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Phase Structure and Properties of Ternary Polylactide/Poly(Methyl Methacrylate)/Polysilsesquioxane Blends

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Phase Structure and Properties of Ternary Polylactide/Poly(Methyl Methacrylate)/Polysilsesquioxane Blends polymers Article Phase Structure and Properties of Ternary Polylactide/ Poly(methyl methacrylate)/Polysilsesquioxane Blends Anna Kowalewska 1,* , Agata S. Herc 1 , Joanna Bojda 1, Maria Nowacka 1 , Mariia Svyntkivska 1, Ewa Piorkowska 1, Witold Kaczorowski 2 and Witold Szyma ´nski 2 1 Centre of Molecular and Macromolecular Studies, Polish Academy of Sciences, Sienkiewicza 112, 90-363 Lodz, Poland; [email protected] (A.S.H.); [email protected] (J.B.); [email protected] (M.N.); [email protected] (M.S.); [email protected] (E.P.) 2 Institute of Materials Science and Engineering, Lodz University of Technology, Stefanowskiego 1/15, 90-924 Lodz, Poland; [email protected] (W.K.); [email protected] (W.S.) * Correspondence: [email protected] Abstract: Ternary blends of polylactide (PLA, 90 wt.%) and poly(methyl methacrylate) (PMMA, 10 wt.%) with functionalized polysilsesquioxanes (LPSQ-R) were obtained by solution blending. R groups in LPSQ containing hydroxyethyl (LPSQ-OH), methylglycolic (LPSQ-COOMe) and pentaflu- orophenyl (LPSQ-F5) moieties of different chemical properties were designed to modify PLA blends with PMMA. The effect of the type of LPSQ-R and their content, 1–3 wt.%, on the structure of the blends was studied with scanning electron microscopy (SEM) combined with energy dispersive spectroscopy (SEM-EDS), dynamic mechanical thermal analysis (DMTA) and Raman spectroscopy. Citation: Kowalewska, A.; Differential scanning calorimetry (DSC) and tensile tests also showed various effects of LPSQ-R on Herc, A.S.; Bojda, J.; Nowacka, M.; the thermal and mechanical properties of the blends. Depth-sensing indentation was used to resolve Svyntkivska, M.; Piorkowska, E.; Kaczorowski, W.; Szyma´nski,W. spatially the micro- and nano-scale mechanical properties (hardness and elastic behaviour) of the Phase Structure and Properties of blends. The results showed clearly that LPSQ-R modulate the structure and properties of the blends. Ternary Polylactide/Poly(methyl methacrylate)/Polysilsesquioxane Keywords: PLA/PMMA blends; ternary polymer blends; polysilsesquioxanes Blends. Polymers 2021, 13, 1033. https://doi.org/10.3390/ polym13071033 1. Introduction Academic Editor: Aziz Biodegradable poly(lactic acid) (PLA) exhibits high strength and stiffness. Brittleness, Mansurovich Muzafarov low toughness, low melt strength, slow crystallization rate and low heat deflection tem- perature largely limit its wide use [1–3]. PLA may be toughened using various methods Received: 28 February 2021 (plasticization, copolymerization, filling and melt blending with other polymers) and the Accepted: 19 March 2021 relationships between PLA-based polymer blends composition, their morphology, mechan- Published: 26 March 2021 ical properties and toughening mechanisms behind the observed phenomena have been thoroughly studied [4–7]. The interfacial compatibility on a nanoscale level and the phase Publisher’s Note: MDPI stays neutral behaviour have a decisive influence on polymer blends. Miscibility may be favoured when with regard to jurisdictional claims in published maps and institutional affil- some special interactions, stronger than van der Waals forces (ionic interactions, dipole- iations. dipole, donor-acceptor and weak hydrogen bonding) exist between the blended materials. The intrinsic properties of the components, as well as the characteristic morphology of the blend determine the improvement of the final properties, e.g., mechanical, thermal and barrier properties. Interesting results were obtained on formation of miscible/immiscible binary blends Copyright: © 2021 by the authors. containing poly(methyl methacrylate) (PMMA). PMMA is known for intrinsic high mechan- Licensee MDPI, Basel, Switzerland. ical properties, UV resistance and long-term durability. Full miscibility of PLA and PMMA This article is an open access article was achieved through solution precipitation [8,9] and melt blending [10] whereas solution distributed under the terms and conditions of the Creative Commons casting resulted in two separate phases (co-continuous or separated inclusions) [8,10,11]. Attribution (CC BY) license (https:// The immiscibility–miscibility transition behaviour of PLA/PMMA blends changes with creativecommons.org/licenses/by/ composition [12,13] and temperature [14]. Rheological, thermomechanical, and mechanical 4.0/). properties of PLA/PMMA miscible blends with different compositions were extensively Polymers 2021, 13, 1033. https://doi.org/10.3390/polym13071033 https://www.mdpi.com/journal/polymers Polymers 2021, 13, x FOR PEER REVIEW 2 of 19 changes with composition [12,13] and temperature [14]. Rheological, thermomechanical, and mechanical properties of PLA/PMMA miscible blends with different compositions were extensively examined. The role of entanglement network in rheological and thermo- mechanical properties was explained [15–20]. The small size of the dispersed inclusions Polymers 2021, 13, 1033 as well as the strong interfacial interactions in PLA/PMMA blends is responsible2 of 19 for in- creased tensile strength. PMMA was also shown to provide increased hydrolytic and structural stability to the PLA/PMMA blends [21–23]. However, the improvement of im- examined.pact toughness The role in of binary entanglement blends network requires in addi rheologicaltion of and quite thermomechanical large amount prop-(>20 wt.%) of ertiesPMMA, was which explained has [15an– 20adverse]. The smalleffect sizeon the of the compostability dispersed inclusions of PLA. as In well addition, as the the im- strongprovement interfacial of impact interactions toughness in PLA/PMMA may be often blends accompanied is responsible by for a increased significant tensile reduction of strength.the tensile PMMA strength. was also shown to provide increased hydrolytic and structural stability to theTernary PLA/PMMA blends blends are [much21–23 ].more However, complex the improvementsystems with of a impactwide range toughness of possible in mi- binarycrostructures. blends requires Many additionvariables of that quite influenc large amounte the morphology, (>20 wt.%) of and PMMA, properties which has include the an adverse effect on the compostability of PLA. In addition, the improvement of impact volume fraction, inherent properties of the components and their miscibility. In the im- toughness may be often accompanied by a significant reduction of the tensile strength. miscibleTernary blends blends the are interfacial much more tension complex between systems withcomponents a wide range can ofbe possibleefficiently mi- reduced crostructures.through compatibilization, Many variables thatwhich influence results the in morphology,a better dispersion and properties of a minor include component the and volumeimproved fraction, interfacial inherent adhesion. properties That of the may components prevent and premature their miscibility. fracture In resulting the immis- from for- ciblemation blends of thelarge interfacial cavities tension inside between a minor components component can inclusions be efficiently or due reduced to separation through of the compatibilization,components. Ternary which resultsPLA/PMMA in a better blends dispersion with of aother minor thermoplastic component and improvedpolymers can be interfacialpromising adhesion. materials. That The may compatibilizers prevent premature should fracture be miscible resulting with from at formationleast one component of largeof the cavities blend. inside Addition a minor of componentcopolymers inclusions containi orng due functionalized to separation ofmethacrylate the components. blocks is an Ternary PLA/PMMA blends with other thermoplastic polymers can be promising materials. effective way to achieve good compatibility and toughening [24–34]. Nanofillers, e.g., na- The compatibilizers should be miscible with at least one component of the blend. Addition ofnosilica copolymers [17,35] containing or other functionalized minerals [36,37], methacrylate also blockshave isa anpositive effective effect way toon achieve properties of goodPLA/PMMA compatibility blends. and It toughening is worth mentioning [24–34]. Nanofillers, that PMMA e.g., nanosilica was also [applied17,35] or as other an effective mineralscompatibilizer [36,37], also that have provided a positive a toughening effect on properties effect ofin PLA/PMMA blends of PLA/polyvinylidene blends. It is worth fluo- mentioningride [38], PLA/polybutadiene-g-poly(styrene-c that PMMA was also applied as an effectiveo-acrylonitrile) compatibilizer [39,40], that PLA/poly(butylene provided a tougheningadipate-co-butylene effect in blends terephthalate) of PLA/polyvinylidene [41], PLA/polystyrene fluoride [38], [42] PLA/polybutadiene-g- or PLA/poly(epichlorohy- poly(styrene-co-acrylonitrile)drin-co-ethylene oxide) [43]. [39 ,40], PLA/poly(butylene adipate-co-butylene terephtha- late) [41We], PLA/polystyrenehave recently [found42] or PLA/poly(epichlorohydrin-co-ethylene that linear, ladder-like polysilsesquioxanes oxide) [43]. (LPSQ-R) We have recently found that linear, ladder-like polysilsesquioxanes (LPSQ-R) (Scheme1 ) (Scheme 1) may be applied as interesting modifiers of PLA [44–47]. LPSQ-R are amor- may be applied as interesting modifiers of PLA [44–47]. LPSQ-R are amorphous substances ofphous low glass substances transition of temperatures low glass transition that are partially temperatures miscible that with are PLA partially [44–46]. miscible Their net with PLA effect[44–46]. may Their be attributed net effect to plasticization may be attributed
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