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After reaction, sufficient quantity of silica functionalized with amine was added to the reactive mixture in order to react with the excess of UPy before filtration. The chloroform was then evaporated under reduced pressure and the polymer was further dried under reduce pressure at 50 °C for 24 h to obtain a white powder UPy2T-PB, vol.2 ,
, 86 (s, 2H, -CH2NH(C=O)NH), vol.11
, CH=CCH3), 5.38 (m, 2mH, -CH2-CH=CH-CH2-), 4.11 (m, 4H, -(C=O)-O-CH2-), 3.65 (t, 4H, -CH2-CH2-OH), 3.26 (m, 4H, -CH2NH(C=O)NH), 3.16 (m, 4H, -CH2NH(C=O)O-), 2.23 (s, 6H, -CH=CCH3), 2.08 (m, 4mH, -CH2-CH=CH-CH2-) with m = 80
, Preparation of the films. Films of PB were obtained after dissolution of the UPy functionalized PB in chloroform (1 g in 1.5 mL of CHCl3) for 24 h. The viscous solution was deposited in a Teflon mold and solvent was let evaporated 24 h. The film was then dried under vacuum for an extra
, All the strips used for DMA and tensile tests analyses were put into a closed glassware (1 g in 1.5 mL of CHCl3) for 24 h. The viscous solution was deposited in a Teflon mold and solvent was let evaporated 24 h. The film was then dried under vacuum for an extra
, Polymer molar masses were determined by size exclusion chromatography (SEC) using tetrahydrofuran (THF) as the eluent (THF with 250 ppm of Butylated hydroxytoluene as inhibitor, Aldrich) at 40°C on a SEC
, Waters RI detector and a Wyatt Light Scattering detector. The separation was achieved on three
, G6000 HXL and a Multipore HXL with an exclusion limits from 500 to 40 000 000 g.mol -1 , at flow rate of 1 mL/min. The injected volume was 100µL. Molar masses were evaluated with polyisoprene standards calibration, Tosoh TSK gel columns (300 × 7.8 mm) G5000 HXL
, Differential scanning calorimetry (DSC) measurements of rubber samples (?10 mg) were performed using a DSC Q100 LN2 apparatus from TA Instruments with a heating and cooling ramp of 10 °C.min -1 . The samples were first heated from 25 °C to 80 °C and held at 80 °C for 10 min in order to eliminate the residual solvent
, The initial grip separation was set at 20 mm and the crosshead speed at 50 mm/min. The results were obtained from at least 4 replicates for each sample. A TA Instrument RSA3 was used to study dynamic mechanical properties of rubber samples
, °C to 200 °C at a heating rate of 4 °C.min -1 . The measurements were performed in tensile mode
, Images were performed at 0.6-0.8 Hz scan rates with a format of 515*512 pixels. Thin film was prepared by microtome cutting of the bulk material or by a drops casted solution (10 mg/mL) and annealed at 130 °C during 10 min. Cooldown was performed at room temperature. the synthesis process. Properties of the material drastically change after the grafting of the UPy moieties. Indeed, at the H4T-PB step, the polymer is a liquid whereas after the Upy modification, the material becomes a solid. These observations allow to confirm that the formation of rubbery network can only be attributed to the UPy dimerization, acting as crosslinking nodes. Therefore, polymer films were prepared by dissolving the Upy modified polymer in chloroform and pouring the viscous solution in Teflon mold to allow the solvent evaporation. Strips were prepared from these films in order to carry out the mechanical characterization. For comparison, linear chain extension based on the UPy telechelic PB was also performed (Figure 68, pathway 2). Surprisingly, conversion of the terminal hydroxyl groups of the H2T-PB into urethane function was not complete while the reaction conditions were identical than for the UPy4T-PB synthesis. Indeed, only 82 % of the hydroxyl signal at 3.65 ppm (Figure S1b) was converted into urethane function, Both topographic and phase images of polished films were obtained in Tapping Mode ? using rectangular silicon cantilever (AC 160-TS, Atomic Force, Germany) with a spring constant of 26 N.m -1 , a resonance frequency in the range 270-320 kHz and a radius of curvature of less than 10 nm
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