High sensitivity measurements of normal force under large amplitude oscillatory shear

Journal article, 2018

The two aims of this publication are to introduce a new and rheometer-independent rheometric tool for measuring the axial normal force in oscillatory shear rheology and to study the normal forces of polyolefin melts under large amplitude oscillatory shear (LAOS). A new plate geometry with an incorporated highly sensitive piezoelectric normal force sensor was designed for a rotational rheometer. The new geometry was used to investigate normal forces of polyethylene (PE) melts under LAOS. The resulting stress and normal force data was compared with the data from measurements in commercial high performance rotational rheometers. The stress and the normal force response were Fourier-transformed and their resulting spectra were analysed. The non-linear contributions to the FT-magnitude spectra (i.e. the intensities of the higher harmonics) were analysed using the framework of the Q-parameter, \(Q=I_{3/1}/{\gamma ^{2}_{0}}\) for both the stress spectrum and the normal force spectrum, resulting in the strain-dependent \(Q\left (\gamma _{0}\right )\) and \(Q_{NF}\left (\gamma _{0}\right )\), respectively. The newly designed normal force geometry had a sensitivity in the measurement starting from \(5\times 10^{-5}\) N up to 20 N, and respectively a signal-to-noise ratio (SNR) of \(1:\) 16.000, which is about a factor of 1.8 times better than the best performing commercial rheometers. The new geometry was used to determine \(Q\left (\gamma _{0}\right )\) and \(Q_{NF}\left (\gamma _{0}\right )\), to characterize the shear rheological behaviour of the PE melts. Even rather simple rheometers, those without normal force detection, can be extended utilizing the here presented tools for high sensitive FT-rheology analysing the normal forces.