Spin-diffusion NMR at low field for the study of multiphase solids

Abstract

The use of spin-diffusion NMR for the measurement of domain sizes in multiphase materials is becoming increasingly popular, in particular for the study of heterogeneous polymers. Under conditions where T 1 relaxation can be neglected, which is mostly the case at high field, analytical and approximate solutions to the evolution of spin diffusion are available. In order to extend the technique to more general conditions, we performed a comprehensive study of the diffusion of magnetization in a model copolymer at low field, where T 1 tends to be of the same order of magnitude as the typical spin-diffusion time. In order to study the effects of T 1 and to delineate the optimal T 1 values for back correction prior to applying the initial-rate approximation, we developed a numerical simulation based on the diffusion equation and including longitudinal relaxation. We present and discuss the limits of simple correction strategies for initial-slope analysis based on apparent relaxation times from saturation-recovery experiments or the spin-diffusion experiments themselves. Our best strategy faithfully reproduces domain sizes obtained by both TEM investigations and full simultaneous fitting of spin-diffusion and saturation-recovery curves. Full fitting of such independent data sets not only yields correct domain sizes, but also the true longitudinal relaxation times, as well as spin-diffusion coefficients. Effects of interphases with distinct mobility on spin-diffusion curves, as well as practical hints concerning the reliable component decomposition of the detected low-resolution FID signal by help of different magnetization filters are also discussed in detail.