Enthalpy Relaxation and Embrittlement of Poly( l -lactide) during Physical Aging
Abstract
The enthalpy relaxation behavior of poly( l -lactide) (PLLA) below glass transition temperature ( T g ) and its effects on the mechanical properties were studied using differential scanning calorimetry (DSC), dynamic mechanical thermal analysis (DMTA), and tensile test. Both the enthalpy loss (δ H ) and peak endothermic temperature ( T p ) in the glass transition region show a linear increase with the logarithm of aging time ( t a ). On the basis of DSC results, the kinetics of the enthalpy relaxation process were analyzed, and the kinetic parameters of PLLA were obtained: relaxation rate of enthalpy at 40 °C β H = 1.77 J g -1 per decade, and apparent activation energy Δ h * = 1107 kJ mol -1 . Besides, analysis on the kinetic of enthalpy relaxation for poly( dl -lactide) (PDLLA) shows that the Δ h * value of PDLLA is similar to that of PLLA. Moreover, it was found that the strength and modulus of PLLA increase gradually; on the contrary, the toughness reduces dramatically during the physical aging. The yield strength and tensile modulus increased respectively 18.8% and 23.1% after being aged at 40 °C for 1008 h, as compared to the unaged sample. Also, the fracture strain of PLLA decreased from more than 300% to about 6% with aging at 25 °C for 24 h. Moreover, the fractographic examination evaluated by scanning electron microscopy showed that the fracture of PLLA changed from the “ductile” to “inductile” manner during physical aging. The drop of ductility in physical aging is correlated to the rearrangement of polymer chains from disordered to more ordered morphology.
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Pure PLLA and 90PLLA:10PLCL(80:20)-PEG samples experience significant enthalpy relaxation, leading to densification, increased stiffness and strength, but lower ductility.
“Pure PLLA and 90PLLA: 10PLCL(80:20)-PEG samples experience significant enthalpy relaxation, leading to densification, increased stiffness and strength, but lower ductility [17].”
From Tuning structural relaxations, mechanical properties, and degradation timescale of PLLA during hydrolytic degradation by blending with PLCL-PEG (2019) · cites this paper as [17]
PLLA can become embrittled over time, which can lead to catastrophic failure of implanted devices.
“PLLA can also become embrittled over time, which can lead to catastrophic failure of implanted devices [17, 18].”
From Tuning structural relaxations, mechanical properties, and degradation timescale of PLLA during hydrolytic degradation by blending with PLCL-PEG (2019) · cites this paper as [17]
Embrittlement of PLLA can be caused by either enthalpy relaxation or crystallisation.
“This embrittlement can be caused by either enthalpy relaxation or crystallisation.”
From Tuning structural relaxations, mechanical properties, and degradation timescale of PLLA during hydrolytic degradation by blending with PLCL-PEG (2019) · cites this paper as [17]
Enthalpy relaxation of PLLA can occur after several days at temperatures below Tg.
“Enthalpy relaxation of PLLA can occur after several days at temperatures below T g [17].”
From Tuning structural relaxations, mechanical properties, and degradation timescale of PLLA during hydrolytic degradation by blending with PLCL-PEG (2019) · cites this paper as [17]
The increased Tg in these blends results from reduced free volume in the densified structure.
“This has also resulted in an increased T g due to the reduced free volume in the densified structure [17].”
From Tuning structural relaxations, mechanical properties, and degradation timescale of PLLA during hydrolytic degradation by blending with PLCL-PEG (2019) · cites this paper as [17]
Lower molecular weight reduces the activation energy and accelerates both enthalpy relaxation and crystallisation.
“The activation energy for structural relaxation is also dependent on the molecular weight of a polymer, with a lower molecular weight known to reduce the activation energy and accelerate both enthalpy relaxation and crystallisation [17, 49, 50].”
From Tuning structural relaxations, mechanical properties, and degradation timescale of PLLA during hydrolytic degradation by blending with PLCL-PEG (2019) · cites this paper as [17]
Enthalpy relaxation and crystallisation are exothermic transformations with an associated activation energy that governs the rate of transformation.
“These are both exothermic transformations which have an associated activation energy, which governs the rate of transformation [17, 49].”
From Tuning structural relaxations, mechanical properties, and degradation timescale of PLLA during hydrolytic degradation by blending with PLCL-PEG (2019) · cites this paper as [17]
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“Pure PLLA and 90PLLA: 10PLCL(80:20)-PEG samples experience significant enthalpy relaxation, leading to densification, increased stiffness and strength, but lower ductility [17].”
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- Authors
- Pan, P., Zhu, B., & Inoue, Y.
- Affiliations
- Tokyo Institute of Technology (JP)
- Corresponding author
- Inoue, Yoshio
- ORCID
- Venue
- Macromolecules
- Publisher
- American Chemical Society (ACS)
- Published
- 2007-11-29
- Volume
- 40
- Issue
- 26
- Pages
- 9664-9671
- ISSN
- 0024-9297 (ISSN-L)
- 1520-5835
- OpenAlex
- W2075190175
- Cited by
- 282
- References
- 69
- Citations by year
- 2026: 21 · 2025: 18 · 2024: 17 · 2023: 15 · 2022: 18 · 2021: 17 · 2020: 17 · 2019: 19 · 2018: 11 · 2017: 19 · 2016: 16 · 2015: 13 · 2014: 26 · 2013: 10 · 2012: 10
- FWCI
- 4.22
- Type
- journal article
- Language
- en
- Open access
- closed
- Locations
- Macromolecules (publishedVersion)
- Topics
- Physical Sciences › Materials Science › Biomaterials › biodegradable polymer synthesis and properties
- Physical Sciences › Materials Science › Materials Chemistry › Material Dynamics and Properties
- Physical Sciences › Materials Science › Polymers and Plastics › Polymer crystallization and properties
- Keywords
- poly(L-lactic acid), poly(D,L-lactide), physical aging, enthalpy relaxation, embrittlement, glass transition, activation energy, mechanical properties, fracture toughness, ductile-to-brittle transition, chain ordering, biodegradable polymers
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