The coagulation of cellulose from solution in N-methylmorpholine-N-oxide by water was studied by stray field magnetic resonance imaging. Changes in composition and diffusion were readily observable at different depths within the cellulose gel. It was found that the composition changed relatively quickly, due to diffusive exchange of water and solvent, such that cellulose precipitation occurred deep within the bi-phasic region of the phase diagram. The expected spinodal decomposition mechanism was supported by electron microscopic observations of the cellulose morphology. Large increases in diffusion coefficient and relaxation times were attributable to the phase separation and the progressive development of pores within the gel. Moreover it appeared that the composition changes and evolution of morphology occurred over separate time-scales.