The different functional groups were examined by Fourier transform infrared spectroscopy (Nicolet AVATAR360, Madison). The prepared samples were cut into thin slices and the reflectance spectra of the samples were tested in the mid-infrared band using the attenuated total reflection mode (ATR). The structure of LPF/NaH modified butyl rubber was observed by scanning and analyzing in the wavelength range of 4000–500/cm.
Determination of the vulcanization characteristic curve of rubber mixing was carried out in GT-M3000AU (GOTECH Testing Machines Inc) type rotorless vulcanizer. After the rubber mix was parked for 24 h, about 5 g of rubber mix was cut and placed between the polycool films for measurement.
The Bruker Ultra Shield 400 plus NMR instrument was used to obtain nuclear magnetic resonance (NMR) hydrogen spectroscopy with deuterated chloroform (CDCL3) as solvent and tetramethylsilane (TMS) as internal standard at room temperature. Small amount of LPF/NaH modified butyl rubber was dissolved in cyclohexane. When the rubber material was completely dissolved, and it was then precipitated with anhydrous ethanol. The dissolution process was repeated for 2–3 times to dissolve the LPF and inorganic fillers out of the rubber material. Finally, the purified NaH modified IIR was obtained and dried in vacuum drying oven for 48 h, after which they could be subjected to NMR characterization.
Micromorphological analysis was performed by scanning electron microscope (SEM, NovaNano450/FEI). A small portion of the fracture was cut off, the section was gold sprayed, and then the micromorphology at the section was observed by the scanning electron microscope.
To conduct the tensile test, the vulcanized sample was cut into dumbbell type pattern with thickness of 1 mm, width of 2 mm and marking distance of 10 mm. The tensile test was carried out on electronic universal testing machine (SHIMADZU AGS-X) at 100 mm/min, and the load-stroke curve was recorded. Each batch of samples was tested three times.
The dynamic thermo-mechanical analyzer was used to perform temperature scanning in tensile mode with frequency of 10 Hz, amplitude of 5 μm, ramp rate of 3 k/min, starting temperature of − 40 °C and termination temperature of 80 °C. The prepared samples with thickness of 1 mm, width of 2 mm and length of 20 mm were placed on the dynamic thermo-mechanical analyzer for the DMA analysis test, and the curves of tanδ, E′, E′′ versus temperature were recorded. The testing procedure followed the standard method. Each batch of samples was tested three times.
The water contact angle of material surfaces was measured by contact angle meter (Dataphysics, OCA15EC-TBU100). After vulcanization, the sample was cut with the size greater than 1 cm*1 cm and fixed on the workbench. The level was dropped water so that the sample surface and water droplets were gently contacted each other, and the image was gained by the software to obtain the contact angle. Samples from each batch were tested three times.
To conduct thermal test, the vulcanized rubber was tested by thermal weight loss analyzer (NETZSCH STA 449 F5) at 10 °C/min rate in nitrogen atmosphere from room temperature to 800 °C.
Determination of the vulcanization characteristic curve of rubber mixing was carried out in GT-M3000AU (GOTECH Testing Machines Inc) type rotorless vulcanizer. After the rubber mix was parked for 24 h, about 5 g of rubber mix was cut and placed between the polycool films for measurement.
The Bruker Ultra Shield 400 plus NMR instrument was used to obtain nuclear magnetic resonance (NMR) hydrogen spectroscopy with deuterated chloroform (CDCL3) as solvent and tetramethylsilane (TMS) as internal standard at room temperature. Small amount of LPF/NaH modified butyl rubber was dissolved in cyclohexane. When the rubber material was completely dissolved, and it was then precipitated with anhydrous ethanol. The dissolution process was repeated for 2–3 times to dissolve the LPF and inorganic fillers out of the rubber material. Finally, the purified NaH modified IIR was obtained and dried in vacuum drying oven for 48 h, after which they could be subjected to NMR characterization.
Micromorphological analysis was performed by scanning electron microscope (SEM, NovaNano450/FEI). A small portion of the fracture was cut off, the section was gold sprayed, and then the micromorphology at the section was observed by the scanning electron microscope.
To conduct the tensile test, the vulcanized sample was cut into dumbbell type pattern with thickness of 1 mm, width of 2 mm and marking distance of 10 mm. The tensile test was carried out on electronic universal testing machine (SHIMADZU AGS-X) at 100 mm/min, and the load-stroke curve was recorded. Each batch of samples was tested three times.
The dynamic thermo-mechanical analyzer was used to perform temperature scanning in tensile mode with frequency of 10 Hz, amplitude of 5 μm, ramp rate of 3 k/min, starting temperature of − 40 °C and termination temperature of 80 °C. The prepared samples with thickness of 1 mm, width of 2 mm and length of 20 mm were placed on the dynamic thermo-mechanical analyzer for the DMA analysis test, and the curves of tanδ, E′, E′′ versus temperature were recorded. The testing procedure followed the standard method. Each batch of samples was tested three times.
The water contact angle of material surfaces was measured by contact angle meter (Dataphysics, OCA15EC-TBU100). After vulcanization, the sample was cut with the size greater than 1 cm*1 cm and fixed on the workbench. The level was dropped water so that the sample surface and water droplets were gently contacted each other, and the image was gained by the software to obtain the contact angle. Samples from each batch were tested three times.
To conduct thermal test, the vulcanized rubber was tested by thermal weight loss analyzer (NETZSCH STA 449 F5) at 10 °C/min rate in nitrogen atmosphere from room temperature to 800 °C.
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