (SEM). Data were analysed using three-way analysis of variance (ANOVA) with appropriate post hoc tests (α = 0.05). Results: Setting time, cement type, and restorative material significantly affected bond strength (p < 0.001). SBS values ranged from 1.74 ± 0.49 MPa in the NeoPUTTY–Dyract XP group at 3 min to 11.55 ± 2.06 MPa in the Biodentine–ACTIVA Kids BioACTIVE Restorative group at 24 h. Bond strength increased progressively with longer setting times, with the lowest values observed at 3 min and the highest at 24 h. Biodentine generally showed higher bond strength than NeoMTA 2 and NeoPUTTY, while ACTIVA Kids BioACTIVE Restorative generally yielded the highest values among the restorative materials. Failure patterns shifted from predominantly adhesive failures at early time points to more mixed or cohesive failures with longer setting times. Conclusions: Bonding to calcium silicate-based cements is time-dependent. Within the limitations of this in vitro study, bond strength was influenced by setting time, cement type, and restorative material type.

Calcium silicate-based cements; Shear bond strength; Biodentine; NeoMTA 2; ACTIVA Kids BioACTIVE Restorative

[1] Cohenca N, Paranjpe A, Berg J. Vital pulp therapy. Dental Clinics of North America. 2013; 57: 59–73.

[2] Pushpalatha C, Dhareshwar V, Sowmya SV, Augustine D, Vinothkumar TS, Renugalakshmi A, et al. Modified mineral trioxide aggregate—a versatile dental material: an insight on applications and newer advancements. Frontiers in Bioengineering and Biotechnology. 2022; 10: 941826.

[3] Albernaz Neves J, Bandeira Lopes L, Alves Duarte M, Mendes JJ, Pimentel T. Systematic review and meta analysis of first and second generation bioceramic materials in primary dentition pulpotomies. Scientific Reports. 2025; 15: 16939.

[4] Parirokh M, Torabinejad M. Mineral trioxide aggregate: a comprehensive literature review—part III: clinical applications, drawbacks, and mechanism of action. Journal of Endodontics. 2010; 36: 400–413.

[5] Murray PE, Hafez AA, Windsor LJ, Smith AJ, Cox CF. Comparison of pulp responses following restoration of exposed and non-exposed cavities. Journal of Dentistry. 2002; 30: 213–222.

[6] Arandi NZ, Thabet M. Minimal intervention in dentistry: a literature review on Biodentine as a bioactive pulp capping material. BioMed Research International. 2021; 2021: 5569313.

[7] Camilleri J. Staining potential of Neo MTA Plus, MTA Plus, and Biodentine used for pulpotomy procedures. Journal of Endodontics. 2015; 41: 1139–1145.

[8] Xavier MT, Costa AL, Caramelo FJ, Palma PJ, Ramos JC. Evaluation of the interfaces between restorative and regenerative biomaterials used in vital pulp therapy. Materials. 2021; 14: 5055.

[9] Hardan L, Mancino D, Bourgi R, Alvarado-Orozco A, Rodríguez-Vilchis LE, Flores-Ledesma A, et al. Bond strength of adhesive systems to calcium silicate-based materials: a systematic review and meta-analysis of in vitro studies. Gels. 2022; 8: 311.

[10] Odabaş ME, Bani M, Tirali RE. Shear bond strengths of different adhesive systems to Biodentine. The Scientific World Journal. 2013; 2013: 626103.

[11] Pradelle-Plasse N, Mocquot C, Semennikova K, Colon P, Grosgogeat B. Interface between calcium silicate cement and adhesive systems according to adhesive families and cement maturation. Restorative Dentistry & Endodontics. 2020; 46: e3.

[12] Camilleri J. Investigation of Biodentine as dentine replacement material. Journal of Dentistry. 2013; 41: 600–610.

[13] Nicholson JW. Polyacid-modified composite resins (“compomers”) and their use in clinical dentistry. Dental Materials. 2007; 23: 615–622.

[14] Maran BM, de Geus JL, Gutiérrez MF, Heintze S, Tardem C, Barceleiro MO, et al. Nanofilled/nanohybrid and hybrid resin-based composite in patients with direct restorations in posterior teeth: a systematic review and meta-analysis. Journal of Dentistry. 2020; 99: 103407.

[15] Radwanski M, Zmyslowska-Polakowska E, Osica K, Krasowski M, Sauro S, Hardan L, et al. Mechanical properties of modern restorative “bioactive” dental materials—an in vitro study. Scientific Reports. 2025; 15: 3552.

[16] Celiksoz O, Irmak O. Delayed vs. immediate placement of restorative materials over Biodentine and RetroMTA: a micro-shear bond strength study. BMC Oral Health. 2024; 24: 130.

[17] Palma PJ, Marques JA, Falacho RI, Vinagre A, Santos JM, Ramos JC. Does delayed restoration improve shear bond strength of different restorative protocols to calcium silicate-based cements? Materials. 2018; 11: 2216.

[18] Candan M, Altinay Karaca FK, Öznurhan F. Evaluation of the shear bond strength of immediate and delayed restorations of various calcium silicate-based materials with fiber-reinforced composite resin materials. Polymers. 2023; 15: 3971.

[19] Ergül R, Aksu S, Çalışkan S, Tüloğlu N. Shear bond strength of calcium silicate-based cements to glass ionomers. BMC Oral Health. 2024; 24: 140.

[20] Jamali Z, Najafpour E, Ebrahim Adhami Z, Sighari Deljavan A, Aminabadi NA, Shirazi S. Does the length of dental procedure influence children’s behavior during and after treatment? A systematic review and critical appraisal. Journal of Dental Research, Dental Clinics, Dental Prospects. 2018; 12: 68–76.

[21] Sano H, Ciucchi B, Matthews WG, Pashley DH. Tensile properties of mineralized and demineralized human and bovine dentin. Journal of Dental Research. 1994; 73: 1205–1211.

[22] Davidson CL, de Gee AJ, Feilzer A. The competition between the composite-dentin bond strength and the polymerization contraction stress. Journal of Dental Research. 1984; 63: 1396–1399.

[23] Camilleri J, Sorrentino F, Damidot D. Investigation of the hydration and bioactivity of radiopacified tricalcium silicate cement, Biodentine and MTA Angelus. Dental Materials. 2013; 29: 580–593.

[24] Palma PJ, Marques JA, Antunes M, Falacho RI, Sequeira D, Roseiro L, et al. Effect of restorative timing on shear bond strength of composite resin/calcium silicate-based cements adhesive interfaces. Clinical Oral Investigations. 2021; 25: 3131–3139.

[25] Alqahtani AS, Sulimany AM, Alayad AS, Alqahtani AS, Bawazir OA. Evaluation of the shear bond strength of four bioceramic materials with different restorative materials and timings. Materials. 2022; 15: 4668.

[26] Hursh KA, Kirkpatrick TC, Cardon JW, Brewster JA, Black SW, Himel VT, et al. Shear bond comparison between 4 bioceramic materials and dual-cure composite resin. Journal of Endodontics. 2019; 45: 1378–1383.

[27] Gündoğar ZU, Keskin G, Yaman Küçükersen M. Shear bond strength of biointeractive restorative materials to NeoMTA Plus and Biodentine. Polymers. 2025; 17: 3070.

[28] Falakaloğlu S, Yeniçeri Özata M, Plotino G. Micro-shear bond strength of different calcium silicate materials to bulk-fill composite. PeerJ. 2023; 11: e15183.

[29] Suharwardy Z, Jain RK, Khetarpal A, Bala A. An in-vitro study comparing the shear bond strength of a self-adhering flowable composite and a bulk-fill flowable composite to various pulp capping materials, including Neo MTA Plus, Dycal, Biodentine, and MTA. Journal of Advances in Medicine and Medical Research. 2024; 36: 1–11.

[30] Martínez-Sabio L, Peñate L, Arregui M, Veloso Duran A, Blanco JR, Guinot F. Comparison of shear bond strength and microleakage between Activa™ Bioactive Restorative™ and bulk-fill composites: an in vitro study. Polymers. 2023; 15: 2840.

[31] Cho K, Rajan G, Farrar P, Prentice L, Prusty BG. Dental resin composites: a review on materials to product realizations. Composites Part B: Engineering. 2022; 230: 109495.

[32] Bağ İ, Çamgöz A, Işılar B, Çalışkan S. The effect of different adhesive applications on the bond strength of new generation primary tooth restoration materials to mineral trioxide aggregate. Black Sea Journal of Health Science. 2023; 6: 690–696. (In Turkish)

[33] John J, Prabath Singh VP. Comparative evaluation of the shear bond strength of MTA and Biodentine to different permanent restorative materials: an in vitro study. International Journal of Prosthodontics & Restorative Dentistry. 2022; 12: 118–124.

[34] Tunç EŞ, Sönmez IŞ, Bayrak Ş, Eğilmez T. The evaluation of bond strength of a composite and a compomer to white mineral trioxide aggregate with two different bonding systems. Journal of Endodontics. 2008; 34: 603–605.