TY - JOUR A1 - Purohit, Purv A1 - Wang, D.-Y. A1 - Wurm, Andreas A1 - Schick, C. A1 - Schönhals, Andreas T1 - Comparison of thermal and dielectric spectroscopy for nanocomposites based on polypropylene and layered double hydroxide - proof of interfaces JF - European polymer journal N2 - Polymer based nanocomposites by melt blending of synthesized ZnAl-Layered Double Hydroxide (ZnAl-LDH) and polypropylene (PP) were investigated by temperature modulated differential scanning calorimetry (TMDSC). The LDH was organically modified by using a surfactant, sodium dodecylbenzene sulfonate (SDBS) to increase the interlayer spacing of the LDH, so that polymer segments can intercalate the inter layer galleries. The glass transition temperature (Tg) and the thermal relaxation strength (Δcp) were determined. The Tg remains constant for concentration till 12 wt% of LDH and a slight reduction of 3 K might be observed for 16 wt% LDH but within the experimental error. The thermal relaxation strength decreases indicating reduction in the amount of mobile polymer segments from amorphous fraction. This finding is supported by the increase in the rigid amorphous fraction (RAF) which is attributed to the polymer molecules which are in close proximity to the crystals and the LDH sheets, as they hinder their mobility. This is analyzed in detail and related to the dielectric relaxation spectroscopy (BDS) results. KW - Polypropylene KW - Layered double hydroxide KW - Nanocomposites KW - Temperature modulated differential scanning calorimetery KW - Dielectric spectroscopy KW - Rigid amorphous fraction PY - 2014 DO - https://doi.org/10.1016/j.eurpolymj.2014.03.005 SN - 0014-3057 SN - 1873-1945 VL - 55 SP - 48 EP - 56 PB - Elsevier CY - Oxford AN - OPUS4-30626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Purohit, Purv A1 - Huacuja Sánchez, Jesús A1 - Wang, D.-Y. A1 - Emmerling, Franziska A1 - Thünemann, Andreas A1 - Heinrich, G. A1 - Schönhals, Andreas T1 - Structure - property relationships of nanocomposites based on polypropylene and layered double hydroxides JF - Macromolecules N2 - Nanocomposites based on polypropylene (PP) and organically modified ZnAl layered double hydroxides (ZnAl-LDH) were prepared by melt blending and investigated by a combination of differential scanning calorimetry (DSC), small- and wide-angle X-ray scattering (SAXS and WAXS), and dielectric relaxation spectroscopy (DRS). An average number of stack size of LDH layers is calculated by analyzing the SAXS data which is close to that of pure organically modified ZnAl-LDH. Scanning microfocus SAXS investigations show that the ZnAl-LDH is homogeneously distributed in the PP matrix as stacks of 4–5 layers with an intercalated morphology. DSC and WAXS results show that the degree of crystallinity decreases linearly with the increasing content of LDH. The extrapolation of this dependence to zero estimates a limiting concentration of ca. 40% LDH where the crystallization of PP is completely suppressed by the nanofiller. The dielectric spectra of the nanocomposites show several relaxation processes which are discussed in detail. The intensity of the dynamic glass transition (β-relaxation) increases with the concentration of LDH. This is attributed to the increasing concentration of the exchanged anion dodecylbenzenesulfonate (SDBS) which is adsorbed at the LDH layers. Therefore, a detailed analysis of the β-relaxation provides information about the structure and the molecular dynamics in the interfacial region between the LDH layers and the polypropylene matrix which is otherwise dielectrically invisible (low dipole moment). As a main result, it is found that the glass transition temperature in this interfacial region is by 30 K lower than that of pure polypropylene. This is accompanied by a drastic change of the fragility parameter deduced from the relaxation map. KW - Nanocomposites KW - Layered double hydroxide KW - Dielectric spectroscopy KW - X-ray scattering KW - Polypropylene PY - 2011 DO - https://doi.org/10.1021/ma200323k SN - 0024-9297 SN - 1520-5835 VL - 44 IS - 11 SP - 4342 EP - 4354 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23921 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -