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dc.contributor.authorMatxinandiarena, Eider
dc.contributor.authorMúgica, Agurtzane
dc.contributor.authorZubitur, Manuela
dc.contributor.authorLadelta, Viko
dc.contributor.authorZapsas, Georgios
dc.contributor.authorCavallo, Dario
dc.contributor.authorHadjichristidis, Nikos
dc.contributor.authorMüller, Alejandro J.
dc.date.accessioned2021-09-19T06:04:18Z
dc.date.available2021-09-19T06:04:18Z
dc.date.issued2021-09-16
dc.date.submitted2021-09-02
dc.identifier.citationMatxinandiarena, E., Múgica, A., Zubitur, M., Ladelta, V., Zapsas, G., Cavallo, D., … Müller, A. J. (2021). Crystallization and Morphology of Triple Crystalline Polyethylene-b-poly(ethylene oxide)-b-poly(ε-caprolactone) PE-b-PEO-b-PCL Triblock Terpolymers. Polymers, 13(18), 3133. doi:10.3390/polym13183133
dc.identifier.issn2073-4360
dc.identifier.doi10.3390/polym13183133
dc.identifier.urihttp://hdl.handle.net/10754/671283
dc.description.abstractThe morphology and crystallization behavior of two triblock terpolymers of polymethylene, equivalent to polyethylene (PE), poly (ethylene oxide) (PEO), and poly (ε-caprolactone) (PCL) are studied: PE227.1-b-PEO4615.1-b-PCL3210.4 (T1) and PE379.5-b-PEO348.8-b-PCL297.6 (T2) (superscripts give number average molecular weights in kg/mol and subscripts composition in wt %). The three blocks are potentially crystallizable, and the triple crystalline nature of the samples is investigated. Polyhomologation (C1 polymerization), ring-opening polymerization, and catalyst-switch strategies were combined to synthesize the triblock terpolymers. In addition, the corresponding PE-b-PEO diblock copolymers and PE homopolymers were also analyzed. The crystallization sequence of the blocks was determined via three independent but complementary techniques: differential scanning calorimetry (DSC), in situ SAXS/WAXS (small angle X-ray scattering/wide angle X-ray scattering), and polarized light optical microscopy (PLOM). The two terpolymers (T1 and T2) are weakly phase segregated in the melt according to SAXS. DSC and WAXS results demonstrate that in both triblock terpolymers the crystallization process starts with the PE block, continues with the PCL block, and ends with the PEO block. Hence triple crystalline materials are obtained. The crystallization of the PCL and the PEO block is coincident (i.e., it overlaps); however, WAXS and PLOM experiments can identify both transitions. In addition, PLOM shows a spherulitic morphology for the PE homopolymer and the T1 precursor diblock copolymer, while the other systems appear as non-spherulitic or microspherulitic at the last stage of the crystallization process. The complicated crystallization of tricrystalline triblock terpolymers can only be fully grasped when DSC, WAXS, and PLOM experiments are combined. This knowledge is fundamental to tailor the properties of these complex but fascinating materials.
dc.description.sponsorshipThis research received funding from MINECO through projects MAT2017-83014-C2-1-P,from the Basque Government through grant IT1309-19, and from ALBA synchrotron facility through granted proposal u2020084441 (March 2020). We would like to thank the financial support provided by the BIODEST project; this project has received funding from the European Union’s Horizon 2020 research and innovation program under the Marie Sklodowska-Curie grant agreement no. 778092. GZ, VL, and NH wish to acknowledge the support of KAUST.
dc.publisherMDPI AG
dc.relation.urlhttps://www.mdpi.com/2073-4360/13/18/3133
dc.rightsThis is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited/
dc.rights.urihttps://creativecommons.org/licenses/by/4.0/
dc.titleCrystallization and Morphology of Triple Crystalline Polyethylene-b-poly(ethylene oxide)-b-poly(ε-caprolactone) PE-b-PEO-b-PCL Triblock Terpolymers
dc.typeArticle
dc.contributor.departmentKAUST Catalysis Center (KCC)
dc.contributor.departmentChemical Science Program
dc.contributor.departmentPhysical Science and Engineering (PSE) Division
dc.identifier.journalPolymers
dc.eprint.versionPublisher's Version/PDF
dc.contributor.institutionPOLYMAT and Department of Polymers and Advanced Materials: Physics, Chemistry and Technology, University of the Basque Country UPV/EHU, Paseo Manuel Lardizábal 3,20018 Donostia-San Sebastián, Spain.
dc.contributor.institutionDepartment of Chemical and Environmental Engineering, University of the Basque Country, UPV/EHU, Plaza Europa 1, 20018 Donostia-San Sebastián, Spain.
dc.contributor.institutionDepartment of Chemistry and Industrial Chemistry, University of Genova, Via Dodecaneso 31, 16146 Genova, Italy.
dc.contributor.institutionIkerbasque, Basque Foundation for Science, Plaza Euskadi 5, 48009 Bilbao, Spain.
dc.identifier.volume13
dc.identifier.issue18
dc.identifier.pages3133
kaust.personLadelta, Viko
kaust.personZapsas, Georgios
kaust.personHadjichristidis, Nikos
dc.date.accepted2021-09-13
refterms.dateFOA2021-09-19T06:05:52Z


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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited/
Except where otherwise noted, this item's license is described as This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited/