Thermogravimetric measurements were carried out using thermogravimetry/differential scanning calorimetry TGA/DSC1 analyzer (Mettler Toledo, Greifensee, Switzerland) in the temperature range of 25–600 °C, with a heating rate of 10 °C/min in an argon atmosphere (flow rate 50 ml/min.). Prior to the measurements, Thermogravimetry (TG) analyzer was calibrated using indium and zinc as standards. Additional analysis was performed using Setsys TG-DTA 16/18 analyser (SETARAM Instrumentation, Caluire-et-Cuire, France) coupled to a Balzers (Pfeiffer) mass spectrometer for evolved gas analysis.
DSC1 analyzer (Mettler Toledo, Greifensee, Switzerland), calibrated with indium and n-octane as standards, was employed to study thermal transitions of pure and DmiBr-modified fillers and the temperature of ionic liquid release/desorption from the surface of filler. The measurements were performed in the temperature range of 25–500 °C, with a heating rate 5 °C /min.
Rubber compounds of ethylene-propylene-diene elastomer (EPDM, Vistalon 8600, Exxon Mobile, Irving, TX, USA) containing 20 phr of DmiBr-modified fillers were prepared using a laboratory two-roll mill. Then, the prepared EPDM compounds were cured at 150 °C using an electrically heated hydraulic press for the optimal vulcanization time, which was determined with rotorless D-RPA 3000 rheometer (MonTech, Buchen, Germany).
SEM images of analyzed filler surface and fractures of EPDM vulcanizates were taken using an LEO1450 SEM microscope (Carl Zeiss AG, Oberkochen, Germany). Prior to the measurement, vulcanizates were broken down using liquid nitrogen; their fractures were coated with carbon and next examined. Based on the SEM images, the morphology and size of filler particles were studied, as well as their dispersion in the elastomer matrix. Energy-dispersive X-ray spectroscopy (EDS) was used to confirm the presence of DmiBr on the surface of modified fillers. Samples of pure fillers were coated with carbon to improve the quality of SEM/EDS results.
DSC1 analyzer (Mettler Toledo, Greifensee, Switzerland), calibrated with indium and n-octane as standards, was employed to study thermal transitions of pure and DmiBr-modified fillers and the temperature of ionic liquid release/desorption from the surface of filler. The measurements were performed in the temperature range of 25–500 °C, with a heating rate 5 °C /min.
Rubber compounds of ethylene-propylene-diene elastomer (EPDM, Vistalon 8600, Exxon Mobile, Irving, TX, USA) containing 20 phr of DmiBr-modified fillers were prepared using a laboratory two-roll mill. Then, the prepared EPDM compounds were cured at 150 °C using an electrically heated hydraulic press for the optimal vulcanization time, which was determined with rotorless D-RPA 3000 rheometer (MonTech, Buchen, Germany).
SEM images of analyzed filler surface and fractures of EPDM vulcanizates were taken using an LEO1450 SEM microscope (Carl Zeiss AG, Oberkochen, Germany). Prior to the measurement, vulcanizates were broken down using liquid nitrogen; their fractures were coated with carbon and next examined. Based on the SEM images, the morphology and size of filler particles were studied, as well as their dispersion in the elastomer matrix. Energy-dispersive X-ray spectroscopy (EDS) was used to confirm the presence of DmiBr on the surface of modified fillers. Samples of pure fillers were coated with carbon to improve the quality of SEM/EDS results.
Free full text: Click here
