Wide-field polarization measurements of the twilight sky background during the several nights with bright and extended noctilucent clouds in central and northern Russia in 2014 and 2015 are used to build the phase dependence of degree of polarization of sunlight scattered by clouds particles in a wide range of scattering angles (from 40° to 130°). This range covers the linear polarization maximum near 90° and large-angle slope of the curve which are most sensitive to the particle size. The method of separation of scattering on clouds particles on the twilight background is presented. Results are compared with T-matrix simulations for different sizes and shapes of ice particles, the best-fit model radius of particles (0.06 μm) and maximum radius (about 0.1 μm) are estimated.