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Assessing the thermo-oxidative degradation of thermosetting polyimides
Luleå University of Technology, Department of Engineering Sciences and Mathematics. (Polymer Composites)
Universidade Federal do Rio Grande do Sul.
Luleå University of Technology, Department of Engineering Sciences and Mathematics. (Polymer composites)
(English)Manuscript (preprint) (Other academic)
Keywords [en]
Polyimide, 6FDA, Thermo-oxidative degradation, TGA, Isoconversional analysis, Thermodynamic parameters
National Category
Textile, Rubber and Polymeric Materials
Identifiers
URN: urn:nbn:se:ltu:diva-93614OAI: oai:DiVA.org:ltu-93614DiVA, id: diva2:1703839
Available from: 2022-10-14 Created: 2022-10-14 Last updated: 2024-04-05
In thesis
1. Studies on the thermal degradation of thermosetting polyimides and their composites
Open this publication in new window or tab >>Studies on the thermal degradation of thermosetting polyimides and their composites
2022 (English)Licentiate thesis, comprehensive summary (Other academic)
Alternative title[sv]
Studier av termisk degradering i härdplastpolyimider och dess kompositer
Abstract [en]

The thesis contains a background and reflections section, an introduction, and three appended articles. The first section is reserved for some of the background and basics on polymers and polymer composites and a discussion on their effect on our everyday lives. The introduction gives a brief recap of the project. The articles contain the research that was performed on the thermal oxidation of thermosetting polyimides and their composites during the project.

The first article covered the thermal oxidative degradation of satin weave and thin-ply composites made by resin transfer molding with carbon fibers and thermosetting polyimide. The degradation was studied by weight loss measurements and X-ray computed microtomography. The weight loss measurements showed that the initial desorption stage during ageing followed Fickian behavior and the proposed model. It was also observed that the satin weave composites formed crack clusters that grew into a network of cracks, voids and delaminations throughout the specimens as the ageing time progressed, while the thin-ply composites only formed delaminations at the free edges.

The second manuscript studied the behavior of the neat polyimide resin when aged for up to 1500 hours in ambient air, and compared it with a newly developed polyimide formulation, with slightly altered chemical composition. The reduced amount of internal crosslinkers in the newer formulation was expected to enhance the fracture toughness of the material. Three-point bending, differential scanning calorimetry, dilatometry, weight loss, light optical microscopy and nanoindentation experiments were performed and highlighted the differences in the thermal and mechanical properties of the two formulations. A slight increase in the fracture toughness was observed, while the glass transition of the new formulation had decreased.

The third manuscript was aimed at continuing the discussion from the second article on the differences between the two thermosetting polyimides. Thermogravimetric scans showed that the polyimide formulations behaved very similarly under thermal oxidative tests. The initial analysis gave indications that the model could capture well the degradation at high temperatures, but is not adequate in predicting long-term degradation at temperatures around 288–400 °C.

Place, publisher, year, edition, pages
Luleå: Luleå tekniska universitet, 2022
Series
Licentiate thesis / Luleå University of Technology, ISSN 1402-1757
Keywords
Polymer composites, Polyimide, Thermal oxidative degradation
National Category
Textile, Rubber and Polymeric Materials Composite Science and Engineering
Research subject
Polymeric Composite Materials
Identifiers
urn:nbn:se:ltu:diva-93613 (URN)978-91-8048-188-5 (ISBN)978-91-8048-189-2 (ISBN)
Presentation
2022-12-20, E632, Luleå tekniska universitet, Luleå, 10:00 (English)
Opponent
Supervisors
Available from: 2022-10-17 Created: 2022-10-17 Last updated: 2023-08-31Bibliographically approved
2. Characterisation of thermally induced degradation of high-temperature polymers and composites
Open this publication in new window or tab >>Characterisation of thermally induced degradation of high-temperature polymers and composites
2024 (English)Doctoral thesis, comprehensive summary (Other academic)
Alternative title[sv]
Karaktärisering av termiskt inducerad degradering av högtemperatur-polymerer och kompositer
Abstract [en]

This project aimed to broaden the knowledge of high-temperature polymers and composites when exposed to elevated temperatures and an oxygen-containing atmosphere. The main accent has been on thermosetting polyimide resins reinforced with carbon fibers. When subjected to harsh atmospheric conditions, such as elevated temperatures and oxygen, polymer resins can undergo thermo-oxidative degradation, often resulting in weight loss and a surface layer with altered properties. High-temperature composites could experience such environments during operation. Therefore, it is crucial to understand how exposure to it could affect their performance. To simulate such an environment in the lab, the materials are aged in a controlled manner in a furnace or other equipment. The ageing of polyimide composites in this project was often performed at temperatures at or above 288 degrees Celsius for extended periods of up to 1500 hours.

The first part of the project, and the first article, delved into the effect of different layups and thicknesses of the carbon fiber bundles on the thermo-oxidative behaviour of two composite materials made with the same thermosetting polyimide. Modelling the desorption during the initial stages of the ageing, showed that it exhibited a Fickian behaviour. X-ray computed tomography experiments were used to investigate the ageing behaviour of the materials and revealed that the satin weave composite formed a network of cracks, voids, and delaminations, that progressed with the ageing time, while the damage in the material made of thin plies was in the form of delaminations at the edges. The analysis of the tomographic datasets was performed using Otsu’s thresholding method for semantic segmentation of the defects within the materials.

In an attempt to counter the crack formation on the surface of the satin weave composite observed during the first study, a new polyimide formulation was developed by the manufacturer. The amount of internal crosslinkers was reduced, aiming to increase the toughness of the resin after curing. The second article compares neat resin samples of the original and newly developed formulations with the help of a three-point bending test, differential scanning calorimetry, dilatometry, weight loss, light optical microscopy and nanoindentation experiments. Samples were aged up to 1500 hours in ambient air. The results showed that while there were hints of a slight increase in the fracture toughness of the new formulation, the glass transition temperature had decreased, compared to the original resin.

The two formulations were further investigated and compared with the help of thermogravimetric analysis in the fourth paper. Experiments were performed in isothermal and non-isothermal conditions for more robust results. It was found that the thermal oxidation of the two materials follows an autocatalytic model. The study highlights the importance of using both isothermal and non-isothermal data in the pursuit of more precise and robust analysis and modelling of the thermal oxidation of high-temperature polymers. Based on the results, a diagram, predicting the weight loss at specific times and temperatures, was created for each material.

An alternative way of studying crack formation within challenging polymer composite tomographic datasets was presented in the fourth article. Instead of using a thresholding method, such as the

previously used Otsu’s in the first study, in this case, a deep learning model was applied to the datasets to follow the progressive micro-cracking within the composite during a series of thermo-mechanical loadings. In contrast to a global thresholding method, which segments all defects within the dataset, the deep learning model, Attention U-Net, made it possible to create a more straightforward and robust way of performing segmentation on transverse cracks. The model was compared to and outperformed both Otsu’s method and a conventional U-Net.

The previously developed methodology for semantic segmentation and the obtained results on transverse cracks were applied in a practical case in the fifth article, where the developed damage prediction model assumes that transverse cracks in thick plies span through the whole width of the specimen. The tomography and deep learning methodology helped shed light on the nature of the cracks and showed that previous assumptions, based on edge observation with light optical microscopy, should be taken as a conservative estimation.

Place, publisher, year, edition, pages
Luleå: Luleå tekniska universitet, 2024
Series
Doctoral thesis / Luleå University of Technology 1 jan 1997 → …, ISSN 1402-1544
National Category
Composite Science and Engineering Textile, Rubber and Polymeric Materials
Research subject
Polymeric Composite Materials
Identifiers
urn:nbn:se:ltu:diva-104993 (URN)978-91-8048-523-4 (ISBN)978-91-8048-524-1 (ISBN)
Public defence
2024-06-13, E632, Luleå University of Technology, Luleå, 10:00 (English)
Opponent
Supervisors
Available from: 2024-04-08 Created: 2024-04-05 Last updated: 2024-05-23Bibliographically approved

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