Crystallization Behavior and Mechanical Properties of Poly(ε-caprolactone) Reinforced with Barium Sulfate Submicron Particles

Poly(ε-caprolactone) (PCL) was mixed with submicron particles of barium sulfate to obtain biodegradable radiopaque composites. X-ray images comparing with aluminum samples show that 15 wt.% barium sulfate (BaSO<sub>4</sub>) is sufficient to present radiopacity. Thermal studies by differe...

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Main Authors: Hegoi Amestoy, Paul Diego, Emilio Meaurio, Jone Muñoz, Jose-Ramon Sarasua
Format: Article
Language:English
Published: MDPI AG 2021-05-01
Series:Materials
Subjects:
Online Access:https://www.mdpi.com/1996-1944/14/9/2368
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author Hegoi Amestoy
Paul Diego
Emilio Meaurio
Jone Muñoz
Jose-Ramon Sarasua
author_facet Hegoi Amestoy
Paul Diego
Emilio Meaurio
Jone Muñoz
Jose-Ramon Sarasua
author_sort Hegoi Amestoy
collection DOAJ
description Poly(ε-caprolactone) (PCL) was mixed with submicron particles of barium sulfate to obtain biodegradable radiopaque composites. X-ray images comparing with aluminum samples show that 15 wt.% barium sulfate (BaSO<sub>4</sub>) is sufficient to present radiopacity. Thermal studies by differential scanning calorimetry (DSC) show a statistically significant increase in PCL degree of crystallinity from 46% to 52% for 25 wt.% BaSO<sub>4</sub>. Non-isothermal crystallization tests were performed at different cooling rates to evaluate crystallization kinetics. The nucleation effect of BaSO<sub>4</sub> was found to change the morphology and quantity of the primary crystals of PCL, which was also corroborated by the use of a polarized light optical microscope (PLOM). These results fit well with Avrami–Ozawa–Jeziorny model and show a secondary crystallization that contributes to an increase in crystal fraction with internal structure reorganization. The addition of barium sulfate particles in composite formulations with PCL improves stiffness but not strength for all compositions due to possible cavitation effects induced by debonding of reinforcement interphase.
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spelling doaj.art-fca3b0aef0ae4087bcd972d11be520a32023-11-21T18:10:48ZengMDPI AGMaterials1996-19442021-05-01149236810.3390/ma14092368Crystallization Behavior and Mechanical Properties of Poly(ε-caprolactone) Reinforced with Barium Sulfate Submicron ParticlesHegoi Amestoy0Paul Diego1Emilio Meaurio2Jone Muñoz3Jose-Ramon Sarasua4Department of Mining-Metallurgy Engineering and Materials Science, POLYMAT, Faculty of Engineering in Bilbao, University of the Basque Country (UPV/EHU), Plaza Torres Quevedo 1, 48013 Bilbao, SpainDepartment of Mining-Metallurgy Engineering and Materials Science, POLYMAT, Faculty of Engineering in Bilbao, University of the Basque Country (UPV/EHU), Plaza Torres Quevedo 1, 48013 Bilbao, SpainDepartment of Mining-Metallurgy Engineering and Materials Science, POLYMAT, Faculty of Engineering in Bilbao, University of the Basque Country (UPV/EHU), Plaza Torres Quevedo 1, 48013 Bilbao, SpainDepartment of Mining-Metallurgy Engineering and Materials Science, POLYMAT, Faculty of Engineering in Bilbao, University of the Basque Country (UPV/EHU), Plaza Torres Quevedo 1, 48013 Bilbao, SpainDepartment of Mining-Metallurgy Engineering and Materials Science, POLYMAT, Faculty of Engineering in Bilbao, University of the Basque Country (UPV/EHU), Plaza Torres Quevedo 1, 48013 Bilbao, SpainPoly(ε-caprolactone) (PCL) was mixed with submicron particles of barium sulfate to obtain biodegradable radiopaque composites. X-ray images comparing with aluminum samples show that 15 wt.% barium sulfate (BaSO<sub>4</sub>) is sufficient to present radiopacity. Thermal studies by differential scanning calorimetry (DSC) show a statistically significant increase in PCL degree of crystallinity from 46% to 52% for 25 wt.% BaSO<sub>4</sub>. Non-isothermal crystallization tests were performed at different cooling rates to evaluate crystallization kinetics. The nucleation effect of BaSO<sub>4</sub> was found to change the morphology and quantity of the primary crystals of PCL, which was also corroborated by the use of a polarized light optical microscope (PLOM). These results fit well with Avrami–Ozawa–Jeziorny model and show a secondary crystallization that contributes to an increase in crystal fraction with internal structure reorganization. The addition of barium sulfate particles in composite formulations with PCL improves stiffness but not strength for all compositions due to possible cavitation effects induced by debonding of reinforcement interphase.https://www.mdpi.com/1996-1944/14/9/2368poly(ε-caprolactone)crystallization kineticsradiopacitybarium sulfate
spellingShingle Hegoi Amestoy
Paul Diego
Emilio Meaurio
Jone Muñoz
Jose-Ramon Sarasua
Crystallization Behavior and Mechanical Properties of Poly(ε-caprolactone) Reinforced with Barium Sulfate Submicron Particles
Materials
poly(ε-caprolactone)
crystallization kinetics
radiopacity
barium sulfate
title Crystallization Behavior and Mechanical Properties of Poly(ε-caprolactone) Reinforced with Barium Sulfate Submicron Particles
title_full Crystallization Behavior and Mechanical Properties of Poly(ε-caprolactone) Reinforced with Barium Sulfate Submicron Particles
title_fullStr Crystallization Behavior and Mechanical Properties of Poly(ε-caprolactone) Reinforced with Barium Sulfate Submicron Particles
title_full_unstemmed Crystallization Behavior and Mechanical Properties of Poly(ε-caprolactone) Reinforced with Barium Sulfate Submicron Particles
title_short Crystallization Behavior and Mechanical Properties of Poly(ε-caprolactone) Reinforced with Barium Sulfate Submicron Particles
title_sort crystallization behavior and mechanical properties of poly ε caprolactone reinforced with barium sulfate submicron particles
topic poly(ε-caprolactone)
crystallization kinetics
radiopacity
barium sulfate
url https://www.mdpi.com/1996-1944/14/9/2368
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