Tytuł pozycji:
Strategy for fabricating multiple-shape memory polymeric materials based on solid state mixing
The deposited data contain results obtained from measurements: DSC, TGA, NMR, DMTA, shape memory and tensile tests.
The attached data are provided in the form of text and Excel files as well as source files typical for the respective software used.
The attached data were obtained using the following instruments: Solid-state NMR spectra were recorded on a Bruker AVANCE III WB 400 MHz spectrometer. The spinning rate for all experiments was 6 kHz. 13C cross-polarization magic-angle spinning spectra were obtained under two-pulse-phasemodulating proton decoupling. A recycle delay is 2 s. 1H spin−lattice relaxation time measurements both in the laboratory and in rotating frames T1 and T1ρ, respectively, were measured at room temperature by a saturation recovery method and a spin lock method, respectively. Thermal behavior of samples was probed with a DSC Q20 differential scanning calorimeter (TA Instruments) during heating with the rate of 10 °C/min. Samples of the 7−8 mg mass were cut out from initial and HPT-processed blends and crimped in standard Al. pans. The DSC cell was purged with dry nitrogen during the measurements (50 mL/min). DMTA measurements were carried out in a tensile mode using a DMTA DMA Q 800 TA Instruments (USA) apparatus at the frequency of 1 Hz and at the heating rate of 2°C/min.The TGA was performed from room temperature to 600 °C at 10 °C/min with a Rigaku Instrument Thermo plus TG 8120 in a nitrogen atmosphere. The X-ray measurements were carried out with an Aeris XRD diffractometer (Malvern Panalytical) operating at 40 kV and 7.5 mA. The material before and after HPT were grinded for the XRD measurements to randomize the polymer crystal orientation. The mechanical properties of initial and HPT processed blends were evaluated using a tensile testing machine (Instron, Model 5582). The samples were cut into a rectangular shape measuring 15 × 5 mm, with an initial distance of 10 mm between the clamps. The crosshead speed was set at 5%/min, and the sample under each condition was tested five times. Thermally-activated shape memory characterization of samples was conducted using Q800 DMA instrument with the film tension clamp under controlled strain and controlled force modes. The triple shape memory properties were enforced by primary strain deformation of 20% applied at 45 or 70 °C. The strain was then kept constant. The strain was then held constant while the sample was cooled. The second deformation was performed at 30 or 60 °C to increase the strain from 20 to 40 %. The strain was held constant until the sample had cooled to room temperature and then released. To observe the memory effect, the samples were heated to 32 or 61 °C for 30 minutes to recover the shape in the first step. Later, the temperature was increased to 47 or 72 °C to visualize the second memory shape. The recovery stress of PP/PS blends was performed under iso-strain conditions (strain=20 %) from 20 °C to the deformation temperature (shape memory programming) at 5 °C/min.