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The environmental conical nozzle levitator (E‐CNL) with dual‐wavelength lasers is an extreme environment materials characterization system that was designed to investigate ultra‐high‐temperature materials: refractory metals, oxides, carbides, and borides above 3000 K in a controlled atmosphere. This article details the characterizations using this system to establish its high‐temperature capabilities and to outline ongoing work on materials under extreme conditions. The system has been used to measure the melting point of several oxide materials (TiO₂, Tm = 2091 ± 3 K; Al₂O₃, Tm = 2310 3 K; ZrO₂, Tm = 2984 31 K; and HfO₂, Tm = 3199 ± 45 K) and several air‐sensitive refractory metals (Ni, Tm = 1740 K; Ti, Tm = 1983 K; Nb, Tm = 2701 K; and Ta, Tm = 3368 K—note: mean ± standard deviation) during levitation which matched literature values within 0.17–2.43 % demonstrating high accuracy and precision. This containerless measurement approach is critical for probing properties without container‐derived contamination, and dual‐wavelength laser heating is essential to heat both relatively poor electrical conductors (some refractory metals and carbides) and insulators (oxides). The highest temperature achieved utilizing both lasers in these experiments was ∼4250 ± 34 K on a 76.6 mg, molten HfO₂sample using a normal spectral emissivity of 0.91. Stable levitation was demonstrated on spherical samples (yttria‐stabilized zirconia) while adjusting levitation gas composition from pure oxygen to pure argon, verifying atmospheric control up to 3173 K on solid or molten samples. These successes demonstrate the viability of in situ high‐temperature environmentally controlled studies potentially up to 4000 K on all classes of ultra‐high‐temperature materials in one system. These measurements highlight the E‐CNL system will be essential for the development of next‐generation ultra‐high‐temperature materials for hypersonic platforms, nuclear fission and fusion, and space exploration.

 

There is an ever-increasing need for material systems to operate in the most extreme environments encountered in space exploration, energy production, and propulsion systems. To effectively design materials to reliably operate in extreme environments, we need an array of tools to both sustain lab-scale extreme conditions and then probe the materials properties across a variety of length and time scales. Within this article, we examine the state-of-the-art experimental systems for testing materials under extreme environments and highlight the limitations of these approaches. We focus on three areas: (1) extreme temperatures, (2) extreme mechanical testing, and (3) chemically hostile environments. Within these areas, we identify six opportunities for instrument and technique development that are poised to dramatically impact the further understanding and development of next-generation materials for extreme environments.

 

High entropy oxides are emerging as an exciting new avenue to design highly tailored functional behaviors that have no traditional counterparts. Study and application of these materials are bringing together scientists and engineers from physics, chemistry, and materials science. The diversity of each of these disciplines comes with perspectives and jargon that may be confusing to those outside of the individual fields, which can result in miscommunication of important aspects of research. In this Perspective, we provide examples of research and characterization taken from these different fields to provide a framework for classifying the differences between compositionally complex oxides, high entropy oxides, and entropy stabilized oxides, which is intended to bring a common language to this emerging area. We highlight the critical importance of understanding a material’s crystallinity, composition, and mixing length scales in determining its true definition. 

Characterization of the thermal expansion in the rare earth di-titanates is important for their use in high-temperature structural and dielectric applications. Powder samples of the rare earth di-titanates R 2 Ti 2 O 7 (or R 2 O 3 ·2TiO 2 ), where R = La, Pr, Nd, Sm, Gd, Dy, Er, Yb, Y, which crystallize in either the monoclinic or cubic phases, were synthesized for the first time by the solution-based steric entrapment method. The three-dimensional thermal expansions of these polycrystalline powder samples were measured by in situ synchrotron powder diffraction from 25°C to 1600°C in air, nearly 600°C higher than other in situ thermal expansion studies. The high temperatures in synchrotron experiments were achieved with a quadrupole lamp furnace. Neutron powder diffraction measured the monoclinic phases from 25°C to 1150°C. The La 2 Ti 2 O 7 member of the rare earth di-titanates undergoes a monoclinic to orthorhombic displacive transition on heating, as shown by synchrotron diffraction in air at 885°C (864°C–904°C) and neutron diffraction at 874°C (841°C–894°C). 

In situ X-ray diffraction measurements at the Advanced Photon Source show that alpha-Al2O3 and MgAl2O4 react nearly instantaneously and completely, and nearly completely to form single-phase high-alumina spinel during voltage-to-current type of flash sintering experiments. The initial sample was constituted from powders of alpha-Al2O3, MgAl2O4 spinel, and cubic 8 mol% Y2O3-stabilized ZrO2 (8YSZ) mixed in equal volume fractions, the spinel to alumina molar ratio being 1:1.5. Specimen temperature was measured by thermal expansion of the platinum standard. These measurements correlated well with a black-body radiation model, using appropriate values for the emissivity of the constituents. Temperatures of 1600-1736 degrees C were reached during the flash, which promoted the formation of alumina-rich spinel. In a second set of experiments, the flash was induced in a current-rate method where the current flowing through the specimen is controlled and increased at a constant rate. In these experiments, we observed the formation of two different compositions of spinel, MgO center dot 3Al(2)O(3) and MgO center dot 1.5Al(2)O(3), which evolved into a single composition of MgO center dot 2.5Al(2)O(3) as the current continued to increase. In summary, flash sintering is an expedient way to create single-phase, alumina-rich spinel. 

The previously unknown experimental HfO₂–Ta₂O₅‐temperature phase diagram has been elucidated up to 3000°C using a quadrupole lamp furnace and conical nozzle levitator system equipped with a CO₂laser, in conjunction with synchrotron X‐ray diffraction. These in‐situ techniques allowed the determination of the following: (a) liquidus, solidus, and invariant transformation temperatures as a function of composition from thermal arrest experiments, (b) determination of equilibrium phases through testing of reversibility via in‐situ X‐ray diffraction, and (c) molar volume measurements as a function of temperature for equilibrium phases. From these, an experimental HfO₂–Ta₂O₅‐temperature phase diagram has been constructed which is consistent with the Gibbs Phase Rule.