The layer compounds WS2and MoS2were exfoliated into single layers suspended in solution, and conditions were adjusted to produce a new homogeneous structure that is believed to be built of alternating layers of WS2and MoS2recrystallized in a 1Tstructure. Evidence for this is provided by the observation of a new hexagonal structure with expanded lattice spacings relative to the identical lattice spacings of the original materials and the fact that if the Mo:W ratio differs from 1:1, the x‐ray diffraction shows that some of the original WS2or MoS2phase is present. The catalytic activity of the alternating layer material is extremely high for the methanation reaction. It is observed and concluded that the alternating material is made up of fine particles, and a model of flocculation is presented to explain why in this material the particles are so fine.