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DOE OSTI2020

Monocrystal-based microchannel plate image intensifier

A monocrystalline scintillator comprises a monocrystal and an optical plate wherein a first side of the monocrystal is adhered to the optical plate. The monocrystal comprises at least one of a rare earth garnet, a perovskite crystal, a rare-earth silicate, and a monocrystal oxysulphide. The scintillator assembly includes an adhesive adhering the optical plate to the first side of the monocrystal. The adhesive can comprise an ultra-high vacuum compatible adhesive. The adhesive is substantially transparent and has a refractive index matching the optical plate. The scintillator assembly can also include a reflective coating on the second side of the monocrystal. The monocrystalline scintillator assembly can be incorporated in a microchannel plate image intensifier tube to provide improved spatial resolution and temporal response.

Lumpkin, Alex H.↗

NASA NTRS2023

An Ensemble Neural Network Model for Predicting Rare-Earth Oxide and Silicate Heat Capacities at High Temperature

In this work, a neural network model was developed to predict the constant pressure heat capacity for materials in the rare-earth oxide—silica material space. Several model architectures were trained and tested on heat capacity data generated from first-principles density functional theory calculations. Hyperparameter optimization was performed, and the optimal model was selected for heat capacity predictions. The optimal model architecture was found to have a root-mean-squared error of 5.12 ± 3.37 J/mol-K. The optimal model architecture was then used in a bagging ensemble model trained using the leave-one-group-out method to provide error estimates for model predictions. The out-of-bag score for the ensemble model was 0.997. The predicted heat capacities agree well with the DFT and experimental results and were computed orders of magnitude faster than DFT simulations. Machine learning shows the potential to provide a suitable surrogate model for thermochemical property predictions for candidate environmental barrier coating materials but refining of input material features and model architectures could further improve accuracy for these models.

environmental barrier coatings↗

NASA NTRS1976

High modulus rare earth and beryllium containing silicate glass compositions

Glass compositions having a Young's modulus of at least 16 million psi and a specific modulus of at least 110 million inches consisting essentially of approximately, by weight, 20 to 43% SiO2, 8 to 21% Al2O3, 4 to 10% BeO, 27 to 58% of at least one oxide selected from a first group consisting of Y2O3, La2O3, Nd2O3, Ce2O3, Ce2O3, and the mixed rare earth oxides, and 3 to 12% of at least one oxide selected from a second group consisting of MgO, ZrO2, ZnO and CaO are described. The molar ratio of BeO to the total content of the first group oxides is from 1.0 to 3.0.

Bacon, J. F.↗

DOE OSTI2022

Dry air cyclic oxidation of mixed Y/Yb disilicate environmental barrier coatings and bare silica formers

Here mixed Y and Yb disilicate coatings (Y/Yb)DS have been proposed as dual function thermal and environmental barrier coatings (EBCs) for protecting SiC-based ceramic matrix composites in gas-turbine environments. As an initial step, the 1350 °C dry air cyclic oxidation of atmospheric plasma sprayed (Y 1.2 /Yb 0.8 )DS and ytterbium disilicate/ytterbium monosilicate (YbDS/YbMS) EBCs deposited onto Si bond coatings was compared. As a baseline for evaluating EBC oxidant permeability, the dry air cyclic oxidation scale growth rates for bare silica formers (SiC, Si) were also measured and were consistently higher than rates previously measured after isothermal oxidation. Regarding Si bond coat oxidation rates underlying (Y/Yb)DS and YbDS/YbMS EBCs, the thinner silica scale formed under the thinner and denser (Y/Yb)DS coatings suggested a lower oxidant permeability than YbDS/YbMS. After 500 1-h cycles, the (Y/Yb)DS coating was comprised of only the β-polymorph disilicate and minor amounts of the X-2 phase monosilicate phase. Negligible differences in oxidation kinetics for (Y/Yb)DS coatings over the 90 – 240 µm thickness range were observed.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Influence of cation species on thermal expansion of Y 2 Si 2 O 7 –Gd 2 Si 2 O 7 solid solutions

Mixtures of Y 2 Si 2 O 7 and Gd 2 Si 2 O 7 were synthesized by solid-state reaction at 1600°C and characterized via in situ x-ray diffraction (XRD) to determine their coefficients of thermal expansion (CTE). All solid solutions within the system exhibited the orthorhombic δ-RE 2 Si 2 O 7 (Pna2 1 ) structure. Thermal expansion measurements of Y 2 Si 2 O 7 and Gd 2 Si 2 O 7 correlated well with reported values in literature, and all synthesized solid solutions exhibited CTEs between Y 2 Si 2 O 7 and Gd 2 Si 2 O 7 . Generally, there was a slight decrease in CTE exhibited by the materials with increasing Gd 2 Si 2 O 7 content, with Gd 2 Si 2 O 7 having the lowest CTEs and Y 2 Si 2 O 7 the highest CTEs. Here, the decrease in CTE was attributed to stronger bonds of Gd-O over Y-O, as determined by calculated crystal orbital Hamilton populations using density functional theory. However, such differences were very small and crystal structure was the dominating factor in CTE trends.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2004

Multilayer Article Characterized by Low Coefficient of Thermal Expansion Outer Layer

A multilayer article comprises a substrate comprising a ceramic or a silicon-containing metal alloy. The ceramic is a Si-containing ceramic or an oxide ceramic with or without silicon. An outer layer overlies the substrate and at least one intermediate layer is located between the outer layer and thc substrate. An optional bond layer is disposed between thc 1 least one intermediate layer and thc substrate. The at least one intermediate layer may comprise an optional chemical barrier layer adjacent the outer layer, a mullite-containing layer and an optional chemical barrier layer adjacent to the bond layer or substrate. The outer layer comprises a compound having a low coefficient of thermal expansion selected from one of the following systems: rare earth (RE) silicates; at least one of hafnia and hafnia-containing composite oxides; zirconia-containing composite oxides and combinations thereof.

Kang N Lee↗

NASA NTRS2013

Calcium-Magnesium-Aluminosilicate (CMAS) Reactions and Degradation Mechanisms of Advanced Environmental Barrier Coatings

The thermochemical reactions between calcium-magnesium-aluminosilicate- (CMAS-) based road sand and several advanced turbine engine environmental barrier coating (EBC) materials were studied. The phase stability, reaction kinetics and degradation mechanisms of rare earth (RE)-silicates Yb2SiO5, Y2Si2O7, and RE-oxide doped HfO2 and ZrO2 under the CMAS infiltration condition at 1500 C were investigated, and the microstructure and phase characteristics of CMAS-EBC specimens were examined using Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD). Experimental results showed that the CMAS dissolved RE-silicates to form crystalline, highly non-stoichiometric apatite phases, and in particular attacking the silicate grain boundaries. Cross-section images show that the CMAS reacted with specimens and deeply penetrated into the EBC grain boundaries and formed extensive low-melting eutectic phases, causing grain boundary recession with increasing testing time in the silicate materials. The preliminary results also showed that CMAS reactions also formed low melting grain boundary phases in the higher concentration RE-oxide doped HfO2 systems. The effect of the test temperature on CMAS reactions of the EBC materials will also be discussed. The faster diffusion exhibited by apatite and RE-doped oxide phases and the formation of extensive grain boundary low-melting phases may limit the CMAS resistance of some of the environmental barrier coatings at high temperatures.

Ahlborg, Nadia L.↗

NASA NTRS2017

Environmental Barrier Coatings for Ceramic Matrix Composites - An Overview

SiC/SiC Ceramic Matrix Composites (CMCs) are increasingly being considered as structural materials for advanced power generation equipment because of their light weight, higher temperature capability, and oxidation resistance. Limitations of SiC/SiC CMCs include surface recession and component cracking and associated chemical changes in the CMC. The solutions pursued to improve the life of SiC/SiC CMCs include the incorporation of coating systems that provide surface protection, which has become known as an Environmental Barrier Coating (EBC). The development of EBCs for the protection of gas turbine hot section CMC components was a continuation of coating development work for corrosion protection of silicon-based monolithics. Work on EBC development for SiC/SiC CMCs has been ongoing at several national laboratories and the original gas turbine equipment manufacturers. The work includes extensive laboratory, rig and engine testing, including testing of EBC coated SiC/SiC CMCs in actual field applications. Another EBC degradation issue which is especially critical for CMC components used in aircraft engines is the degradation from glassy deposits of calcium-magnesium-aluminosilicate (CMAS) with other minor oxides. This paper addresses the need for and properties of external coatings on SiC/SiC CMCs to extend their useful life in service and the retention of their properties.

EBC↗

NASA NTRS2023

Influence of Cation Species on Thermal Expansion of Y2Si2O7–Gd2Si2O7 Solid Solutions

Mixtures of Y 2 Si 2 O 7 and Gd 2 Si 2 O 7 were synthesized by solid-state reaction at 1600°C and characterized via in situ x-ray diffraction (XRD) to determine their coefficients of thermal expansion (CTE). All solid solutions within the system exhibited the orthorhombic δ-RE 2 Si 2 O 7 (Pna2 1 ) structure. Thermal expansion measurements of Y 2 Si 2 O 7 and Gd 2 Si 2 O 7 correlated well with reported values in literature, and all synthesized solid solutions exhibited CTEs between Y 2 Si 2 O 7 and Gd 2 Si 2 O 7 . Generally, there was a slight decrease in CTE exhibited by the materials with increasing Gd 2 Si 2 O 7 content, with Gd 2 Si 2 O 7 having the lowest CTEs and Y 2 Si 2 O 7 the highest CTEs. The decrease in CTE was attributed to stronger bonds of Gd-O over Y-O, as determined by calculated crystal orbital Hamilton populations using density functional theory. However, such differences were very small and crystal structure was the dominating factor in CTE trends.

rare earth silicates↗

NASA NTRS2024

Theoretical Prediction of Thermal Expansion Anisotropy for Y 2 Si 2 O 7 Environmental Barrier Coatings Using a Deep Neural Network Potential and Comparison to Experiment

Environmental barrier coatings (EBCs) are an enabling technology for silicon carbide (SiC)-based ceramic matrix composites (CMCs) in extreme environments such as gas turbine engines. However, development of new coating systems is hindered by the large design space and difficulty in predicting properties for these materials. Density Functional Theory (DFT) has successfully been used to model and predict some thermodynamic and thermo-mechanical properties of high-temperature ceramics for EBCs, although these calculations are challenging due to their high computational costs. In this work, we use machine learning to train a deep neural network potential (DNP) for Y 2 Si 2 O 7 , which is then applied to calculate thermodynamic and thermo-mechanical properties at near-DFT accuracy much faster and using less computational resources than DFT. We use this DNP to predict phonon-based thermodynamic properties of Y 2 Si 2 O 7 with good agreement to DFT and experiments. We also utilize the DNP to calculate the anisotropic, lattice direction-dependent coefficients of thermal expansion (CTEs) for Y 2 Si 2 O 7 . Molecular dynamics trajectories using the DNP correctly demonstrate accurate prediction of the anisotropy of the CTE in good agreement with diffraction experiments. In the future, this DNP could be applied to accelerate additional property calculations for Y 2 Si 2 O 7 compared to DFT or experiments.

rare earth silicates↗

NASA NTRSDate not supplied

SiO2 Activity Measurements in the Gd2O3-SiO2 System Via Knudsen Effusion Mass Spectrometry (KEMS)

Environmental barrier coatings (EBCs) are required for the use of silicon carbide (SiC)-based ceramic matrix composites (CMCs) in gas turbine engines, as they protect the SiO 2 thermally grown oxide (TGO) formed at the CMC/coating interface from volatilization in a combustion environment. Current-generation EBCs consist of a silicon bond coat and a rare earth (RE) silicate topcoat. The RE silicate topcoat is exposed to high-velocity steam during engine operation, and SiO 2 within the coating can preferentially volatilize to form Si(OH) 4 gas species, albeit at a lesser degree than SiO 2 alone. Therefore, it is of interest to investigate the stability of these materials in steam as a function of their RE. In this study, SiO 2 activity, which can be related to the partial pressure of Si(OH) 4 , was measured across the Gd 2 O 3 -SiO 2 phase diagram, which includes Gd 2 SiO 5 , Gd 9.33 (SiO 4 ) 6 O 2 , and Gd 2 Si 2 O 7 as line compounds, via Knudsen Effusion Mass Spectrometry (KEMS). Values obtained for the Gd 2 O 3 -SiO 2 system were compared to those of other RE2O3-SiO2 systems and contextualized in terms of EBC viability.

EBCs↗

NASA NTRS2014

NASA's Advanced Environmental Barrier Coatings Development for SiC/SiC Ceramic Matrix Composites: Understanding Calcium Magnesium Alumino-Silicate (CMAS) Degradations and Resistance

Environmental barrier coatings (EBCs) and SiCSiC ceramic matrix composites (CMCs) systems will play a crucial role in next generation turbine engines for hot-section component applications because of their ability to significantly increase engine operating temperatures with improved efficiency, reduce engine weight and cooling requirements. The development of prime-reliant environmental barrier coatings is essential to the viability and reliability of the envisioned CMC engine component applications, ensuring integrated EBC-CMC system durability and designs are achievable for successful applications of the game-changing component technologies and lifing methodologies.This paper will emphasize recent NASA environmental barrier coating developments for SiCSiC turbine airfoil components, utilizing advanced coating compositions, state-of-the-art processing methods, and combined mechanical and environment testing and durability evaluations. The coating-CMC degradations in the engine fatigue-creep and operating environments are particularly complex; one of the important coating development aspects is to better understand engine environmental interactions and coating life debits, and we have particularly addressed the effect of Calcium-Magnesium-Alumino-Silicate (CMAS) from road sand or volcano-ash deposits on the durability of the environmental barrier coating systems, and how the temperature capability, stability and cyclic life of the candidate rare earth oxide and silicate coating systems will be impacted in the presence of the CMAS at high temperatures and under simulated heat flux conditions. Advanced environmental barrier coating systems, including HfO2-Si with rare earth dopant based bond coat systems, will be discussed for the performance improvements to achieve better temperature capability and CMAS resistance for future engine operating conditions.

Environmental barrier coatings↗

NASA NTRS2014

The Development of HfO2-Rare Earth Based Oxide Materials and Barrier Coatings for Thermal Protection Systems

Advanced hafnia-rare earth oxides, rare earth aluminates and silicates have been developed for thermal environmental barrier systems for aerospace propulsion engine and thermal protection applications. The high temperature stability, low thermal conductivity, excellent oxidation resistance and mechanical properties of these oxide material systems make them attractive and potentially viable for thermal protection systems. This paper will focus on the development of the high performance and high temperature capable ZrO2HfO2-rare earth based alloy and compound oxide materials, processed as protective coating systems using state-or-the-art processing techniques. The emphasis has been in particular placed on assessing their temperature capability, stability and suitability for advanced space vehicle entry thermal protection systems. Fundamental thermophysical and thermomechanical properties of the material systems have been investigated at high temperatures. Laser high-heat-flux testing has also been developed to validate the material systems, and demonstrating durability under space entry high heat flux conditions.

Ceramic Matrix Composites↗

NASA NTRS2017

Development of Advanced Environmental Barrier Coatings for SiC/SiC Ceramic Matrix Composites: Path Toward 2700 F Temperature Capability and Beyond

Advanced environmental barrier coating systems for SiC-SiC Ceramic Matrix Composite (CMC) turbine and combustor hot section components are currently being developed to meet future turbine engine emission and performance goals. One of the significant coating development challenges is to achieve prime-reliant environmental barrier coating systems to meet the future 2700F EBC-CMC temperature stability and environmental durability requirements. This presentation will emphasize recent NASA environmental barrier coating system testing and down-selects, particularly the development path and properties towards 2700-3000F durability goals by using NASA hafnium-hafnia-rare earth-silicon-silicate composition EBC systems for the SiC-SiC CMC turbine component applications. Advanced hafnium-based compositions for enabling next generation EBC and CMCs capabilities towards ultra-high temperature ceramic coating systems will also be briefly mentioned.

Ceramic Matrix Composite↗

DOE OSTI2022

Rare Earth and Transition Metal Containing Glasses

Transition metal (TM) and rare earth (RE) ions have been incorporated into many glass systems such as silicate, phosphate, and borosilicate-based oxide glasses, as well as in halide and chalcogenide glasses, that find applications ranging from optical, photonic, and magnetic devices, solid-state battery, to nuclear waste disposal. Understanding the structural role of RE and TM in these glasses can help to develop glass compositions for targeted applications with either high-optical emission efficiency, electrical conductivity, or chemical durability. In this chapter, we first provide a general introduction of the applications and structural features of RE and TM in glasses, then the critical aspects of molecular dynamics (MD) simulations of these glasses such as interatomic potentials, structural analysis tools to study RE and TM ions in glasses and their clustering behaviors, Quantitative Structure–Property Analysis (QSPR), diffusion and dynamic property calculations, and electronic structure calculations to understand electronic defects such as charge trapping and radiation effects are introduced. Three representative case studies are presented: the first one is on MD simulations of erbium- and europium-doped silica and silicate glasses, as well as cerium doped aluminophosphate glasses, that revealed the effect of glass composition on RE ion local structure and clustering behavior. Electronic structure calculations of cerium-doped glass show how the existence of multioxidation states help to mediate radiation-induced damages caused by excited electron–hole pairs was also discussed. The second one focuses on alkali vanadophosphate glasses where the existence of two vanadium oxidation states help to provide electronic conduction in the glasses while alkali ions provide ionic conduction. MD simulations were used to understand vanadium environments and other structural aspects in the phosphate glasses, as well as the ionic transport behaviors of alkali ions. The third case study is on zirconium-containing borosilicate and aluminosilicate glasses that find wide applications in nuclear waste disposal. MD simulations help to provide structural details of zirconium ions that are validated by diffraction and EXAFS spectra. The structural information was used to interpret changes of mechanical properties and chemical durability by using QSPR and other analyses-based MD-generated structure models.

Du, Jincheng↗

DOE OSTI2026

High Entropy Rare-earth Oxide (HERO) Coatings for Refractory Alloys

The HERO coating was developed to protect refractory alloys for application in the harsh hot section of the turbine engine environment addressing ARPA-E ULTIMATE Project Topic 2: Coating Development. The effort was both innovative in its utilization of high entropy rare earth oxides as well as transformational in our approach: holistic design of a single layer thermal/environmental barrier coating (T/EBC) for refractory alloys, with an excellent coefficient of thermal expansion (CTE) match to the alloy substrate, chemical compatibility with the underlying alloy, low oxidant permeability, stability in combustion environments, low thermal conductivity, thermal shock resistance, and resistance to degradation by siliceous debris (calcium magnesium alumino-silicates-CMAS). The high entropy rare earth oxide approach enables two critical coating properties: tailoring CTE match to the substrate and, most significantly, substantially reduced thermal conductivity. The summation of these proposed coating capabilities goes well beyond the technical requirements specified in the ULTIMATE program objectives, and additionally is essential for a successful first stage turbine blade application.

36 MATERIALS SCIENCE↗

NASA NTRS1994

The evolution of enstatite and chondrules in unequilibrated enstatite chondrites: Evidence from iron-rich pyroxene

FeO-rich (Fs(sub 6)-34) pyroxene lacking cathodoluminescence (CL), hereafter black pyroxene, is a major constituent of some of the chondrules and fragments in unequilibrated (type 3) enstatite chondrites (UECs). It contains structurally oriented zones of Cr-, Mn-, V-rich, FeO-poor enstatite with red CL, associated with mm-sized blebs of low-Ni, Fe-metal and, in some cases, silica. These occurrences represent clear evidence of pyroxene reduction. The black pyroxene is nearly always rimmed by minor element (Cr, Mn, V)-poor enstatite having a blue CL. More commonly, red and blue enstatites, unassociated with black pyroxene, occur as larger grains in chondrules and fragments, and these constitute the major silicate phases in UECs. The rare earth element (REE) abundance patterns of the black pyroxene are LREE-depleted. The blue enstatite rims, however, have a near-flat to LREE-enriched pattern, approx. 0.5-4x chondritic. The petrologic and trace element data indicate that the black pyroxene is from an earlier generation of chondrules that formed in a nebular region that was more oxidizing than that of the enstatite chondrites. Following solidification, these chondrules experienced a more reducing nebular environment and underwent reduction. Some, perhaps most, of the red enstatite that is common throughout the UECs may be the product of solid-state reduction of black pyroxene. The blue enstatite rims grew onto the surfaces of the black pyroxene and red enstatite as a result of condensation from a nebular gas. The evolutionary history of some of the enstatite and chondrules in enstatite chondrites can be expressed in a four-stage model that includes: Stage 1. Formation of chondrules in an oxidizing nebular environment. Stage 2. Solid-state reduction of the more oxidized chondrules and fragments to red enstatite in a more reducing nebular environment. Stage 3. Formation of blue enstatite rims on the black pyroxene as well as on the red enstatite. Stage 4. Reprocessing, by various degrees of melting, of many of the earlier-formed materials.

Weisberg, Michael K.↗

NASA NTRS1998

Technologies for Non-Destructive Evaluation of Surfaces and Thin Coating

A study was made on two commercially available terbium-doped silicate glasses. There is an increased interest in silicate glasses doped with rare-earth ions for use in high-energy particle detection and radiographic applications. These glasses are of interest due to the fact that they can be formed into small fiber sensors; a property that can be used to increase the spatial resolution of a detection system. Following absorption of radiation, the terbium ions become excited and then emit photons via 4f-4f electronic transitions as they relax back to the ground state. The lifetime of these transitions is on the order of milliseconds. A longer decay component lasting on the order of minutes has also been observed. While radiative transitions in the 4f shell of rare-earth ions are generally well understood by the Judd-Olfelt theory, the presence of a longer luminescence decay component is not. Experimental evidence that the long decay component is due, in part, to the thermal release of trapped charge carriers will be presented. In addition, a theoretical model describing the time evolution of the radiation-induced luminescence will be presented.

Manos, Dennis M.↗