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Ultra-high temperature ceramics (UHTCs), most notably transition metal carbides and borides, exhibit melting temperatures exceeding 3000 °C, making them appropriate candidates to withstand the extreme temperatures (∼2000 °C) expected to occur at the leading edges of hypersonic vehicles. However, their propensity to react rapidly with oxygen limits their sustained application. The high entropy paradigm enables the exploration of novel UHTC compositions that may improve on the oxidation resistance of conventional refractory mono-carbides and -diborides. The oxidation kinetics of candidate high entropy group IV + V (HfZrTiTaNb)C and (HfZrTiTaNb)B2 materials were evaluated at 1500–1800 °C using Joule heating in one atmosphere 0.1%–1% oxygen/argon gas mixtures for times up to 15 min. Possible mechanisms based on the resulting complex time, temperature, and oxygen partial pressure dependencies are discussed. The carbides formed porous and intergranular oxides. Oxidation resistance was improved upon a continuous external scale formation. The diborides formed dense external scales and exhibited better oxidation resistance compared to the carbides. This improvement was attributed to the formation of liquid boria. Both compositions showed an unexpected reduction in material consumption at 1800 °C for all times tested, compared to results at lower temperatures. An in-depth analysis of the composition and morphology of the oxide scale and sub-surface regions for specimens tested at 1800 °C revealed that the formation of denser group IV-rich (Hf, Zr, Ti) oxides mitigated the formation of the otherwise detrimental liquid-forming group V (Ta, Nb) oxides, leading to the improved oxidation resistance. [ABSTRACT FROM AUTHOR]

Ultra-high temperature ceramics (UHTCs), most notably transition metal carbides and borides, exhibit melting temperatures exceeding 3000 °C, making them appropriate candidates to withstand the extreme temperatures (∼2000 °C) expected to occur at the leading edges of hypersonic vehicles. However, their propensity to react rapidly with oxygen limits their sustained application. The high entropy paradigm enables the exploration of novel UHTC compositions that may improve on the oxidation resistance of conventional refractory mono-carbides and -diborides. The oxidation kinetics of candidate high entropy group IV + V (HfZrTiTaNb)C and (HfZrTiTaNb)B2 materials were evaluated at 1500–1800 °C using Joule heating in one atmosphere 0.1%–1% oxygen/argon gas mixtures for times up to 15 min. Possible mechanisms based on the resulting complex time, temperature, and oxygen partial pressure dependencies are discussed. The carbides formed porous and intergranular oxides. Oxidation resistance was improved upon a continuous external scale formation. The diborides formed dense external scales and exhibited better oxidation resistance compared to the carbides. This improvement was attributed to the formation of liquid boria. Both compositions showed an unexpected reduction in material consumption at 1800 °C for all times tested, compared to results at lower temperatures. An in-depth analysis of the composition and morphology of the oxide scale and sub-surface regions for specimens tested at 1800 °C revealed that the formation of denser group IV-rich (Hf, Zr, Ti) oxides mitigated the formation of the otherwise detrimental liquid-forming group V (Ta, Nb) oxides, leading to the improved oxidation resistance. [ABSTRACT FROM AUTHOR]

This work reports on a pump–probe laser-based heating and sensing metrology to study the failure mechanisms of materials during extreme heat fluxes localized near surfaces, the localization of which is controlled by the focus of the laser beam and sensed by the reflection of a secondary probe laser. We focus the demonstration of these power density at failure tests on the damage mechanisms of commercially pure titanium metal during and after high heat fluxes induced from the absorbed laser energy. Using this steady-state thermoreflectance pump–probe metrology, a localized region of the material was irradiated at a low modulated frequency, while the average change in the thermoreflectance signal was monitored. We observe surface and cross-sectional oxidation of the titanium, revealing correlations between microstructural evolution events and shifts in thermoreflectance trends as a function of absorbed power density. Furthermore, the damage morphology was shown to be heavily influenced by the size of the heater (dictated by the radius of the pump laser beam), which controlled the relative degree of thermomechanical, melting, and oxidative decohesion failure mechanisms in the samples. The analysis of the temperature distribution coupled with the observed microstructural damage gives rise to a high-throughput experimental technique to induce desired deformation modes through cyclic thermal testing. [ABSTRACT FROM AUTHOR]