A B S T R A C TIn a companion paper, it has been demonstrated the remarkably beneficial effect of palygorskite clay (Pal) fibers as support material coupled to appropriate thermal treatments and aging under CO 2 atmosphere in monitoring the phase composition of Ag 2 CO 3 -Pal composite. In this new nanocomposite material, the structure of the functional component Ag 2 CO 3 can be controlled from 100% stable monoclinic (m) to 100% metastable hexagonal β through an adjusted mixture of m-and β-Ag 2 CO 3 . The present study deals with the assessment of the visible photocatalytic properties of these various nanocomposite materials towards the removal of Orange G dye from aqueous solutions. It was found that the Ag 2 CO 3 -Pal nanocomposite in which Ag 2 CO 3 was single-phased and crystallized with the stable monoclinic structure was more active than the one crystallizing entirely with the metastable β-Ag 2 CO 3 structure. Nevertheless, the composite material containing a mixture of both Ag 2 CO 3 phases with a relative content of 32% of β-and 68% of m-phase was found to be the most photoactive compound of the series. This behavior reveals likely a synergetic effect between both phases in the photocatalytic degradation of the dye under visible light.