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All sources NASA NTRS DOE OSTI

DOE OSTI2020

Atomic Layer Deposition (ALD) to Extend Catalyst Lifetime for Biobased Adipic Acid Production

Robust heterogeneous catalysts are essential for enabling biomass conversion; however, harsh reaction environments introduce durability challenges for many conventional catalyst materials [1]. The hydrogenation of biobased muconic acid to adipic acid is one such emerging chemistry that faces PGM catalyst stability challenges [2]. Muconic acid is a heavily-investigated biobased platform chemical that can be converted into an array of large-market commodity chemicals [2]. PGM catalysts are exceptionally effective for muconic acid hydrogenation to adipic acid, with Pd the most active to date. [2] However, Pd leaches in an acidic environment and this chemistry has a high propensity for fouling. Atomic layer deposition (ALD) is one such material design strategy that has emerged to stabilize supported metal catalysts [3]. ALD coatings are theorized to stabilize supported metal active sites by i) covering high-energy facets most susceptible to degradation, ii) disrupting the physical mobility of active sites, and iii) reinforcing the structure of the underlying catalyst support [3]. However, ALD coatings for catalyst durability with carboxylic acids remains an underdeveloped area of research and literature reports have yet to consider the techno-economic tradeoffs between the ALD manufacturing cost and catalyst lifetime productivity. This study examines low-cycle Al2O3 ALD coatings to stabilize Pd/TiO2 against deactivation during muconic acid hydrogenation. The unique harshness of muconic acid for Pd leaching was evaluated by both experiment and computation. Based on batch reactor screening results, uncoated and ALD coated catalysts were evaluated in a continuous flow reactor for their productivity, stability, and post-reaction regenerability at 700 degrees C. Characterization was performed to assess the impact of ALD coatings on catalyst morphology, as well as following regeneration. Finally, techno-economic analysis models evaluated the value proposition for ALD-coated catalysts within an nth-generation adipic acid biorefinery.

09 BIOMASS FUELS↗

NASA NTRS2017

Revisiting the Birth of 7YSZ Thermal Barrier Coatings: Steve Stecura

Thermal barrier coatings are widely used in all turbine engines, typically using a 7 wt% Y2O3-ZrO2 formulation. Extensive research and development over many decades have refined the processing and structure of these coatings for increased durability and reliability. New compositions demonstrate some unique advantages and are gaining in application. However, the "7YSZ" formulation predominates and is still in widespread use. This special composition has been universally found to produce nanoscale precipitates of metastable t' tetragonal phase, giving rise to a unique toughening mechanism via ferro-elastic switching under stress. This note recalls the original study that identified superior properties of 6 to 8 wt% YSZ plasma sprayed thermal barrier coatings, published in 1978. The impact of this discovery, arguably, continues in some form to this day. At one point, 7YSZ thermal barrier coatings were used in every new aircraft and ground power turbine engine produced worldwide. It is a tribute to its inventor, Dr. Stephan J. Stecura, NASA retiree.

turbine blades↗

NASA NTRSDate not supplied

Metrological and Spectral Characterization of the Aspera Flight Optics

Aspera is a NASA's Astrophysics Pioneers mission, led by the University of Arizona. The aim of this mission is to study the presence of hot gasses (T=10^5-10^6 K) in the circumgalactic medium (CGM) and how the flow of these gasses affects galactic formation. One key enabling technology in the Aspera optical system is the use of more efficient UV-reflective optical coatings particularly at around 103.2 nm where the O VI emission line is located . In order to meet radiometric effective area requirements, the Goddard Space Flight Center (GSFC) code 551 Optics Branch applied Al (aluminum) + eLiF (enhanced lithium fluoride) on these optics, where the Al+LiF is annealed at elevated temperature (~250˚C) after the deposition and thus providing an improved version of the Al+LiF used in FUSE . Furthermore, these optics are encapsulated with a thin film of atomic layer deposited MgF2 at the Jet Propulsion Laboratory for enhanced durability . The efficiency and durability of these coatings depends on the quality of the optical surface in terms of cleanliness and roughness. Roughness increases the scatter off the coating and reduces the specular reflectance, and surface contaminants can accommodate moisture and other contaminants, increase scattering, and are weak points in the coating that may affect adhesion and subsequently the longevity of these coatings. Extensive optical metrology is necessary to minimize and quantify the impact of surface roughness and contaminants on optical surfaces. In this proceeding we report the inspection procedure implemented for Aspera optics at GSFC, from initial receiving of the optics to post-coating. Inspection includes Atomic Force Microscopy (AFM), Scanning White Light Interferometry (SWILI), Dark Field Microscopy (DFM), Phase Shifting Interferometry (PSI), and Vacuum ultraviolet (VUV) spectroscopy. Combinations of these techniques are used to inspect flight optics at each of the following steps: i) as-received, pre-cleaning inspection, ii) pre-coating, post-cleaning inspection, and iii) post-coating inspection. The evolution of roughness and other surface inspections such as contaminants are compared between each step to quantify the effect each step has on the flight optics. The final far ultraviolet (FUV) spectral performance of witness samples coated with the flight optics are presented.

Far Ultraviolet (FUV)↗

NASA NTRSDate not supplied

Permanent, Transparent Anti-Fog Coating for Spacesuit Helmet

Fogging of polycarbonate spacesuit helmets is detrimental to astronaut safety and to mission success. Currently used anti-fogging methods are temporary and require the reapplication of a coating before each use. These temporary solutions have been shown to delaminate during use and have led to eye irritation and temporary blindness during spacewalks. Potential permanent solutions NASA has previously tested lack in durability and are prone to coating damage and delamination during cleaning. Lynntech is leveraging its experience with coating development to fabricate an anti-fog coating with the durability necessary for permanent use, to be applied to polycarbonate. In this SBIR Phase I project, Lynntech has demonstrated the proof of concept by applying our coating to flat polycarbonate and characterized the durability of its anti-fogging properties. Toward this end, Lynntech has developed a breath simulating testbed, exposing coatings to conditions they would experience on the interior of a spacesuit helmet during use. Additionally, Lynntech is developing an application method to uniformly deposit their coating on non-planar objects, such as a prototype spacesuit helmet.

spacesuit↗

NASA NTRS2008

MISSE Results Used for RF Plasma Ground Testing-To-Space-Exposure Correlation for Coated Kapton

The ability to predict the durability of materials in the low Earth orbit (LEO) environment by exposing them in ground-based facilities is important because one can achieve test results sooner, expose more types of materials, and do it much more cost effectively than to test them in flight. However, flight experiments to determine the durability of groups or classes of materials that behave similarly are needed in order to provide correlations of how much time in ground-based facilities represents certain durations in LEO for the material type of interest. An experiment was designed and flown on the Materials International Space Station Experiment (MISSE) 2 (3.95 yr in LEO) and MISSE 4 (1.04 yr in LEO) in order to develop this type of correlation between ground-based RF plasma exposure and LEO exposure for coated Kapton. The experiment consisted of a sample of Kapton H (DuPont) polyimide coated with 1300 of silicon dioxide by Sheldahl, Inc. The samples were exposed to atomic oxygen in a radio frequency (RF) generated atomic oxygen plasma. Mass change was measured for the samples and then the same samples were exposed in flight on MISSE and the mass change was again recorded post-flight. After documentation, the samples were exposed again in the ground-based RF plasma in order to determine if the erosion would be the same as it had been in the same facility pre-flight which would indicate whether or not the sample had been damaged during flight and if the defects on the surface were those that were there preflight. The slopes of the mass change versus fluence plots were then used to develop a correlation factor that can be used to help predict the durability of coated Kapton in ground-based isotropic atomic oxygen plasma systems. This paper describes the experiment and presents the correlation factor results.

Miller, Sharon K. R.↗

NASA NTRS2004

Furnace Cyclic Oxidation Behavior of Multi-Component Low Conductivity Thermal Barrier Coatings

Ceramic thermal barrier coatings will play an increasingly important role in advanced gas turbine engines because of their ability to further increase engine operating temperatures and reduce cooling, thus helping achieve future engine low emission, high efficiency and improved reliability goals. Advanced multi-component zirconia-based thermal barrier coatings are being developed using an oxide defect clustering design approach to achieve the required coating low thermal conductivity and high temperature stability. Although the new composition coatings were not yet optimized for cyclic durability, an initial durability screening of the candidate coating materials was conducted using conventional furnace cyclic oxidation tests. In this paper, furnace cyclic oxidation behavior of plasma-sprayed zirconia-based defect cluster thermal barrier coatings was investigated at 1163 C using 45 min hot cycles. The ceramic coating failure mechanisms were studied using scanning electron microscopy (SEM) combined with X-ray diffraction (XRD) phase analysis after the furnace tests. The coating cyclic lifetime is also discussed in relation to coating processing, phase structures, dopant concentration, and other thermo-physical properties.

Zhu, Dong-Ming↗

NASA NTRSDate not supplied

Expanding the Capability of A Legacy Combustion Flametube to Test High Temperature Engine Materials in Relevant Environments

New materials and component designs are needed to advance gas turbine engine technology and provide the performance and efficiency needs for future applications. In order to advance these materials, testing in combustion environments is a critical step prior to engine testing. In this work, we detail the design and the fabrication of a materials test sector in a flametube combustor facility. The facility simulates a combustion environment similar to that experienced by components in gas turbine engines. The flow regime is characterized by a combination of high-temperature, high-velocity, high-heat flux, and high-velocity that components experience in gas turbine engines. Exposure of components in this facility allows for the study of combined environmental effects and the impact on both coating and substrate durability. The test facility may operate across a wide range of pressures from 275-400 psig (1,896-2,758 kPa) and an air flow rate of 5 lb/s (2.27 kg/s). While combustion gas temperature is expected in excess of 3,000°F (1,649°C), 900°F (482°C) cooling air may be supplied to the backside of components or test articles. The flametube combustor was previously used to evaluate fuel injectors and combustion products, and the new test configuration will also allow for materials exposure to complex, engine-like conditions. The interior of the Test Section was additively manufactured from GRCop-84 and cryogenically fit and brazed to a stainless steel 304 housing. The use of a copper liner minimizes welds and with active cooling, is expected to provide better durability over traditional hardware using stainless steel or Inconel with a ceramic liner. The Test Section has two opposing removable windows approximately 230 mm x 80 mm that can accommodate articles up to 85 mm tall. This modular design allows for custom platforms to hold coupons, panels, or airfoil shapes to be tested with minimal re-engineering or fabrication. The bolted joint and sealing remains consistent, so any new testing only needs to work within the existing design footprint. This paper will provide an overview of the facility capabilities, design considerations, as well as thermal and structural analysis of the hardware. Future testing of ceramic matrix composite (CMC) airfoils and advanced environmental barrier coatings (EBCs) will also be discussed.

Combustion↗

NASA NTRS1995

Mechanical properties testing and results for thermal barrier coatings

The paper reports on several years of mechanical testing of thermal barrier coatings. The test results were generated to support the development of durability models for the coatings in heat engine applications. The test data that are reviewed include modulus, static strength, and fatigue strength data. The test methods and results are discussed, along with the significant difficulties inherent in mechanical testing of thermal barrier coating materials. The materials include 7 percent wt. and 8 percent wt. yttria, partially stabilized zirconia as well as a cermet material. Both low pressure plasma spray and electron-beam physical vapor deposited coatings were tested. The data indicate the basic trends in the mechanical properties of the coatings over a wide range of isothermal conditions. Some of the trends are correlated with material density.

Thomas A. Cruse↗

NASA NTRS2018

E-Beam Generated Plasma Etching for Developing High-Reflectance Mirrors for Far-Ultraviolet Astronomical Instrument Applications

Astronomical space telescopes to study astrophysical phenomena from the far-ultraviolet (FUV) to the near infrared (NIR) will require mirror coatings with high reflectance over this entire spectral region. While coatings for the optical and NIR part of the spectrum are fairly well developed with proven performance, the FUV presents significant challenges. The U.S. Naval Research Laboratory (NRL) has developed a processing system based on an electron beam-generated plasma that provides for controlled fluorination and/or etching of surfaces with near monolayer precision and minimal changes to surface morphology. In this paper, we report recent results of samples treated in the NRL Large Area Plasma Processing System (LAPPS) where restoration of the high intrinsic reflectance in the FUV spectral range have been observed of aluminum (Al) mirrors protected with a magnesium di-fluoride (MgF2) overcoat. This paper will also extend these studies to other Al mirrors protected with aluminum tri-fluoride (AlF3) in order to realize the high intrinsic reflectance Al down to FUV wavelengths (100−200 nm), while still maintaining the high reflectance in the optical and NIR spectral regions. Laboratory test data and optical diagnostic techniques used to verify surface scattering and durability of selected coatings will be presented. Finally, we will discuss the scalability of the LAPPS etching process in order to realize these high-reflectivity coatings on mirror segments as large as those proposed for the Large Ultraviolet, Optical, and Infrared (LUVOIR) astronomical telescope system (1+meter class).

LUVOIR↗

DOE OSTI2026

Designing the Platinum Catalyst Layer for Improved Performance and Durability in Anion Exchange Membrane Water Electrolysis

To lower the cost of hydrogen produced by anion exchange membrane water electrolysis (AEMWE), it is critical to reduce the use of platinum group metal (PGM) catalysts within the device. While iridium has been successfully replaced with PGM-free catalysts at the anode, platinum-based (Pt) cathode catalysts are still required to meet the activity and durability targets. This study investigates the impact of commercial Pt/C catalyst loading, ionomer type and content, and electrode fabrication method on the cathode catalyst layer properties and AEMWE performance with the aim of determining the feasibility of reduced Pt loadings. While increased Pt loading is found to improve beginning-of-life performance, the effects are minimal above 0.6 mg/cm 2 . Ink characterization shows that ionomer type and content affect the ink stability, particle size, and percent of unbound ionomer, which further impact the homogeneity of the sprayed catalyst layers. The 5% PiperION cathode exhibited the highest performance, which may be attributed to a balance between the small particle size and the low proportion of unbound ionomer, minimizing kinetic and transport losses. Theoretical calculations show that the ionomers interact differently with the Pt surface, causing different surface charges and water adsorption strength and activating different mechanisms for hydrogen evolution. Pt-PiperION lowered the enthalpy of water-splitting by 0.1 eV compared to Pt alone and allowed for equal site access between adsorbed H* and OH* (both adsorbed at circa −2.2 eV). Although catalyst-coated membrane (CCM) fabrication techniques are desirable for scale-up, no performance enhancement is observed compared with the catalyst-coated substrate approach. Durability, as measured by degradation rates, Pt loss, and catalyst layer restructuring, was found to improve with increased Pt loadings, higher ionomer content, and CCM architectures. These findings provide important insight into the significant role of the cathode in AEMWE and strategies for maintaining the performance with low Pt loading or PGM-free catalysts.

08 HYDROGEN↗

DOE OSTI2014

Fracture toughness of plasma-sprayed thermal barrier ceramics: Influence of processing, microstructure, and thermal aging

Fracture toughness has become one of the dominant design parameters that dictates the selection of materials and their microstructure to obtain durable thermal barrier coatings (TBCs). Much progress has been made in characterizing the fracture toughness of relevant TBC compositions in bulk form, and it has become apparent that this property is significantly affected by process-induced microstructural defects. In this investigation, a systematic study of the influence of coating microstructure on the fracture toughness of atmospheric plasma sprayed (APS) TBCs has been carried out. Yttria partially stabilized zirconia (YSZ) coatings were fabricated under different spray process conditions inducing different levels of porosity and interfacial defects. Fracture toughness was measured on free standing coatings in as-processed and thermally aged conditions using the double torsion technique. Results indicate significant variance in fracture toughness among coatings with different microstructures including changes induced by thermal aging. Comparative studies were also conducted on an alternative TBC composition, Gd 2 Zr 2 O 7 (GDZ), which as anticipated shows significantly lower fracture toughness compared to YSZ. Furthermore, the results from these studies not only point towards a need for process and microstructure optimization for enhanced TBC performance but also a framework for establishing performance metrics for promising new TBC compositions.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Energy Efficiency Improvement Approaches in Ice Related Processes

A detailed survey of ice mold and evaporator metal surfaces, physical structures, operational conditions, materials of construction, design of different equipment was reviewed and analyzed. A reliable test methodology was developed to measure the ice adhesion strength of different materials and geometries identified. The developed test setup was successfully employed in measuring the ice adhesion strength on both tubular and planar substrate geometries of metals including copper, aluminum, stainless steel. Application of advanced polymer materials in lowering the adhesion strength of ice was confirmed where the measured strength was lowered by 50-70% depending on the material and geometry. Additionally, utilization of induced ultrasonic vibration in further lowering the ice harvesting energy was confirmed on multiple materials and geometries. Durability of the coating enhancement was also confirmed in a thermal cycling test under realistic operating conditions.

36 MATERIALS SCIENCE↗

NASA NTRS1993

Space propulsion

Lewis Research Center is developing broad-based new technologies for space chemical engines to satisfy long-term needs of ETO launch vehicles and other vehicles operating in and beyond Earth orbit. Specific objectives are focused on high performance LO2/LH2 engines providing moderate thrusts of 7,5-200 klb. This effort encompasses research related to design analysis and manufacturing processes needed to apply advanced materials to subcomponents, components, and subsystems of space-based systems and related ground-support equipment. High-performance space-based chemical engines face a number of technical challenges. Liquid hydrogen turbopump impellers are often so large that they cannot be machined from a single piece, yet high stress at the vane/shroud interface makes bonding extremely difficult. Tolerances on fillets are critical on large impellers. Advanced materials and fabricating techniques are needed to address these and other issues of interest. Turbopump bearings are needed which can provide reliable, long life operation at high speed and high load with low friction losses. Hydrostatic bearings provide good performance, but transients during pump starts and stops may be an issue because no pressurized fluid is available unless a separate bearing pressurization system is included. Durable materials and/or coatings are needed that can demonstrate low wear in the harsh LO2/LH2 environment. Advanced materials are also needed to improve the lifetime, reliability and performance of other propulsion system elements such as seals and chambers.

Kazaroff, John M.↗

NASA NTRS2004

The Office of the Materials Division

I was assigned to the Materials Division, which consists of the following branches; the Advanced Metallics Branch/5120-RMM, Ceramics Branch/5130-RMC, Polymers Branch/5150-RMP, and the Durability and Protective Coatings Branch/5160-RMD. Mrs. Pamela Spinosi is my assigned mentor. She was assisted by Ms.Raysa Rodriguez/5100-RM and Mrs.Denise Prestien/5100-RM, who are both employed by InDyne, Inc. My primary assignment this past summer was working directly with Ms. Rodriguez, assisting her with setting up the Integrated Financial Management Program (IFMP) 5130-RMC/Branch procedures and logs. These duties consisted of creating various spreadsheets for each individual branch member, which were updated daily. It was not hard to familiarize myself with these duties since this is my second summer working with Ms Rodriguez at NASA Glenn Research Center. RMC ordering laboratory, supplies and equipment for the Basic Materials Laboratory (Building 106) using the IF'MP/Purchase Card (P-card), a NASA-wide software program. I entered into the IFMP/Travel and Requisitions System, new Travel Authorizations for the 5130-RMC Civil Servant Branch Members. I also entered and completed Travel Vouchers for the 5130-RMC Ceramics Branch. I assisted in the Division Office creating new Emergency Contact list for the Materials Division. I worked with Dr. Hugh Gray, the Division Chief, and Dr. Ajay Misra, the 5130-RMC Branch Chief, on priority action items, with a close deadline, for a large NASA Proposal. Another project was working closely with Ms. Rodriguez in organizing and preparing for Dr. Ajay K. Misra's SESCDP (two year detail). This consisted of organizing files, file folders, personal information, and recording all data material onto CD's and printing all presentations for display in binders. I attended numerous Branch meetings, and observed many changes in the Branch Management organization.

Ramsey, amanda J.↗

NASA NTRS2004

Foreign Object Damage Resistance of Uncoated and EBC Coated SiC/SiC Composites

SiC/SiC composites fabricated by the melt infiltration method are candidate materials for the turbine components such as combustor liners, nozzle vanes and blades because of their high temperature strength, and thermal conductivity. To avoid surface recession in a combustion environment containing moisture, these materials also require an environmental barrier coating (EBC). Under thermal loading condition alone, the EBC coated SiC/SiC components show microstructural and strength stability after -1 5000 hr exposure to 12OO0C in combustion environment. However, the stability of SiC/SiC composites under impact conditions is not fully understood. In this study, both uncoated and EBC coated SiC/SiC composite specimens were impact tested by steel-ball projectiles at room temperature and at 1300 C in air. After impact, the specimens were analyzed under a scanning electron microscope to assess coating damage, and then tensile and bend tested at room temperature to determine their residual strength. The extent of coating and substrate damage with increasing projectile velocity was imaged and analyzed using nondestructive evaluation (NDE) methods such as micro focus x-ray radiography, tomography, and thermal wave imaging. The mechanical property results of impacted specimens are correlated with the NDE results and the scanning electron microscopy (SEM) observations. Influence of projectile velocity on impact damage of the coating/substrate, and the implication coating damage on durability of the composite will be discussed.

Bhatt, R. T.↗

NASA NTRS2008

Thermal and Environmental Barrier Coating Development for Advanced Propulsion Engine Systems

Ceramic thermal and environmental barrier coatings (TEBCs) are used in gas turbine engines to protect engine hot-section components in the harsh combustion environments, and extend component lifetimes. Advanced TEBCs that have significantly lower thermal conductivity, better thermal stability and higher toughness than current coatings will be beneficial for future low emission and high performance propulsion engine systems. In this paper, ceramic coating design and testing considerations will be described for turbine engine high temperature and high-heat-flux applications. Thermal barrier coatings for metallic turbine airfoils and thermal/environmental barrier coatings for SiC/SiC ceramic matrix composite (CMC) components for future supersonic aircraft propulsion engines will be emphasized. Further coating capability and durability improvements for the engine hot-section component applications can be expected by utilizing advanced modeling and design tools.

Zhu, Dongming↗

NASA NTRS2011

Mach 0.3 Burner Rig Facility at the NASA Glenn Materials Research Laboratory

This Technical Memorandum presents the current capabilities of the state-of-the-art Mach 0.3 Burner Rig Facility. It is used for materials research including oxidation, corrosion, erosion and impact. Consisting of seven computer controlled jet-fueled combustors in individual test cells, these relatively small rigs burn just 2 to 3 gal of jet fuel per hour. The rigs are used as an efficient means of subjecting potential aircraft engine/airframe advanced materials to the high temperatures, high velocities and thermal cycling closely approximating actual operating environments. Materials of various geometries and compositions can be evaluated at temperatures from 700 to 2400 F. Tests are conducted not only on bare superalloys and ceramics, but also to study the behavior and durability of protective coatings applied to those materials.

Fox, Dennis S.↗

NASA NTRS2013

CMC Technology Advancements for Gas Turbine Engine Applications

CMC research at NASA Glenn is focused on aircraft propulsion applications. The objective is to enable reduced engine emissions and fuel consumption for more environmentally friendly aircraft. Engine system studies show that incorporation of ceramic composites into turbine engines will enable significant reductions in emissions and fuel burn due to increased engine efficiency resulting from reduced cooling requirements for hot section components. This presentation will describe recent progress and challenges in developing fiber and matrix constituents for 2700 F CMC turbine applications. In addition, ongoing research in the development of durable environmental barrier coatings, ceramic joining integration technologies and life prediction methods for CMC engine components will be reviewed.

Grady, Joseph E.↗