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At least 181 records · Page 10

Improving the damage tolerance of Si 3 N 4 by forming laminate composites with refractory metals

The objective of this research was to demonstrate that the damage tolerance of Si 3 N 4 could be significantly improved by forming laminate composites with refractory metals, providing materials that undergo graceful failure, rather than the fast-fracture mechanism exhibited by monolithic Si 3 N 4 . A damage tolerant Si 3 N 4 could be used as a ring material in an all-ceramic bearing, decreasing the chance for catastrophic failure if the ring is stressed in tension during operation. The technical approach formed a laminate composite material using alternating Si 3 N 4 -metallic layers, with both outer layers being Si 3 N 4 to take advantage of its greater wear resistance, chemical stability, and thermal stability. The metallic layers are designed to arrest any cracks in the outer layers, thus producing a toughened Si 3 N 4 and avoiding the catastrophic failure behavior exhibited by monolithic ceramics. The laminate composites were fabricated using a combination of tape-casting Si 3 N 4 and metals from slurries, as well as metal foils, followed by hot pressing at 1500°C. The metallic materials employed were chromium, titanium, and tantalum. Analysis confirmed that the interfaces were well formed, and the laminates with chromium and titanium formed intermetallic compounds more readily than the composites with tantalum. The Si 3 N 4 -Ta laminates demonstrated crack deflection and bridging behavior during failure and flexural strength of 800–900 MPa. The hardness and elastic modulus of Si 3 N 4 -Ta laminates measured by nanoindentation were similar to those reported in literature. The hardness across the interface of the Si 3 N 4 -Ta composite varied according to the composition of the interface, which displayed a profile indicative of a diffusion bond.

36 MATERIALS SCIENCE↗

Atmospheric Cold Plasma Jet Coating and Surface Treatment for Improved Adhesive Bonding Performance of Dissimilar Material Joints Subject to Harsh Environmental Exposure

The program goal was the development and demonstration of a novel material coating system using an innovative atmospheric cold microwave plasma jet to enable surface functionalization for corrosion protection, wear resistance and improved bonding strength. The technical approach was directed towards proof-of-concept demonstration of advanced point-of-manufacturing material bonding to improve adhesive joint performance subject to harsh environmental exposure. The assembled team, consisting of the researchers at the University of Illinois, end-users at General Motors and small business manufacturer Starfire Industries, successfully demonstrated a single, cost-effective, high-volume production process that meets the requirements of multi-material combinations relevant to the energy-intensive transportation industry (e.g. Al-steel, Mg-steel, Al-Mg and Al-CFRP joints for body-in-white structures) while eliminating offline pretreatment for Al and Mg alloy substrates that are energy intensive, have chemical waste disposal issues, and add cost. Technical demonstration of dissimilar material joining while maintaining bonding strength and cohesion after long-duration environmental exposure was accomplished for all materials of interest. This novel approach has broad applicability for manufacturing in automotive, aerospace, marine, railcar, and specialty consumer goods, etc.

36 MATERIALS SCIENCE↗

Laboratory-Scale Coal-Derived Graphene Process (Final Report)

The Energy & Environmental Research Center (EERC) conducted a laboratory-scale coal-derived graphene (CDG) project focused on developing a technological process for making graphene from four U.S. domestic coal or coal wastes, including lignite from North Dakota, subbituminous coal from Wyoming, bituminous coal from Utah, and anthracite from Pennsylvania. The project was divided into two performance or budget periods (BPs), with BP1 comprising the up-front laboratory experiments to make graphene materials from coal beginning on May 1, 2020, to April 30, 2022. BP2 was conducted from May 1, 2022, to April 30, 2023, and was focused on analyzing the CDG process economic feasibility and the technical gaps for technological scale-up and commercialization. During this project, a few different coal-derived high-value products have been demonstrated, including graphite, graphene oxide (GO), reduced graphene oxide (rGO), and graphene quantum dots (GQDs). A new graphite microstructure was discovered and named “croissant graphite” because of the exterior morphological and textural resemblance to croissant food items sold in commercial groceries stores. The new graphite structure and the associated preparation from coal or coal waste feedstocks has been the subject of a U.S. patent application. The systematic experimental processes involving coal cleaning, upgrading, and conversion to high-value carbon products culminated into a developed upgraded coal-to-products (UCP) technology that is being pursued for potential fast-track commercialization, if funding is available. It is envisioned that commercialization of the UCP technology would increase consumption of U.S. domestic coals or coal wastes to make environmentally sustainable high-value products for the electronics industry, high-energy-storage applications, and clean energy technologies such as electric vehicle (EV) lithium-ion batteries (LIBs), for which graphite has become a critical mineral commodity. Croissant graphite microstructures, when observed by field emission scanning electron microscopy (FESEM), display wavy surface morphology and often grow from a base that is made of graphitized particles with honeycomb-like layers, which are believed to be graphene layers. While more studies are needed to fully ascertain the mechanisms of the croissant graphite microstructure formation, it is postulated that their growth may begin from curling of the graphene sheets into ribbon-like structures, and continuous growth and densification of the ribbon-like structures forms croissant microstructures. Additional studies are ongoing to evaluate the electrochemical performance of croissant graphite for LIB applications and to determine the experimental conditions necessary to tune on/off croissant formation so that it can be either optimized or suppressed depending on performance evaluation results. In addition to the discovery of croissant graphite, the graphitization process from the four coal ranks in general was successful. X-ray diffraction (XRD) analysis showed that the degree of graphitization (DoG) ranged from 12% to 80% in an early sample set, and further optimization on lignite coal produces a DoG of about 92%, which was spectacular to see as lignite is the lowest-rank coal. Thus, it is expected that the graphitization performance for higher-rank coals will be similar or better when optimized as well. The coal-derived graphite was used to make GO and rGO. Analytical characterization, e.g., by methods such as Raman spectroscopy, XRD, Fourier transform infrared (FTIR) spectroscopy and FESEM, showed that the sequence of converting the coal to graphite, exfoliating it to GO, and then chemically reducing the GO to rGO was successful. Although coal naturally contains aromatic compounds and some relatively small-sized condensed aromatic units, it does not contain graphene sheets. In the UCP process, the aromatic domains in the coals, particularly low-rank coals, are concentrated and condensed further into graphene sheets, which are ordered into a 3D stack during graphitization. The synthesized graphite is then unpacked by methods such as exfoliation to various graphene products. GQDs were synthesized from all four coal types, and their optical properties were demonstrated to be tunable by the coal precursor preprocessing treatments. In all four coal types, enhanced optical properties were observed for the produced GDQs with incremental improvements made to the coal precursors. GQDs produced from raw coal samples displayed lower ultraviolet–visible (UV–Vis) spectroscopy absorbance intensity compared to those obtained from cleaned and upgraded coal residues. The photoluminescence (PL) intensities also varied with pretreatment conditions and with the concentration of GQDs in aqueous solutions. GQDs obtained from anthracite show longer emission wavelengths and can be excited by visible light as opposed to GQDs derived from the other coal ranks. UV fluorescence 3D maps and spectra revealed that the emission wavelength at which the GQDs solutions display the highest intensity was slightly redshifted based on the coal precursor pretreatments. In low-rank coal (lignite and subbituminous) samples, two clusters were observed in the maps for GQDs, which may suggest that there are potentially two types of fluorophores in solution or two main size populations. The ability to tune the properties of GQDs based on processing methods can be exploited to make GQDs for various optical display or optoelectronics applications. The results also highlight the importance of removing coal-borne impurities to improve the quality of the coal precursor for preparation of graphene products. Coal and/or coal wastes preprocessing methods were developed and applied to clean and upgrade the coal precursors prior to graphitization and subsequent conversion to graphene products. The preprocessing methods involve high specific-gravity separations, mineral acid cleaning (no hydrofluoric acid), and subsequent upgrading by reducing the coal-borne heteroatom (nitrogen, sulfur, and oxygen) content using proprietary chemical agents. Analytical characterization revealed that the preprocessing steps were successful, with ash reductions that range from 38% to 80% and residual ash content that was below the 5 wt% initial target. Based on proximate and ultimate analysis, the heteroatom reduction reactions produced upgraded coal residues with the oxygen content reduced by 8% to 24%, with additional reductions in the nitrogen and sulfur contents. An initial assessment of the waste streams from the UCP process shows very small to negligible environmental impact due to CO 2 , NO x , and SO x because most process steps are performed under inert atmosphere with argon. Consequently, reactive oxygen environments that tend to create these species are avoided. The inorganic and potentially hazardous species are released into aqueous waste streams that are easy to handle for proper disposal. The liquid waste streams were found to contain low-level concentrations of rare-earth elements (REEs), which could be concentrated and recovered as value-added by-products. Additionally, the volatile and gaseous fractions from carbonization and heat treatment contain useful organic compounds that can also be recovered as potential valuable by-products. Thus, the UCP technology is considered an environmentally sustainable and promising emerging technology for making high-value products from coal and coal wastes, with potential additional value-added by-products. Analysis of potential markets for the coal-derived carbon products shows a strong demand in both niche market sectors and across a wide variety of other industrial sectors. Graphite is currently considered a critical mineral commodity that has a large and growing demand in the LIB industry for EV applications. Based on data from Fortune Business Insights (2022) and Marketwatch (2023) reports, the average global graphite market is projected to reach about 33 billion by 2028, growing at a compound annual growth rate (CAGR) of about 7%, with much of this growth expected to be in the LIB industry. GO and rGO have strong market potentials in various application areas, such as coatings for anticorrosion, anti-icing, and antimicrobial protection, thermal barriers, wear resistance, sensors, additive manufacturing such as 3D inks, and others. GQDs are the emerging key player in the bioimaging, photovoltaics, and light-emitting diodes (LEDs) applications, with the potential to replace traditional semiconductor quantum dots (SQDs), which are based on metallic systems that are more toxic and more expensive. Biomedical applications of GQDs are becoming more attractive because of low to no toxicity and extremely low cost compared to SQDs. The major challenges for scale-up and commercialization of coal-derived carbon products such as graphene vary from the inherent attributes of graphene itself to reluctance to accept graphene in new manufacturing processes because of the uncertainty of the unknown. The 2D nature of graphene materials with a thickness of one atom presents significant challenges to proper handling/processing, and process scale-up becomes difficult because it requires high-end, expensive equipment, even for routine handling and analysis for quality assurance and control. Pristine graphene can also be extremely difficult to work into other matrices, thus hindering downstream processibility, especially at large scale. Currently, the cost of graphene and graphene products is still high and presents an economic risk that tends to slow down investment in scaling up emerging technologies. The lack of a standard for graphene materials for quality assurance and quality control poses a great challenge not only for the markets but also for commercialization efforts. A first-look economic feasibility analysis of the UCP technology provided valuable information that suggests the UCP process would be feasible, especially when it is scaled to a pilot scale and could be more competitive at the full scale. Graphitization was found to be the most energy-consuming and most capital-intensive step in the overall process. In small laboratory- and bench-scale experiments, labor is a significant contributor to the total process costs. Although these energy, capital, and labor constraints contribute to a higher selling price for the product, a preliminary economic model suggests that the process would be feasible at large scale when the process is fully integrated, optimized, and automated.

01 COAL, LIGNITE, AND PEAT↗

Quality Control Metrics to Assess MoS 2 Sputtered Films for Tribological Applications [Slides]

Easily measured metrics that could assign quantifiable values to coating batches for quality control have started to be developed. High-density is an attribute of quality films. Increased density results in harder, more wear resistant coatings in inert and humid environments. Denser films are more resistant to oxidation from aging, limiting the severity and depth of oxide into the coating. Future work includes using metrics for quality. The next step is to develop in house deposition capabilities to develop process-structure relationships.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Development of Surface Treatment Solutions for Stamping Tools Fabricated via Additive Manufacturing

Oak Ridge National Laboratory (ORNL) and H.E.F. USA, Inc. (HEF) partnered to develop wear resistant surface treatment of additive manufactured steels for stamping die applications under CRADA agreement NFE-19-07909. This project aimed at evaluating the ARCOR® process, developed by HEF, to improve the surface behavior of 410SS (stainless steel), 410NiMo SS, 630 SS, and Maraging 250 steel coupons and demo components, fabricated via wire arc additive manufacturing (WAAM), with and without post print heat treatment. The peak hardness achieved was ~1000 HV and above (Up to 1300 HV) for all materials under proper processing parameters, and far exceeded the target hardness of 746 HV (60 HRC). Finally, stamping tools were printed and nitrocarburized with the optimum parameters, and then went through 500 fabrication cycles. Characterization of the used 17-4PH stamping tool discovered no crack or delamination in the nitrocarburized layer and the interface between the nitrocarburized layer and substrate.

36 MATERIALS SCIENCE↗

H2 Materials Compatibility of Low Cost, High Pressure, Polymer H2 Dispensing Hoses

NanoSonic was recently awarded a DOE Phase IIB SBIR program for the commercialization of an innovative metal-free polymer based H2 dispensing hose to make H2 an economically viable fuel alternative to gasoline. During the Phase I and Phase II base programs, NanoSonic's H2 hose demonstrated ultra-high hydrostatic burst strength values > 31,000 psi where failure occurred due to fitting slippage, rather than hose burst. Additionally, our hoses survived > 51,000 pressure impulse cycles at 12,000 psi over a thermal cycle of -40 °C to 85 °C. These hoses also failed due to fitting slippage. Thus, our Phase IIB program is centralized on the addition of a new fitting, polymer hose refinement, and validation of a complete hose and fitting system certified for use with H2. While NanoSonic has partnered with the National Renewable Energy Laboratory (NREL) to test our hose on their robotic H2 dispensing system, we are also seeking durability with the H2 environment at the molecular level. Here, NanoSonic proposes a CRADA with Pacific Northwest National Laboratory (PNNL), who has expertise in H2 polymer materials compatibility. Together, we will determine the lifetime of our H2 hose polymer and composite constituents via: 1) time-temperature superposition (TTS) studies via dynamic mechanical analysis (DMA) under H2, 2) friction and wear resistance under in situ H2 tribometry, and 3) multi-axis strain testing under cryogenic conditions. PNNL has the unique test equipment essential to gain this type of insight and lifetime prediction data. Importantly, the work conducted under the proposed CRADA will increase the safety and reliability of our H2 hoses while expanding the market for use of our low H2 permeation polymers and durable cryogenic composites to realize the H2@Scale objectives to reduce the cost of H2.

08 HYDROGEN↗

High-density SSiC 3D-printed Lattices for Compact HTHP Aero-engine Recuperators

The proposed project utilizes advanced ceramic-based 3D-printing technology to develop light, low-cost, ultra-compact, high-temperature high-pressure (HTHP) heat exchangers (HX) for the harsh oxidizing environment of aircraft gas-turbine engines. Typical 3D printing technologies (powder bed or lithographic techniques) cannot produce large high-density, monolithic ceramic material with intricate internal features and channels required for high-temperature, high-pressure recuperators. Furthermore, typical 3D printing technologies are not yet economical for large high-density components. A high-density material is required for hermeticity, high-temperature strength, and oxidation, corrosion, and wear resistance. The team has invented an extrusion-based additive manufacturing technology (referred to as robocasting) and developed processing techniques to tailor composition and rheological mix properties for rapid 3D printing of high-density alumina and SiC parts. The goal of the proposed project is to use robocasting technology to demonstrate commercializable high-density 3D-printed ceramic HX modules with high durability and quality, thereby reducing the risk of thermo-mechanical failure under extreme environments. In addition, the proposed project improves the quality of the ceramic 3D-printing process over a large printed area and HTHP operating conditions. Ceramic 3D printing technology also provides a means to create advanced topologies that are unobtainable with conventional manufacturing.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

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↗

Graphene oxide gluing layer enabling macroscale tribology applications of pristine graphene

In recent studies of two-dimensional (2D) nanomaterial-based solid lubricants, the importance of durability has been emerging for real engineering-scale applications. To achieve this, a transfer layer formation is essential to prevent the wear of the mechanical systems. However, it has been challenging for pristine graphene (PG) to induce a material transfer due to chemical inertness. In this study, we suggest an easy-to-process strategy to promote the huge material transfer of the PG onto the counterpart contacting material. We utilized graphene oxide (GO) as a gluing layer between the PG film and the counterpart contact surface to realize the superior tribological performance. The high interaction energy of the GO from its functional groups makes a contribution to the material transfer of PG, which is unveiled by a systematic analysis of the counterpart contact surface and the wear track. The huge solid transfer layer not only makes a wear-resistant contact interface between the transfer layer and the underlying film by densification and oxidation, but also reduces surface interaction energies, finally resulting in a significant improvement in durability.

graphene oxide (GO)↗

Peening Techniques for Surface Modification: Processes, Properties, and Applications

Surface modification methods have been applied to metals and alloys to change the surface integrity, obtain superior mechanical properties, and improve service life irrespective of the field of application. In this review paper, current state-of-the-art of peening techniques are demonstrated. More specifically, classical and advanced shot peening (SP), ultrasonic impact peening (UIP), and laser shock peening (LSP) have been discussed. The effect of these techniques on mechanical properties, such as hardness, wear resistance, fatigue life, surface roughness, and corrosion resistance of various metals and alloys, are discussed. This study also reports the comparisons, advantages, challenges, and potential applications of these processes.

microstructure↗

Structural, Optical and Mechanical Properties of Nanocrystalline Molybdenum Thin Films Deposited under Variable Substrate Temperature

Molybdenum (Mo), which is one among the refractory metals, is a promising material with a wide variety of technological applications in microelectronics, optoelectronics, and energy conversion and storage. However, understanding the structure–property correlation and optimization at the nanoscale dimension is quite important to meet the requirements of the emerging nanoelectronics and nanophotonics. In this context, we focused our efforts to derive a comprehensive understanding of the nanoscale structure, phase, and electronic properties of nanocrystalline Mo films with variable microstructure and grain size. Molybdenum films were deposited under varying temperature (25–500 °C), which resulted in Mo films with variable grain size of 9–22 nm. The grazing incidence X-ray diffraction analyses indicate the (110) preferred growth behavior the Mo films, though there is a marked decrease in hardness and elastic modulus values. In particular, there is a sizable difference in maximum and minimum elastic modulus values; the elastic modulus decreased from ~460 to 260–280 GPa with increasing substrate temperature from 25–500 °C. The plasticity index and wear resistance index values show a dramatic change with substrate temperature and grain size. Additionally, the optical properties of the nanocrystalline Mo films evaluated by spectroscopic ellipsometry indicate a marked dependence on the growth temperature and grain size. This dependence on grain size variation was particularly notable for the refractive index where Mo films with lower grain size fell in a range between ~2.75–3.75 across the measured wavelength as opposed to the range of 1.5–2.5 for samples deposited at temperatures of 400–500 °C, where the grain size is relatively higher. The conductive atomic force microscopy (AFM) studies indicate a direct correlation with grain size variation and grain versus grain boundary conduction; the trend noted was improved electrical conductivity of the Mo films in correlation with increasing grain size. The combined ellipsometry and conductive AFM studies allowed us to optimize the structure–property correlation in nanocrystalline Mo films for application in electronics and optoelectronics.

36 MATERIALS SCIENCE↗

Carbide Nanoparticle Dispersion Techniques for Metal Powder Metallurgy

Nanoparticles (NP) embedded into a matrix material have been shown to improve mechanical properties such as strength, hardness, and wear-resistance. However, the tendency of NPs to agglomerate in the powder mixing process is a major concern. This study investigates five different mechanochemical processing (MCP) routes to mitigate agglomeration to achieve a uniform dispersion of ZrC NPs in an Fe-based metal matrix composite. Our results suggest that MCP with only process controlling agents is ineffective in avoiding aggregation of these NPs. Instead, the uniformity of the carbide NP dispersion is achieved by pre-dispersing the NPs under ultrasonication using suitable surfactants followed by mechanically mixing of the NPs with iron powders in an alcohol solvent which is then dried. High-energy MCP is then used to embed the NPs within the powders. These collective steps resulted in a uniform dispersion of ZrC in the sintered (consolidated) Fe sample.

08 HYDROGEN↗

Valve seat pores sealed with thermosetting monomer

Hard anodic coating provides a smooth wear resistant value seating surface on a cast aluminum alloy valve body. Vacuum impregnation with a thermosetting monomer, diallyl phthalate, seals the pores on the coating to prevent galvanic corrosion.

Olmore, A. B.↗

Status of reusable surface insulation thermal protection system technology programs

The development of three low-density rigidized insulation materials for the shuttle TPS application is reported. These materials consist of one high purity silica system and two systems based on mullite, an aluminum silicate. Both systems consist of fibers joined together with appropriate binders to obtain a rigidized insulation composite. Both material systems require the application of a glassy coating to provide a wear resistant, high emittance surface and to prevent the absorption of water by the fiber matrix. The technology program has addressed the development of water impervious coatings, methods of assembling the materials in design concepts while minimizing the thermal stress in the insulation, achieving compatibility between the RSI material and the structural system, and test evaluations to demonstrate the feasibility of the surface insulation concept.

Greenshields, D. H.↗

Performance of 40-millimeter-bore ball bearings with lead- and lead-alloy-plated retainers in liquid hydrogen at 1.2 million DN

Forty-millimeter-bore ball bearings with lead- and lead-alloy-coated retainers were operated in liquid hydrogen at 30,000 rpm under a thrust load of 1780 N (400 lb.) Four different substrate materials were used for the retainer. Longer bearing run times were achieved with a lead-tin-copper alloy coating plated onto a leaded-bronze material (22.5 hr) and an aluminum-bronze alloy (19.3 hr). One bearing with a pure lead coating achieved the desired objective of 10 hr. This bearing had an aluminum - bronze substrate retainer and ran successfully for 12.4 hr. Additions of antimony to the lead provided an alloy coating with better wear resistance than pure lead; however, this coating was abrasive to the outer-race lands.

Brewe, D. E.↗

Seals

Seal configurations generally found in fluid systems are given. Special attention is given to material selection and the process for achieving a seal. Seal material characteristics including wear resistance, creep, and cold flow properties are discussed.

Source record↗

Microstructural and wear properties of sputtered carbides and silicides

Sputtered Cr3C2, Cr3Si2, and MoSi2 wear-resistant films (0.05 to 3.5 microns thick) were deposited on metal and glass surfaces. Electron transmission, electron diffraction, and scanning electron microscopy were used to determine the microstructural appearance. Strong adherence was obtained with these sputtered films. Internal stresses and defect crystallographic growth structures of various configurations within the film have progressively more undesirable effects for film thicknesses greater than 1.5 microns. Sliding contact and rolling element bearing tests were performed with these sputtered films. Bearings sputtered with a duplex coating (0.1-micron-thick undercoating of Cr3Si2 and subsequently 0.6-micron coating of MoS2) produced marked improvement over straight MoS2 films.

Spalvins, T.↗