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Overview of high temperature materials testing within the ART Gas Cooled Reactor Program. Covers 800H weldment creep testing and Alloys 617 and 709 creep and creep-fatigue crack growth rate testing.
Abstract Complex shapes are created from Yb 14 MnSb 11 , a high‐temperature thermoelectric Zintl phase, via a two‐step process: i) layer‐by‐layer 3D‐extrusion of ink containing partially‐reacted powders which are ball‐milled from a blend of Yb, MnSb, and Sb powders; ii) heat treatment to synthesize the ternary compound Yb 14 MnSb 11 and densify the extruded powders. A high phase purity for Yb 14 MnSb 11 (83–94%) is achieved in both cast and 3D‐extruded ink specimens via a solid‐state reaction between Yb, MnSb, and Yb 4 Sb 3 during reactive sintering. Pressure‐free sintering at temperatures of 1200–1400 °C densifies the powders to 82% relative density but can also induce the decomposition of the Yb 14 MnSb 11 phase due to Yb sublimation. A process window with optimized sintering temperature and time is identified, achieving both low porosity and high phase purity and reaching a maximum zT = 0.61 at 1000 °C, about half of the maximum zT value for bulk Yb 14 MnSb 11 made via conventional processes (pressure sintering of precursor powders). The present approach – direct ink writing of ball‐milled powders, combined with reactive sintering – is a scalable and affordable method to fabricate thermoelectric legs with intricate 3D shapes, for enhanced performances in high‐temperature thermoelectric applications.
MAB phases are popular as high-temperature materials with high damage tolerance and excellent electrical conductivity that are used to exfoliate two-dimensional (2D) transition metal borides (MBenes); a promising material for developing next- generation nanodevices. In this report, we explore the correlation between the formation energy, exfoliation energy and structural factors of MAB phases using DFT and machine learning. In order to do so, we developed three different machine learning models based on the support vector machine, deep neural network, and random forest regressor to study the stability of the MAB phases by calculating their formation energies. Furthermore, our support vector machine and deep neural network models are capable of predicting the formation energies with mean absolute errors less than 0.1 eV/atom. We demonstrated that the stability of a MAB phase for a given transition metal decreases when the A element changes from Al to Tl. The density functional theory (DFT) re- vealed that M-A and M-B bond strength strongly correlates with the stability of MAB phases. In addition, the exfoliation possibility of 2D MBenes becomes higher when the A element changes from Al to Tl due to weakening of M-A and M-B bonds.
The present invention relates, in part, to a discovery of a method for using atomic layer deposition (ALD) to improve the stability of refractory materials in high temperature steam, and compositions produced by the method.
Through this collaborative effort, a new 3D printing platform for ceramics called laser-induced slip casting (LIS) was explored and developed for improving the processing and manufacture of silicon carbide (SiC), a high temperature ceramic material. This method prints layers of ceramic slips/slurries with subsequent selective-laser heating to dry each layer to build a 3D structure. The completed and dried part is then sintered. This manufacturing process is inherently lower cost than alternative ceramic printing methods such as binder jet technology or stereolithography when it comes to the feedstock material but is more expensive than robocasting or direct ink writing. However, it has the potential to make more controlled parts with less defects compared to robocasting. The largest cost is the heating source for the printer. With this technique, there is potential to make large ceramic parts in a near-net shape. Further, there is no known commercial manufacturing of 3D printed ceramics that creates a large range of different high-density ceramics at large scale. The goals and outcomes for the development of the new printing technology were: 1) assessing the technology with alumina by characterizing coupons, 2) printing and sintering of silicon carbide (SiC), and 3) characterization and properties testing of materials printed and a scale-up of SiC part(s). Through this collaborative project, it was sought to provide the best solution to achieving highly dense and near-net shaped ceramic parts at large scale and reduced cost. The goal was to produce high density sintered materials for applications in defense, energy generating systems, armor, and wear parts using 3D printing methods. Variables including powder particle sizes, dispersant molecular weights (MWs), binders, printing parameters, and post processing were explored as well as the characterization of the physical properties (add specifics here).
The High-Temperature Gas-cooled Reactor (HTGR) is a Generation IV concept designed to produce electricity and hydrogen at high efficiencies via high operating temperatures (700 °C or higher). Helium, the primary coolant for HTGRs, contains impurities (e.g., CO, H2O and CH4) that can induce corrosion reactions at high temperatures such as oxidation and (de)carburization, which in turn can affect the tribological behavior of components. Incoloy® 800HT (Ni-Fe-Cr austenitic solid-solution alloy) and Inconel® 617 (Ni-Cr-Co-Mo solid-solution alloy) are two high-temperature superalloys currently selected as candidate structural materials for the HTGR. The objective of this study is to evaluate the high-temperature tribological performance of these two candidate alloys after conditioning them in HTGR environments. Four regimes of corrosion were considered: a non-conditioned regime (Regime I), an oxidizing regime (Regime II), a carburizing and oxidizing regime (Regime III), and a carburizing regime (Regime IV). To simulate oxidation in HTGR, samples were conditioned for 22 days at elevated temperatures in a once-through helium loop with 4 ppmv H2O. Carburization of the samples was achieved by the commercial process, Kolsterising®. In addition, two surface treatments – shot peening and aluminization – were considered as potential routes of improving the alloys’ wear resistance. Surface-treated samples were tested both before and after conditioning in Regime II. Tribological testing of the samples was performed via a pin-on-disk tribometer at elevated temperatures in ambient environment – 650 and 750°C for 800HT; 850 and 900°C for 617 – with applied loads of 1N, 2N and 5N. The wear behavior of the alloys was assessed via wear volume and friction coefficient measurements, supported by morphological, structural and compositional analyses of the wear tracks. Conditioning the samples in Regime II led to the formation of a chromium oxide on both alloys. This protective scale increased the wear resistance compared to that of as-received samples (Regime I) due to the formation of a compacted ‘glaze’ oxide layer during sliding, rendering the wear track nearly undistinguishable from the unworn background and resulting in wear volumes below the detection limits of the measurement technique. The variability of the friction coefficients of the conditioned samples was also considerably reduced compared to that of the as-received samples due to the glaze layer. Additionally, the initial friction coefficients of the samples conditioned in Regime II were reduced by 45% and 54% compared to those of as-received samples for alloys 800HT and 617, respectively. Carburizing the samples (Regime IV) hardened the surfaces of both alloys and promoted the formation of an iron oxide on 800HT during tribological testing, thereby increasing the wear resistance and decreasing the initial friction coefficient by a factor of two compared to those of as-received 800HT. Alloy 617 exhibited an enhanced wear resistance but similar initial friction coefficient compared to those of as-received samples due to the increased surface hardness. The Mn-Cr oxide developed during Regime III conditioning of 800HT did not develop a glaze layer during tribotesting, even at lower loads. Thus, it was not as protective as the oxide produced during conditioning of Regime II samples, leading to lower wear resistance of 800HT in Regime III compared to that measured in the Regime II condition. 800HT benefited from the aluminization surface treatment, particularly before conditioning in Regime II, due to the promotion of a wear-resistant aluminum oxide layer during testing and the increase in surface hardness due to the presence of a FeAl intermetallic phase. The presence of this phase caused an order-of-magnitude reduction in wear volumes compared to those of as-received 800HT. Aluminization of 617 decreased its wear resistance, particularly after conditioning in Regime II, due to significant wear of the aluminum oxide via a ceramic wear mechanism. This aluminum oxide was removed during sliding, causing the wear volumes to increase by a factor of five compared to those of 617 conditioned in Regime II. Shot-peened 800HT exhibited a tribological behavior similar to that of as-received 800HT, despite an enhancement in the rate of chromium oxide formation. Shot-peened 800HT conditioned in Regime II showed lower wear resistance compared to that of 800HT conditioned in Regime II due to the poor adhesion between the oxide and the underlying metal, preventing the formation of the glaze layer during sliding. Shot peening of 617 increased its wear resistance at higher load, reducing worn volumes by 60% compared to that measured with as-received 617. Tribotesting of shot-peened 617 in Regime II revealed that the glaze-oxide layer was formed at every load, resulting in negligible wear, similar to what was observed from testing 617 after conditioning in Regime II. Overall, alloy 617 exhibited tribologically superior behavior compared to that of alloy 800HT, as demonstrated by its lower friction coefficients and its order-of-magnitude lower wear volumes when measurable.
This report describes a framework for storing, processing, and displaying qualification data for high temperature mechanical properties. The framework automates the process of generating design data from mechanical test results, for example for a data qualification report for the ASME Boiler \& Pressure Vessel Code. The framework has three parts: a data storage model with common formats for several types of typical mechanical property tests, a backend based on the \pycreep Python library for correlating and extrapolating the data to generate design material properties and allowable stresses, and a demonstration user interface for displaying, sorting, and filtering the data and exploring different options for modeling the design mechanical properties. The report discusses the options available for data processing, with illustrations from real test data on Alloy 617, Alloy 709, Alloy 740H, and Laser-Powder Bed Fusion 316H. The framework is complete for ASME type data analysis and will be used to store test data generated by the Department of Energy, Office of Nuclear Energy, Advanced Materials and Manufacturing Technologies sponsored qualification programs. Future work could extend the tool to other types of material properties and/or expand the demo user interface to make it accessible across the AMMT program.
Technologies that function at room temperature often require magnets with a high Curie temperature, $T$ C , and can be improved with better materials. Discovering magnetic materials with a substantial $T$ C is challenging because of the large number of candidates and the cost of fabricating and testing them. Using the two largest known datasets of experimental Curie temperatures, we develop machine-learning models to make rapid $T$ C predictions solely based on the chemical composition of a material. We train a random-forest model and a k -NN one and predict on an initial dataset of over 2500 materials and then validate the model on a new dataset containing over 3000 entries. The accuracy is compared for multiple compounds' representations (“descriptors”) and regression approaches. A random-forest model provides the most accurate predictions and is not improved by dimensionality reduction or by using more complex descriptors based on atomic properties. Further, a random-forest model trained on a combination of both datasets shows that cobalt-rich and iron-rich materials have the highest Curie temperatures for all binary and ternary compounds. An analysis of the model reveals systematic error that causes the model to over-predict low-$T$ C materials and under-predict high-$T$ C materials. For exhaustive searches to find new high-$T$ C materials, analysis of the learning rate suggests either that much more data is needed or that more efficient descriptors are necessary.
Graphitic matrix material encapsulates tristructural isotropic (TRISO) coated fuel particles and is a structural component for both pebble and cylindrical fuel compacts in high temperature gas reactor (HTGR) designs. In an off-normal event involving steam exposure, the matrix material is exposed to oxidants, leading to degradation of the fuel compact and subsequent exposure of the TRISO particle fuel to oxidizing species. This study presents microstructural characterization of matrix material after exposure to high temperature (1200°C), 48 kPa steam in which the evolved microstructure demonstrated nonuniform degradation. Subsequent Raman spectroscopy determined the nature of the remaining material post-exposure. Finally, the electron microscopy characterization suggests and Raman spectroscopic analysis confirms, under off-normal conditions, the carbonized phenolic resin binder is preferentially oxidized ahead of the graphite flake filler and is responsible for the nonuniform degradation and enhanced depth of attack.
High temperature ferritic-martensitic steels are candidate materials for heavy-duty diesel engine pistons. The envisioned transition to hydrogen blended fuels is expected to alter the post-combustion atmosphere in the engines, primarily resulting in a higher water vapor content (> 20 vol%) and potentially higher exhaust gas temperatures. The oxidation resistance of existing and newly developed alloys will be a critical life-limiting mechanism under these conditions. In the present work, the oxidation behavior of candidate piston alloys was evaluated in air+10 vol.% H2O and air+30 vol.% H2O at 700°C. Thermal cyclic (1h cycle) exposures were conducted for two variants of commercial UNSS42200 ferritic-martensitic steel and two developmental alloy steels for up to 300h. The developmental alloys each have similar compositions but with one containing elevated Cu levels of 3 wt.%, A significant reduction in resistance to breakaway oxidation was observed for the commercial alloys in the higher water vapor atmosphere. Microstructural characterization (optical metallography, scanning electron microscopy and electron microprobe analysis) revealed the formation of thick Fe-rich oxides even for the high Cr (~12 wt.%) steels after an initial stage of protective oxidation with MnCr-rich spinels. The impact of the evaporation-induced loss of Cr on the time and temperature dependent compositional changes in the alloys was correlated with experimental findings. For the developmental alloys, Cu additions appear to play a role in significantly reducing oxidation kinetics in air+30 vol.% H2O at 700°C.
Understanding the formation mechanism of layered oxide cathodes via solid-state synthesis is imperative to achieving controllability over their materials properties and electrochemical behaviors. In this work, we investigate the phase and microstructure evolution during the synthesis of NaNi 1/3 Fe 1/3 Mn 1/3 O 2 , a model sodium-ion layered oxide cathode, using a combination of imaging, diffraction, and spectroscopic techniques. We unravel the synthetic mechanistic pathways involved in the high-temperature calcination reaction, as well as elaborate the synthesis-microstructure-performance relationship of this material. The formation of the final layered oxide phase involves a gradual transformation through a sodiated oxyhydroxide intermediate. During the reaction, the precursor dehydration reaction dominates at 250–550 °C, while the major sodiation reaction occurs at 550–850 °C. Alongside multiple stages of phase transformations, the final grain structure formation occurs through the continuous growth of the (003) and (104) facets. During the reaction, Mn acts as the charge-compensating element and exhibits depth-dependent characteristics. When the sodiation reaction dominates over dehydration, the reaction intermediates undergo gradual electronic structure changes with increasing temperature, as indicated by the spectral features of TM3d-O2p hybrid states. Calcination duration is also a critical parameter governing the microstructure, surface reactivity, phase fraction distribution and electrochemical performance of the material. The optimal calcination duration was determined to be 18 hours at 850 °C under the conditions evaluated here. Calcination beyond this duration was found to be detrimental to electrochemical performance due to Na and O loss and heterogeneous sodium distribution throughout the particles. Our work sheds light on the complex crystallographic-chemical-microstructural evolution of sodium ion layered oxide cathodes and provides insight into precisely tuning material properties which are intimately linked to battery performances.
Among many efforts in the research of van der Waals (vdW) magnetic materials, increasing the Curie temperature above room temperature has been at the center of research in developing spintronics technology using vdW materials. Here an effective and reliable method of increasing the Curie temperature of ferromagnetic Fe3GeTe2 vdW materials by Ga implantation is reported. It is found that implanting Ga into Fe3GeTe2 by the amount of 10-3 Ga Å-3 could greatly enhance the Fe3GeTe2 Curie temperature by almost 100%. Spatially resolved microdiffraction and element-resolved X-ray absorption spectroscopy show little changes in the Fe3GeTe2 crystal structure and Fe valence state. In addition, the Ga implantation changes the Fe3GeTe2 magnetization from out-of-plane direction at low temperature to in-plane direction at high temperature. The result opens a new opportunity for tailoring the magnetic properties of vdW materials beyond room temperature.
Thermal energy storage (TES) is a broad-based technology for reducing CO₂ emissions and advancing concentrating solar, fossil, and nuclear power through improvements in efficiency and economics. Phase change materials (PCMs) are of interest as TES media because of their ability to store large amounts of heat in relatively small volumes. The volume expansion during a phase change, typically between a solid and liquid, can cause breakage of protective coatings. This paper reports on the fabrication of a ceramic encapsulated metal (CEM) high temperature TES technology using a rotary calcining furnace and a fluidized bed chemical vapor deposition coating technique. Aluminum beads were chosen as the PCM because Al has a high melting point (660 °C), low cost, high heat of fusion, and an ability to form a thin, strong alumina layer capable of supporting the Al melt for subsequent processing. Quite remarkably, this study shows that 1 mm diameter Al can be fluidized up to at least 1500 °C in an appropriate atmosphere while maintaining a spheroid geometry. This allowed for producing a first of a kind CEM whereby Al particles were encapsulated in pyro-carbon (PyC) and high purity, dense chemical vapor deposited SiC. The CEM with a PyC only coating was exposed to thermal cycling to test the performance with a differential scanning calorimeter; the melting point and latent heat were measured to be 648.4 ± 2.8 °C and 293.3 ± 6.2 J/g respectively. It was demonstrated that the CEM design is possible to produce, laying the foundation for manufacturing of high temperature, tunable, TES media.
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Fiber-reinforced ceramic matrix composites are attractive for high-temperature nuclear applications due to excellent thermal and mechanical properties as well as reasonable-to-outstanding radiation resistance. Over the past 20 years, the use of ceramic matrix composite applications expanded to many commercial non-nuclear industries as fabrication and application of the technologies mature. The ASME Boiler Pressure Vessel Code, under Section III Division 5, provides the design and construction rules for High Temperature Reactor components. It published the first rules for ceramic matrix composites to be used for reactor core components. The rules lay out the quality requirements together with the design and materials criteria for the use and application of silicon carbide- and carbon-based matrix material technologies. As with the established graphite rules, the ceramic composite material rules are structured in Subsection HH (from Section III), that addresses the criteria for class SN nonmetallic core components. The code rules rely heavily on the development and publication of standards for composite specification, classification, and testing of mechanical, thermal, and other properties. These test methods are developed in ASTM Committee C28 on Advanced Ceramics, with a current focus on ceramic composite tubes. This article describes the detail of the composites code, the design methodology and similarities to the graphite code, the guidance for the development of specifications for ceramic composites (for nuclear applications) including recent standard developments, and it mentions the next steps to support licensing aspects by validating the code with benchmarking data.
Realizing higher operating temperatures to increase efficiency of future applications for energy conversion and storage while minimizing cost is a challenge for development of high-temperature materials. Simultaneous optimization of mechanical properties and corrosion resistance continues to be a difficult task but is essential due to the need to significantly accelerate the transition between technology readiness levels in the future. Furthermore, oxidation-induced degradation will be a critical life-limiting mechanism at increased operating temperatures. Suitable high-temperature materials cannot be solely identified by time-consuming experiments and reliable computational methods incorporating the relevant physics of processes must be considered to complement the experimental efforts. In the present work, a review of the methods employed to model oxidation-induced material degradation described in literature will be discussed. Furthermore, their capability to predict lifetime and aid in material selection will be evaluated.
This report describes the development of simplified, universal constitutive model that captures the high temperature monotonic and cyclic behavior of a range of commonly-used high temperature materials. The goal of the work is to provide a simple, universal constitutive model to replace the current bespoke models for Grade 91, 316H, and Alloy 617 included in Nonmandatory Appendix HBB-Z of the ASME Boiler & Pressure Vessel Code, and to extend this model to cover Alloy 800H. We initiated this work in response to feedback from reactor vendors and other Code users requesting simplified models, compared to the current models, that are easier to implement and use in commercial finite element analysis software. This report describes the completion of this effort by developing a model to correct the defects in standard model forms presently used for high temperature material modeling, described in past work, developing and implementing new numerical methods to train this model against test data, and then actually training the model for the four materials. The report provides a complete mathematical description of the model along with the tabulated material coefficients for the four materials. The final step will be to formulate an ASME Code change to introduce the new models into the Code.