Confinement in Extruded Nanocomposites Based on PCL and Mesoporous Silicas: Effect of Pore Sizes and Their Influence in Ultimate Mechanical Response
In this study, nanocomposites based on polycaprolactone (PCL) and two types of mesoporous silicas, MCM-41 and SBA-15, were attained by melt extrusion. The effect of the silica incorporated within the PCL matrix was observed, firstly, in the morphological characteristics and degradation behavior of t...
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MDPI AG
2021-12-01
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| Series: | Journal of Composites Science |
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| Online Access: | https://www.mdpi.com/2504-477X/5/12/321 |
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| author | Tamara M. Díez-Rodríguez Enrique Blázquez-Blázquez Nadine L. C. Antunes Maria do Rosário Ribeiro Ernesto Pérez María L. Cerrada |
| author_facet | Tamara M. Díez-Rodríguez Enrique Blázquez-Blázquez Nadine L. C. Antunes Maria do Rosário Ribeiro Ernesto Pérez María L. Cerrada |
| author_sort | Tamara M. Díez-Rodríguez |
| collection | DOAJ |
| description | In this study, nanocomposites based on polycaprolactone (PCL) and two types of mesoporous silicas, MCM-41 and SBA-15, were attained by melt extrusion. The effect of the silica incorporated within the PCL matrix was observed, firstly, in the morphological characteristics and degradation behavior of the resultant composites. DSC experiments provided information on the existence of confinement in the PCL–SBA-15 materials through the appearance of an additional small endotherm, located at about 25–50 °C, and attributed to the melting of constrained crystallites. Displacement to a slightly lower temperature of this endothermic event was observed in the first heating run of PCL–MCM-41 composites, attributed to the inferior pore size in the MCM-41 particles. Thus, this indicates variations in the inclusion of PCL chains within these two mesostructures with different pore sizes. Real-time variable-temperature small-angle X-ray scattering (SAXS) experiments with synchrotron radiation were crucial to confirm the presence of PCL within MCM-41 and SBA-15 pores. Accurate information was also deduced from these measurements regarding the influence of these two mesoporous MCM-41 and SBA-15 silicas on PCL long spacing. The differences found in these morphological and structural features were responsible for the ultimate mechanical response exhibited by the two sets of PCL nanocomposites, with a considerably higher increase of mechanical parameters in the SBA-15 family. |
| first_indexed | 2024-03-10T03:50:06Z |
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| id | doaj.art-cb4cca835fdb4959a9d0f529858a1cf5 |
| institution | Directory Open Access Journal |
| issn | 2504-477X |
| language | English |
| last_indexed | 2024-03-10T03:50:06Z |
| publishDate | 2021-12-01 |
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| series | Journal of Composites Science |
| spelling | doaj.art-cb4cca835fdb4959a9d0f529858a1cf52023-11-23T08:59:24ZengMDPI AGJournal of Composites Science2504-477X2021-12-0151232110.3390/jcs5120321Confinement in Extruded Nanocomposites Based on PCL and Mesoporous Silicas: Effect of Pore Sizes and Their Influence in Ultimate Mechanical ResponseTamara M. Díez-Rodríguez0Enrique Blázquez-Blázquez1Nadine L. C. Antunes2Maria do Rosário Ribeiro3Ernesto Pérez4María L. Cerrada5Instituto de Ciencia y Tecnología de Polímeros (ICTP-CSIC), Juan de la Cierva 3, 28006 Madrid, SpainInstituto de Ciencia y Tecnología de Polímeros (ICTP-CSIC), Juan de la Cierva 3, 28006 Madrid, SpainCentro de Química Estrutural, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa, PortugalCentro de Química Estrutural, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa, PortugalInstituto de Ciencia y Tecnología de Polímeros (ICTP-CSIC), Juan de la Cierva 3, 28006 Madrid, SpainInstituto de Ciencia y Tecnología de Polímeros (ICTP-CSIC), Juan de la Cierva 3, 28006 Madrid, SpainIn this study, nanocomposites based on polycaprolactone (PCL) and two types of mesoporous silicas, MCM-41 and SBA-15, were attained by melt extrusion. The effect of the silica incorporated within the PCL matrix was observed, firstly, in the morphological characteristics and degradation behavior of the resultant composites. DSC experiments provided information on the existence of confinement in the PCL–SBA-15 materials through the appearance of an additional small endotherm, located at about 25–50 °C, and attributed to the melting of constrained crystallites. Displacement to a slightly lower temperature of this endothermic event was observed in the first heating run of PCL–MCM-41 composites, attributed to the inferior pore size in the MCM-41 particles. Thus, this indicates variations in the inclusion of PCL chains within these two mesostructures with different pore sizes. Real-time variable-temperature small-angle X-ray scattering (SAXS) experiments with synchrotron radiation were crucial to confirm the presence of PCL within MCM-41 and SBA-15 pores. Accurate information was also deduced from these measurements regarding the influence of these two mesoporous MCM-41 and SBA-15 silicas on PCL long spacing. The differences found in these morphological and structural features were responsible for the ultimate mechanical response exhibited by the two sets of PCL nanocomposites, with a considerably higher increase of mechanical parameters in the SBA-15 family.https://www.mdpi.com/2504-477X/5/12/321mesoporous silicaMCM-41 and SBA-15PCL nanocompositessynchrotron SAXS measurementscrystallitesrigidity modulus |
| spellingShingle | Tamara M. Díez-Rodríguez Enrique Blázquez-Blázquez Nadine L. C. Antunes Maria do Rosário Ribeiro Ernesto Pérez María L. Cerrada Confinement in Extruded Nanocomposites Based on PCL and Mesoporous Silicas: Effect of Pore Sizes and Their Influence in Ultimate Mechanical Response Journal of Composites Science mesoporous silica MCM-41 and SBA-15 PCL nanocomposites synchrotron SAXS measurements crystallites rigidity modulus |
| title | Confinement in Extruded Nanocomposites Based on PCL and Mesoporous Silicas: Effect of Pore Sizes and Their Influence in Ultimate Mechanical Response |
| title_full | Confinement in Extruded Nanocomposites Based on PCL and Mesoporous Silicas: Effect of Pore Sizes and Their Influence in Ultimate Mechanical Response |
| title_fullStr | Confinement in Extruded Nanocomposites Based on PCL and Mesoporous Silicas: Effect of Pore Sizes and Their Influence in Ultimate Mechanical Response |
| title_full_unstemmed | Confinement in Extruded Nanocomposites Based on PCL and Mesoporous Silicas: Effect of Pore Sizes and Their Influence in Ultimate Mechanical Response |
| title_short | Confinement in Extruded Nanocomposites Based on PCL and Mesoporous Silicas: Effect of Pore Sizes and Their Influence in Ultimate Mechanical Response |
| title_sort | confinement in extruded nanocomposites based on pcl and mesoporous silicas effect of pore sizes and their influence in ultimate mechanical response |
| topic | mesoporous silica MCM-41 and SBA-15 PCL nanocomposites synchrotron SAXS measurements crystallites rigidity modulus |
| url | https://www.mdpi.com/2504-477X/5/12/321 |
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