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DOE OSTI2022

A Molten Salt Electrochemical Process for the Preparation of Cost-Effective p-Block (Coating) Materials

Solar energy applications rely heavily on p-block elements and transition metals. Silicon is, by far, the most commonly used material in photovoltaic cells and accounts for about 85% of modules sold presently. Of late, thin film photovoltaic cells have gained momentum because of their higher efficiencies. Most of these thin film devices are made out of just five elements, namely, cadmium, tellurium, selenium, indium, gallium and copper. The present manuscript describes an elegant and inexpensive molten salt-based electrolytic process for fabricating a tellurium-coated metallic substrate. A three-electrode set up was employed to coat iridium with tellurium from a molten bath containing lithium chloride, lithium oxide and tellurium tetrachloride (LiCl-Li 2 O-TeCl 4 ) at 650 °C for a duration ranging from 30 to 120 min under a galvanostatic mode. The tellurium coating was observed to be thick, uniform, smooth and homogeneous. Additionally, the deposited tellurium did not chemically react with the iridium substrate to form intermetallic compounds, which is a good feature from the standpoint of the device’s performance characteristics. The present process, being generic in nature, shows the potential for the manufacture of both the coated substates and high-purity elements not just for tellurium but also for other p-block elements.

36 MATERIALS SCIENCE↗

NASA NTRS2001

Inherent and Apparent Scattering Properties of Coated or Uncoated Spheres Embedded in an Absorbing Host Medium

The conventional Lorenz-Mie formalism is extended to the scattering process associated with a coated sphere embedded in an absorbing medium. It is shown that apparent and inherent scattering cross sections of a scattering particle, which are identical in the case of transparent host medium, are different if the host medium is absorptive. Here the inherent single-scattering properties are derived from the near-field information whereas the corresponding apparent counterparts are derived from the far-field asymptotic form of the scattered wave with scaling of host absorption that is assumed to be in an exponential form. The formality extinction and scattering efficiencies defined in the same manner as in the conventional sense can be unbounded. For a nonabsorptive particle embedded in an absorbing medium, the effect of host absorption on the phase matrix elements associated with polarization is significant. This effect, however, is largely reduced for strongly absorptive particles such as soot. For soot particles coated with water, the impurity can substantially reduce the single-scattering albedo of the particle if the size parameter is small. For water-coating soot and hollow ice spheres, it is shown that the phase matrix elements -P(sub 12)/P(sub 11) and P(sub 33)/P(sub 11) are unique if the shell is thin, as compared with the case for thick shell. Furthermore, the radiative transfer equation regarding a multidisperse particle system in an absorbing medium is discussed. It is illustrated that the conventional computation algorithms can be applied to solve the multiple scattering process if the scaled apparent single-scattering properties are applied.

Yang, P.↗

NASA NTRS2010

Advanced Vacuum Plasma Spray (VPS) for a Robust, Longlife and Safe Space Shuttle Main Engine (SSME)

In 1984, the Vacuum Plasma Spray Lab was built at NASA/Marshall Space Flight Center for applying durable, protective coatings to turbine blades for the space shuttle main engine (SSME) high pressure fuel turbopump. Existing turbine blades were cracking and breaking off after five hot fire tests while VPS coated turbine blades showed no wear or cracking after 40 hot fire tests. Following that, a major manufacturing problem of copper coatings peeling off the SSME Titanium Main Fuel Valve Housing was corrected with a tenacious VPS copper coating. A patented VPS process utilizing Functional Gradient Material (FGM) application was developed to build ceramic lined metallic cartridges for space furnace experiments, safely containing gallium arsenide at 1260 degrees centigrade. The VPS/FGM process was then translated to build robust, long life, liquid rocket combustion chambers for the space shuttle main engine. A 5K (5,000 Lb. thrust) thruster with the VPS/FGM protective coating experienced 220 hot firing tests in pristine condition with no wear compared to the SSME which showed blanching (surface pulverization) and cooling channel cracks in less than 30 of the same hot firing tests. After 35 of the hot firing tests, the injector face plates disintegrated. The VPS/FGM process was then applied to spraying protective thermal barrier coatings on the face plates which showed 50% cooler operating temperature, with no wear after 50 hot fire tests. Cooling channels were closed out in two weeks, compared to one year for the SSME. Working up the TRL (Technology Readiness Level) to establish the VPS/FGM process as viable technology, a 40K thruster was built and is currently being tested. Proposed is to build a J-2X size liquid rocket engine as the final step in establishing the VPS/FGM process TRL for space flight.

Holmes, Richard R.↗

DOE OSTI2023

Exploring the process-structure-property relationship of Aerosol Deposition to phosphor coatings for non-contact thermometry

Full-field, multi-measurand diagnostics provide rich validation data necessary to improve the product life cycle time of nuclear safety components. Thermophosphor digital image correlation (TP+DIC) is a method of simultaneously measuring strain and temperature fields using patterned phosphor coatings deposited with aerosol deposition (AD). While TP+DIC produces a functional diagnostic, the coating’s reproducibility and the effect of the patterned features on the inferred temperature remains uncharacterized. This NSR&D project provided the opportunity to study two areas: 1) the tunability and repeatability of aerosol deposition and 2) the robustness of aerosol deposition phosphor on deforming substrates. The first area explores the process-property relationship of parameters elucidating the significance of each on the coating. The second area explores the relationship between the features’ characteristics (namely thickness) and the phosphor emission and inferred temperature. Together, the results will lead to the improved accuracy and functionality of TP+DIC for qualification testing of nuclear safety components.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Ultrahigh-Rate and Long-Life Zinc–Metal Anodes Enabled by Self-Accelerated Cation Migration

Aqueous zinc ion batteries are receiving unprecedented attention owing to their markedly high safety and sustainability, yet their lifespan particularly at high rates is largely limited by the poor reversibility of zinc (Zn) metal anodes, due to the random ion diffusion and sluggish ion replenishment at reaction interface. In this work, we propose a tunnel-rich and corona-poled ferroelectric thin film coating for Zn metal anode to tackle above conundra. It is demonstrated that the poled ferroelectric coating can better deconcentrate and self-accelerate ion migration at coating/Zn interface upon electroplating process than untreated ferroelectric coating and bare Zn, thus enabling a compact and horizontally-aligned Zn morphology even at ultrahigh rates. Notably, a maximal cumulative plating capacity of over 6500 mAh cm -2 (at 10 mA cm -2 ) is achieved for the surface-modified Zn metal anode, showing extraordinary reversibility of Zn plating/stripping. This work provides new insights in stabilizing Zn metal electrodeposition at the scale of interfacial ion diffusion.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

NASA NTRS2019

Using Defects to Create Ceramics with Giant Permittivity as Ultracapacitors

Dielectrics with a high and weakly- temperature-dependent permittivity are highly desirable for the development of high performance energy storage devices. It is well known that ferroelectrics (FEs) exhibit a high permittivity that is strongly dependent on the temperature due to phase transition. In this project, the FE BaTiO3 (BTO), based ceramics are developed as ultra-capacitors by introducing defects to eliminate the phase transition and enhance the permittivity. The ceramics are fabricated using a unique process: BTO nanoparticles are coated with a nano-layer of SiO2 and, then, sintered in vacuum using SPS process. The ceramics exhibit a giant permittivity and many other unique properties.

Talebinezhad, H.↗

NASA NTRS1992

ASRM Process Development in Aqueous Cleaning

Viewgraphs are included on process development in aqueous cleaning which is taking place at the Aerojet Advanced Solid Rocket Motor (ASRM) Division under a NASA Marshall Space and Flight Center contract for design, development, test, and evaluation of the ASRM including new production facilities. The ASRM will utilize aqueous cleaning in several manufacturing process steps to clean case segments, nozzle metal components, and igniter closures. ASRM manufacturing process development is underway, including agent selection, agent characterization, subscale process optimization, bonding verification, and scale-up validation. Process parameters are currently being tested for optimization utilizing a Taguci Matrix, including agent concentration, cleaning solution temperature, agitation and immersion time, rinse water amount and temperature, and use/non-use of drying air. Based on results of process development testing to date, several observations are offered: aqueous cleaning appears effective for steels and SermeTel-coated metals in ASRM processing; aqueous cleaning agents may stain and/or attack bare aluminum metals to various extents; aqueous cleaning appears unsuitable for thermal sprayed aluminum-coated steel; aqueous cleaning appears to adequately remove a wide range of contaminants from flat metal surfaces, but supplementary assistance may be needed to remove clumps of tenacious contaminants embedded in holes, etc.; and hot rinse water appears to be beneficial to aid in drying of bare steel and retarding oxidation rate.

Swisher, Bill↗

DOE OSTI2024

Effect of post-deposition heat treatment on microstructure and mechanical properties of NASA HR-1 cold spray coatings

The primary goal of this work was to examine the impact of heat treatment on the evolution of microstructure and mechanical properties of NASA HR-1 cold spray coatings. Coatings were produced employing a high pressure cold spray system using N2 and He process gases and the effect of process gas and deposition temperature on the microstructure and mechanical properties of the coatings was examined. Microstructural characterization was performed using optical microscopy, scanning electron microscopy, micro X-ray computed tomography, and electron backscatter diffraction. NASA HR-1 coatings produced with He process gas exhibited improved plastic deformation and resulted in the lowest porosity compared to those deposited with N2 process gas. All coatings showed brittle failure with limited ductility in the as-deposited condition. Heat treatment of the NASA HR-1 cold spray coatings was performed at 550°C and 950°C for 1 h to improve the mechanical strength of the coatings. Heat treatment improved the particle bonding and enhanced the mechanical properties of the cold spray coatings. Heat treatment performed at 550°C resulted in higher mechanical strength of coatings, whereas the heat treatment performed at 950°C resulted in recrystallized microstructure and improved ductility of the coatings. However, heat treatment at 950°C resulted in forming the Eta (η) phase and Ni-Ti intermetallics in all the NASA HR-1 cold spray coatings. Here, the overall results suggest that using He as process gas contributed to reduced porosity and enhanced mechanical properties of the cold spray coatings.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

NASA NTRS2000

Investigation of Potential Thermal Processing Techniques for the Enhancement of PS300 High Temperature Solid Lubricant Coatings

Contemporary trends in rotating machinery development have produced a continuous evolution towards ever increasing speeds and higher operating temperatures. This process has been particularly evident in aerospace and automotive applications such as turbochargers. The combination of high temperature and high speed has exceeded the capacity of mainstream liquid lubrication technology. The NASA Glenn Research Center has been at the forefront in developing innovative solid lubricants for the oil free protection of rotating machinery under these extreme environmental conditions. The most recent of these is the PS 300 series of plasma sprayed solid lubricant coatings. St Louis University and NASA Glenn Research Center entered into this cooperative agreement to investigate potential thermal processing techniques for the enhancement of the PS 304 solid lubricant.

Benoy, Patricia A.↗

DOE OSTI2023

Metal (Cu,Al)/CNT Composite Wires for Energy Efficient Motors

This report summarizes the main results of research project on Metal/CNT nanocomposites conducted at University of Central Florida (UCF). It should be noted that the project was budgeted for three years, but the budget period 3 was unfortunately not funded and conducted in COVID19 pandemic years due to many reasons. The demonstration plan on the small motors was also removed according to the discussion with the DOE program manager. All research activities were focused on the (Cu,Al)/CNT material development and wire extrusion. Existing methods to fabricate Metal/CNTs were usually suffering from agglomeration of CNTs due to their density and stiffness differences. A new method is studied by the UCF research team, where CNTs are surface treated firstly, then coated with pure metals (i.e., Al, Cu, and Nickle). The metal encapsulation on CNT is expected to significantly improve the interfacial bonding between CNTs and the intimated metal matrices. The coated CNT powders were used to make sample materials through sintering, then a customized wire extrusion process was employed to fabricate wires. Measurement of material property improvements in mechanical strength, thermal conductivity, and electrical conductivity were conducted on both cylinder samples and extruded wires. In addition to the sintering process, casting on metal coated CNT powder was also investigated. The best results we achieved are summarized as follows. (1) The measured thermal conductivity of Al/CNT composite made with Ni-encapsulated CNTs and pure Al powders is about 85% better than that of pure aluminum fabricated. The measured electrical conductivity of fabricated Al/CNT is about 14-20% better than that of pure aluminum. (2) The measured electrical conductivity of Cu/CNT is about 14.5% better than that of pure copper fabricated. (3) The mechanical strengths of both Cu/CNT and Al/CNT (with about 1% wt. CNTs) are 70% better than pure metals although losing some material ductility. (4) Two-stage wire extrusion at high temperatures were designed and successfully conducted to fabricate wires of Metal/CNTs.

36 MATERIALS SCIENCE↗

NASA NTRS1974

Adhesive coating eliminated in new honeycomb-core fabrication process

Technique eliminates use of silicone-based adhesive material as bonding medium. Adhesive requires precise time-temperature cure. Prepreg resin is used as bonding medium, and each layer is laminated together to form honeycomb billet. Process can be used in any application where nonmetallic honeycomb core is being fabricated.

Batty, W. L.↗

NASA NTRS1995

Process for non-contact removal of organic coatings from the surface of paintings

The present invention discloses a method of removing organic protective coatings from a painting. In the present invention degraded protective coatings such as lacquers, acrylics, natural resins, carbons, soot, and polyurethane are safely removed from the surface of a painting without contact to the surface of the painting. This method can be used for restoration of paintings when they have been damaged, through age, fire, etc.

Banks, Bruce A.↗

NASA NTRS1996

Process for Non-Contact Removal of Organic Coatings from the Surface of Paintings

Banks, Bruce A.↗

NASA NTRS2003

CVD aluminiding process for producing a modified platinum aluminide bond coat for improved high temperature performance

A method of depositing by chemical vapor deposition a modified platinum aluminide diffusion coating onto a superalloy substrate comprising the steps of applying a layer of a platinum group metal to the superalloy substrate; passing an externally generated aluminum halide gas through an internal gas generator which is integral with a retort, the internal gas generator generating a modified halide gas; and co-depositing aluminum and modifier onto the superalloy substrate. In one form, the modified halide gas is hafnium chloride and the modifier is hafnium with the modified platinum aluminum bond coat comprising a single phase additive layer of platinum aluminide with at least about 0.5 percent hafnium by weight percent and about 1 to about 15 weight percent of hafnium in the boundary between a diffusion layer and the additive layer. The bond coat produced by this method is also claimed.

Nagaraj, Bangalore A.↗

DOE OSTI2021

Lamination of transparent conductive adhesives for tandem solar cell applications

A transparent conductive adhesive (TCA) interlayer for mechanically stacked multijunction solar cells provides adhesive strength and electrical connection between sub-cells when stacked. The fabrication of TCA sheets from an ethyl-vinyl acetate (EVA) matrix and silver coated compliant conductive microspheres, similar to industry-standard EVA encapsulant sheets, compatible with a standard lamination process was developed. Blade coating TCA sheets using 3D printed blades and testing of vertical conduction through the interlayer with a TCA conductivity jig allowed for reproducible measurements and low-cost fabrication. The supplemental information provides design files to enable other researchers to produce their own blades and testing jigs. We identified 0.5 mm as an optimal blade height for producing lab-scale TCA sheets and 120 °C at 3 psi for 10 min as the optimal vacuum lamination process to minimize resistance and possible damage to samples. For TCA sheets with coverages between 0.75% and 9%, the series resistance was approximately 0.2 O cm2 which should result in minimal losses for one-sun photovoltaic applications.

14 SOLAR ENERGY↗

NASA NTRS2017

Residual Stresses in a NiCrY-Coated Powder Metallurgy Disk Superalloy

Protective ductile coatings will be necessary to mitigate oxidation and corrosion attack on superalloy disks exposed to increasing operating temperatures in some turbine engine environments. However, such coatings must be resistant to harmful surface cracking during service. The objective of this study was to investigate how residual stresses evolve in such coatings. Cylindrical gage fatigue specimens of powder metallurgy-processed disk superalloy LSHR were coated with a NiCrY coating, shot peened, and then subjected to fatigue in air at room and high temperatures. The effects of shot peening and fatigue cycling on average residual stresses and other aspects of the coating were assessed. Shot peening did induce beneficial compressive residual stresses in the coating and substrate. However, these stresses became more tensile in the coating with subsequent heating and contributed to cracking of the coating in long intervals of cycling at 760 C. Substantial compressive residual stresses remained in the substrate adjacent to the coating, sufficient to suppress fatigue cracking. The coating continued to protect the substrate from hot corrosion pitting, even after fatigue cracks initiated in the coating.

superalloy↗

NASA NTRS2001

Thermal Processing Effects on the Adhesive Strength of PS304 High Temperature Solid Lubricant Coatings

In this paper the effects of post deposition heat treatments on the cohesive and adhesive strength properties of PS304, a plasma sprayed nickel-chrome based, high temperature solid lubricant coating deposited on stainless steel, are studied. Plasma spray deposited coating samples were exposed in air at temperatures from 432 to 650 C for up to 500 hr to promote residual stress relief, enhance particle to particle bonding and increase coating to substrate bond strength. Coating pull-off strength was measured using a commercial adhesion tester that utilizes 13 mm diameter aluminum pull studs attached to the coating surface with epoxy. Pull off force was automatically recorded and converted to coating pull off strength. As deposited coating samples were also tested as a baseline. The as-deposited (untreated) samples either delaminated at the coating-substrate interface or failed internally (cohesive failure) at about 17 MPa. Samples heat treated at temperatures above 540 C for 100 hr or at 600 C or above for more than 24 hr exhibited strengths above 31 MPa, nearly a two fold increase. Coating failure occurred inside the body of the coating (cohesive failure) for nearly all of the heat-treated samples and only occasionally at the coating substrate interface (adhesive failure). Metallographic analyses of heat-treated coatings indicate that the Nickel-Chromium binder in the PS304 appears to have segregated into two phases, a high nickel matrix phase and a high chromium precipitated phase. Analysis of the precipitates indicates the presence of silicon, a constituent of a flow enhancing additive in the commercial NiCr powder. The exact nature and structure of the precipitate phase is not known. This microstructural change is believed to be partially responsible for the coating strength increase. Diffusion bonding between particles may also be playing a role. Increasing the heat treatment temperature, exposure time or both accelerate the heat treatment process. Preliminary measurements indicate that the heat treatment also results in a one time, permanent coating thickness increase of about 3%. Based upon these results, the incorporation of a heat treatment prior to final finishing has been incorporated in the application process of this coating technology.

DellaCorte, Christopher↗

DOE OSTI2020

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↗