An investigation of oxidation resistant solid lubricant materials
Wear tests of oxide and fluoride oxidation resistant solid lubricants for use in high temperature gaseous environments
Sliney, H. E.↗
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Assessment of the State of the Art of Ultra High Temperature Ceramics
Ultra High Temperature Ceramics (UHTCs) are a family of materials that includes the borides, carbides and nitrides of hafnium-, zirconium- and titanium-based systems. UHTCs are famous for possessing some of the highest melting points of known materials. In addition, they are very hard, have good wear resistance, mechanical strength, and relatively high thermal conductivities (compared to other ceramic materials). Because of these attributes, UHTCs are ideal for thermal protection systems, especially those that require chemical and structural stability at extremely high operating temperatures. UHTCs have the potential to revolutionize the aerospace industry by enabling the development of sharp hypersonic vehicles or atmospheric entry probes capable of the most extreme entry conditions.
Johnson, Sylvia↗
Ferrographic analysis of wear debris generated in accelerated rolling element fatigue tests
The types and quantities of wear particles generated during accelerated ball rolling contact fatigue tests were determined. Ball specimens were made of AMS 5749, a corrosion resistant, high-temperature bearing steel. The lubricant was a super-refined naphthenic mineral oil. Conditions included a maximum Hertz stress of 5.215 times 10 to the 9th power Pa and a shaft speed of 10,000 rpm. Four types of wear particles were observed; normal rubbing wear particles, fatigue spall particles, spheres, and friction polymer.
Jones, W. R., Jr.↗
A new chromium carbide-based tribological coating for use to 900 deg C with particular reference to the Stirling engine
A new chromium carbide-based coating (PS 200) is described. This coating is shown to have good friction and wear properties over a wide temperature range. A nickel alloy-bonded chromium carbide coating was used as a baseline material for comparison with experimental formulated coatings. Coatings were plasma sprayed onto metal disks, then diamond ground to a thickness of 0.025 cm. Friction and wear were determined using a pin on disk tribometer at temperatures from 25 to 900 C in hydrogen, helium, and air. Pin materials included several metallic alloys and silicon carbide. It was found that appropriate additions of metallic silver and of barium fluoride/calcium fluoride eutectic to the baseline carbide composition significantly reduced friction coefficients while preserving, and in some cases, even enhancing wear resistance. The results of this study demonstrate that PS 200 is a promising coating composition to consider for high temperature aerospace and advanced heat engine applications. The excellent results in hydrogen make this coating of particular interest for use in the Stirling engine.
Sliney, H. E.↗
A new chromium carbide-based tribological coating for use to 900 C with particular reference to the Stirling engine
A new chromium carbide-based coating (PS 200) is described. This coating is shown to have good friction and wear properties over a wide temperature range. A nickel alloy-bonded chromium carbide coating was used as a baseline material for comparison with experimentally formulated coatings. Coatings were plasma sprayed onto metal disks, then diamond ground to a thickness of 0.025 cm. Friction and wear were determined using a pin on disk tribometer at temperatures from 25 to 900 C in hydrogen, helium, and air. Pin materials included several metallic alloys and silicon carbide. It was found that appropriate additions of metallic silver and of barium fluoride/calcium fluoride eutectic to the baseline carbide composition significantly reduced friction coefficients while preserving, and in some cases, even enhancing wear resistance. The results of this study demonstrate that PS 200 is a promising coating composition to consider for high temperature aerospace and advanced heat engine applications. The excellent results in hydrogen make this coating of particular interest for use in the Stirling engine.
Sliney, Harold E.↗
Degradation science: Integrating modeling and experiments to predict localized corrosion processes (Annual Progress Report)
Additively manufactured (AM) eutectic high-entropy alloys (EHEAs), such as nano-lamellar AlCoCrFeNi 2.1 , have excellent strength, ductility, and wear resistance even at elevated temperatures, but their corrosion behavior in aggressive acids at different length scales remain poorly understood. This work investigates the corrosion behavior of laser powder bed–fused (L-PBF) AlCoCrFeNi 2.1 as a function of annealing temperatures, probing degradation mechanisms from nanoscopic to macroscopic length scales. The alloy is dual phase consisting of a ductile FCC L1 2 phase and a high-strength BCC B2 phase. Rapid solidification during L-PBF produces a far-from-equilibrium nano-lamellar structure with nearly homogeneous elemental distribution, which tends to evolve upon annealing toward Cr/Co/Fe-enriched FCC and Al/Ni-enriched B2. Three conditions were studied: as-printed, 600 °C/5 h, and 1000 °C/1 h, over which B2 lamellae coarsen, lamellar spacing increases, and elemental segregation becomes more prominent. Microstructure and chemistry were characterized by scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS), while in-situ electrochemical atomic force microscopy (EC-AFM) was used to link early (<5 h) local dissolution to microstructure after exposure in sulfuric acid. EC-AFM highlights preferential dissolution of the BCC/B2 phase where the surrounding matrix is Cr-depleted and directly quantifies the dissolution rates within individual phases, tracks the transition from early nano-scale attack to partial repassivation, to correlate height differences with current and impedance responses. To monitor longer-term behavior (up to 96 h), ex-situ AFM, SEM, and confocal imaging were combined with conventional bulk electrochemical tests, bridging nanoscale observations to micro/meso-scale damage morphologies. At the meso-scale, the deepest dissolution channels align with the build-direction lamellae and melt-pool boundaries, indicating that printing directionality guides the propagation of these localized corrosion sites. Annealing modifies corrosion by restructuring BCC/FCC phase fractions, lamellar spacing, and Cr/Al segregation, thereby changing the cathode/anode ratio and passive film stability. The results clarify how as-printed and annealed nano-lamellar architectures differ in their susceptibility to selective dissolution; how elemental segregation competes with residual stresses along the build direction. With these insights, future work will use CALPHAD-guided alloy modification to stabilize higher Cr contents in the B2 phase while retaining a dominant FCC+B2/BCC microstructure, with the goal of designing mechanically robust, corrosion-resistant EHEAs for safety-critical applications to leverage the LLNL’s broader national and global security mission.
36 MATERIALS SCIENCE↗
Exceptional strength and wear resistance in an AA7075/TiB 2 composite fabricated via friction consolidation
The friction consolidation method successfully reinforced aluminum 7075 alloy (AA7075) with high-volume fractions (12 and 24 vol%) of titanium diboride (TiB 2 ) by high pressure and severe plastic deformation at elevated temperatures. The consolidated AMCs have a uniform dispersion of submicron- and micron-sized TiB 2 particles in the AA7075 matrix, with significant refinement of the matrix grain size and the particles. The addition of TiB 2 significantly increases hardness by up to 50 %, Young’s modulus by up to 62 %, and ultimate tensile strength by up to 28 % to 672 MPa, while reducing ductility by 80 %. Wear resistance of 7075/24 vol% TiB 2 improves seven-fold compared to baseline, making it comparable to that of carburized steels. Microstructure-based finite element modeling provided a theoretical strength limit of ~730 MPa for the composites and indicated that high triaxiality in conjunction with severe equivalent plastic strain in a narrow area between the TiB 2 particles led to early fracture initiations, limiting the ductility.
36 MATERIALS SCIENCE↗
Characterization of wear debris generated in accelerated rolling-element fatigue tests
A ferrographic analysis was used to determine the types and quantities of wear debris generated during accelerated rolling contact fatigue tests. The five-ball rolling contact fatigue tester was used. Ball specimens were made of a corrosion resistant, high-temperature bearing steel. The lubricant was a superrefined naphthenic mineral oil. Conditions included a maximum Hertz stress of 5.52 10 to the 9th power Pa and a shaft speed of 10,000 rpm. Four types of wear debris were observed: (1) normal rubbing wear particles, (2) fatigue microspall particles, (3) spheres, and (4) friction polymer deposits. The characterization of wear debris as a function of time was of limited use in predicting fatigue failures in these accelerated tests.
Jones, W. R., Jr.↗
Effect of annealing on the tribological behavior of Zr-based bulk metallic glass
Bulk Metallic Glasses (BMGs) are promising materials for several applications owing to their high elastic limit and resistance to permanent deformation. However, BMGs have lower wear resistance than their crystalline counterparts during dry sliding. The formation of a composite material with crystalline phases dispersed in the BMG matrix through devitrification and partial crystallization at elevated temperatures has recently been proposed as an effective way to improve the wear resistance. However, our understanding of the origin of the improved wear behavior of annealed BMGs is still elusive. Here, a systematic evaluation of the effect of annealing temperature (from temperatures lower than the BMG glass transition temperature to temperatures higher than the BMG recrystallization temperature) on the friction and wear response of a Zr-based BMG, namely Vit105 (Zr 52.5 Cu 17.9 Ni 14.6 Al 10 Ti 5 ), was performed. The results indicate that annealing Vit105 improves its wear resistance while also reducing the steady-state friction response when the annealing temperature is close to the glass transition temperature. Notably, the formation of a transfer film on the sapphire countersurface is highly dependent on the applied normal load and sliding time. Finally, the wear mechanism was found to be strongly dependent on the annealing temperature as a transition from a predominantly adhesive wear mechanism to an abrasive-dominated one was observed as the annealing temperature crossed the glass transition temperature. Altogether, the results of this work aid to our understanding of the tribological behavior of Zr-based BMGs in general, while also providing clues to strategies for the effective use of BMGs in tribological applications.
Lien, Hsu-Ming [Univ. of Texas, Austin, TX (United↗
Ferrographic analysis of wear debris generated in accelerated rolling element fatigue tests
Ferrographic analysis was used to determine the types and quantities of wear particles generated during accelerated rolling contact fatigue tests. The NASA five-ball rolling contact fatigue tester was used. Ball specimens were made of AMS 5749, a corrosion-resistant high-temperature bearing steel. The lubricant was a super-refined naphthenic mineral oil. Conditions included a maximum Hertz stress of 5.52 billion Pa and a shaft speed of 10,000 rpm. Four types of wear particles were observed: normal rubbing wear particles, fatigue spall particles, spheres, and friction polymer.
Jones, W. R., Jr.↗
Boride-Carbon Hybrid Technology to Produce Ultra-Wear and Corrosion Resistant Surfaces for Applications in Harsh Conditions (Final Technical Report)
Engineered functional surfaces play an important role to enable new products and manufacturing processes that can endure harsh service conditions such as high impact and contact loads, highly abrasive wear, extreme temperatures, and corrosive environments. Engineered surfaces can also be instrumental to improving the efficient use of energy by reducing frictional losses and extending service life. The main objective of this project was to develop a hybrid surface engineering technology that combines the advantages of a novel ultrafast boriding process with the next generation of superhard carbon coatings. The hypothesis was that this hybrid process will offer an unprecedented combination of wear and corrosion resistance, low frictional losses and affordability for treated parts so that it can be utilized in many applications. During this project, a duplex process was developed that combines the advantages of ultra-fast electrochemical boriding with those of hard tetrahedral amorphous carbon coatings. Both technologies can be combined to form a hybrid technology that is characterized by low friction and wear properties combined with corrosion and fatigue resistance. Good adhesion of both layers to each other was one main goal of this project, that has been achieved with HF1 adhesion through the Rockwell-C adhesion test. In this project, the mechanical properties of the hybrid coating were modeled through a finite-element analysis approach. We can conclude that the FEA model resembles the actual samples and be utilized to predict mechanical behavior under impacts. Based on this model, application-oriented load conditions can be simulated for optimal layer design regarding thickness and mechanical properties. To exemplify, one conclusion that can be drawn from the nanoindentation model is a boride layer thickness of 50 µm is sufficient to effectively support the carbon coating on the identified AISI 1045 low carbon steel substrate material. The duplex treatment yields wear rates as low as 6 x 10 -8 mm 3 N -1 m -1 and a coefficient of friction of 0.14 when tested against a steel counter face in a ball-on-disk test setup. On the other hand, the wear rate of the only-borided AISI 1045 steel was 5 x 10 -5 mm 3 N -1 m -1 , about three orders of magnitude higher than the duplex coating. At the same time, duplex treated samples experience corrosion resistance, which could not be achieved with single-layer carbon coatings. The developed surface treatment withstands a 3-hour exposure to 15% HCl, while the only carbon coated counter sample shows severe delamination of the coating due to pin hole corrosion. The boride layer is chemically stable and pin hole free because it is formed through an electrochemical process under high current densities (700 mA/cm 2 ) and high temperature. Additionally, the hybrid coating led to at least 3x increase in fatigue strength of the steel substrate, which exceeds the target performance of 30% improvement. There are numerous potential applications for the duplex coatings. A representative application is bearing ball coatings for off-shore windmills. Compared to currently employed surface technologies in this field, the initial costs of applying our technology might be higher due to more process steps but the performance benefits lead to an increased life time of treated parts, which will lower the maintenance and replacement costs in the long-term. To validate the technology for this specific application, the team is currently investigating the process of white etching crack initiation of the duplex coating in collaboration with ANL. Overall, this project successfully validated that the boride-carbon hybrid technology can withstand harsh conditions. One possible approach to commercialization under consideration is to transfer the technology to a startup or an existing coatings company.
36 MATERIALS SCIENCE↗
Characterization of Rhenium Oxides Using ESCA
Rhenium as an engineering material has the following properties: (1) high melting point (one of the refractory metals); (2) high strength at elevated temperatures; (3) excellent toughness at room temperature; (4) low vapor pressure at melting point; (5) low coefficient of thermal expansion; (6) high impact and wear resistance; (7) compatibility with elements such as carbon and platinum; (8) conservation of properties in the presence of hydrogen, water vapor, and nitrogen oxides; and (9) poor oxidation resistance. This viewgraph presentation gives an overview of rhenium oxide characterization, including details on its history, experimental procedure using ESCA, and the analysis of the oxides (spectra and effects of ion sputtering).
Panda, Binayak↗
Application of hard coatings to substrates at low temperatures
BIRL, the industrial research laboratory of Northwestern University, has conducted unique and innovative research, under sponsorship from the NASA Marshall Space Flight Center (MSFC), in the application of hard, wear resistant coatings to bearing steels using the high-rate reactive sputtering (HRRS) process that was pioneered by Dr. William Sproul, the principal investigator on this program. Prior to this program, Dr. Sproul had demonstrated that it is possible to apply hard coatings such as titanium nitride (TiN) to alloy steels at low temperatures via the HRRS process without changing the metallurgical properties of the steel. The NASA MSFC program at BIRL had the specific objectives to: apply TiN to 440C stainless steel without changing the metallurgical properties of the steel; prepare rolling contact fatigue (RCF) test samples coated with binary hard coatings of TiN, zirconium nitride (ZrN), hafnium nitride (HfN), chromium nitride (CrN), and molybdenum nitride (MoN), and metal coatings of copper (Cu) and gold (Au); and develop new alloyed hard coatings of titanium aluminum nitride (Ti(0.5)Al(0.5)N), titanium zirconium nitride (Ti(0.5)Zr(0.5)N), and titanium aluminum vanadium nitride.
Sproul, William D.↗
High Kinetic Energy Penetrator Shielding and High Wear Resistance Materials Fabricated with Boron Nitride Nanotubes (BNNTS) and BNNT Polymer Composites
Boron nitride nanotubes (BNNTs), boron nitride nanoparticles (BNNPs), carbon nanotubes (CNTs), graphites, or combinations, are incorporated into matrices of polymer, ceramic or metals. Fibers, yarns, and woven or nonwoven mats of BNNTs are used as toughening layers in penetration resistant materials to maximize energy absorption and/or high hardness layers to rebound or deform penetrators. They can be also used as reinforcing inclusions combining with other polymer matrices to create composite layers like typical reinforcing fibers such as Kevlar.RTM., Spectra.RTM., ceramics and metals. Enhanced wear resistance and usage time are achieved by adding boron nitride nanomaterials, increasing hardness and toughness. Such materials can be used in high temperature environments since the oxidation temperature of BNNTs exceeds 800.degree. C. in air. Boron nitride based composites are useful as strong structural materials for anti-micrometeorite layers for spacecraft and space suits, ultra strong tethers, protective gear, vehicles, helmets, shields and safety suits/helmets for industry.
Kang, Jin Ho↗
Advanced Coating Compositions and Microstructures to Improve Uptime and Operational Flexibility in Cyclic, Low-Load Thermal Utility Plants
GE, the University of Tennessee, and Oak Ridge National Laboratory collaborated from 2020 to 2023 developing two key technologies for improving the viability of fuel switching and load following in thermal utility plants: a) cost-effective weld overlay compositions for boiler tubing b) cathodic arc coatings that deliver improvements in both erosion resistance and oxidation resistance in high temperature steam for HP turbine blades The team worked through a robust, logical project map to de-risk these two technologies and advance them from TRL 3 to TRL 6. For the cost-effective weld overlay, the team developed a ferritic filler material which was fabricated at a vendor for 18% the average market cost of Inconel 625 wire, had a corrosion rate 3x lower in conditions simulating a biomass-fired superheater and 10x lower in conditions simulating a coal-fired superheater, and was fabricated into prototype overlaid tubing that passed ASME requirements including transverse bending, dye penetrant inspection, and ASTM G-76 evaluation. For the cathodic arc coatings applied to steam turbine blades, the team developed a novel composition that was successfully transferred to a qualified vendor. The vendor was able to produce coated prototypes with 4x the as-deposited erosion resistance and 10.4x the post-steam-exposure erosion resistance of the TiN coating the vendor currently applies on GE steam turbine components, without significantly increasing process cost. These coated prototypes also passed a GE inspection and showed favorable performance in high temperature erosion, nanoindentation, sliding wear, scratch adhesion, and high cycle fatigue testing. If successfully deployed by GE, it is anticipated that the technologies will enable the following: • 25%-50% increase in time between outages for both boilers and HP turbines. • 50% decrease in cost for weld overlay on a per foot basis relative to todays NiCr alloys. • Adequate oxidation resistance and erosion for HP turbine inlet steam at >620°C and >220 bar. • No need for changes in component supply chain or any notable Capital Expenditures. 5 Decreasing component cost, increasing performance, and extending time between outages represent direct value propositions to GE and their customers. For the American consumer, these objectives translate into increased grid reliability (fewer unexpected outages), decreased Levelized Cost of Electricity, and improved environmental health (low-loading/load following to accelerate penetration of renewables). The results also have implications for wear resistant tooling, wire arc additive manufacturing, more durable components for syngas cleanup, and deployment of more efficient thermochemical pathways for carbon negative fuel production
09 BIOMASS FUELS↗
Low Cost Al-Si Casting Alloy As In-Situ Composite for High Temperature Applications
A new aluminum-silicon (Al-Si) alloy has been successfully developed at NASA- Marshall Space Flight Center (MSFC) that has significant improvement in tensile and fatigue strength at elevated temperatures (500 F-700 F). The alloy offers a number of benefits such as light weight, high hardness, low thermal expansion and high surface wear resistance. In hypereutectic form, this alloy is considered as an in-situ Al-Si composite with tensile strength of about 90% higher than the auto industry 390 alloy at 600 F. This composite is very economically produced by using either conventional permanent steel molds or die casting. The projected material cost is less than $0.90 per pound, and automotive components such as pistons can be cast for high production rate using conventional casting techniques with a low and fully accounted cost. Key Words: Metal matrix composites, In-situ composite, aluminum-silicon alloy, hypereutectic alloy, permanent mold casting, die casting.
Lee, Jonathan A.↗
Improved Mo-Re VPS Alloys for High-Temperature Uses
Dispersion-strengthened molybdenum- rhenium alloys for vacuum plasma spraying (VPS) fabrication of high-temperature-resistant components are undergoing development. In comparison with otherwise equivalent non-dispersion-strengthened Mo-Re alloys, these alloys have improved high-temperature properties. Examples of VPS-fabricated high-temperature-resistant components for which these alloys are expected to be suitable include parts of aircraft and spacecraft engines, furnaces, and nuclear power plants; wear coatings; sputtering targets; x-ray targets; heat pipes in which liquid metals are used as working fluids; and heat exchangers in general. These alloys could also be useful as coating materials in some biomedical applications. The alloys consist of 60 weight percent Mo with 40 weight percent Re made from (1) blends of elemental Mo and Re powders or (2) Re-coated Mo particles that have been subjected to a proprietary powder-alloying-and-spheroidization process. For most of the dispersion- strengthening experiments performed thus far in this development effort, 0.4 volume percent of transition-metal ceramic dispersoids were mixed into the feedstock powders. For one experiment, the proportion of dispersoid was 1 volume percent. In each case, the dispersoid consisted of either ZrN particles having sizes <45 m, ZrO2 particles having sizes of about 1 m, HfO2 particles having sizes <45 m, or HfN particles having sizes <1 m. These materials were chosen for evaluation on the basis of previously published thermodynamic stability data. For comparison, Mo-Re feedstock powders without dispersoids were also prepared.
Hickman, Robert↗
An investigation of oxidation-resistant solid lubricant materials.
Recent research at NASA-Lewis on solid lubricants for use at high temperatures in air and other gaseous environments is presented. The characteristics of oxide and fluoride lubricants at temperatures to 1700 F are described. Data is presented for fluoride coatings with silicate and other additives incorporated to give improved wear life and better oxidation protection to the substrate metal. Experience is described for fluoride-metal self-lubricating composites with improved metal oxidation resistance to 1700 F. The concept of cast, self-lubricating ceramics is also explored.
Sliney, H. E.↗