Journal of the Australian Ceramic Society

, Volume 55, Issue 1, pp 235–245 | Cite as

Characterization of hybrid light-cured resin composites reinforced by microspherical silanized DCPA/nanorod HA via thermal fatigue

  • Yu-Ren Wu
  • Chin-Wei Chang
  • Kai-Chi Chang
  • Chia-Ling Ko
  • Hui-Yu Wu
  • Jiin-Huey Chern Lin
  • Wen-Cheng ChenEmail author


The mechanical and self-mineralized properties of nanohybrid composite resins used for the dental restoration of class V caries are investigated. The nanorod hydroxyapatite (Nr-HA) hybrid and the microspherical granular dicalcium phosphate anhydrate (DCPA) after silanization were mixed and used as fillers in different kinds of composite resins (abbreviated as DCPA, DCPA+5Nr-HA, and DCPA+10Nr-HA). Their composite strengths were measured via 3-point flexure. Their properties were characterized from environmental samples after water immersion for 24 h and exposure to thermal fatigue between 5 and 55 °C for 600 and 2400 cycles. The resin reinforced with high amounts of Nr-HA (DCPA+10Nr-HA) showed a significant increase in mineralization of the sample surfaces, which consequently enhanced microhardness. The presence of Nr-HA also increased the residual energy of samples during preparation and enhanced their capacity to reprecipitate after immersion and through thermal fatigue. However, the presence of Nr-HA also resulted in high ductility and early failure of the sample, especially in the reinforced group with the highest amount of Nr-HA (DCPA+10Nr-HA). The appropriate additive Nr-HA (DCPA+5Nr-HA) balanced the properties with less difference of strength and residual energy compared with the DCPA group. The additive showed superior capability in enhancing the release of ions and initiating mineralization after immersion with thermal fatigue in vitro. This newly developed composite resin may provide an excellent combination of stress bearing, improved residual energy before the sample fracture, enhanced mineralization capacity, and improved caries-inhibiting capabilities.


Composite resin Calcium phosphate Mineralization Flexural strength Hybrid nanorod 



The authors would like to thank the Precision Instrument Support Center of Feng Chia University, which provided the fabrication and measurement facilities. The assistance of the participants in this research is also acknowledged.


This work was supported by the Ministry of Science and Technology, Taiwan (grant numbers MOST103-2221-E-035-099-, 105-2221-E-035-021-MY3, and MOST106-2622-E-035-002-CC2).


  1. 1.
    Liu, F., Wang, R., Cheng, Y., Jiang, X., Zhang, Q., Zhu, M.: Polymer grafted hydroxyapatite whisker as a filler for dental composite resin with enhanced physical and mechanical properties. Mater. Sci. Eng. C. 33, 4994–5000 (2013)CrossRefGoogle Scholar
  2. 2.
    Xu, H.H.K., Moreau, J.L., Sun, L., Chow, L.C.: Strength and fluoride release characteristics of a calcium fluoride based dental nanocomposite. Biomaterials. 29, 4261–4267 (2008)CrossRefGoogle Scholar
  3. 3.
    Taheri, M.M., Kadir, M.R.A., Shokuhfar, T., Hamlekhan, A., Assadian, M., Shirdar, M.R., Mirjalili, A.: Surfactant-assisted hydrothermal synthesis of fluoridated hydroxyapatite nanorods. Ceram. Int. 41, 9867–9872 (2015)CrossRefGoogle Scholar
  4. 4.
    Sarrett, D.C.: Clinical challenges and the relevance of materials testing for posterior composite restorations. Dent. Mater. 21, 9–20 (2005)CrossRefGoogle Scholar
  5. 5.
    Sakaguchi, R.L.: Review of the current status and challenges for dental posterior restorative composites: clinical, chemistry, and physical behavior considerations. Dent. Mater. 21, 3–6 (2005)CrossRefGoogle Scholar
  6. 6.
    Xu, H.H.K., Weir, M.D., Sun, L.: Nanocomposites with Ca and PO4 release: effects of reinforcement, dicalcium phosphate particle size and silanization. Dent. Mater. 23, 1482–1491 (2007)CrossRefGoogle Scholar
  7. 7.
    Weir, M.D., Ruan, J., Zhang, N., Chow, L.C., Zhang, K., Chang, X., Bai, Y., Xu, H.H.K.: Effect of calcium phosphate nanocomposite on in vitro remineralization of human dentin. Dent. Mater. 33, 1033–1044 (2017)CrossRefGoogle Scholar
  8. 8.
    Yerro, O., Radojević, V., Radović, I., Kojović, A., Uskoković, P.S., Stojanović, D.B., Aleksić, R.: Enhanced thermo-mechanical properties of acrylic resin reinforced with silanized alumina whiskers. Ceram. Int. 42, 10779–10786 (2016)CrossRefGoogle Scholar
  9. 9.
    Chen, W.C., Wu, H.Y., Chen, H.S.: Evaluation of reinforced strength and remineralized potential of resins with nanocrystallites and silica modified filler surfaces. Mater. Sci. Eng. C. 33, 1143–1151 (2013)CrossRefGoogle Scholar
  10. 10.
    Arcís, R.W., López-Macipe, A., Toledano, M., Osorio, E., Rodríguez-Clemente, R., Murtra, J., Fanovich, M.A., Pascual, C.D.: Mechanical properties of visible light-cured resins reinforced with hydroxyapatite for dental restoration. Dent. Mater. 18, 49–57 (2002)CrossRefGoogle Scholar
  11. 11.
    Domingo, C., Arcís, R.W., López-Macipe, A., Osorio, R., Rodríguez-Clemente, R., Murtra, J., Fanovich, M.A., Toledano, M.: Dental composites reinforced with hydroxyapatite: mechanical behavior and absorption/elution characteristics. J Biomed Mater Res Part A. 56, 297–305 (2001)CrossRefGoogle Scholar
  12. 12.
    Sadat-Shojai, M., Atai, M., Nodehi, A., Khanlar, L.N.: Hydroxyapatite nanorods as novel fillers for improving the properties of dental adhesives: synthesis and application. Dent. Mater. 26, 471–482 (2010)CrossRefGoogle Scholar
  13. 13.
    Ferracane, J.L.: Resin composite—state of the art. Dent. Mater. 27, 29–38 (2011)CrossRefGoogle Scholar
  14. 14.
    Chen, W.C., Ko, C.L., Wu, H.Y., Lai, P.L., Shih, C.J.: Thermal cycling effects on adhesion of resin–bovine enamel junction among different composite resins. J. Mech. Behav. Biomed. Mater. 38, 105–113 (2014)CrossRefGoogle Scholar
  15. 15.
    Zhang, C., Yang, J., Quan, Z., Yang, P., Li, C., Hou, Z., Lin, J.: Hydroxyapatite nano- and microcrystals with multiform morphologies: controllable synthesis and luminescence properties. Cryst. Growth Des. 9, 2725–2733 (2009)CrossRefGoogle Scholar
  16. 16.
    Monteiro, C.A., Levy, R.B., Claro, R.M., Castro, I.R.R., Cannon, G.: Increasing consumption of ultra-processed foods and likely impact on human health: evidence from Brazil. Public Health Nutr. 14, 5–13 (2010)CrossRefGoogle Scholar
  17. 17.
    Dickens-Venz, S.H., Takagi, S., Chow, L.C., Bowen, R.L., Johnston, A.D., Dickens, B.: Physical and chemical properties of resin reinforced calcium phosphate cements. Dent. Mater. 10, 100–106 (1994)CrossRefGoogle Scholar
  18. 18.
    Wu, Y.R., Chang, C.W., Ko, C.L., Wu, H.Y., Chen, W.C.: The morphological effect of calcium phosphates on reinforcing the mechanical strength of methacrylate-based dental composite resins through thermal cycling. Ceram. Int. 43, 14389–14394 (2017)CrossRefGoogle Scholar
  19. 19.
    Sampaio, F.N., Pinto, J.R., Turssi, C.P., Basting, R.T.: Effect of sealant application and thermal cycling on bond strength of tissue conditioners to acrylic resin. Braz. Dent. J. 24, 247–252 (2013)CrossRefGoogle Scholar
  20. 20.
    Anil, N., Hekimoglu, C., Buyukbas, N., Ercan, M.T.: Microleakage study of various soft denture liners by autoradiography: effect of accelerated aging. J. Prosthet. Dent. 84, 394–399 (2000)CrossRefGoogle Scholar
  21. 21.
    Pinto, J.R., Mesquita, M.F., Nóbilo, M.A., Henriques, G.E.: Evaluation of varying amounts of thermal cycling on bond strength and permanent deformation of two resilient denture liners. J. Prosthet. Dent. 92, 288–293 (2004)CrossRefGoogle Scholar
  22. 22.
    Borsatto, M.C., Martinelli, M.G., Contente, M.M.M.G., Mallara, T.d.S., Pécora, J.D., Galo, R.: Bond durability of Er:YAG laser-prepared primary tooth enamel. Braz. Dent. J. 24, 330–334 (2013)CrossRefGoogle Scholar
  23. 23.
    García-Contreras, R., Scougall-Vilchis, R., Acosta-Torres, L., Arenas-Arrocena, M., García-Garduño, R., de la Fuente-Hernández, J.: Vickers microhardness comparison of 4 composite resins with different types of filler. J Oral Res. 4, 313–320 (2015)CrossRefGoogle Scholar
  24. 24.
    Xu, H.H., Weir, M.D., Sun, L., Takagi, S., Chow, L.C.: Effects of calcium phosphate nanoparticles on CaPO4 composite. J. Dent. Res. 86, 378–383 (2007)CrossRefGoogle Scholar
  25. 25.
    Suchanek, W., Yashima, M., Kakihana, M., Yoshimura, M.: Hydroxyapatite/hydroxyapatite-whisker composites without sintering additives: mechanical properties and microstructural evolution. J. Am. Ceram. Soc. 80, 2805–2813 (1997)CrossRefGoogle Scholar

Copyright information

© Australian Ceramic Society 2018

Authors and Affiliations

  1. 1.Advanced Medical Devices and Composites Laboratory, Department of Fiber and Composite MaterialsFeng Chia UniversityTaichungTaiwan
  2. 2.Department of Materials Science and EngineeringNational Cheng-Kung UniversityTainanTaiwan
  3. 3.Department of Dental HygieneChina Medical UniversityTaichungTaiwan

Personalised recommendations