RESUMEN
To describe the evolution of residual stresses in epoxy resin during the curing process, a more detailed characterization of its viscoelastic properties is necessary. In this study, we have devised a simplified apparatus for assessing the viscoelastic properties of epoxy resin. This apparatus employs a confining cylinder to restrict the circumferential and radial deformations of the material. Following the application of load by the testing machine, the epoxy resin sample gradually reduces the gap between its surface and the inner wall of the confining cylinder, ultimately achieving full contact and establishing a continuous interface. By recording the circumferential stress-strain on the outer surface of the confining cylinder, we can deduce the variations in material bulk and shear moduli with time. This characterization spans eight temperature points surrounding the glass transition temperature, revealing the bulk and shear relaxation moduli of the epoxy resin. Throughout the experiments, the epoxy resin's viscoelastic response demonstrated a pronounced time-temperature dependency. Below the glass transition temperature, the stress relaxation response progressively accelerated with increasing temperature, while beyond the glass transition temperature, the stress relaxation time underwent a substantial reduction. By applying the time-temperature superposition principle, it is possible to construct the relaxation master curves for the bulk and shear moduli of the epoxy resin. By fitting the data, we can obtain expressions for the constitutive model describing the viscoelastic behavior of the epoxy resin. In order to validate the reliability of the test results, a uniaxial tensile relaxation test was conducted on the epoxy resin casting body. The results show good agreement between the obtained uniaxial relaxation modulus curves and those derived from the bulk and shear relaxation modulus equations, confirming the validity of both the device design and the testing methodology.
RESUMEN
To meet the environmental protection and flame retardancy requirements for epoxy resins (EPs) in certain fields, in this study, a novel triazine-ring-containing DOPO-derived compound (VDPD), derived from vanillin, 2,4-Diamino-6-phenyl-1,3,5-triazine, and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), was synthesized using a one-pot method. Flame-retardant epoxy resin (FREP) was prepared by adding various ratios of VDPD to EP and curing with 4,4-diaminodiphenylmethane (DDM). The curing behavior, thermal stability, mechanical properties, and flame-retardant properties of the FREP were examined in various tests. According to the results, when the amount of VDPD added to the EP increased, the glass transition temperature of the FREP decreased linearly, and the flame-retardant properties gradually improved. With a 0.4 wt.% P content, the vertical burning rating of EP/DDM/VDPD-0.4 (according to the theoretical content of VDPD) reached the V-0 level, and the LOI value reached 33.1%. In addition, the results of a CCT showed that the peak heat release rate (PHRR) of EP/DDM/VDPD-0.4 decreased by 32% in comparison with that of the EP. Furthermore, compared with those of the EP, the tensile strength of EP/DDM/VDPD-0.4 decreased from 80.2 MPa to 74.3 MPa, only decreasing by 6 MPa, and the tensile modulus increased. Overall, VDPD can maintain the mechanical properties of EP and effectively improve its flame-retardant properties.
RESUMEN
The hygroscopic behavior of vinylester resin and high strength glass fiber reinforced vinylester resin composites were examined here, including weight change and the resulting degradation of mechanical properties. The prepared resin and composites specimens were immersed in deionized water and artificial seawater with an applied temperature of 70 °C, and then the specimens were weighed at specified time intervals in combination with the observation of surface morphologies using a scanning electron microscope. Identification of variations of functional groups was also carried out using Fourier-transform infrared spectroscopy. Meanwhile, the mechanical properties for resin and the composite specimens were tested periodically. The observations on surficial morphologies and the test on weight change display that the vinylester resin hydrolyzes seriously after immersion in deionized water, and that the embedment of glass fiber effectively inhibits the moisture absorption and hydrolysis for resin matrix in composites. The results from the mechanical properties test reveal that the tensile strength of pure resin decreases by 35.3% after 7 days' immersion and keeps small fluctuation in the sequent immersion duration. However, the compressive strength of pure resin consistently dwells at 100 ± 2 MPa during immersion. After immersion for 90 days, the tensile strength decreases by 28.5% and 38.4%, the compressive strength reduces by 7.2% and 16.6%, and the in-plane shear strength reduces by 16.6% and 15.2% for the composites immersed into deionized water and artificial seawater, respectively. The main highlights of this paper are that it provides a more comprehensive mechanical properties test in combination with the microscopic characterization on a matrix and its composites to reveal the aging behavior of composites under a hygroscopic environment.
RESUMEN
In order to improve the efficiency of intumescent flame retardants (IFRs), a novel macromolecular charring agent named poly(ethanediamine-1,3,5-triazine-p-4-amino-2,2,6,6-tetramethylpiperidine) (PETAT) with gas phase and condense phase synergistic flame-retardant capability was synthesized and subsequently dispersed into polypropylene (PP) in combination with ammonium polyphosphate (APP) via a melt blending method. The chemical structure of PETAT was investigated by Fourier transform infrared spectroscopy (FTIR), and ¹H nuclear magnetic resonance (NMR) spectroscopy. Thermal properties of the PETAT and IFR systems were tested by thermogravimetric-derivative thermogravimetric analysis (TGA-DTG) and thermogravimetry-Fourier transform infrared spectroscopy (TG-FTIR). The mechanical properties, thermal stability, flame-retardant properties, water resistance, and structures of char residue in flame-retardant composites were characterized using tensile and flexural strength property tests, TGA, limiting oxygen index (LOI) values before and after soaking, underwritten laboratory-94 (UL-94) vertical burning test, cone calorimetric test (CCT), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDXS), and FTIR. The results indicated that PETAT was successfully synthesized, and when the ratio of APP to PETAT was 2:1 with 25 wt % loading, the novel IFR system could reduce the deterioration of tensile strength and enhance the flexural strength of composites. Meanwhile, the flame-retardant composite was able to pass the UL-94 V-0 rating with an LOI value of 30.3%, and the peak of heat release rate (PHRR), total heat release (THR), and material fire hazard values were considerably decreased compared with others. In addition, composites also exhibited excellent water resistance properties compared with traditional IFR composites. SEM-EDXS and FTIR analyses of the char residues, as well as TG-FTIR analyses of IFR were used to investigate the flame-retardant mechanism of the APP/PETAT IFR system. The results indicated that the efficient flame retardancy of PP/IFR composites could be attributed to the synergism of the free radical-quenching and char layer-protecting mechanisms in the gas phase and condense phase, respectively.