Heat-resistant molding of compounds is an indispensable part in encapsulating future electronic power devices. Herein, it is used for polyfunctional epoxy resin (EP) and diamine-phenol benzoxazine (BOZ) as resin matrix, 4,4'-diaminodiphenylmethane (DDM) as curing agent, and iron acetylacetonate (Fe(acac) 3 ) as curing accelerator, as well as inorganic fillers and other auxiliaries, to prepare heat-resistant molding compounds. The curing behavior, processability and thermal performance of the EP/DDM/BOZ (EDB) resin blends containing different contents of DDM, BOZ, and Fe(acac) 3 are first systematically investigated. The EDB molding compounds (MC EDB ) with suitable BOZ content show good processability, and the molding process can be compatible with that of commercial epoxy molding compounds (EMC). With increasing the BOZ content, the glass transition temperature of cured MC EDB is greatly enhanced to a maximum of 261 °C determined by dynamic mechanical analyzer, owing to the hydrogen-bond interaction generated after polymerization of BOZ increasing the rigidity of network chains. Moreover, the cured MC EDB also exhibits higher thermal decomposition stability, better high-temperature (200 °C) mechanical properties, and lower water absorption compared to the cured EMC. After high-temperature (200 °C) aging for 500 h, the cured MC EDB with suitable BOZ content still maintains outstanding performance. This study provides a promising strategy for preparing heat-resistant electronic packaging molding compounds.
Benzoxazine incorporating an aniline dimer in its structure has satisfactory electroactivity and undergoes both amine-catalyzed and autocatalytic polymerization.
Ammonium polyphosphate microcapsules (BM (polybenzoxazine modified) APP) were prepared through the in situ ring-opening polymerization of allyl group containing benzoxazine monomers on the surfaces of ammonium polyphosphate (APP), and they were significantly hydrophobic than the APP. A flame retardant system of epoxy (EP) resin was prepared with BMAPP and expanded graphite (EG). Flame retardancy, the thermal degradation behavior, a mechanical property of EP and EP/BMAPP/EG composites was investigated through limited oxygen index, vertical burning test, cone calorimetry (CONE), and the thermogravimetric analysis (TGA). The flame retardancy tests indicated that the EG could improve the thermal performance, promote the charring, and enhance the char quality of EP/BMAPP. Scanning electron microscopy (SEM) and Fourier-transform infrared spectroscopy (FTIR) were employed to analyze the morphology and composition of the char residue formed during CONE testing, and to understand the mechanism of char formation. The results of TG-FTIR confirmed the possible mechanism of flame retardancy of EP/BMAPP/EG in the gas phase during combustion. The EG content effects on Young’s modulus, the tensile strength, and the fracture toughness ( KIC) of the EP/BMAPP composites were also investigated. The KIC of the composites containing 1% of EG and 10% of BMAPP increased by approximately 76% and 153%, respectively, compared to the neat matrix and EP/BMAPP-10%. The SEM images of the fractured surface indicated that the enhanced toughness of EP/BMAPP/EG composites mainly attributed to the debonding of the BMAPP and the subsequent plastic void growth of the matrix, as well as the crack deflection effect of the BMAPP/EG.
Latent curing accelerators are essential for application to one-component epoxy systems in various industries, such as coatings, adhesives and electronic packaging. Herein, we developed organic-inorganic hybrid microcapsules encapsulating triphenylphosphine (TPP) by Pickering emulsion polymerization of styrene and methoxyethyl methacrylate with dimethoxydiphenylsilane-modified silica nanoparticles as emulsifiers. The microcapsules were further surface-modified by epoxy silane and employed as a thermal latent curing accelerator for an epoxy/anhydride system. Good dispersibility and interfacial bonding of the hybrid microcapsules with the resin matrix were observed. Compared with TPP, the microcapsule-type accelerator endowed the one-component epoxy curing system with significantly enhanced storage stability at room temperature of 25 °C (a pot life of 20 days) and a comparable curing activity at high temperature. The activity of the encapsulated accelerator can be blocked and released rapidly and effectively with increasing temperature to trigger the segmental motion of the polymeric microcapsules. Furthermore, the addition of microcapsules increased the glass transition temperature and thermal stability of the epoxy thermosets owing to the organic-inorganic hybrid character. Moreover, the toughness of the cured resin was also improved. Therefore, the latent curing accelerator demonstrated a promising prospect for application in highperformance one-pot epoxy formulations.
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