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Cure Cycle Development for High Temperature Thermosetting Resins

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Cure Cycle Development for High Temperature Thermosetting Resins for Fused Deposition Modeling

 

Limitations of current state-of-the-art thermoplastics for fused deposition modeling (FDM) are low glass transition temperatures (< 250 °C), poor thermo-oxidative stability and solubility in organic solvents, fuel and oil. The goal of this research is to investigate high temperature polyimide thermosets (HTPI-Ts) as potential candidates for FDM additive manufacturing of aerospace-grade parts with higher thermo-oxidative stability (TOS) and higher service temperatures.  A key requirement for the FDM process is that material must be in filament form. Tuning the chemistry and rheology of existing phenylethynyl terminated imides (PETIs) is therefore necessary to obtain ductile filament. To address the minimum viscosity resulting due to crosslinking exotherms of the thermoset, degree of cure (DoC) progression for in-line cure (i.e. crosslinking during the FDM process) and pre-cure cycles were explored.  Experiments were also conducted to determine critical print parameters for optimal processing and minimum required DoC during FDM that led to self-supporting builds that will facilitate post-cure cycles of printed specimens with minimal distortions.  Differential scanning calorimetry (DSC) on reacted crosslink sites were used to acquire DoC and glass transition temperature (Tg).  Extrusion temperature and speed were found to be the primary constraints that limited in-line cure; and pre-curing feedstock was found to be an effective measure to mitigate in-line cure limitations. DSC pre-cure results showed that ≥ 46 % DoC was too high for FDM processing. Successful FDM extrusion was achieved with filament that was less than or equal to 34.3 % pre-cured.

 

Authors: Robyn L. Bradford, Sarah N. Izor, Andrew C. Abbott, Hilmar Koerner, Gyaneshwar P. Tandon, and Katie E. Thorp

 

Conference: CAMX 2016 – Anaheim

 

SKU/Code: TP16-0142

 

Pages: 16



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