Cure Kinetics and Thermal Decomposition Behavior of Novel Phenylacetylene-Capped Polyimide Resins.

Based on a novel phenylacetylene capped polyimide (PI) with unique high-temperature resistance, its curing kinetics and thermal decomposition behavior were investigated. The curing mechanism and kinetics were studied by differential scanning calorimetry (DSC), and the activation energy (Ea) and pre-exponential factor (A) of the curing reaction were calculated based on the Kissinger equation, Ozawa equation, and Crane equation. According to the curve of conversion rate changing with temperature, the relationship between the dynamic reaction Ea and conversion rate (α) was calculated by the Friedman equation, Starink equation, and Ozawa-Flynn-Wall (O-F-W) equation, and the reaction Ea in different stages was compared with the results of molecular dynamics. Thermogravimetric analysis (TGA) and a scanning electron microscope (SEM) were used to analyze the thermal decomposition behavior of PI resins before and after curing. Temperatures at 5% and 20% mass loss (T5%, T20%), peak decomposition temperature (Tmax), residual carbon rate (RW), and integral process decomposition temperature (IPDT) were used to compare the thermal stability of PI resins and cured PI resins. The results display that the cured PI has excellent thermal stability. The Ea of the thermal decomposition reaction was calculated by the Coats-Redfern method, and the thermal decomposition behavior was analyzed. The thermal decomposition reaction of PI resins at different temperatures was simulated by molecular dynamics, the initial thermal decomposition reaction was studied, and the pyrolysis mechanism was analyzed more comprehensively and intuitively.

The Performance and Synthesis of Alkynyl-Functionalized Benzoxazine Containing Phthalide Side Groups and Cyano Groups with Different Molecular Weights.

Benzoxazine resins are widely employed in a variety of applications due to their exceptional heat resistance and treatment properties. However, traditional benzoxazine resins still confront hurdles in today's engineering applications, such as their inability to provide long-term service in high-temperature settings and their inadequate toughness. In this study, four alkyne-functionalized benzoxazines with phthalide side groups and cyano groups of varying molecular weights were produced. Fourier transform infrared spectroscopy (FT-IR) and hydrogen nuclear magnetic resonance spectroscopy (1H-NMR) were used to characterize the resin structure, and differential scanning calorimetry (DSC) was used to investigate the thermal curing kinetics at different warming rates. The apparent activation energy was 116.9 kJ/mol. In-situ FT-IR was used to investigate the cure mechanism. Dynamic mechanical analysis (DMA) was used to evaluate the gelation time of BOZ series resins at various temperatures, and the curing process was designed by combining the results with DSC. The Tg of the composites made using BOZ-1N21 as the matrix was 336 °C, which was much higher than the Tg of the BP-a resin made with aniline, phenolphthalein, and formaldehyde (Tg = 251 °C). As a result, the resin system is expected to be employed in applications requiring high-temperature resistance and toughness.

Experimental Study of Thermal and Fire Reaction Properties of Glass Fiber/Bismaleimide Composites for Aeronautic Application.

Thermal behavior and fire reaction properties of aerial glass fiber (GF)/bismaleimide (BMI) composites were tested using thermogravimetric analysis (TGA), thermogravimetric coupled with Fourier transform infrared spectroscopy (TG-FTIR), cone calorimeter, limiting oxygen index, and smoke density chamber. The results showed that the pyrolysis process was one stage in a nitrogen atmosphere with the prominent volatile components of CO2, H2O, CH4, NOx, and SO2. The release of heat and smoke increased with the increase in heat flux, while the time required to reach hazardous conditions decreased. The limiting oxygen index decreased monotonically from 47.8% to 39.0% with increasing experimental temperature. The maximum specific optical density within 20 min in the non-flaming mode was greater than that in the flaming mode. According to the four kinds of fire hazard assessment indicators, the greater the heat flux, the higher the fire hazard, for the contribution of more decomposed components. The calculations of two indices confirmed that the smoke release in the early stage of fire was more negative under flaming mode. This work can provide a comprehensive understanding of the thermal and fire characteristics of GF/BMI composites used for aircraft.

Flame-Synthesis of Carbon Nanotube Forests on Metal Mesh Structure: Dependence, Morphology, and Application.

Multi-walled carbon nanotubes (MWCNTs) in the form of "forests" were synthesized directly on the surface of stainless steel (SS) mesh from ethanol flame volume. The growth dependence of the MWCNT forests on the porosity of SS mesh substrate and the morphologies and growth mechanism of the MWCNT forests were investigated in detail by a combination of turbulent flow simulation, scanning electron microscopy (SEM), transmission electron microscope (TEM), and Raman and X-ray diffraction (XRD) spectroscopy. The growth height of the MWCNT forests exhibited a strong dependence on the flame gas flow rate controlled by the porosity of SS mesh substrate, and the maximum averaged height of the MWCNT forests reached 34 µm. Most MWCNTs grew perpendicularly on the surface of SS wires, and some branch, welded, and spiral structures were observed by SEM and TEM. The MWCNT-decorated mesh was used as a novel heating element to weld glass-fabric-reinforced polyetherimide (GF/PEI) thermoplastics. We found that the maximum tensile lap-shear strength (LSS) of the welded joints could reach 39.21 MPa, an increase of 41% in comparison with that of conventional SS mesh-based joints.

Self-assembly of ternary hollow microspheres with strong wideband microwave absorption and controllable microwave absorption properties.

In this study, we report a simple and efficient two-step method consisting of water-in-oil (W/O) emulsion technique and subsequent annealing process for synthesizing the hollow reduced graphene oxide microspheres embedded with Co nanoparticles (Air@rGO€Co). The microspheres showed good electromagnetic properties because of the coexistence of magnetic loss and dielectric loss to microwaves. The minimum reflection loss (RLmin) value of S1.5 reaches -68.1 dB at 13.8 GHz with a thickness of 2.2 mm, and the absorption bandwidth (lower than -10 dB) is 7.1 GHz covering from 10.9 GHz to 18.0 GHz. More interestingly, we can easily controll the microwave absorbing properties of the microspheres by changing the ratio of the two components in the composites. The excellent electromagnetic match at the corresponding resonance peaks for dielectric and magnetic loss play an important role in improving microwave absorption property. Our study provides a good potential method for preparation of lightweight microwave absorbing materials.