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Open AccessArticle

Hierarchical Surface Texturing of Hydroxyapatite Ceramics: Influence on the Adhesive Bonding Strength of Polymeric Polycaprolactone

1
Department of Materials Science (Institute of Glass and Ceramics), University of Erlangen-Nuernberg, Martensstr. 5, D-91058 Erlangen, Germany
2
School of Advanced Materials Science & Engineering, Sungkyunkwan University (SKKU), Suwon 16149, Korea
3
Frontier Research Institute for Materials Science, Nagoya Institute of Technology, Gokiso-cho, Showa-ku, Nagoya 466-8555, Japan
*
Authors to whom correspondence should be addressed.
J. Funct. Biomater. 2020, 11(4), 73; https://doi.org/10.3390/jfb11040073
Received: 8 September 2020 / Revised: 29 September 2020 / Accepted: 30 September 2020 / Published: 3 October 2020
(This article belongs to the Special Issue Bioceramics and Bioactive Glass-Based Materials)
The tailored manipulation of ceramic surfaces gained recent interest to optimize the performance and lifetime of composite materials used as implants. In this work, a hierarchical surface texturing of hydroxyapatite (HAp) ceramics was developed to improve the poor adhesive bonding strength in hydroxyapatite and polycaprolactone (HAp/PCL) composites. Four different types of periodic surface morphologies (grooves, cylindric pits, linear waves and Gaussian hills) were realized by a ceramic micro-transfer molding technique in the submillimeter range. A subsequent surface roughening and functionalization on a micron to nanometer scale was obtained by two different etchings with hydrochloric and tartaric acid. An ensuing silane coupling with 3-aminopropyltriethoxysilane (APTES) enhanced the chemical adhesion between the HAp surface and PCL on the nanometer scale by the formation of dipole–dipole interactions and covalent bonds. The adhesive bonding strengths of the individual and combined surface texturings were investigated by performing single-lap compressive shear tests. All individual texturing types (macro, micro and nano) showed significantly improved HAp/PCL interface strengths compared to the non-textured HAp reference, based on an enhanced mechanical, physical and chemical adhesion. The independent effect mechanisms allow the deliberately hierarchical combination of all texturing types without negative influences. The hierarchical surface-textured HAp showed a 6.5 times higher adhesive bonding strength (7.7 ± 1.5 MPa) than the non-textured reference, proving that surface texturing is an attractive method to optimize the component adhesion in composites for potential medical implants.
Keywords: hierarchical surface texturing; surface functionalization; hydroxyapatite; polycaprolactone; acid etching; tartaric acid; silane; adhesive bonding strength hierarchical surface texturing; surface functionalization; hydroxyapatite; polycaprolactone; acid etching; tartaric acid; silane; adhesive bonding strength
MDPI and ACS Style

Biggemann, J.; Müller, P.; Köllner, D.; Simon, S.; Hoffmann, P.; Heik, P.; Lee, J.H.; Fey, T. Hierarchical Surface Texturing of Hydroxyapatite Ceramics: Influence on the Adhesive Bonding Strength of Polymeric Polycaprolactone. J. Funct. Biomater. 2020, 11, 73.

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