This study investigates and compares the thermal stability of two 6FDA-based thermosetting polyimide formulations with varied amounts of internal crosslinkers. The baseline formulation is a commercially available polyimide with good resin transfer molding processability and a high glass transition temperature, Tg, in the range of 340°C–466°C. The altered formulation has a reduced amount of internal crosslinkers. In the current study, the materials are studied through multiple thermogravimetric analysis (TGA) scans to investigate how the polyimide formulation affects the thermo-oxidative properties in the cured state. The measurements and the subsequent analyses reveal that the two polyimides have similar thermal oxidation behavior after curing, despite the changes. A combined model-based approach, utilizing both isothermal and non-isothermal TGA data, is used for the analysis and to create conversion-time–temperature diagrams for both materials. The combined method is compared to pure isoconversional and non-isothermal model-based methods and shows improvement in the ability to model the degradation of the materials.

The effect of test temperature, maximum stress, and stress-ratio on transverse cracking development in cross-ply laminates subjected to tension–tension cyclic loading was analysed. A two-parameter Weibull distribution model was used to predict transverse cracking, wherein the Weibull scale parameter was assumed to be test temperature and number of cycles dependent. By introducing an equivalent stress in the model, it was possible to account for the effect of the stress ratio in cyclic loading over a range of different loading conditions. To verify the model, tests on temperature resistant cross-ply composites were performed at room temperature and at 150 °C with different stress levels and local 90-layer stress ratios. For both test temperatures, increase in stress level increased the transverse cracking tendency. At 150 °C, despite the lower maximum thermo-mechanical ply-stress level compared to room temperature, transverse cracking tendency was found to be higher.

Accumulation of transverse cracks in carbon fiber heat resistant polymer (with bismaleimide formulation) cross-ply laminates during tensile loading at elevated temperatures and after long heat treatment is analysed. Data shows that both the iso-thermal heat treatment and testing at elevated temperatures reduce the transverse cracking resistance. A two-parameter Weibull failure stress distribution model with scale parameter degrading with heat treatment and elevated temperature is used for crack initiation analysis. The degradation is described by polynomial expansion including interaction terms. Data shows that the scale parameter dependence on the heat treatment time and the test temperature is rather linear. The same expansion parameters have been successfully used for laminates with the same constituents but with a different layup and fiber content.

Presented test results on transverse cracking in cross-ply laminates upon tension–tension cyclic loading show that the increase of crack density depends not only on the maximum transverse stress in the cycle but also on the local cyclic stress ratio RTloc in the analyzed layer. To include the effect of the RTloc in the model with statistical failure stress distribution for crack initiation (based on Weibull distribution) adapted for fatigue, an equivalent stress is introduced in a similar manner as the equivalent strain energy release rate has been used for delamination crack propagation. The equivalent stress in the layer is defined as a power function of the maximum stress and the stress ratio in the layer. It was found, testing laminates with two different fiber contents that higher the local stress ratio in 90-layer, higher the transverse cracking resistance. Transverse crack density simulation using the developed equivalent stress model has been validated against test results. 

The present study delivers a methodology for investigating the gradual damage development in a carbon fibre-reinforced cross-ply polymer composite during a sequence of thermo-mechanical loadings with the help of X-ray computed tomography. The procedure allows an in-depth analysis of the occurrence and nature of the multiple cracks that form within layers oriented perpendicular, or transverse, to the loading direction. This is achieved by using Attention U-Net architecture for semantic segmentation of the transverse cracks. The model shows promising results, through an ability to identify all the transverse cracks and reflect the damage progression. The described method provides a robust routine for analysing challenging polymer composite tomographic datasets.

Two 4,4′-(hexafluoroisopropylidene)diphthalic anhydride-based thermosetting polyimide formulations with varied amounts of crosslinking sites were compared to understand the influence of crosslinking density on fracture toughness, glass transition temperature and thermal oxidative stability. The thermal and mechanical properties of both materials were investigated through a series of single-edge notched beams, differential scanning calorimetry, dilatometry, weight loss, light optical microscopy and nanoindentation experiments. It was found out that the reduced crosslinking resulted in slightly increased fracture toughness but decreased the Tg of the material. No significant difference could be observed in the thermal oxidative stability with the experimental techniques considered.

A novel thermosetting polyimide, NEXIMID R300, is introduced and compared with the commercial MHT-R in terms of fracture toughness, thermal properties and ageing behaviour. The new R300 formulation has an altered chemical composition compared to the MHT-R, resulting in a reduced cross-linking density, and was presented as a less susceptible to cracking and a more processable alternative during composite manufacturing with resin transfer moulding. The study uses fracture toughness with single edge notched beam setup, DSC, dilatometry, weight loss measurements and optical microscopy for investigation of the neat resin properties of both material. A slight increase in fracture toughness and a decrease in glass transition temperature for the R300 formulation is observed.