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<p>Polycaprolactone (PCL) offers interesting properties (i.e., ease of processing, biocompatibility and biodegradability), making it a promising material. However, its slow degradation rate and poor strength and stiffness limit its use. In this study, a PCL-RHA composite was developed using micro-hydroxyapatite (mHAp) as a reinforcing agent, and the mechanical and bioactive properties were optimised using the Taguchi Design of Experiment technique. The effects of mHAp concentration and holding time on the hardness, fracture toughness, swelling ratio and biodegradation rate were studied using the signal-to-noise (S/N) ratio and analysis of variance (ANOVA). The thermal stability and textural properties of the developed biocomposite were studied through Thermogravimetric analysis (TGA) and Brunauer-Emmett-Teller (BET) analysis. The regression analysis shows that the mHAp concentration had a greater impact on the studied properties than the holding time. Using the Taguchi Grey Relational Analysis (GRA), the condition with the best performance is 5 wt% HAp microparticle and 2&#xa0;h holding time, resulting in 20.37 Hv, 0.42 MPam1/2, 21.88% and 40.50% for hardness, fracture toughness, degradation rate and swelling ratio, respectively. The TGA analysis shows that the Pure PCL and the optimal sample had a major thermal degradation process above 300&#xa0;°C, showing the samples break down at a high temperature. The optimal sample exhibited a higher specific surface area (510.68 m2/g) and pore volume (0.25 cm2/g) than pure PCL, which could help improve the bioactivity of the sample through ion exchange, protein adsorption, and osteoblast attachment. SEM analysis showed that the optimal sample exhibited a rough surface, an interconnected porous structure, and good particle dispersion with minimal agglomeration prior to immersion. Following 28 days of immersion, the scaffold retained its structural integrity while developing apatite-like mineral deposits, indicating enhanced bioactivity and mineralisation. Overall, the findings highlight the potential of PCL-RHA biocomposite reinforced with hydroxyapatite microparticles as a mechanically competent, bioactive material for bone tissue engineering applications.</p> Graphical abstract <p></p>

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Taguchi design of experiment-assisted optimisation of sustainable polycaprolactone–rice husk ash composites reinforced with micro hydroxyapatite

  • 期刊论文

  • 发表日期：

    2026年7月31日

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  • M. A. Adamu,
  • M. Dauda,
  • M. Sumaila,
  • T. Ause,
  • K. A. Salami

摘要

Polycaprolactone (PCL) offers interesting properties (i.e., ease of processing, biocompatibility and biodegradability), making it a promising material. However, its slow degradation rate and poor strength and stiffness limit its use. In this study, a PCL-RHA composite was developed using micro-hydroxyapatite (mHAp) as a reinforcing agent, and the mechanical and bioactive properties were optimised using the Taguchi Design of Experiment technique. The effects of mHAp concentration and holding time on the hardness, fracture toughness, swelling ratio and biodegradation rate were studied using the signal-to-noise (S/N) ratio and analysis of variance (ANOVA). The thermal stability and textural properties of the developed biocomposite were studied through Thermogravimetric analysis (TGA) and Brunauer-Emmett-Teller (BET) analysis. The regression analysis shows that the mHAp concentration had a greater impact on the studied properties than the holding time. Using the Taguchi Grey Relational Analysis (GRA), the condition with the best performance is 5 wt% HAp microparticle and 2 h holding time, resulting in 20.37 Hv, 0.42 MPam1/2, 21.88% and 40.50% for hardness, fracture toughness, degradation rate and swelling ratio, respectively. The TGA analysis shows that the Pure PCL and the optimal sample had a major thermal degradation process above 300 °C, showing the samples break down at a high temperature. The optimal sample exhibited a higher specific surface area (510.68 m2/g) and pore volume (0.25 cm2/g) than pure PCL, which could help improve the bioactivity of the sample through ion exchange, protein adsorption, and osteoblast attachment. SEM analysis showed that the optimal sample exhibited a rough surface, an interconnected porous structure, and good particle dispersion with minimal agglomeration prior to immersion. Following 28 days of immersion, the scaffold retained its structural integrity while developing apatite-like mineral deposits, indicating enhanced bioactivity and mineralisation. Overall, the findings highlight the potential of PCL-RHA biocomposite reinforced with hydroxyapatite microparticles as a mechanically competent, bioactive material for bone tissue engineering applications.

Graphical abstract