Characterization of Biodegradable Polycaprolactone Containing Titanium Dioxide Micro and Nanoparticles

Authors: Emi Govorčin Bajsić, Vesna Ocelić Bulatović, Miroslav Slouf, Ana Šitum

Abstract:

Composites based on a biodegradable polycaprolactone (PCL) containing 0.5, 1.0 and 2.0 wt % of titanium dioxide (TiO₂) micro and nanoparticles were prepared by melt mixing and the effect of filler type and contents on the thermal properties, dynamic-mechanical behaviour and morphology were investigated. Measurements of storage modulus and loss modulus by dynamic mechanical analysis (DMA) showed better results for microfilled PCL/TiO₂ composites than nanofilled composites, with the same filler content. DSC analysis showed that the T_g and T_c of micro and nanocomposites were slightly lower than those of neat PCL. The crystallinity of the PCL increased with the addition of TiO₂ micro and nanoparticles; however, the c_c for the PCL was unchanged with micro TiO₂ content. The thermal stability of PCL/TiO₂ composites were characterized using thermogravimetric analysis (TGA). The initial weight loss (5 wt %) occurs at slightly higher temperature with micro and nano TiO₂ addition and with increasing TiO₂ content.

Keywords: Morphology, polycaprolactone, thermal properties, titanium dioxide.

Digital Object Identifier (DOI): doi.org/10.5281/zenodo.1093568

References:

[1] L. Cabedo, J. L. Feijoo, M. P. Villanueva, J. M. Lagarόn, E. Giménez "Optimization of Biodegradable nanocomposites Based on aPLA/PCL Blends for Food packaging Application”, Macromol. Symp., Vol. 233, no. 1 , pp. 191-197, Febr. 2006.
[2] D. Walsh, T. Furuzono, J. Tanaka, "Preparation of porous composite implant materials by in situ polymerization of porous apatite containing -caprolactone or methyl methacrylate”, Biomaterials, Vol. 22, no. 11, pp. 1205-1212, Jun. 2001.
[3] J. Y. Liu, L. Reni, Q. Wei, J. L. Wu, S. Liu, Y. J. Wang, G. Y. Li, "Fabrication and characterization of polycaprolactone/calcium sulfate whisker composites”, eXPRESS Polym. Lett., Vol. 5, no. 8, pp. 742-752, 2011.
[4] C. S. Wu, "In situ polymerization of titanium isopropoxide in polycaprolactone: Properties and characterization of the hybrid nanocomposites”, J. Appl. Polym. Sci., Vol. 92, no. 3, pp. 1749-1757, May 2004.
[5] G. J. Nohynek, J. Lademann, C. Riband, M. S. Roberts, "Grey goo on the skin? Nanotechnology, cosmetic and sunscreen safety”, Crit. Rev. Toxicol., Vol. 37, no. 3 , pp. 251-277, Mar. 2007.
[6] A. M.-Bonilla, M. L. Cerrada, M. Fernández-García, A. Kubacka, M. Ferrer, M. Fernández-García, "Biodegradable Polycaprolactone-Titania Nanocomposites: Preparation, Characterization and Antimicrobial Properties”, Int. J. Mol. Sci., Vol. 14, no. 5, pp. 9249-9266, Apr. 2011.
[7] A. Kubacka, C. Serrano, M. Ferrer, H. Lünsdorf, P. Bielecki, M. L. Cerrada, M. Fernández-García, M. Fernández-García, "High performance dual action polymer TiO2 nanocomposites films via melting processing”, Nano Lett., Vol. 7, no. 8 , pp. 2529-2534, July 2007.
[8] M. L. Cerrada, C. Serrano, M. Sánchez-Chaves, M. Fernández-García, F. Fernández-Martín, A. de Andrés, R. J. Jiménez Riobόo, A. Kubacka, M. Ferrer, M. Fernández-García, "Biocidal capability optimization in organic inorganic nanocomposites based on titania”, Environ. Sci. Techn., Vol. 18, no. 5, pp. 1630-1634, Jan 2009.
[9] H. Tsuji, T. Ishizaka, "Porous biodegradable polyesters, 3a preparation of porous poly(ε-caprolactone) films from blends by selective enzymatic removal of poly(L-lactide)”, Macromal. Biosci., Vol. 1, pp. 59-65, 2001.
[10] V. Crescenzi, G. Manzini, G. Galzolari, C. Borri, "Thermodynamics of fusion of poly-β-propiolactone and poly-ε-caprolactone. Comparative analysis of the melting of aliphatic polylactone and polyester chains”, Eur. Polym. J., Vol. 8, no. 3, pp. 449-463, March 1972.
[11] J. Jancar, J. F. Douglas, F. W. Starr; S. K. Kumar, P. Cassagnau, A. J. Lesser, S. S. Sternstein, M. J. Buehler, "Current Issues in Research on Structure-Property Relationships in Polymer Nanocomposites”, Polymer, Vol. 51, no. 15, pp. 3321-3343, July 2010.
[12] Y. Ding, S. Pawlus, A. P. Sokolov, J. F. Douglas, A. Karim, C. L. Soles, "Dielectric Spectroscopy Investigation of Relaxation in C60-Polyisoprene Nanocomposites”, Macromolecules, Vol. 42, no.8, pp. 3201-3206, March 2009.
[13] K. Fukushima, D. Tabuai, G. Camino, "Nanocomposites of PLA and PCL based on montmorillonite and sepiolite”, Mater. Sci. Eng., Vol. 29, no.4, pp. 1433-1441, May 2009.