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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 109 records · Page 6

Tailoring plasticity mechanisms in compositionally graded hierarchical steels fabricated using additive manufacturing

Abstract While there exists in nature abundant examples of materials with site-specific gradients in microstructures and properties, engineers and designers have traditionally used monolithic materials with discrete properties. Now, however, additive manufacturing (AM) offers the possibility of creating structures that mimic some aspects of nature. One example that has attracted attention in the recent years is the hierarchical structure in bamboo. The hierarchical architecture in bamboo is characterized by spatial gradients in properties and microstructures and is well suited to accommodate and survive complex stress states, severe mechanical forces, and large deformations. While AM has been used routinely to fabricate functionally graded materials, this study distinguishes itself by leveraging AM and physical metallurgy concepts to trigger cascading deformation in a single sample. Specifically, we have been successful in using AM to fabricate steel with unique spatial hierarchies in structure and property to emulate the structure and deformation mechanisms in natural materials. This study shows an improvement in the strength and ductility of the nature-inspired “hierarchical steel” compared with conventional cast stainless steels. In situ characterization proves that this improvement is due to the sequential activation of multiple deformation mechanisms namely twinning, transformation-induced plasticity, and dislocation-based plasticity. While significantly higher strengths can be achieved by refining the chemical and processing technique, this study sets the stage to achieve the paradigm of using AM to fabricate structures which emulate the flexibility in mechanical properties of natural materials and are able to adapt to in-service conditions.

36 MATERIALS SCIENCE↗

Electrochemical lithium extraction from hectorite ore

Electrochemical technologies add a unique dimension for ore refinement, representing tunable methods that can integrate with renewable energy sources and existing downstream process flows. However, the development of electrochemical extraction technologies has been impeded by the technological maturity of hydro- and pyro-metallurgy, as well as the electrical insulating properties of many metal oxide ores. The fabrication and use of carbon/insulating material composite electrodes has been a longstanding method to enable electrochemical activation. Here, using real hectorite ore, we employ this technical approach to fabricate hectorite-carbon black composite electrodes (HCCEs) and achieve electrochemical activation of hectorite. Anodic polarization results in lithium-ion release through a multi-step chemical and electrochemical mechanism that results in 50.7 ± 4.4% removal of lithium from HCCE, alongside other alkaline ions. This technical proof-of-concept study underscores that electrochemical activation of ores can facilitate lattice deterioration and ion removal from ores.

25 ENERGY STORAGE↗

Unraveling the structure of molten salts: a review of high-energy x-ray diffraction (HEXRD) studies

High energy x-ray diffraction (HEXRD) has emerged as a pivotal technique for examining the structural properties of molten salts, which play vital roles in various high-temperature applications, such as energy storage, nuclear reactors, and metallurgy. This review provides a comprehensive analysis of recent progress in HEXRD studies of various molten salt systems, including molten halide salts, their mixtures, and salts with molecular anions, focusing on the insights into their atomic-scale arrangements. Additionally, we discuss methodological advancements that have improved the resolution and accuracy of HEXRD measurements, as well as recent developments in computational simulations, such as machine learning interatomic potentials, for interpreting results. This review aims to serve as a valuable resource for researchers in this field, offering a detailed overview of the progress of HEXRD studies of molten salts and suggesting pathways for further exploration.

Blockmon, Avery L. [Argonne National Laboratory (A↗

A code-to-code benchmark for magneto-convection in a horizontal duct

Liquid metals and magnetic fields are used in many technical applications such as metallurgy, crystal growth and nuclear fusion reactors. When an electrically conducting fluid moves in a magnetic environment, electric currents and electromagnetic forces are generated that affect velocity and pressure losses in the flow. These magnetohydrodynamic (MHD) interactions have to be investigated to optimize the engineering processes. The characteristics of MHD flows depend on the geometrical configuration, the strength of the applied magnetic field, the electrical properties of fluid and structural materials and the thermal conditions. In the so-called blankets for fusion reactors, where liquid metals are used to breed the plasma fuel component tritium and to extract the generated heat, magneto-convective flows play a crucial role in determining heat and mass transfer. Therefore, the availability of numerical codes to simulate this type of flow is mandatory and their validation is a necessary step to guarantee the reliability of the results. For that reason, a benchmark problem has been defined to simulate liquid metal flows in a horizontal rectangular duct heated from below and exposed to a non-uniform magnetic field. Results obtained by five research groups using different codes are compared.

benchmark↗

Microstructure and Hard Magnetic Properties of Sm 1-x Zr x (Fe,Co) 11.3-y Ti 0.7 By Ingots and Thick Melt-Spun Ribbons

Permanent magnets made from Sm(Fe,Co) 12 -based compounds are being actively pursued through nanostructuring and powder metallurgy. This study was aimed at the development of hard magnetic properties in bulk as-cast alloys and in melt-spun alloys for very low wheel speeds. Slower solidification rates and alloying with Zr promote the tetragonal ThMn 12 -type crystal structure, whereas higher solidification rates and alloying with B replace the ThMn 12 structure type with the TbCu 7 structure type. When introduced simultaneously, Zr and B dramatically reduce the alloy solidification rates required for both the refinement of the 1:12 crystallites and their replacement with the 1:7 phase. In bulk arc-melted alloys, this allowed for a microstructure of separated 1:12 crystallites 1–3 μm in size, although, because of the ferromagnetic nature of a minority phase, the coercivity of these fine-grained alloys reached only 0.73 kOe. A moderately accelerated solidification further refined the 1:12 crystallites and increased the coercivity; a Sm 0.7 Zr 0.4 (Fe,Co) 10.8 Ti 0.7 B 0.5 alloy exhibited a coercivity of 1.5 kOe and a maximum energy product of 3.4 MGOe when it was melt-spun into a 0.26-mm-thick ribbon. A more rapid solidification suppressed the 1:12 phase and after annealing at 800–850 °C, the alloys modified with Zr and B developed reasonably high coercivity and maximum energy product even when melt-spun at a wheel speed of 6 m/s. For the above-mentioned alloy, these values were 4.1 kOe and 7.8 MGOe, respectively. Further, a similarly processed very-Sm-lean Sm 0.5 Zr 0.6 (Fe,Co) 10.6 Ti 0.7 B 0.7 alloy exhibited a remanence of 8.8 kG and an energy product of 7.4 MGOe.

36 MATERIALS SCIENCE↗

Accessing pluripotent materials through tempering of dynamic covalent polymer networks

Pluripotency, which is defined as a system not fixed as to its developmental potentialities, is typically associated with biology and stem cells. Here, inspired by this concept, we report synthetic polymers that act as a single “pluripotent” feedstock and can be differentiated into a range of materials that exhibit different mechanical properties, from hard and brittle to soft and extensible. To achieve this, we have exploited dynamic covalent networks that contain labile, dynamic thia-Michael bonds, whose extent of bonding can be thermally modulated and retained through tempering, akin to the process used in metallurgy. In addition, we show that the shape memory behavior of these materials can be tailored through tempering and that these materials can be patterned to spatially control mechanical properties.

36 MATERIALS SCIENCE↗

Electrochemical Recovery of Iron from Spent Pickle Liquor by Chloride-Based Molten Salt Electrolysis

Spent pickle liquor (SPL) is a waste stream generated in the steel industry that presents both a disposal challenge and a potential resource for metal recovery. This study investigates the electrochemical extraction of high-purity iron metal from SPL using chloride-based molten salt electrolysis (CMSE). Electrochemical characterization of diluted SPL confirmed Fe 2+ as the dominant species. Thermal dehydration of SPL under inert atmosphere yielded FeCl 2 -rich solids, which were directly employed as feedstock for electrolysis in LiCl–KCl eutectic melts at 500 °C. Cyclic voltammetry of FeCl 2 in this melt revealed well-defined Fe 2+ /Fe 0 redox behavior within the electrochemical stability window of the supporting electrolyte. High coulombic efficiency (>85%) electrodeposition was achieved demonstrating that iron metal can be produced from dehydrated SPL by CMSE. The electrodeposited iron exhibited >98 wt% purity, which was further enhanced to 99.9 wt% via arc melting. The resulting iron powder was ferromagnetic, and its size distribution was found to be suitable for powder metallurgy applications. This work demonstrates a scalable, energy-efficient pathway for valorizing SPL into high-purity iron metal, advancing circular economy strategies in the steel industry.

Materials science↗

High-entropy materials

We report that primarily over the last decade, the concept of multiple-principal-element metallic materials, commonly referred to as high-entropy alloys, or more generally, high-entropy materials, has taken the field of materials science, particularly structural metallurgy, by storm, at least as measured by the plethora of publications that are focused on this topic. In this article and the following six articles, we attempt to distill what all this is about, with a description of why these materials may be important, why they may differ from traditional materials and how theoretical, computational, and experimental studies can shed light on the science underlying their behavior and potential application.

36 MATERIALS SCIENCE↗

An engineering perspective on evaluating mechanisms governing ductility in pure molybdenum

The United States lacks a stable domestic supply of 99 mTc, a critical medical imaging isotope generated from 99 Mo. Accelerator-based production using 100 Mo targets (aMo) introduces mechanical concerns due to the ductile-to-brittle transition temperature inherent to refractory metals like Mo. This study evaluates the tensile behavior of aMo targets from 25 to 1000 °C, compared to powder-metallurgy-processed natural Mo (PMo) and cast-and-rolled Mo (RMo), both as-received and after 5 ppm O 2 exposure in flowing He. RMo showed superior ductility (7.3% at 25 °C, 48% at 1000 °C) and strength, attributed to its fine, elongated grains and high geometrically necessary dislocation density. PMo exhibited variable ductility (up to 33%), while aMo remained brittle, with a maximum elongation of 10.4% at 600 °C. EBSD analysis revealed weak texture in PMo and aMo, but high defect density in aMo limited dislocation mobility. This work links processing, microstructure, and deformation mechanisms to guide fabrication of ductile refractory targets.

Hyer, Holden C. [Oak Ridge National Laboratory (OR↗

CHARACTERIZING AND CONTROLLING RECOVERY AND RECRYSTALLIZATION IN NIOBIUM FOR IMPROVED SRF CAVITY PERFORMANCE

Crystal defects, such as dislocations and low-angle boundaries, provide sources of magnetic flux trapping in the Nb materials used for superconducting radio frequency (SRF) resonating cavities. Improving the performance of SRF cavities, as measured through the quality factor, requires reducing these defects. SRF cavity production involves deformation processing, such as rolling and forming, and strategic annealing heat treatments. The resulting microstructures can be recovered, recrystallized, or both. Because recovery leaves many defects that can trap flux, recrystallization should improve cavity performance. Thus, processing schedules that produce complete recrystallization without excessive grain growth need to be designed. Solutions to this problem require understanding physical metallurgy and differentiating between recovered and recrystallized regions of microstructure. Backscattered electron microscopy techniques are applied to this end. We demonstrate that the conditions required to produce fully recrystallized microstructures depend on Nb impurity content, suggesting that processing schedules may need to be adjusted by material heat or lot. We also demonstrate that processing can be used to control growth of recrystallized grains to maintain mechanical strength in fully recrystallized materials. Forming cavities from cold-rolled Nb sheet material may provide strategic new routes to obtain microstructures that improve SRF cavity performance.

Taleff, E. [The University of Texas at Austin]↗

Hydrogen Transport in a Model 9979 Shipping Package with Inner Convenience Cans

Radiolytic hydrogen production and accumulation inside containment packages is a concern at any facility responsible for their packaging, storage, transportation, and/or disposal. When hydrogen gas accumulates to concentrations above the Lower Flammability Limit (LFL) which is 4% or 40,000 ppm in air, the possibility of a deflagration or explosion increases. This concern persists over the course of the package lifetime which is unlimited when disposed of by burial or in permanent repositories. Here, we report on a numerical model used to predict the concentration of hydrogen within each layer of a Model 9979 package containing a convenience can assembly. Simulations show the hydrogen concentration to always be highest in the inner convenience can containing the radioactive source. When the radioactive source is within the Los Alamos National Laboratory (LANL) Packaging Limits, the hydrogen concentration is shown to remain well below the LFL at all times including packaging, storage, transportation, and disposal. A hydrogen transport model is presented for a Model 9979 package system containing a nested arrangement of convenience cans, which are tin oxide coated steel cans of various sizes with a slip-lid assembly. The inner convenience can contains the radioactive source material along with an unknown quantity of incidental water acquired from humid air or processing. While visible organic materials such as paper and plastics were purposely excluded from the inner can, it is not possible to claim the wastes are entirely organic free. The inner convenience can is tape sealed and placed into a plastic bag which is horsetail closed (i.e., twisted and taped). The bagged can is placed into an outer convenience can that is also tape sealed. The can assembly is then placed into the 30 gallon drum and subsequently placed inside the 55 gallon drum in the 9979 package. Here we assume hydrogen gas is produced in the inner convenience can from alpha radiolysis of water at a rate dependent on the quantity of uranium isotopes and water present. The hydrogen transport model was used to calculate hydrogen accumulations within the package’s five layers at different times and conditions. These simulations serve two purposes; (i) to build confidence in the model by comparing predicted values to measured values, and (ii) to check the steady state hydrogen concentrations that are approached at long times in the package’s lifetime. Model simulations were compared to gas samples taken from the 30 gallon drum after storage at LANL’s Chemistry and Metallurgy Research (CMR) building for around 500 days. Hydrogen concentration calculations over much longer periods (i.e., more than 270 years) included extreme storage durations, transportation at extreme cold temperatures, and disposal of packages assuming different average temperatures.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Molten Chloride Thermophysical Properties, Chemical Optimization, and Purification

Next-generation concentrating solar power (CSP) technology requires high-temperature heat-transfer fluids and thermal energy storage that can operate in the temperature range of 500°–720°C. This high temperature demands a new chemistry for the heat-transfer fluids that must have high-temperature thermal and chemical stabilities, high energy density, and low corrosion rate on metallic materials used in the heat exchangers, piping, and thermal energy storage tanks. A ternary MgCl 2 -KCl-NaCl chloride-salt system has been proposed to achieve such goals, given its high-temperature thermal stability. The chloride-salt-based systems have been used by the metallurgy industry as the electrolyte to electrolytically extract metallic magnesium. They have also attracted attentions from the nuclear industry for developing the molten salt fast reactors that can operate at close to atmospheric pressure and at higher temperature than traditional light-water reactors. However, the corrosion properties of the ternary salt are not well known. The corrosion mechanism is believed to be correlated to the presence of MgOHCl impurity at the operation temperature. MgOHCl is fundamentally caused by the hygroscopic nature of the MgCl 2 component. Therefore, the first key objective of this project is to understand the nature of the corrosiveness of the ternary chloride-salt system and its prevention by designing new lab-scale purification processes. Because of its importance, a working group called the Chloride Salt Collective across multiple U.S. Department of Energy national laboratories is established to gain experimental agreement on the corrosion behaviors. In addition, water generation during salt dehydration could lead to highly corrosive HCl/water mixture via a hydrolysis process between water and anhydrous MgCl 2 or MgCl 2 hydrates. MgOHCl will eventually be converted to MgO particulates regardless of the chemical path chosen (i.e., by thermal decomposition, chemical purification with an active metal, or electrochemical purification utilizing the reduction power of electron flows). Large MgO particles with high hardness can wear out bearing and bushing and even clog the delicate channels in the primary heat exchanger. Because of this, a second objective is to understand the chemistry behind salt purification and transfer the scientific understanding to a set of engineering know-how for large-scale salt melter design. Because there is limited information on the thermophysical properties and the sensitivity of these properties around the targeted salt composition, a third objective is to measure thermophysical properties relevant to system and component design and support Topic 1 Liquid Pathway development. For example, composition shift due to salt reaction with water can be a potential issue because it can lead to changes of thermophysical properties, such as (1) melting point (or freeze point), which can jeopardize safe operation of the supercritical CO 2 power cycle proposed for next-generation CSP, and (2) heat capacity and density, which can decrease the overall power-generation capability of the plants. The value of the thermal conductivity of the selected salt composition is also a critical criterion for the solar receiver design.

14 SOLAR ENERGY↗

TA-55 FOD Waste Management Requirements

Virtually all activities conducted in the TA-55 FOD (Facility Operations Division) (TA-55, TA-50,RLWTF[Radioactive Liquid Waste Treatment Facility], RLUOB[Radiological Laboratory/Utilities/Office Building], TWF, TA-63 [Transuranic Waste Facility], RANT, TA-54 West [Radioassay Nondestructive Testing Facility], WCRRF [Waste Characterization, Reduction, and Repackaging Facility]and CMR[Chemistry and Metallurgy Research])facilities generate waste. Generation and management of waste arecomplex activitiessubject toFederal and State regulations as well as DOE(Department of Energy)and Laboratory requirements. Improper management of waste can result in civiland/or criminal penalties as well as potential significant impacts to operations.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Development of Repair Techniques for Cast Iron Engine Blocks by Additive Manufacturing

ORNL partnered with Cummins Inc to demonstrate the feasibility of using additive manufacturing techniques to deposit large volume of new material on cast iron in the context of remanufacturing. Remanufacturing at Cummins Inc is carried out to repair any field damage and, in some cases, provide additional value by adding new features. Large volume deposition on difficult to weld materials is a challenging problem due to involved metallurgy. Phase-1 of this work evaluated the feasibility of using laser directed energy deposition technique to deposit new material layer by layer on cast iron engine blocks. During phase-1 deposits were made using Inconel-718, Nickel, Nr-Cr-B braze filler. Leveraging the knowledge gained during Phase-1, Phase-2 focused on developing a low- cost crack resistant ferrous alloy to repair cast iron via volume deposition techniques without preheating. Three different alloy chemistries were identified, and trials were performed on cast iron substrates to identify the optimal chemistry that provided adequate resistance to cracking in both, the deposits as well as the cast iron substrate.

42 ENGINEERING↗

Operational and Mission Highlights: A Monthly Summary of Top Achievements September 2021

Laboratory personnel working on a years-long Confinement Vessel Disposition (CVD) Project at the Chemistry and Metallurgy Research (CMR) facility recently shipped its first vessel after closing the emptying and dispositioning portion of the project in 2020. During the 1970s and 1980s, the Laboratory conducted experiments that produced data used in computer modeling. Scientists used these models to evaluate the performance of nuclear weapons.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Shear Assisted Processing and Extrusion (ShAPE) of Aluminum Alloy 7075, 2024, and Al-12.4TM

The most common aluminum alloys utilized in the aerospace industry are 7075 and 2024 due to their high strength-to-weight ratio compared to advanced high strength steels and other aluminum alloys. Despite excellent performance, these aluminum alloys have seen limited use outside of the aerospace industry due in part to high cost. If high-performance aluminum extrusions could be made more cost effectively by eliminating energy intensive process steps typical of conventional extrusion, then numerous opportunities exist for more widespread adoption. A key reason for the high cost of 7075 and 2024 extrusions (25-75% higher than 6061) is their slow extrusion speed. 7075 and 2024 are limited to 2 m/min and 3.5 m/min respectively, in contrast to 6061 which can be extruded at 20–80 m/min. In addition to slow speed, aluminum alloys require numerous thermal treatments throughout the extrusion process including homogenization and pre-heating prior to extrusion, and solution heat treating and artificial aging after extrusion. Each of these steps contribute to the total energy consumed during manufacturing of extruded components. This project investigates the use of ShAPE to improve extrusion speed and reduce, or even eliminate, the typical thermal treatments for high strength aluminum alloys, all while improving material performance. The overarching goal of this project was to demonstrate that Shear Assisted Processing and Extrusion (ShAPE) can manufacture high-performance aluminum alloy tubing with lower manufacturing energy and improved mechanical properties compared to conventional extrusion. Unlike conventional extrusion where the billet is rammed against a stationary die using a strictly linear motion, the ShAPE process superimposes a rotational shear force by spinning the die while the billet is plunged. Compared to conventional linear extrusion, the ShAPE process imparts significantly more strain into the feedstock material, which enables the formation of novel microstructures. These microstructures manifest an array of property and process improvements for extrusion of high-performance aluminum alloys. The following accomplishments were achieved for this project: Extrusion of 7075 at 12.2 meters/min compared to 2 meters/min for conventional extrusion; Elimination of 7075 billet homogenization (430 °C for 20 hours) which is required prior to conventional extrusion; Elimination of 7075 billet pre-heating (400 °C for 1 hour) in a separate furnace which is required prior to conventional extrusion; Achieved 7075-T6with yield strength = 595 MPa, ultimate tensile strength = 531MPa, and elongation = 17.4% for extrusions made from unhomogenized billets. Exceeds the ASTM and ASM standard, and typical industry values; Achieved 7075-T5 (i.e., no solution heat treatment) with yield strength = 588 MPa, ultimate tensile strength = 535 MPa, and elongation = 14.8% for extrusions made from homogenized billets; Extrusion of 2024 at 7.4 meters/min compared to 3.5 meters/min for conventional extrusion; Achieved 2024-T8510 yield strength = 522 MPa, ultimate strength = 510MPa, and elongation = 7.1% for extrusions made from wrought billets. Exceeds the ASTM and ASM standard, and typical industry values; Extrusion of Al-12.4TM high-performance aluminum powder directly into tubing, in a single step, which eliminates process steps typical of powder metallurgy extrusion.

36 MATERIALS SCIENCE↗

Pseudo-Hot-Isostatic Pressing (P-HIP)

Researchers at Los Alamos National Laboratory developed a technology to produce high performance ceramic or metal with a combination of major key properties such as versatile-complicated shape, high density, uniform density distribution, and minimal amounts of starting material. The novel pseudo-hot-isostatic-pressing (P-HIP) uses graphite or boron nitride flakes as the stress transmission media to transmit stress instead of the conventional solid graphite punch. The graphite and boron nitride flakes are solid lubricants and can slide among one another to re-distribute the stress from high stress concentration area to the low stress concentration areas, resulting in a self-stress-relief action. This innovative P-HIP enables the manufacturing of complicated shapes with near-net-shape capability while minimizing the energy used and reducing waste. This is a revolutionary breakthrough to the ceramics and powder metallurgy industries.

36 MATERIALS SCIENCE↗

Development & Validation of Low-Cost, Highly-Durable, Spinel-Based Materials for SOFC Cathode-Side Contact (Final Report)

A cathode-side contact layer is required to provide and maintain stable electrical conduction paths between the interconnect and cathode in a solid oxide fuel cell (SOFC) stack assembly and thus minimize the ohmic resistance and stack power loss. Current cathode-interconnect contact materials are based on noble metals, electrically-conductive perovskites, their composite materials, etc. These materials are either too expensive or do not possess the overall balanced performance required for the cathode-side contact application. To achieve the DOE SOFC system cost and performance stability goals, a new generation of low-cost, high-performance contact materials needs to be developed. In this project, spinel-based materials thermally converted from the Fe-Ni and Co-Mn based alloy precursors were developed and validated for the cathode-side contact application. The precursor alloy compositions were optimized via a combination of composition screening in the (Ni,Fe) 3 O 4 and (Mn,Co) 3 O 4 spinel system, alloy design using physical metallurgy principles, and cost considerations. The alloy powders with the desired composition and particle size were manufactured via gas atomization. The optimal process parameters for thermal conversion of these alloy precursor layers to a spinel-based layer were identified, i.e., 900°C x 2h in air, which is close to the initial stack firing condition. The area-specific resistances (ASRs) of the interconnect/contact/cathode test assemblies with the developed contact layer were determined for various durations (up to 5000 h) under simulated cathodic operation conditions. Some of the alloy-derived spinel contacts exhibited the lowest ASR and ASR degradation rate. The in-stack performance of the most promising alloy-derived contact layer is currently being evaluated via stack testing. To reduce the stack cost, the Co-Mn based alloy powders were utilized as the precursor for synthesis of dense spinel-based interconnect coating. By optimizing both the initial powder size/distribution and the alloy powder composition, a dense (Mn,Co) 3 O 4 -based spinel coating was achieved. Furthermore, co-sintering of the coating/contact dual-layer structure under the initial stack firing condition was realized by utilizing the tailored Co-Mn alloy precursors. Cost analysis of the developed technology indicated a total stack cost reduction of around 10.6% with the implementation of co-sintering of the interconnect coating and the contact layer during initial stack firing. Since low-cost processes such as screen printing is utilized in the precursor application and no reduction heat treatment is needed for the coating formation, the developed technology can be readily implemented at the industrial partner’s manufacturing facilities with no additional capital investment needed.

08 HYDROGEN↗