Characterization of the polycaprolactone melt crystallization: Complementary optical microscopy, DSC, and AFM studies
Open accessAbstract
The first stages of the crystallization of polycaprolactone (PCL) were studied using several techniques. The crystallization exotherms measured by differential scanning calorimetry (DSC) were analyzed and compared with results obtained by polarized optical microscopy (POM), rheology, and atomic force microscope (AFM). The experimental results suggest a strong influence of the observation scale. In particular, the AFM, even if limited on time scale, appears to be the most sensitive technique to detect the first stages of crystallization. On the contrary, at least in the case analysed in this work, rheology appears to be the least sensitive technique. DSC and POM provide closer results. This suggests that the definition of induction time in the polymer crystallization is a vague concept that, in any case, requires the definition of the technique used for its characterization.
The claims and statistics of this paper haven’t been checked yet.
Run the check — free, no account needed. It reads the open-access text and checks the sources it cites.
Integrity signals
Registry
Cites
Statistics
Claims the paper makes
The claims and statistics of this paper haven’t been checked yet.
Run the check — free, no account needed. It reads the open-access text and checks the sources it cites.
Claims other papers make about this one
Each is checked against this paper’s own text: does it say what the citing paper says it does?
PCL is in the rubbery state at room temperature, with a glass transition temperature at about −60 °C and a melting point at about 65 °C.
“the poly(ε-caprolactone) (PCL) is in the rubbery state at room temperature, showing a glass transition temperature at about −60 °C and a melting point at about 65 °C [12].”
From Thermo-Rheological and Shape Memory Properties of Block and Random Copolymers of Lactide and ε-Caprolactone (2021) · cites this paper as [12]
The Experimental section (2.4 and 2.6; page unavailable) describes PCL’s melting temperature as about 60 °C, close to the claimed approximate 65 °C. Our copy does not state a glass-transition temperature of about −60 °C or describe PCL as rubbery at room temperature; searches for those terms found no supporting passage. (LLM, conf=0.83)
Experimental — accuracy not yet measured
Self-check
Percentages, sums and reported differences re-computed from the paper’s own numbers.
The self-check needs the paper’s full text.
Cites
Gee, G. (1972) · Polymer · doi:10.1016/0032-3861(72)90025-0 · Cited by 1,367 · see citing works
Modeling of morphology evolution in the injection molding process of thermoplastic polymers
Pantani, R., Coccorullo, I., Speranza, V., & Titomanlio, G. (2005) · Progress in Polymer Science · doi:10.1016/j.progpolymsci.2005.09.001 · Cited by 291 · see citing works
Pogodina, N. V., Lavrenko, V. P., Srinivas, S., & Winter, H. H. (2001) · Polymer · doi:10.1016/s0032-3861(01)00402-5 · Cited by 197 · see citing works
Direct Observation of Growth of Lamellae and Spherulites of a Semicrystalline Polymer by AFM
Li, L., Chan, C., Yeung, K. L., Li, J., Ng, K., & Lei, Y. (2000) · Macromolecules · doi:10.1021/ma000273e · Cited by 158 · see citing works
Rheological mechanism and overview of nucleated crystallization kinetics
Khanna, Y. P. (1993) · Macromolecules · doi:10.1021/ma00066a024 · Cited by 124 · see citing works
Hobbs, J., McMaster, T. J., Miles, M. J., & Barham, P. (1998) · Polymer · doi:10.1016/s0032-3861(97)00586-7 · Cited by 120 · see citing works
Ivanov, D. A., Amalou, Z., & Magonov, S. (2001) · Macromolecules · doi:10.1021/ma010809b · Cited by 119 · see citing works
Pearce, R., & Vancso, G. J. (1997) · Macromolecules · doi:10.1021/ma970463y · Cited by 119 · see citing works
Real-time crystallization study of poly(ϵ-caprolactone) by hot-stage atomic force microscopy
Beekmans, L. G. M., & Vancso, G. J. (2000) · Polymer · doi:10.1016/s0032-3861(00)00240-8 · Cited by 82 · see citing works
Zhou, W., Cheng, S. Z. D., Putthanarat, S., Eby, R. K., Reneker, D. H., Lotz, B., Magonov, S., Hsieh, E. T., Geerts, R. G., Palackal, S. J., et al. (2000) · Macromolecules · doi:10.1021/ma000802e · Cited by 72 · see citing works
Real-time imaging of melting and crystallization in poly(ethylene oxide) by atomic force microscopy
Pearce, R., & Vancso, G. J. (1998) · Polymer · doi:10.1016/s0032-3861(97)00420-5 · Cited by 67 · see citing works
Crystal Growth in Poly( L ‐lactide) Thin Film Revealed by in situ Atomic Force Microscopy
Kikkawa, Y., Abe, H., Fujita, M., Iwata, T., Inoue, Y., & Doi, Y. (2003) · Macromolecular Chemistry and Physics · doi:10.1002/macp.200350044 · Cited by 64 · see citing works
AFM study of morphological development during the melt-crystallization of poly(ethylene oxide)
Schultz, J. M., & Miles, M. J. (1998) · Journal of Polymer Science Part B Polymer Physics · doi:10.1002/(sici)1099-0488(19980930)36:13 · Cited by 63 · see citing works
Jiang, Y. D., Yan, D., Gao, X., Han, C. C.-C., Jin, X., Li, L., Wang, Y., & Chan, C. (2003) · Macromolecules · doi:10.1021/ma0341061 · Cited by 49 · see citing works
Molecular orientation and strain in injection moulding of thermoplastics
Pantani, R., Speranza, V., Sorrentino, A., & Titomanlio, G. (2002) · Macromolecular Symposia · doi:10.1002/1521-3900(200208)185:1 · Cited by 40 · see citing works
Pearce, R., & Vancso, G. J. (1998) · Journal of Polymer Science Part B Polymer Physics · doi:10.1002/(sici)1099-0488(199810)36:14 · Cited by 38 · see citing works
Nucleation and Growth of Poly(ε-caprolactone) on Poly(tetrafluoroethylene) by in-Situ AFM
Beekmans, L. G. M., Vallée, R. A. L., & Vancso, G. J. (2002) · Macromolecules · doi:10.1021/ma020237a · Cited by 36 · see citing works
Structure development during crystallization of polycaprolactone
Acierno, S., Maio, E. D., Iannace, S., & Grizzuti, N. (2005) · Rheologica Acta · doi:10.1007/s00397-005-0054-2 · Cited by 34 · see citing works
Sorrentino, A., Pantani, R., & Titomanlio, G. (2006) · Journal of Polymer Science Part B Polymer Physics · doi:10.1002/polb.21039 · Cited by 33 · see citing works
Nagatake, W., Takahashi, T., Masubuchi, Y., Takimoto, J., & Koyama, K. (2000) · Polymer · doi:10.1016/s0032-3861(99)00226-8 · Cited by 32 · see citing works
Depolarization of linearly polarized light by a polycrystalline specimen
Binsbergen, F. L. (1970) · Journal of Macromolecular Science Part B · doi:10.1080/00222347008217126 · Cited by 30 · see citing works
Relevance of Crystallisation Kinetics in the Simulation of the Injection Molding Process
Pantani, R., Speranza, V., & Titomanlio, G. (2001) · International Polymer Processing · doi:10.3139/217.1620 · Cited by 29 · see citing works
AFM study of in situ real time polymer crystallization and spherulite structure
McMaster, T. J., Hobbs, J., Barham, P., & Miles, M. J. (1997) · Probe Microscopy · Cited by 21 · see citing works
Applicability of light depolarization technique to crystallization studies
Ziabicki, A., & Misztal-Faraj, B. (2005) · Polymer · doi:10.1016/j.polymer.2005.01.021 · Cited by 18 · see citing works
Applicability of light transmission technique to studies of crystalline polymers texture
Ziabicki, A. (1967) · Colloid & Polymer Science · doi:10.1007/bf02086089 · Cited by 13 · see citing works
Martins, J. A., Zhang, W., Brito, A. M., Infante, U., Romero, M., & Soares, F. (2005) · Review of Scientific Instruments · doi:10.1063/1.2083087 · Cited by 11 · see citing works
Santis, F. D., Vietri, A. R., & Pantani, R. (2006) · Macromolecular Symposia · doi:10.1002/masy.200650202 · Cited by 8 · see citing works
Flagged first, then by citations
1 of the 28 references couldn’t be matched to a known paper.
Cited by
Sorted by citations
Charoo, N. A., Ali, S. F. B., Mohamed, E. M., Kuttolamadom, M. A., Ozkan, T., Khan, M. A., & Rahman, Z. (2020) · Drug Development and Industrial Pharmacy · doi:10.1080/03639045.2020.1764027 · Cited by 270 · see citing works
Structural Evolution of PCL during Melt Extrusion 3D Printing
Liu, F., Vyas, C., Poologasundarampillai, G., Pape, I., Hinduja, S., Mirihanage, W. U., & Bártolo, P. (2017) · Macromolecular Materials and Engineering · doi:10.1002/mame.201700494 · Cited by 110 · see citing works
3D‐Printed Polymeric Biomaterials for Health Applications
Zhu, Y., Guo, S., Ravichandran, D., Ramanathan, A., Sobczak, M. T., Sacco, A. F., Patil, D., Thummalapalli, S. V., Pulido, T. V., Lancaster, J. N., et al. (2024) · Advanced Healthcare Materials · doi:10.1002/adhm.202402571 · Cited by 100 · see citing works
Johnson, L. M., Krovi, S. A., Li, L., Girouard, N., Demkovich, Z. R., Myers, D., Creelman, B., & van der Straten, A. (2019) · Pharmaceutics · doi:10.3390/pharmaceutics11070315 · Cited by 82 · see citing works
de Cassan, D., Hoheisel, A. L., Glasmacher, B., & Menzel, H. (2019) · Journal of Materials Science Materials in Medicine · doi:10.1007/s10856-019-6245-7 · Cited by 48 · see citing works
The Effect of Inkjet Printing over Polymeric Films as Potential Buccal Biologics Delivery Systems
Montenegro-Nicolini, M., Reyes, P. E., Jara, M. O., Vuddanda, P. R., Neira‐Carrillo, A., Butto-Miranda, N., Velaga, S. P., & Morales, J. O. (2018) · AAPS PharmSciTech · doi:10.1208/s12249-018-1105-1 · Cited by 35 · see citing works
Naddeo, M., Sorrentino, A., & Pappalardo, D. (2021) · Polymers · doi:10.3390/polym13040627 · Cited by 25 · see citing works
“On the contrary, the poly(ε-caprolactone) (PCL) is in the rubbery state at room temperature, showing a glass transition temperature at about −60 ◦C and a melting point at about 65 ◦C [12].”
BackgroundLizarazo-Fonseca, L., Correa-Araujo, L., Prieto-Abello, L., Camacho, B., & Silva-Cote, I. (2023) · Regenerative Therapy · doi:10.1016/j.reth.2023.05.005 · Cited by 26 · see citing works
Matos, B. N., Lima, A. L., Cardoso, C. O., Cunha‐Filho, M., Gratieri, T., & Gelfuso, G. M. (2023) · Pharmaceuticals · doi:10.3390/ph16091322 · Cited by 23 · see citing works
Policicchio, A., Meduri, A., Simari, C., Lazzaroli, V., Stelitano, S., Agostino, R. G., & Nicotera, I. (2017) · Journal of CO2 Utilization · doi:10.1016/j.jcou.2017.03.017 · Cited by 22 · see citing works
Paetzold, R., Coulter, F. B., Singh, G., Kelly, D. J., & O’Cearbhaill, E. D. (2022) · Bioprinting · doi:10.1016/j.bprint.2022.e00206 · Cited by 19 · see citing works
3D Printed Composite Scaffolds in Bone Tissue Engineering: A Systematic Review
Rad, M. R., Khojasteh, A., Mohaghegh, S., & Hosseini, S. F. (2021) · Current Stem Cell Research & Therapy · doi:10.2174/1574888x16666210810111754 · Cited by 18 · see citing works
Pompa-Monroy, D. A., Figueroa-Marchant, P. G., Dastager, S. G., Thorat, M. N., Iglesias, A. L., Miranda‐Soto, V., Pérez-González, G. L., & Villarreal-Gómez, L. J. (2020) · Materials · doi:10.3390/ma13235556 · Cited by 18 · see citing works
Li, L., Areson, C., van der Straten, A., & Johnson, L. M. (2021) · International Journal of Molecular Sciences · doi:10.3390/ijms22126529 · Cited by 17 · see citing works
Iglesias-Echevarria, M., Durante, L., Johnson, R., Rafuse, M., Ding, Y., Bonani, W., Maniglio, D., & Tan, W. (2019) · Biomaterials Science · doi:10.1039/c9bm00388f · Cited by 16 · see citing works
Ku, K.-L., Grøndahl, L., Dao, H., Du, K., Puttick, S. G., Lai, P., Peng, H., Chu, I., & Whittaker, A. K. (2017) · Polymer Degradation and Stability · doi:10.1016/j.polymdegradstab.2017.04.021 · Cited by 16 · see citing works
Formela, K., Marć, M., Namieśnik, J., & Zabiegała, B. (2016) · Microchemical Journal · doi:10.1016/j.microc.2016.02.001 · Cited by 15 · see citing works
High performance resorbable composites for load-bearing bone fixation devices
Heimbach, B., Tonyali, B., Zhang, D., & Wei, M. (2018) · Journal of the mechanical behavior of biomedical materials/Journal of mechanical behavior of biomedical materials · doi:10.1016/j.jmbbm.2018.01.031 · Cited by 15 · see citing works
Bicy, K., Geethamma, V. G., Kalarikkal, N., Rouxel, D., & Thomas, S. (2018) · Macromolecular Symposia · doi:10.1002/masy.201800140 · Cited by 14 · see citing works
Avaliação morfológica de fibras eletrofiadas de policaprolactona em função do tipo de solvente
Anaya‐Mancipe, J. M., Dias, M. L., & Thiré, R. M. D. S. M. (2019) · Matéria (Rio de Janeiro) · doi:10.1590/s1517-707620190003.0713 · Cited by 12 · see citing works
Furushima, Y., Nakada, M., Masuda, A., OKADA, K., Iwata, N., & Ohkura, M. (2020) · Polymer Crystallization · doi:10.1002/pcr2.10102 · Cited by 12 · see citing works
Chitosan-coated poly(є-caprolactone) nanocapsules for mucoadhesive applications of perillyl alcohol
Penteado, L. D. O., Lopes, V. F., Karam, T. K., Nakamura, C. V., Khalil, N. M., & Mainardes, R. M. (2021) · Soft Materials · doi:10.1080/1539445x.2021.1906702 · Cited by 10 · see citing works
Brennan, D. A., Flamini, M. D., Posselt, J. D., Wagner, C. T., & Beachley, V. Z. (2022) · Materials Today Communications · doi:10.1016/j.mtcomm.2022.104990 · Cited by 9 · see citing works
Loo, S. S. L., Tan, K. Y., Zahid, N. I., Foo, C. Y., Neoh, Y. X., Chong, K. Y., Tan, S. T., & Choo, Y. S. L. (2024) · ACS Applied Engineering Materials · doi:10.1021/acsaenm.4c00495 · Cited by 7 · see citing works
Analysis of Polymer Crystallization by Calorimetry
Lorenzo, M. L. D., Androsch, R., Rhoades, A. M., & Righetti, M. C. (2018) · Handbook of thermal analysis and calorimetry · doi:10.1016/b978-0-444-64062-8.00007-3 · Cited by 7 · see citing works
Polycaprolactone‐based hotmelt adhesive for hernia‐mesh fixation
Roisman, S., Dotan, A. L., & Lewitus, D. Y. (2020) · Polymers for Advanced Technologies · doi:10.1002/pat.5044 · Cited by 7 · see citing works
Gritsch, L., Askanian, H., Bednarzig, V., Schrüfer, S., Kaschta, J., Blavignac, C., Peuble, S., Gallice, F., Jallot, É., Boccaccini, A. R., et al. (2023) · Progress in Additive Manufacturing · doi:10.1007/s40964-023-00505-9 · Cited by 4 · see citing works
Putri, O. D., Petchsuk, A., Buchatip, S., Supmak, W., Kaewsaneha, C., Thananukul, K., Nim, B., Bayram, S., Thumanu, K., & Opaprakasit, P. (2023) · Nanomaterials and Nanotechnology · doi:10.1155/2023/9832904 · Cited by 3 · see citing works
Yang, C. Z., Shu, X., Hou, S., & Mao, Y. (2021) · Computational Materials Science · doi:10.1016/j.commatsci.2021.110382 · Cited by 3 · see citing works
Lizarazo-Fonseca, L., Prieto, E. M., Graziano, R. V., Camacho, B., Salguero, G., & Silva-Cote, I. (2019) · CIENCIA EN DESARROLLO · doi:10.19053/01217488.v10.n2.2019.9841 · Cited by 3 · see citing works
Yang, X., Yang, C. Z., Hou, S., & Mao, Y. (2021) · Journal of Mechanical Science and Technology · doi:10.1007/s12206-021-1025-y · Cited by 2 · see citing works
Antunes, J., Ribeiro, A., Lemos, D., Miranda, T., Santos, J. G., & Soares, G. M. B. (2022) · Materials science forum · doi:10.4028/p-72ck25 · Cited by 1 · see citing works
Jesús-Téllez, M. A. D., Robles-González, F., de León-Gómez, R. E. D., Ledezma-Pérez, A. S., & López-González, H. R. (2023) · Revista Ciencia UANL · doi:10.29105/cienciauanl25.113-2 · Cited by 1 · see citing works
Start-up Stage for an Electric Field Assisted Fused Deposition
Xu, R., Bao, W., Yin, T., Wang, Z., & Wang, Y. (2020) · IEEE International Conference on Mechatronics and Automation (ICMA) · doi:10.1109/icma49215.2020.9233678
Start-up stage with improved resolution for an electric field-assisted fused deposition
Xu, R., Bao, W., Zhihai, W., & Wang, Y. (2021) · RSC Advances · doi:10.1039/d0ra07795j
Gleadall, A., & Ruiz‐Cantu, L. (2020) · Elsevier eBooks · doi:10.1016/b978-0-08-102542-0.00011-7
Crystallization in PCL ‐Based Blends and Composites
Hegde, M., Chandrashekar, A., Nataraja, M., Gopi, J. A., Prabhu, N., & Parameswaranpillai, J. (2023) · Polymer Crystallization · doi:10.1002/9783527839247.ch7
Rheology as a Tool to Investigate Anti‐Nucleation in Semicrystalline Polymers
Tov, O. S., Bacharuzi, N., Dotan, A. L., & Lewitus, D. Y. (2025) · Journal of Applied Polymer Science · doi:10.1002/app.56873
- Authors
- Speranza, V., Sorrentino, A., De Santis, F., & Pantani, R.
- Affiliations
- University of Salerno (IT)
- National Research Council (IT)
- Department of Industrial Engineering (DIIN), University of Salerno, Via Giovanni Paolo II, 84084 Fisciano, Italy
- Corresponding author
- Sorrentino, A.
- Venue
- The Scientific World JOURNAL
- Publisher
- Hindawi Limited
- Published
- 2014
- Volume
- 2014
- Pages
- 1-9
- ISSN
- 1537-744X (ISSN-L)
- 2356-6140
- PMC
- PMC3913191
- OpenAlex
- W2011040873
- Cited by
- 42
- References
- 28
- Citations by year
- 2026: 1 · 2025: 1 · 2024: 2 · 2023: 6 · 2022: 3 · 2021: 7 · 2020: 6 · 2019: 6 · 2018: 4 · 2017: 3 · 2016: 2 · 2015: 1
- FWCI
- 1.40
- Type
- journal article
- Language
- en
- Open access
- gold
- doi.org
- Locations
- The Scientific World JOURNAL (publishedVersion, cc-by)
- Europe PMC (PubMed Central) (publishedVersion, cc-by)
- PubMed Central (publishedVersion, cc-by)
- PubMed (publishedVersion)
- DOAJ (DOAJ: Directory of Open Access Journals) (submittedVersion, cc-by-sa)
- 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 › Crystallization and Solubility Studies
- Keywords
- polycaprolactone, melt crystallization, crystallization induction time, crystallization exotherm, polymer crystallization kinetics, atomic force microscopy, polarized light microscopy, rheology, differential scanning calorimetry
- MeSH terms
- Calorimetry, Differential Scanning, Crystallization, Microscopy, Polyesters, Microscopy, Atomic Force
About these checks
Registry, retraction, Cites and statistics results are computed, not judged, with one exception: a printed reference that no index lists is read once by a model before it counts as a citation error. Claims are extracted by a model and kept only when their quote appears verbatim in the text; each cited source is then checked, with a model’s help, for whether it says what the claim relies on. Those verdicts can be wrong — read the claim’s quote and the cited source before relying on one.
Statistics and arithmetic are recomputed, not judged.
Confidence bands are shown only for fields calibrated on our annotated test set. None is calibrated yet, so no band is shown.
What counts as a claim ›How we measure confidence ›How we check this ›
Are you an author, or do you see a problem with this page? Request a review
