o ‐ZrW 1.6 Mo 0.4 O 8 : A Novel Orthorhombic Intermediate Phase Formed During the Synthesis of the Negative Thermal Expansion Cubic ZrW 1.6 Mo 0 . 4 O 8 Material by the Precursor Dehydration Route

The mechanism of the precursor dehydration route was revealed for the synthesis of NTE c‐ZrW 1.6 Mo 0.4 O 8 . The hydrate precursor was dehydrated at 473 K and transformed to a NTE cubic compound above 800 K. A novel intermediate phase o ‐ZrW 1.6 Mo 0 . 4 O 8 occurs between the temperature range of 573–800 K. The XRD pattern of novel intermediate was refined with the structural model of LT‐ZrMo 2 O 8 by using Rietveld method. The residuals are R wp = 7.80% and R p = 5.79%. The space group is Pmn 2 1 and the lattice parameters are a = 0.5917(4) nm, b =0.7273(4) nm, c =0.9148(6) nm, and Z = 2.