As an important nuclear reactor material, Zr-2.5Nb (all concentrations in mass%, unless otherwise stated) has a low neutron absorption cross-section, high corrosion resistance, and high strength and creep resistance. [1] The phase diagram of the binary system is shown in Figure 1. [2] In thermodynamic equilibrium at room temperature it consists of a-Zr phase (hcp) and b-Nb phase (bcc), while a-Zr and Zr-rich, b-Zr(Nb) co-exist between the eutectoid temperature of T eu ¼ 893 K and the solvus temperature of T b ¼ 1 087 K in Zr-2.5Nb. A b-phase solid solution is stable above T b . The alloy has been studied widely, considering aspects of the chemistry, texture and morphology of the microstructure following different heat treatments, high temperature deformation as well as variant selection during phase transformation. However, the underlying crystal properties such as the lattice parameters and thermal expansion of the different phases during the phase transformations, have not been determined in situ and in real time.In the current study, a high-intensity neutron diffractometer in combination with a vacuum furnace has been used to determine for the first time, the crystalline properties of a Zr-2.5Nb alloy in situ during the a-b phase transformation. By combining thermal expansion and Vegard's law in a novel approach, the phase transformations and the diffusion of alloying elements can be tracked and the results compared to the phase diagram. The outcomes of this investigation are consistent with earlier thermal expansion experiments and time-temperature transformation curves recently determined for Zr-2.5Nb nuclear reactor pressure tubes by using X-ray diffraction analysis. [3] In Situ AnalysisThe initial Zr-2.5Nb material is presented in Figure 2, revealing a typical fine microstrucure, composed of laths of a-phase interfacing with very fine filaments of b-phase regions between the matrix of the a phase.While undergoing heat treatments, in situ neutron diffraction tests were conducted on both the high-intensity powder diffractometer Wombat [4] and the high-resolution powder diffractometer Echidna [5] at ANSTO. Details of the sample preparation and the measurements are given further down in the Experimental Section.
ResultsA diffraction pattern obtained at room temperature is shown at the top of Figure 3. In addition to the majority of a-Zr phase, the pattern reveals a relatively large amount of retained b-Zr(Nb) phase of eutectoid composition and a small amount of b-Nb rich phase with lattice parameters of a ¼ 3.4361 and 3.3016 Å , respectively.The bottom part of Figure 3 shows a stacked sequence of such individual diffraction patterns. Temperature is shown on the vertical axis and the diffraction intensity is indicated by grayscale values. It follows that the amount of the b-Zr(Nb) phase starts to increase above T eu ¼ 893 K while the a-Zr phase vanishes totally at 1133 K, which is 46 K above T b . We attribute this sluggish behavior to the kinetics of the displace character
COMMUNICATIONThe a-b phase transforma...