Molecular origins of Epoxy-Amine/Iron oxide interphase formation

Morsch, Suzanne; Wand, Charlie R.; Emad, Seyedgholamreza; Lyon, S.B.; Siperstein, Flor R.; Malanin, Mikhail; Muche, Julia; Caspari, Anja; Drechsler, Astrid; Eichhorn, Klaus‐Jochen; Gibbon, Simon

doi:10.1016/j.jcis.2022.01.016

Cited by 15 publications

(27 citation statements)

References 62 publications

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“…For thermoplastic polymer nanocomposites, the polymer/nanoparticle interaction strength is believed to play a critical role in controlling the thermomechanical properties of the interfacial polymer layer . For example, the interfacial layer in polymer nanocomposites with a strong nanoparticle/polymer interaction generally exhibits an increase in the T g and stiffness compared with that for unfilled polymers and vice versa. − However, such a well-established relationship might not be applicable to predict the modification of the thermomechanical properties of the interfacial layer in epoxy nanocomposites. , Many studies have demonstrated that the presence of solid particles alters not only the dynamics of epoxy resin precursors but also their stoichiometric ratio from the corresponding unfilled systems, especially in regions near the particle surface. − Indeed, recent simulation and experimental studies by Tanaka and co-workers have proven a dependence of the stoichiometric ratio between epoxy and amine molecules on the distance to a solid interface, at which an excess amount of amine molecules was observed. , Such changes in both the dynamics and ratio of the epoxy precursors can significantly influence the curing kinetics of the network formation around the particles, giving rise to a complex structural and mechanical behavior for the interfacial epoxy layer. Unfortunately, a direct quantification of the local properties at the nanoparticle/epoxy interface remains challenging, and, thus, information about the true mechanical response at this nanoscale interface is still limited …”

Section: Introductionmentioning

confidence: 99%

Unraveling Nanoscale Elastic and Adhesive Properties at the Nanoparticle/Epoxy Interface Using Bimodal Atomic Force Microscopy

Nguyen

Shundo

Liang

et al. 2022

ACS Appl. Mater. Interfaces

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The addition of a small fraction of solid nanoparticles to thermosetting polymers can substantially improve their fracture toughness, while maintaining various intrinsic thermomechanical properties. The underlying mechanism is largely related to the debonding process and subsequent formation of nanovoids at a nanoscale nanoparticle/epoxy interface, which is thought to be associated with a change in the structural and mechanical properties of the formed epoxy network at the interface compared with the matrix region. However, a direct characterization of the local physical properties at this nanoscale interface remains significantly challenging. Here, we employ a recently developed bimodal atomic force microscopy technique for the direct mapping of nanoscale elastic and adhesive responses of an amine-cured epoxy resin filled with ∼50 nm diameter silica nanoparticles. The obtained elastic modulus and dissipated energy maps with high spatial resolution evidence the existence of a ∼20-nm-thick interfacial epoxy layer surrounding the nanoparticles, which exhibits a reduced modulus and weaker adhesive response in comparison with the matrix properties. While the presence of such a soft and weak-adhesive interfacial layer is found not to affect the architecture of structural heterogeneities in the epoxy matrix, it conceivably supports the toughening mechanism related to the debonding and plastic nanovoid growth at the silica/epoxy interface. The incorporation of this soft interfacial layer into the Halpin–Tsai model also provides a good explanation for the effect of the silica fraction on the tensile modulus of cured epoxy nanocomposites.

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Section: Introductionmentioning

confidence: 99%

Unraveling Nanoscale Elastic and Adhesive Properties at the Nanoparticle/Epoxy Interface Using Bimodal Atomic Force Microscopy

Nguyen

Shundo

Liang

et al. 2022

ACS Appl. Mater. Interfaces

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“…The cross‐linking reaction was characterized by the consumption of the characteristic epoxy band at 907 cm −1 , attributed to the asymmetric ether stretch of glycidyl groups, Figure 2 30,31 . This was found to occur at the same time as the growth of a band at 1108 cm −1 , assigned to the asymmetric stretch of the secondary hydroxyl groups produced during the epoxy‐phenolic reaction 13,14,32 …”

Section: Resultsmentioning

confidence: 96%

“…30,31 This was found to occur at the same time as the growth of a band at 1108 cm À1 , assigned to the asymmetric stretch of the secondary hydroxyl groups produced during the epoxyphenolic reaction. 13,14,32 Integration of the characteristic epoxy band at 907 cm À1 , and normalization to the aromatic band at 1504 cm À1 , allowed epoxy consumption to be compared in each case, Figure 3a. For the higher temperature cure reactions, epoxy levels are rapidly depleted (within 10 and 1 min at 150 and 200 C, respectively) and then level off, indicating a complete reaction.…”

Section: In-situ Fourier Transform Infrared Spectroscopymentioning

confidence: 99%

Internal topology and water transport in tetrafunctional epoxy resins

Morsch

Lyon

Gibbon

et al. 2022

J of Applied Polymer Sci

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Water sorption into epoxy resins limits the performance lifetime of many composites, adhesives, and coatings. One hypothesis for the well‐known hygroscopicity of epoxies is that the well‐known internal nodular topology of epoxy networks enhances permeability. This theory has however remained untested to date, since previous attempts to manipulate the internal topology have been accompanied by changes in the hydrogen bonding capability of resins, which dominates water uptake. Here, the nanostructure of highly cross‐linked network polymers based on tetra glycidyl diaminodiphenyl methane is varied in the absence of significant polarity effects by careful optimization of the cure schedule. The internal morphology of resins cured at 100, 150, and 200°C are characterized using Peakforce tapping mode atomic force microscopy, whilst the cure progression at each temperature is analyzed using in‐situ transmission mode infrared spectroscopy. Distinct nodular morphologies are found to form at high cure temperatures (150 and 200°C), where spectroscopic analysis demonstrates that excess epoxy consumption occurs prior to the gel point, as a result of intra‐cluster cross‐linking and reduced reaction selectivity. Surprisingly, the establishment of an internal nanostructure is, however, found to have negligible effect on the extent and kinetics of moisture sorption.

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“…It was found that the addition of nanosized BaTiO 3 particles into a ferroelectric polymer enlarged the size of local conformational disorder in the matrix, suggesting that the all-trans conformation was locally stabilized in the polymer nanocomposite. Morsch et al 171,172 used NanoIR to illustrate the curing process of the interface between epoxy-amine and iron oxide. Hauffman et al probed the chemical interactions at the poly(acrylic acid) (PAA)/Al 2 O 3 interface.…”

Section: Detection Of Localmentioning

confidence: 99%

Polymer Nanocomposite Dielectrics: Understanding the Matrix/Particle Interface

et al. 2022

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Polymer nanocomposite dielectrics possess exceptional electric properties that are absent in the pristine dielectric polymers. The matrix/particle interface in polymer nanocomposite dielectrics is suggested to play decisive roles on the bulk material performance. Herein, we present a critical overview of recent research advances and important insights in understanding the matrix/particle interfacial characteristics in polymer nanocomposite dielectrics. The primary experimental strategies and stateof-the-art characterization techniques for resolving the local property− structure correlation of the matrix/particle interface are dissected in depth, with a focus on the characterization capabilities of each strategy or technique that other approaches cannot compete with. Limitations to each of the experimental strategy are evaluated as well. In the last section of this Review, we summarize and compare the three experimental strategies from multiple aspects and point out their advantages and disadvantages, critical issues, and possible experimental schemes to be established. Finally, the authors' personal viewpoints regarding the challenges of the existing experimental strategies are presented, and potential directions for the interface study are proposed for future research.

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Molecular origins of Epoxy-Amine/Iron oxide interphase formation

Cited by 15 publications

References 62 publications

Unraveling Nanoscale Elastic and Adhesive Properties at the Nanoparticle/Epoxy Interface Using Bimodal Atomic Force Microscopy

Unraveling Nanoscale Elastic and Adhesive Properties at the Nanoparticle/Epoxy Interface Using Bimodal Atomic Force Microscopy

Internal topology and water transport in tetrafunctional epoxy resins

Polymer Nanocomposite Dielectrics: Understanding the Matrix/Particle Interface

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