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. 2024 Mar 6;16(5):719.
doi: 10.3390/polym16050719.

The Structural, Thermal and Morphological Characterization of Polylactic Acid/Β-Tricalcium Phosphate (PLA/Β-TCP) Composites upon Immersion in SBF: A Comprehensive Analysis

Sondes Ftiti  1 , Sandra C Cifuentes  2 , Awatef Guidara  1 , Joaquín Rams  2 , Hassib Tounsi  1 , Juan P Fernández-Blázquez  3
Affiliations

The Structural, Thermal and Morphological Characterization of Polylactic Acid/Β-Tricalcium Phosphate (PLA/Β-TCP) Composites upon Immersion in SBF: A Comprehensive Analysis

Sondes Ftiti et al. Polymers (Basel). .

Abstract

Biocomposite films based on PLA reinforced with different β-TCP contents (10%, 20%, and 25%wt.) were fabricated via solvent casting and immersed in SBF for 7, 14, and 21 days. The bioactivity, morphological, and thermal behavior of composites with immersion were studied using scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) microanalysis, weight loss (WL), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and gel permeation chromatography (GPC). This broad analysis leads to a deeper understanding of the evolution of the polymer-filler interaction with the degradation of the biocomposites. The results showed that β-TCP gradually evolved into carbonated hydroxyapatite as the immersion time increased. This evolution affected the interaction of β-TCP with PLA. PLA and β-TCP interactions differed from PLA and carbonated hydroxyapatite interactions. It was observed that β-TCP inhibited PLA hydrolysis but accelerated the thermal degradation of the polymer. β-TCP retarded the cold crystallization of PLA and hindered its crystallinity. However, after immersion in SBF, particles accelerated the cold crystallization of PLA. Therefore, considering the evolution of β-TCP with immersion in SBF is crucial for an accurate analysis of the biocomposites' degradation. These findings enhance the comprehension of the degradation mechanism in PLA/β-TCP, which is valuable for predicting the degradation performance of PLA/β-TCP in medical applications.

Keywords: crystallinity; gel permeation chromatography; polylactic acid; solvent casting technique; β-tricalcium phosphate.

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Conflict of interest statement

The authors declare no conflicts of interest.

Figures

Figure 1
Figure 1
Preparation process of PLA/n β-TCP biocomposites.
Figure 2
Figure 2
SEM micrographs of the surfaces of PLA (A0–A2) and PLA/nβ-TCP composites as a function of the β-TCP content: 10 wt.% (B0–B2), 20 wt.% (C0–C2), and 25 wt.% (D0–D2) before and after incubation in SBF.
Figure 3
Figure 3
XRD profiles of PLA and PLA/nβ-TCP biocomposites before and after immersion in SBF solution: (a) PLA; (b) PLA/10β-TCP; (c) PLA/20β-TCP; (d) PLA/25β-TCP. (red dot lines refer to the main peaks of PLA (a) and β-TCP (b–d)).
Figure 4
Figure 4
FTIR spectra of PLA and PLA/nβ −TCP biocomposites with immersion time: (a) PLA; (b) PLA/10β −TCP; (c) PLA/20β −TCP; (d) PLA/25β −TCP.
Figure 5
Figure 5
Evolution of calcium (a) and phosphorous concentrations (b) during the immersion of PLA/nβ-TCP biocomposites in SBF solution; (c) percentage of mass losses after 21 days of immersing PLA and PLA/nβ-TCP biocomposites in SBF; (d) evolution of pH with immersion time.
Figure 6
Figure 6
Percentage of water uptake after immersion in SBF of PLA and PLA/nβ-TCP biocomposites.
Figure 7
Figure 7
The molecular weight distribution of PLA and PLA/25β-TCP.
Figure 8
Figure 8
Thermogravimetric analysis of PLA and PLA/nβ-TCP biocomposites before and after immersion in SBF for 21 days.
Figure 9
Figure 9
DTG curves of PLA and PLA/nβ-TCP before and after immersion in SBF for 21 days.
Figure 10
Figure 10
DSC curves during the first heating cycle of PLA/β-TCP films at a scanning rate of 5 °C/min: (a) PLA; (b) PLA/10β-TCP; (c) PLA/20β-TCP; (d)PLA/25β-TCP.
Figure 11
Figure 11
DSC curves during the second heating cycle of PLA/β-TCP films at a scanning rate of 5 °C/min. Glass transition (Tg), cold crystallization (Tcc), and melting temperature (Tm) are marked with black dashed lines: (a) PLA; (b) PLA/10β-TCP; (c) PLA/20β-TCP; (d) PLA/25β-TCP.
Figure 12
Figure 12
DSC curves during the second heating cycle of PLA and PLA/nβ-TCP films before immersion in SBF.
Figure 13
Figure 13
Schematic illustrating the proposed degradation mechanism of neat PLA and PLA with β-TCP particles.
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