Tuneable phase behaviour and glass transition <i>via</i> polymerization-induced phase separation in crosslinked step-growth polymers

Leguizamon, Samuel C.; Ahn, Juhong; Lee, Sang‐Woo; Jones, Brad H.

doi:10.1039/d2sm00485b

Cited by 7 publications

(9 citation statements)

References 57 publications

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“…In the process of curing, due to the difference in solubility parameters between silicone and PR, the phase separation rate is greater than the curing rate. In order to meet the minimum surface energy requirement, hybrid resin often ends up with a sea-island morphology. − To avoid this situation, herein, a novel PIS was designed by introducing imide rings as well as ethoxy groups into the silicone chain. The high compatibility between PIS and PR ensures that the phase separation rate matches the curing rate, resulting in a final nano co-continuous structure.…”

Section: Resultsmentioning

confidence: 99%

Nano Co-Continuous Structure Poly(imide-siloxane)/Phenolic Hybrid Resin Fabricated by Copolymerization for the Thermal Protection System

Yuan,

Wang,

Huang

et al. 2023

Ind. Eng. Chem. Res.

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Organic–inorganic hybridization is an important way to improve the ablation resistance of phenolic resin (PR). However, it is difficult to form a continuous inorganic liquid film on the resin surface during ablation, thus limiting the further improvement of ablation performance. In this work, a new poly(imide-siloxane) (PIS) was designed by introducing imide rings and terminal ethoxy groups into the main chain of silicone, and then it was introduced into PR. The imide rings can increase the polarity of the chain, and the terminal ethoxy groups can react with hydroxyl groups in PR, which can improve the compatibility of PIS with PR. SEM and AFM showed that nano co-continuous and sea-island structures of hybrid resins were prepared, respectively. Then, the influence of different structures on thermal stability and ablation-resistant properties was investigated by using TGA, tube furnace heat treatment, and oxyacetylene ablation test. Compared to the sea-island structure, the nano co-continuous structure of resin can form a continuous and dense SiO2 film in situ, giving the resin superior thermal stability and ablation-resistant properties. The present work provides an available way to manipulate hybrid resin’s phase structure and develop high-performance ablation-resistant resin in aerospace applications.

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Section: Resultsmentioning

confidence: 99%

Nano Co-Continuous Structure Poly(imide-siloxane)/Phenolic Hybrid Resin Fabricated by Copolymerization for the Thermal Protection System

Yuan,

Wang,

Huang

et al. 2023

Ind. Eng. Chem. Res.

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“…The chemical structure of the TDI-T GLDE was examined by 13 C-NMR at room temperature on a Bruker 400 NMR spectrometer using DMSO-d6 as the solvent.…”

Section: Nmrmentioning

confidence: 99%

“…The reactants (TDI-T) and products (TDI-T GL, TDI-T GLDE) during different reaction stages were taken for infrared analysis and the infrared spectrum is shown Figure 3. The chemical structure of the TDI-T GLDE was also studied by 13 C-NMR (Figure 3). Comparing the infrared spectra of TDI-T and TDI-T GL, the characteristic peak of the isocyanate group stretching vibration at 2268 cm À1 disappeared, and the carbon peak on the carbamate group generated by the block reaction was observed at 13 C-NMR 154.9 ppm.…”

Section: Characterization Of Tdi-t Glde Structurementioning

confidence: 99%

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Study on a novel epoxy‐terminated dendritic modifier as an active toughening agent for epoxy resin

Zhang,

Li,

Huang

et al. 2024

J of Applied Polymer Sci

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Although significant efforts have been undertaken to explore the toughening of epoxy resins, it remains challenges to establish a simple and effective toughening technique which does not compromise its strength, thermal stability and processing performance. In this paper, toluene‐diisocyanate‐trimer (TDI‐T) was utilized to manufacture a novel epoxy‐terminated dendritic modifier TDI‐T glycol diglycidyl ether (TDI‐T GLDE). When the addition of TDI‐T GLDE reaches 20% of the resin mass, the tensile strength, tensile elongation, compressive strength and impact strength were increased by 28.1%, 75%, 24.8%, and 138.0% respectively, compared to E‐51. The thermal properties of the samples have been improved, including an increased glass transition temperature (Tg) from 68.2 to 73.2°C, as well as an increase in the initial decomposition temperature from 240.6 to 257.7°C. The toughening mechanism of TDI‐T GLDE was studied through a combination of mechanical performance tests, thermal performance tests, and resin fracture surface morphology analysis.

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“…Depending on functionality degree, the siloxane may remain dissolved in the matrix or may undergo phase separation [32][33][34]. In most cases, at least compositional gradients are observed in the cured material [35][36][37], though some homogeneous materials have been developed [38][39][40].…”

Section: Introductionmentioning

confidence: 99%

Mechanism of Morphology Development in HDGEBA/PAMS Hybrid Thermosets: Monte Carlo Simulation and LSCM Study

et al. 2022

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Reactive combinations of aliphatic epoxy resins and functional polysiloxanes form a class of hybrid thermosetting materials with properties that may come from both the organic and the inorganic phases. The two typically immiscible phases form a suspension whose morphology, composition, and thermal properties vary with curing time. The aim of this research was to elucidate the mechanism by which morphology changed with time and to simulate it through Metropolis-Monte Carlo. The selected system was hydrogenated epoxy (HDGEBA) and a synthetic polyaminosiloxane (PAMS). It was studied by DSC, FTnIR, gel point, viscometry, and in-situ laser scanning confocal microscopy. A mechanism for morphology generation was proposed and simulated, exploring a wide range of values of the “a priori” relevant variables. The essential features were captured by simulations with a reasonable agreement with experimental data. However, the complete process was more complex than the geometrical approach of the simulation. The main deviations that were found and qualitatively explained are: (i) the induction period on the rate of coalescence, and (ii) PAMS-rich domain average size increases faster than predictions.

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Tuneable phase behaviour and glass transition via polymerization-induced phase separation in crosslinked step-growth polymers

Abstract: A universal approach to tune polymerization-induced phase separation is expanded and studied by X-ray scattering and dynamic mechanical analysis.

Cited by 7 publications

References 57 publications

Nano Co-Continuous Structure Poly(imide-siloxane)/Phenolic Hybrid Resin Fabricated by Copolymerization for the Thermal Protection System

Nano Co-Continuous Structure Poly(imide-siloxane)/Phenolic Hybrid Resin Fabricated by Copolymerization for the Thermal Protection System

Study on a novel epoxy‐terminated dendritic modifier as an active toughening agent for epoxy resin

Mechanism of Morphology Development in HDGEBA/PAMS Hybrid Thermosets: Monte Carlo Simulation and LSCM Study

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