Phase transformations in Ti-15Mo single crystal investigated by synchrotron X-ray diffraction

J. Šmilauerová, P. Zháňal, L. Horák, P. Harcuba, J. Veselý, V. Holý

Faculty of Mathematics and Physics, Charles University, Ke Karlovu 5, 121 16, Prague, Czech Republic

smilauerova@karlov.mff.cuni.cz

In metastable titanium alloys, the transformation from the high-temperature β phase (bcc) to the low-temperature α phase (hcp) can be suppressed upon quenching to room temperature [1]. Due to the thermodynamically metastable nature of the β phase, particles of the so-called ω phase form in the material by a diffusionless shuffle mechanism already during quenching. The crystallographic structure of ω phase is either trigonal or hexagonal, depending on the completeness of the β → ω transformation, and there are four crystallographic orientations (variants) of the ω phase [2]. ω particles are coherent with the parent β phase, their size ranges from a few nanometres to a few tens of nanometres [3] and they were found to be spatially weakly ordered in a cubic array [4]. With increasing temperature, ω particles evolve and grow by a diffusion-assisted process until they reach a stability limit at which the precipitation of α phase becomes the dominant transformation.

The main goal of this research is to investigate the sequence of transitions occurring in single-crystals of Ti-15Mo (in wt.%) alloy during linear heating by synchrotron X-ray diffraction. For this purpose, a single crystal was prepared using the floating zone method [5], solution treated above the β-transus temperature and quenched to water to produce a well-defined starting condition for the heating experiments.

X-ray diffraction was measured at the high-energy beamline ID11 at ESRF, Grenoble. The photon energy was 60 keV and the primary beam was parallel to [100]β direction in the studied crystal. The heating was performed in a dedicated furnace equipped with a quartz chamber, allowing to reach high vacuum (approx. 10-6 mbar). The diffracted signal was collected in situ during linear heating with the rate of 5°C/min. An example of a measured diffraction pattern together with calculated pattern explaining the origin of individual peaks is displayed in Fig. 1.

Figure 1. a) Measured diffraction pattern at room temperature and b) calculated pattern showing the positions of observed β and ω diffraction spots (square and ellipse symbols, respectively).

The set of measured data allowed us to determine the sequence of phase transformations by following the evolution in regions around selected ω diffraction spots during linear heating, see Fig. 2. The intensity in these regions first decreases with increasing temperature, but the ω reflections do not disappear completely. On the contrary, around 673 K (400 °C), the ω peaks sharpen and their intensity increases – this is most visible in Fig. 2 c) which shows an ω spot closest to the Ewald sphere (Figs. 2 a) and b) display ω peaks further from the Ewald sphere, so the intensity increase is not readily apparent due to their sharpening). At 833 K (560 °C, denoted by a black vertical line in Fig. 2), all ω reflections disappear, suggesting a complete dissolution of the ω phase. The intensity observed at the highest measured temperatures corresponds to α phase diffraction spots which lie close to the original ω reflections.

Figure 2. Evolution of a) , b)  and c)  diffraction spots.

Figure 3. Evolution of ω phase fraction of the ω phase (red points) and the β/ω interface area (blue points).

Numerical fitting of measured diffraction peaks allowed us to estimate the temperature dependence of ω phase fraction (red points in Fig. 3) and interface area between the β matrix and ω particles (blue points in Fig. 3). Both quantities depend linearly on the number of irradiated ω particles; the steeper decrease of S/S0 above 523 K (250 °C) suggests that while ω particles grow, their number decreases (a process similar to Ostwald ripening). The increasing trend observed in Fig. 3 is caused by progressive coarsening of ω particles. As the temperature nears the stability limit of the ω phase at 833 K (560 °C), both the phase fraction and the interface area decrease rapidly. More information on this topic and a comparison with complementary data from electrical resistivity measurements can be found in [6].

 

[1] G. Lutjering a J. C. Williams, Titanium, 2nd editor, Berlin: Springer, 2007.

[2] D. De Fontaine, „Simple models for the omega transformation,“ Metallurgical Transactions A 19, 169-175, 1988.

[3] B. S. Hickman, „The formation of omega phase in titanium and zirconium alloys: A review,“ Journal of Materials Science 4, 554-563, 1969.

[4] J. Šmilauerová, P. Harcuba, J. Stráský, J. Stráská, M. Janeček, J. Pospíšil, R. Kužel, T. Brunátová, V. Holý a J. Ilavský, „Ordered array of ω particles in β-Ti matrix studied by small-angle X-ray scattering,“ Acta Materialia 81, 71-82, 2014.

[5] J. Šmilauerová, J. Pospíšil, P. Harcuba, V. Holý a M. Janeček, „Single crystal growth of TIMETAL LCB titanium alloy by a floating zone method,“ Journal of Crystal Growth 405, 92-96, 2014.

[6] P. Zháňal, P. Harcuba, M. Hájek, J. Stráský, J. Šmilauerová, J. Veselý, L. Horák, M. Janeček a V. Holý, „In situ detection of stability limit of ω phase in Ti-15Mo alloy during linear heating,“ Journal of Applied Crystallography 52, 1061-1071, 2019.