Sequential crystallization and morphology of triple crystalline biodegradable PEO-b-PCL-b-PLLA triblock terpolymers
Open accessAbstract
The sequential crystallization of poly(ethylene oxide)- b -poly(ε-caprolactone)- b -poly( l -lactide) (PEO- b -PCL- b -PLLA) triblock terpolymers, in which the three blocks are able to crystallize separately and sequentially from the melt, is presented.
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The proposed lamellar arrangement includes the alternation of only one lamella of either PCL or PEO in between two lamellae of PLLA.
“From our observations, we proposed a lamellar arrangement that includes the alternation of only one lamella of either PCL or PEO in between two lamellae of PLLA.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The Morphology section reports PCL lamellar crystals in the interlamellar regions of PLLA spherulites and subsequent PEO crystallization there. The Conclusions describe three types of lamellae coexisting, but the paper does not specify that exactly one PCL or PEO lamella lies between two PLLA lamellae. (LLM, conf=0.85)
Experimental — accuracy not yet measuredA tri-lamellar self-assembly that included lamellae of the three phases was indirectly elucidated from AFM observations complemented with SAXS experiments and theoretical simulations.
“A tri-lamellar self-assembly that included lamellae of the three phases was indirectly elucidated from AFM observations complemented with SAXS experiments and theoretical simulations.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The SAXS characterization section proposes a morphology with three types of crystalline lamellae, and the Morphology section reports SAXS evidence for a complex triple-lamellar structure. Our copy does not support the claimed use of AFM observations or theoretical simulations: it describes polarized-light microscopy and rough theoretical calculations of melt miscibility instead. Page numbers are unavailable in the indexed copy. (LLM, conf=0.87)
Experimental — accuracy not yet measuredDuring the final cooling to 25 °C, the PEO block can crystallize, forming the thinnest lamellae of the three components.
“Finally, the sample was quenched to 25 ºC at 100 ºC min -1 (during this cooling, the PEO block can crystallize 35 , forming the thinnest lamellae of the three components).”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The Morphology section reports that PEO can crystallize after a final quench to room temperature, supporting the cooling portion of the claim. It describes three types of lamellae but does not say that PEO forms the thinnest; a search for comparative lamellar thickness found no such statement in our copy. Page numbers were not available. (LLM, conf=0.86)
Experimental — accuracy not yet measuredPEO23PCL34PLLA43 is melt miscible.
“the SAXS analysis proved the melt miscibility.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
In the SAXS characterization section (page not available), the authors report that PEO23PCL34PLLA43 had a broad, weak reflection at 140 °C and conclude that the terpolymers are “most likely miscible in the melt.” The SAXS analysis supports melt miscibility, but the citing sentence overstates that qualified conclusion as proof. (LLM, conf=0.86)
Experimental — accuracy not yet measuredUpon cooling from the melt, PLLA crystallizes first, creating a spherulitic superstructural template.
“Upon cooling from melt, PLOM and WAXS experiments confirmed that PLLA crystallizes first, creating a spherulitic superstructural template.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The WAXS results say PLLA crystallizes first, and the Conclusions say its crystallization templates the morphology upon cooling from the melt. However, the Conclusions also report that PLOM shows a composition-dependent shape: the template is spherulite-like at higher PLLA content but resembles axialites at lower PLLA content. (LLM, conf=0.88)
Experimental — accuracy not yet measured
The thickest lamellae (15 nm) belong to the PLLA block, while the thinnest lamellae (10 nm) belong to the PCL block.
“We established that the thickest lamellae (15 nm, red) should belong to the PLLA block because this block is the one that crystallizes first, while the thinnest lamellae (10 nm, green) should belong to the PCL block.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The morphology section (page unavailable) reports that PLLA crystallizes before PCL, supporting the sentence’s rationale. It does not assign 15 nm lamellae to PLLA or 10 nm lamellae to PCL; the same section says the exact origin of the SAXS reflections needs further investigation. (LLM, conf=0.85)
Experimental — accuracy not yet measuredThe templated morphology did not change during the successive crystallization of the PEO and PCL blocks, and only a slight change in the magnitude of the birefringence was observed.
“The templated morphology did not change during the successive crystallization of the other PEO and PCL blocks, and only a slight change in the magnitude of the birefringence was observed.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The Morphology section and Conclusions (page not provided) say that PCL and PEO crystallization do not alter the PLLA-templated superstructure. They describe clear changes in birefringence, including intense brightness after PCL crystallization, rather than only a slight change. (LLM, conf=0.88)
Experimental — accuracy not yet measuredThe PEO block crystallizes during the final quench treatment by cooling the sample to 25 °C at 100 °C.min-1.
“Finally, the PEO block will crystallize during the last final quench treatment applied by cooling the sample to 25 °C at 100 °C.min-1 .35”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The morphology section says the final quench was to room temperature, where the PEO block can crystallize. It does not specify 25 °C or a cooling rate of 100 °C min⁻¹ for that quench; the paper reports other cooling rates for its DSC and WAXS measurements. (LLM, conf=0.88)
Experimental — accuracy not yet measuredThe melting point values reported are a range because they depend on previous thermal history and scanning rates.
“The melting point values reported here are a range because they depend on previous thermal history (controlled cooling or isothermal crystallization) and scanning rates employed during their determination (1, 5 or 20 ºC/min)”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The DSC methods and Tables 3 and 5 (page not specified) report melting temperatures after different thermal histories, supporting the idea that the reported values can form a range. But the paper uses 1 °C/min for cooling, not for determining melting points, and its isothermal crystallization protocol concerns morphological observations; the claim overstates the stated basis for the range. (LLM, conf=0.84)
Experimental — accuracy not yet measuredA previous SAXS analysis suggested that a lamella of either PEO or PCL randomly inserts between two adjacent PLLA lamellae.
“In our previous publication, 35 an exhaustive theoretical analysis of SAXS characterization upon heating suggested that a lamella of either PEO or PCL randomly inserts between two adjacent PLLA lamellae.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The SAXS characterization section reports measurements during heating and suggests a structure containing three types of crystalline lamellae. The Morphology section places PCL crystallization in regions between PLLA lamellae and describes PEO crystallization within the same spherulites, but it does not propose that a PEO or PCL lamella randomly inserts between each pair of adjacent PLLA lamellae. It says further investigation is needed to explain the exact origin of the SAXS reflections; the claimed exhaustive theoretical analysis is not supported. (LLM, conf=0.85)
Experimental — accuracy not yet measuredThe Dimension Icon AFM microscope showed to some extent the random lamellar arrangement proposed earlier and gives clear evidence of the multi-crystalline morphology of triple crystalline PEO-b-PCL-b-PLLA triblock terpolymers.
“What is significant is that the Dimension Icon AFM microscope not only showed to some extent the random lamellar arrangement proposed earlier, 35 but in addition, it gives clear evidence of the multi-crystalline morphology of triple crystalline PEO-b-PCL-b-PLLA triblock terpolymers.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The citation follows the reference to an earlier proposed lamellar arrangement, not the citing authors’ Dimension Icon AFM observation. In the SAXS characterization section (page unavailable), the source proposes three types of crystalline lamellae within spherulites; the Morphology section describes an irregular superstructure. It does not specifically propose that the lamellae are randomly arranged. (LLM, conf=0.77)
Experimental — accuracy not yet measuredWAXS showed both PLLA and PEO reflections, but some PLLA and PEO reflections overlap, so the presence of PEO crystals could only be indirectly confirmed.
“Both PLLA and PEO reflections were observed.However, some reflections of PLLA and PEO crystals overlap (more details are in 35 ).Therefore, after the WAXS experiment, the presence of the PEO crystals could only be indirectly confirmed.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The Non-Isothermal Crystallization section reports that the PLLA 203 reflection coincides with the PEO 120 reflection, supporting the overlap claim. But it also identifies a separate PEO reflection as evidence of PEO crystallization and says the WAXS patterns confirm the terpolymers’ triple-crystalline nature beyond doubt. It does not support the claim that PEO crystals could only be indirectly confirmed. (LLM, conf=0.88)
Experimental — accuracy not yet measuredUpon cooling from the melt, WAXS and DSC analysis showed that the PLLA block crystallizes first, followed by the PCL and lastly the PEO in the diblock and triblock.
“Wide-angle X-Ray scattering (WAXS) measurements, carried out during cooling, confirmed that the PLLA block is the one that crystallizes first, followed by the PCL and lastly, the PEO.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The PEO-b-PCL-b-PLLA is a triblock terpolymer with an alternating superstructure of three crystalline phases.
“The PEO-b-PCL-b-PLLA is a triblock terpolymer with an alternating superstructure of three crystalline phases, as we had reported in previous publications.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The melting points of each component determined by DSC previously are given in Table 1.
“The melting points of each component determined by DSC previously [33][34][35][36] are also given in Table 1.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
Both samples are most probably melt miscible.
“Both samples are most probably melt miscible.SAXS observations in the melt showed no scattering, 33,35 , although the electron density between these blocks is quite similar.26”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The three blocks in PEO23PCL34PLLA43 are able to crystallize.
“In our previous reports, 33,35 , we demonstrated by DSC and WAXS that the three blocks in PEO23PCL34PLLA43 are able to crystallize”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
PEO crystallizes last, growing its lamellar crystals inside the available interlamellar spaces beside PCL and PLLA lamellae, because it is covalently bonded to the PCL block.
“The last block to crystallize is the PEO block, and it has no other option but to grow its lamellar crystals inside the available interlamellar spaces aside PCL and PLLA lamellae, as it is covalently bonded to the PCL block.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
After PLLA, the PCL block crystallizes inside the interlamellar spaces of the PLLA spherulites or axialites.
“Then, the next block to crystallize is the PCL block, which must crystallize inside the interlamellar spaces of the PLLA spherulites (or axialites).”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
Based on the different melting temperatures of each block (PCL melts at around 55 °C and PLLA at around 120 °C), if the sample is heated above the melting point of PCL but below that of PLLA, the PCL phase should disappear while PLLA lamellae remain intact.
“Based on the different melting temperatures of each block (the PCL block melts at around 55 °C and PLLA block at around 120 °C, see Table 1 and our previous work 35 ), the premise is that if the sample is heated until a temperature above the melting point of the PCL lamellae but sufficiently low to keep the PLLA phase crystallized, we should be able to see the disappearance of the PCL phase, while”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
After using a more diluted 0.1 wt% sample solution, AFM height images at 25 °C show a clear trilayered morphology with three lamellar thickness populations: 18, 14, and 10 nm.
“After employing a more diluted sample solution, the Dimension Icon AFM microscope confirms the multiphasic lamellar morphology that the authors hypothesized earlier.35 An extraordinary view of the tri-lamellar arrangement is given by the AFM height images taken at 25 °C (see Figure 9a).”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
In a previous report, three different lamellar thicknesses of 15, 10, and 7 nm were identified by AFM.
“In our previous report 35 , we were able to identify three different lamellar thicknesses by AFM (15, 10, and 7 nm), and we hypothesized about their origin.”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
The SAXS characterization and morphology sections discuss lamellar structures and SAXS long periods, but do not report AFM measurements of lamellar thickness. Searches for AFM, lamellar thickness, and 15, 10, and 7 nm found no passage in our copy establishing the claimed measurements. (LLM, conf=0.75)
Experimental — accuracy not yet measuredThe measured lamellar thickness values of 18, 14, and 10 nm are slightly higher than the previously reported values of 15, 10, and 7 nm.
“These values are slightly higher than those that were previously reported: 15, 10, and 7 nm.35”
From Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy (2020) · cites this paper as [35]
Table 6 in the copy (page not clearly labeled) reports SAXS long-period distances for the terpolymers, not the claimed previously reported lamellar thicknesses of 15, 10, and 7 nm. Searches for those three values and for lamellar thickness found no passage that establishes the attributed comparison. (LLM, conf=0.74)
Experimental — accuracy not yet measured
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Flagged first, then by citations
1 of the 61 references couldn’t be matched to a known paper.
Research works printed but not linked: 4
- A. J. Müller , M. L.Arnal and A. T.Lorenzo, in Handbook of Polymer Crystallization, ed. E. Piorkowska and G. C. Rutledge, John Wiley and Sons, Hoboken, New Jersey, 2013, ch. 12, pp. 347–372
- Hamley, 2004, Prog. Polym. Sci., 29, 909
- A. J. Muller , M.Avila, G.Saenz and J.Salazar, in Poly(lactic acid) Science and Technology: Processing, Properties, Additives and Applications, ed. A. Jimenez, M. Peltzer and R. Ruseckaite, The Royal Society of Chemistry, Cambridge, 2015, vol. 12, ch. 3, pp. 66–98
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Cited by
Sorted by citations
Fractionated crystallization in semicrystalline polymers
Sangroniz, L., Wang, B., Su, Y., Liu, G., Cavallo, D., Wang, D., & Müller, A. J. (2021) · Progress in Polymer Science · doi:10.1016/j.progpolymsci.2021.101376 · Cited by 102 · see citing works
Self-citationLi, L., Cao, Z.-Q., Bao, R., Xie, B., Yang, M., & Yang, W. M. (2017) · European Polymer Journal · doi:10.1016/j.eurpolymj.2017.10.025 · Cited by 54 · see citing works
Recent progress in block copolymer crystallization
Horn, R. M. V., Steffen, M. R., & O’Connor, D. (2018) · Polymer Crystallization · doi:10.1002/pcr2.10039 · Cited by 49 · see citing works
Palacios, J. K., Zhao, J., Hadjichristidis, N., & Müller, A. J. (2017) · Macromolecules · doi:10.1021/acs.macromol.7b02148 · Cited by 41 · see citing works
Self-citationTrilayered morphology of an ABC triple crystalline triblock terpolymer
Palacios, J. K., Tercjak, A., Liu, G., Wang, D., Zhao, J., Hadjichristidis, N., & Müller, A. J. (2017) · Macromolecules · doi:10.1021/acs.macromol.7b01576 · Cited by 37 · see citing works
Self-citationSachan, R., Warkar, S. G., & Purwar, R. (2022) · Polymer-Plastics Technology and Materials · doi:10.1080/25740881.2022.2113890 · Cited by 36 · see citing works
Single crystals and two‐dimensional crystalline assemblies of block copolymers
Yang, C., Li, Z., & Xu, J. (2022) · Journal of Polymer Science · doi:10.1002/pol.20210866 · Cited by 26 · see citing works
Tetracrystalline Tetrablock Quarterpolymers: Four Different Crystallites under the Same Roof
Ladelta, V., Zapsas, G., Abou‐hamad, E., Gnanou, Y., & Hadjichristidis, N. (2019) · Angewandte Chemie International Edition · doi:10.1002/anie.201908688 · Cited by 22 · see citing works
Self-citationZaldua, N., Múgica, A., Zubitur, M., Iturrospe, A., Arbe, A., Re, G. L., Raquez, J., Dúbois, P., & Müller, A. J. (2016) · CrystEngComm · doi:10.1039/c6ce02005d · Cited by 22 · see citing works
Self-citationPalacios, J. K., Mugica, A., Zubitur, M., & Müller, A. J. (2018) · Crystallization in Multiphase Polymer Systems · doi:10.1016/b978-0-12-809453-2.00006-2 · Cited by 18 · see citing works
Self-citationCrystallization, morphology and self-assembly of double, triple and tetra crystalline block polymers
Palacios, J. K., Michell, R. M., & Müller, A. J. (2023) · Polymer Testing · doi:10.1016/j.polymertesting.2023.107995 · Cited by 17 · see citing works
Self-citationMatxinandiarena, E., Múgica, A., Tercjak, A., Ladelta, V., Zapsas, G., Hadjichristidis, N., Cavallo, D., Flores, A., & Müller, A. J. (2021) · Macromolecules · doi:10.1021/acs.macromol.1c01186 · Cited by 16 · see citing works
Self-citationBlock Copolymers with Crystallizable Blocks: Synthesis, Self-Assembly and Applications
Schmalz, H., & Abetz, V. (2022) · Polymers · doi:10.3390/polym14040696 · Cited by 16 · see citing works
Palacios, J. K., Liu, G., Wang, D., Hadjichristidis, N., & Müller, A. J. (2019) · Macromolecular Chemistry and Physics · doi:10.1002/macp.201900292 · Cited by 15 · see citing works
Self-citationCrystallization of Polymers in Confined Space
Samanta, P., Liu, C., Nandan, B., & Chen, H. (2017) · Elsevier eBooks · doi:10.1016/b978-0-12-809453-2.00013-x · Cited by 13 · see citing works
Matxinandiarena, E., Múgica, A., Zubitur, M., Ladelta, V., Zapsas, G., Cavallo, D., Hadjichristidis, N., & Müller, A. J. (2021) · Polymers · doi:10.3390/polym13183133 · Cited by 12 · see citing works
Self-citationPalacios, J. K., Zhang, H., Zhang, B., Hadjichristidis, N., & Müller, A. J. (2020) · Polymer · doi:10.1016/j.polymer.2020.122863 · Cited by 11 · see citing works
Self-citationLadelta, V., Zapsas, G., Gnanou, Y., & Hadjichristidis, N. (2019) · Journal of Polymer Science Part A Polymer Chemistry · doi:10.1002/pola.29492 · Cited by 9 · see citing works
Self-citationCan five chemically different lamellar crystals self-assemble in a single spherulite?
Matxinandiarena, E., Pérez‐Camargo, R. A., Sebastián, V., Zhang, P., Ladelta, V., Hadjichristidis, N., & Müller, A. J. (2025) · Nature Communications · doi:10.1038/s41467-025-64845-6 · Cited by 4 · see citing works
Self-citationLiu, X., Huang, M., Zhu, P., Dong, S., Dong, X., & Wang, D. (2018) · Polymer International · doi:10.1002/pi.5653 · Cited by 4 · see citing works
Self-citationTetracrystalline Tetrablock Quarterpolymers: Four Different Crystallites under the Same Roof
Ladelta, V., Zapsas, G., Abou‐Hamad, E., Gnanou, Y., & Hadjichristidis, N. (2019) · Angewandte Chemie · doi:10.1002/ange.201908688 · Cited by 3 · see citing works
Self-citationPolymer blends and multiphase systems
Lorenzo, M. L. D., Passaglia, E., & Righetti, M. C. (2026) · Elsevier eBooks · doi:10.1016/b978-0-443-33228-9.00020-8
- Authors
- Palacios, J. K., Mugica, A., Zubitur, M., Iturrospe, A., Arbe, A., Liu, G., Wang, D., Zhao, J., Hadjichristidis, N., & Müller, A. J.
- Affiliations
- University of the Basque Country (ES)
- POLYMAT and Polymer Science and Technology Department
- Material Physics Center (ES)
- Chinese Academy of Sciences (CN)
- King Abdullah University of Science and Technology (SA)
- Ikerbasque (ES)
- Corresponding author
- Hadjichristidis, Nikos
- Müller, Alejandro J.
- ORCID
- Venue
- RSC Advances
- Publisher
- Royal Society of Chemistry (RSC)
- Published
- 2016
- Volume
- 6
- Issue
- 6
- Pages
- 4739-4750
- ISSN
- 2046-2069 (ISSN-L)
- OpenAlex
- W2228175695
- Cited by
- 23
- References
- 61
- Citations by year
- 2026: 1 · 2025: 1 · 2023: 1 · 2022: 4 · 2021: 3 · 2020: 1 · 2019: 4 · 2018: 2 · 2017: 5 · 2016: 1
- FWCI
- 2.67
- Type
- journal article
- Language
- en
- Open access
- bronze
- doi.org
- Locations
- RSC Advances (publishedVersion)
- DIGITAL.CSIC (Spanish National Research Council (CSIC)) (submittedVersion, other-oa)
- King Abdullah University of Science and Technology Repository (King Abdullah University of Science and Technology) (submittedVersion)
- Funders
- Eusko Jaurlaritza (GIC IT-586-13)
- Topics
- Physical Sciences › Materials Science › Polymers and Plastics › Polymer crystallization and properties
- Physical Sciences › Materials Science › Biomaterials › biodegradable polymer synthesis and properties
- Physical Sciences › Materials Science › Materials Chemistry › Block Copolymer Self-Assembly
- Keywords
- sequential crystallization, triblock terpolymers, poly(ethylene oxide), polycaprolactone, poly(L-lactic acid), biodegradable polymers, polymer morphology, block copolymers, melt crystallization
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