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NASA NTRS2019

Extreme-Temperature Carbon- and Ceramic-Matrix Composite Nozzle Extensions for Liquid Rocket Engines

The United States (US) National Aeronautics and Space Administration (NASA) and its US industry partners are developing extreme-temperature composite nozzle extensions for a variety of cryogenic liquid rocket engine propulsion systems. Applications under consideration at the NASA Marshall Space Flight Center (MSFC) include launch vehicle (upper stage), in-space, and lunar lander descent/ascent propulsion systems. Composite material systems of interest include carbon-carbon (C-C) and carbon/silicon-carbide (C-SiC) composites, as well as modified versions of such composites (coatings, mixed matrices, oxidation inhibitors, etc.). Missions addressed include access to low Earth orbit, the lunar surface, and more distant destinations. Cryogenic upper-stage and in-space liquid rocket engines are optimized for performance through the use of high area ratio nozzles to fully expand combustion gases to low exit pressures, increasing exhaust velocities. As a result of the large size of such nozzles, and the related engine performance requirements, composite nozzle extensions are being considered to reduce mass impacts. Currently, metallic and foreign composite nozzle extensions used on the Atlas V, Delta IV, Falcon 9, and Ariane 5 launch vehicles represent the state-of-the-art. Such extensions are limited to use at or slightly above 2000°F (1093°C). Materials under development by MSFC and its industry partners have the potential to operate at temperatures up to (or above) 4250°F (2343°C). Marshall Space Flight Center efforts are aimed at (a) further developing the technology and databases needed to enable the use of composite nozzle extensions on cryogenic liquid rocket engines, (b) developing and demonstrating low-cost capabilities for testing and qualifying such nozzle extensions, and (c) advancing the US domestic supply chain for nozzle extensions. Through the Small Business Innovation Research (SBIR) and Small Business Technology Transfer (STTR) Programs, low-level internal MSFC research projects, and teaming arrangements with domestic industry partners, composite material design, development, hot-fire test, and evaluation efforts are progressing. Hot- fire engine tests of subscale hardware have been conducted using oxygen/hydrogen (LOX/H2), oxygen/methane (LOX/CH4), and oxygen/kerosene (LOX/RP-1) propellants. These engine tests at MSFC have enabled the evaluation of both heritage and state-of-the-art material systems, demonstrating the initial capabilities of the extreme temperature materials and their fabrication methods. Recent, ongoing, and potential future work supporting cryogenic propulsion systems development will be presented. The composite nozzle extension technology and test capabilities being developed are intended to support both NASA and US Department of Defense requirements, as well as those of the broader Commercial Space industry.

Valentine, Peter G.↗

NASA NTRS2017

Environmental Testbed Development to Evaluate Power Distribution Materials in Electrified Aircraft (EA)

NASA is pursuing the development of electrified propulsion (EP) technologies to improve air transportation in terms of efficiency, affordability, and sustainability. The power requirements are expected to reach 20 megawatts for large EP commercial airliners. A key challenge is transmission and distribution of the high voltage (20 kilovolts) needed for some EP systems. This is a challenge because the risk of electrical failure in aircraft at high altitude (low pressure) due to corona discharge and other forms of partial discharge increases significantly when voltages exceed 327 V. Corona discharge is a form of partial discharge in which gaseous molecules are ionized by strong electric fields. Corona discharge leads to aging in power transmission lines. Aging is a leading cause of electrical failure in electrical insulation materials. In particular, aging from electrical, vibrational, and thermal stresses decrease the performance life of insulation materials. There are currently no test standards or equipment that can effectively age materials under high altitude, voltage and frequency conditions. This poster proposes a design for a test system including an environmental chamber that can simulate the environment of future EP systems for material and component aging tests.

Materials Test chamber Design↗

DOE OSTI2025

Development of Engine Valve Materials for Next Generation Higher Efficiency Engines

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

NASA NTRS2002

Environment-Conscious Ceramics (Ecoceramics) Technology Received 2001 R&D 100 Award

Since the dawn of human civilization, there has been a delicate balance between the use of resources as human frontiers expanded and the need to have a minimum influence on the ecosystem. The first 200 years of the industrial revolution essentially solved the problem of production. However, the massive production of goods also generated tremendous amounts of byproducts and wastes. In the new millennium, to sustain a healthy life in harmony with nature, it will be extremely important for us to develop various materials, products, and processes that minimize any harmful influence on the environment. Environment-conscious ceramics (ecoceramics) are a new class of materials that can be fabricated with renewable resources (wood) and wood waste material (wood sawdust). Wood is a "lignocellulosic" material formed by the photosynthetic reaction within the needles or leaves of trees. The photosynthesis process uses sunlight to take carbon dioxide from air and convert it into oxygen and organic materials. Wood has been known to be one of the best and most intricate engineering materials created by nature and known to mankind. In addition, natural woods of various types are available throughout the world. On the other hand, wood sawdusts are generated in abundant quantities by sawmills. Environment-conscious ceramic materials, fabricated via the pyrolysis and infiltration of natural wood-derived preforms, have tailorable properties with numerous potential applications. The experimental studies conducted to date on the development of materials based on biologically derived structures indicate that these materials behave like ceramic materials manufactured by conventional approaches. These structures have been shown to be quite useful in producing porous or dense materials having various microstructures and compositions.

Singh, Mrityunjay↗

DOE OSTI2023

Advancing radioactive material research method: the development of a novel in situ particle-attached microfluidic electrochemical cell

This study aims to develop a microgram-scale microfluidic electrochemical cell (E-cell) for investigating the redox behavior of uranium oxide (UO 2 ). The traditional bulk electrochemical methods may require shielded facilities to investigate the hazardous materials, e.g., spent nuclear fuel, due to high radiation levels. Microfluidic E-cells offer advantages such as reduced radiation exposure, control over fluid flow rates, and high-throughput capabilities. Methods: The design of the E-cell considers electrode morphology, adhesion to a thin membrane, electrode configuration, and vacuum compatibility. Three techniques, including FIB-SEM lift-out, Au coating, and polyvinylidene fluoride (PVDF) binder, are explored for fabricating and attaching microgram quantities of UO 2 as working electrodes. The PVDF binder method proves to be the most effective, enabling the creation of a vacuum-compatible microfluidic E-cell. Results and discussion: The PVDF binder method demonstrates successful electrochemical responses and allows for real-time monitoring of UO 2 electrode behavior at the microscale. It offers chemical imaging capabilities using in situ SEM/EDS analysis. The technique provides consistent redox outcomes similar to bulk electrochemical analysis. Conclusion: The development of a microgram-scale microfluidic electrochemical cell using the PVDF binder technique enables the investigation of UO 2 redox behavior. It offers a low-risk approach with reduced radiation exposure and high-throughput capabilities. The technique provides real-time monitoring and chemical imaging capabilities, making it valuable for studying spent nuclear fuel systems and material characterization.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2007

Developing Carbon Nanotube Standards at NASA

Single wall carbon nanotubes (SWCNTs) are currently being produced and processed by several methods. Many researchers are continuously modifying existing methods and developing new methods to incorporate carbon nanotubes into other materials and utilize the phenomenal properties of SWCNTs. These applications require availability of SWCNTs with known properties and there is a need to characterize these materials in a consistent manner. In order to monitor such progress, it is critical to establish a means by which to define the quality of SWCNT material and develop characterization standards to evaluate of nanotube quality across the board. Such characterization standards should be applicable to as-produced materials as well as processed SWCNT materials. In order to address this issue, NASA Johnson Space Center has developed a protocol for purity and dispersion characterization of SWCNTs. The NASA JSC group is currently working with NIST, ANSI and ISO to establish purity and dispersion standards for SWCNT material. A practice guide for nanotube characterization is being developed in cooperation with NIST. Furthermore, work is in progress to incorporate additional characterization methods for electrical, mechanical, thermal, optical and other properties of SWCNTs.

Nikolaev, Pasha↗

NASA NTRS2007

Developing Carbon Nanotube Standards at NASA

Single wall carbon nanotubes (SWCNTs) are currently being produced and processed by several methods. Many researchers are continuously modifying existing methods and developing new methods to incorporate carbon nanotubes into other materials and utilize the phenomenal properties of SWCNTs. These applications require availability of SWCNTs with known properties and there is a need to characterize these materials in a consistent manner. In order to monitor such progress, it is critical to establish a means by which to define the quality of SWCNT material and develop characterization standards to evaluate of nanotube quality across the board. Such characterization standards should be applicable to as-produced materials as well as processed SWCNT materials. In order to address this issue, NASA Johnson Space Center has developed a protocol for purity and dispersion characterization of SWCNTs (Ref.1). The NASA JSC group is currently working with NIST, ANSI and ISO to establish purity and dispersion standards for SWCNT material. A practice guide for nanotube characterization is being developed in cooperation with NIST (Ref.2). Furthermore, work is in progress to incorporate additional characterization methods for electrical, mechanical, thermal, optical and other properties of SWCNTs.

Nikolaev, Pasha↗

NASA NTRS2019

NASA’s In-Space Manufacturing Project: Update on Manufacturing Technologies and Materials to Enable More Sustainable and Safer Exploration

NASA’s In-Space Manufacturing (ISM) project seeks to develop the materials, processes, and manufacturing technologies needed to provide an on-demand manufacturing capability for deep space exploration missions. The ability to manufacture and recycle some parts on demand rather than launch them from earth has the potential to reduce logistics requirements on long duration missions and enhance crew safety. With the launch of the first 3D printer (built and operated by Made in Space through a Small Business Innovative Research – SBIR -- contract) to the International Space Station (ISS) in 2014, the ISM project demonstrated the feasibility of operating an on-demand manufacturing system in a microgravity environment. This paper will provide an update on recent advancements in ISM under three key technology areas: manufacturing, recycling, and development of a design database. ISM continues to pursue development of manufacturing technologies for space applications and use the ISS as a critical test bed to prove out these technologies before deploying them on next generation exploration systems. Activities under this focus area include: characterization of materials manufactured using the Additive Manufacturing Facility (AMF), the second generation commercial 3D-printer on ISS, also owned and operated by Made in Space; development of prototype payloads for metal manufacturing through phase II SBIR contracts with Tethers Unlimited, Made in Space, and Ultra Tech Machinery; development of a multi-material fabrication laboratory capable of processing metals and providing inspection of manufactured parts through a Broad Agency Announcement (Techshot, Interlog, and Tethers Unlimited); an in-line sensing system for ISM platforms; and development of higher strength feedstocks for 3D polymer printers. In the area of recycling, the Tethers Unlimited Refabricator payload (an integrated 3D printer and recycler for ULTEM 9085) launched to ISS in November 2018 and began operating in early 2019. This payload represents the first demonstration of on-orbit recycling; down massed specimens will assess material degradation in the polymer over multiple recycling cycles to define limits on material re-use. Other work in the recycling area includes development of common use materials intended to be reused and recycled on space missions (Tethers Unlimited and Cornerstone Research Group) and a sterilization capability for multiple-use materials (ERASMUS from Tethers Unlimited). Concurrent with manufacturing technology and materials development work is creation of a design database, a curated list of parts that can be manufactured using the suite of In-Space Manufacturing capabilities.

Tracie Prater↗

NASA NTRS1992

Permeability of rayon based polymer composites

Several types of anomalous rayon based phenolic behavior have been observed in post-fired nozzles and exit cones. Many of these events have been shown to be related to the development of internal gas pressure within the material. The development of internal gas pressure is a function of the amount of gas produced within the material and the rate at which that gas is allowed to escape. The latter property of the material is referred to as the material's permeability. The permeability of two dimensional carbonized rayon based phenolic composites is a function of material direction, temperature, and stress/strain state. Recently significant differences in the permeability of these materials has been uncovered which may explain their inconsistent performance. This paper summarizes what is known about the permeability of these materials to date and gives possible implications of these finding to the performance of these materials in an ablative environment.

Stokes, E. H.↗

DOE OSTI2017

Plasma source development for fusion-relevant material testing

Plasma facing materials in the divertor of a magnetic fusion reactor will have to tolerate steady-state plasma heat fluxes in the range of 10 MW/m2 for ~107 sec, in addition to fusion neutron fluences, which can damage the plasma facing materials to high displacements per atom (dpa) of ~50 dpa . Material solutions needed for the plasma facing components are yet to be developed and tested. The Materials Plasma Exposure eXperiment (MPEX) is a newly proposed steady state linear plasma device that is designed to deliver the necessary plasma heat flux to a target for this material testing, including the capability to expose a-priori neutron damaged material samples to those plasmas. The requirements of the plasma source needed to deliver this plasma heat flux are being developed on the Proto-MPEX device, which is a linear high-intensity radio frequency (RF) plasma source that combines a high-density helicon plasma generator with electron and ion heating sections. It is being used to study the physics of heating over-dense plasmas in a linear configuration. The helicon plasma is operated at 13.56 MHz with RF power levels up to 120 kW. Microwaves at 28 GHz (~30 kW) are coupled to the electrons in the over-dense helicon plasma via Electron Bernstein Waves (EBW), and ion cyclotron heating at 7-9 MHz (~30 kW) is via a magnetic beach approach. High plasma densities >6x1019/m3 have been produced in deuterium, with electron temperatures that can range from 2 to >10 eV. Operation with on-axis magnetic field strengths between 0.6 and 1.4 T is typical. The plasma heat flux delivered to a target can be > 10 MW/m2, depending on the operating conditions.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2025

Development of Engine Valve Materials for Next Generation Higher Efficiency Engines

The growing demand to increase the performance and efficiency of light-, medium-, and heavy-duty engines continues to drive increases in combustion intensities and cylinder pressures, which result in higher exhaust gas temperatures. Thus, there is a critical need for new materials that can meet the performance and cost targets for components such as exhaust valves which are exposed to these higher exhaust gas temperatures. Oak Ridge National Laboratory (ORNL) has developed several lower-cost, high-strength alloys that have the potential to be adopted into intake and/or exhaust valves in the next generation, high-efficiency engines and other high temperature applications. These alloys are covered by two issued patents: 1. G. Muralidharan, U. S. Patent No. 9,605,565 B2, “Low-cost Fe--Ni--Cr alloys for high temperature valve applications,” March 28, 2017. 2. G. Muralidharan, U. S. Patent 9,752, 468 B2, “Low-Cost, High-Strength Fe-Ni-Cr Alloys for High Temperature Exhaust Valve Applications, Issued Sep. 5, 2017. The overall scope of this CRADA project was for Oak Ridge National Laboratory to collaborate with Tenneco Powertrain to: 1) better define the properties required for intake and/or exhaust valves for next generation vehicles, 2) fabricate industrial scale heats of alloys down-selected from existing patents, 3) generate critical high temperature property data that will help evaluate the suitability of these new alloys for high temperature intake and/or exhaust valves, and finally to 4) fabricate and evaluate the performance of prototype intake/and or exhaust valves.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

NASA NTRS1996

PICA Forebody Heatshield Qualification for the Stardust Discovery Class Mission

This paper presents the qualification of the light weight Phenolic Impregnated Carbon Ablators (PICA) as the forebody heatshield for the Stardust Discovery Class Mission. The Stardust spacecraft will be launched in early 1999 and fly by Comet Wild-2 to collect cometary and interstellar dust and return them back to earth in the Sample Return Capsule (SRC). This earth re-entry will be the fastest to date, at 12.6 km/s, and therefore requires a heatshield that can withstand very high heating rates and stagnation pressures, as well as provide the necessary insulation to the vehicle structure. The PICA material was developed as part of the Lightweight Ceramic Ablators program at NASA Ames Research Center, and was baselined as the forebody heatshield because of its low density and superior ablation and thermal performance at severe aerothermodynamic conditions. Under a Small Business Innovative Research (SBIR) program with NASA Ames, Fiber Materials, Inc. developed a process to manufacture a single-piece PICA heatshield for the forebody of the SRC, along with witness material for the fabrication of the test models. The test models were fabricated and instrumented by the staff of Lockheed Martin Astronautics in Denver, Colorado. Full body preliminary aerothermal CFD calculations were performed at NASA Ames to determine the heating and stagnation pressure conditions. The Heat shield sizing was also performed at NASA Ames by using a new material response code that accounts for the highly porous characteristics of the PICA material. The ablation and thermal performance of PICA was qualified in the NASA Ames Interaction Heating Arc Jet Facility. A total of 24 models and four test conditions were used to qualify PICA at the predicted peak heat flux, heat load, shear, and stagnation pressure conditions. Surface and in-depth temperatures were measured using optical pyrometers and thermocouples. Surface recession was measured by using a template and a height gage. Several models were tested to evaluate repair procedures, and two models were cold soaked in liquid nitrogen, prior th testing, to investigate the effect of the cold space environment on the performance of the material. In addition, material cored from a demonstration single-piece heatshield was tested to verify that the PICA process can be successfully completed on a large, complex heatshield shape.

Tran, Huy K.↗

DOE OSTI2019

Review of high-throughput approaches to search for piezoelectric nitrides

Piezoelectric materials are commonplace in modern devices, and the prevalence of these materials is poised to increase in the years to come. The majority of known piezoelectrics are oxide materials, due in part to the related themes of a legacy of ceramists building off of mineralogical crystallography and the relative simplicity of fabricating oxide specimens. However, diversification beyond oxides offers exciting opportunities to identify and develop new materials perhaps better suited for certain applications. Aluminum nitride (and recently, its Sc-modified derivative) is the only commercially integrated piezoelectric nitride in use today, although this is likely to change in the near future with increased use of high-throughput techniques for materials discovery and development. This review covers modern methods—both computational and experimental—that have been developed to explore chemical space for new materials with targeted characteristics. Here, the authors focus on the application of computational and high-throughput experimental approaches to discovering and optimizing piezoelectric nitride materials. While the focus of this review is on the search for and development of new piezoelectric nitrides, most of the research approaches discussed in this article are both chemistry- and application-agnostic.

36 MATERIALS SCIENCE↗

DOE OSTI2024

A review of antimicrobial implications for improving indoor air quality

The frequent outbreak of infectious respiratory diseases, such as the recent COVID-19 epidemic, raised the importance of indoor air quality. Removing microorganisms from indoor air is critical to improve indoor air quality. Numerous studies in recent years have been published on developing antimicrobial materials and technologies for antibacterial and antiviral applications. Further, this study critically reviews the recent antimicrobial advances for improving indoor air quality. This paper provides a comprehensive analysis of the antimicrobial mechanisms, development of materials, and deployment strategies, as well as a performance evaluation of the antimicrobial implication for indoor air quality. Furthermore, the challenges and opportunities of future research directions are also highlighted.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2025

The Path towards Plasma Facing Components: A Review of State-of-the-art in W-Based Refractory High-Entropy Alloys

Developing advanced materials for plasma-facing components (PFCs) in fusion reactors is a crucial aspect for achieving sustained energy production. Tungsten (W) - based refractory high-entropy alloys (RHEAs) have emerged as promising candidates due to their superior radiation tolerance and high-temperature strength. This review paper will focus on recent advancements in W-based RHEA research, particularly emphasizing the key role of modelling using machine learning (ML) in the stage of discovery by predicting properties for each composition and expediting the identification of optimal RHEA compositions with desired properties. Additionally, the application of additive manufacturing (AM) techniques for fabricating W-based RHEAs is explored, highlighting their advantages for rapid prototyping and multi-compositional sample production in a high throughput manner. The review critically evaluates the current understanding of mechanical properties relevant to PFC applications, including high-temperature strength and ductility. Furthermore, the radiation tolerance of W-based RHEAs under irradiated conditions is discussed. Finally, the validity of current AM-manufactured W-based RHEAs as PFC materials is assessed, and key challenges and opportunities for future research are identified. This review aims to provide a comprehensive overview of W-based RHEAs for fusion applications and their potential to guide the development and validation of advanced refractory high entropy alloys.

Hatler, Caleb [University of Wisconsin-Madison]↗

DOE OSTI2018

Final report for Assembling Microorganisms into Energy Converting Materials

The goal of this project was to integrate microorganisms capable of reversible energy transduction in response to changing relative humidity with non-biological materials to create hybrid energy conversion systems. While plants and many other biological organisms have developed structures that are extraordinarily effective in converting changes in relative humidity into mechanical energy, engineered energy transduction systems rarely take advantage of this powerful phenomenon. Rather than developing synthetic materials that can convert changes in relative humidity in to mechanical energy, we developed approaches to assemble bacterial spores into larger materials. These materials can convert energy from evaporation of water in dry atmospheric conditions, which we demonstrated by building energy harvesters from these materials. We have also developed experiments to investigate the interaction of water with the spore material, and to determine how this interaction imposes limits on energy conversion. In addition, we carried out theoretical calculations to investigate the limits imposed by the environmental conditions to the power available in the energy harvesting process. These calculations took into account heat and water vapor transfer in the atmosphere surrounding the spore based materials. Overall, our results suggest that biomolecular materials are promising candidates to convert energy from evaporation.

36 MATERIALS SCIENCE↗

NASA NTRS1966

Development of sensors to obtain in-flight ablation measurements of thermal-protection materials

Design and development of sensors for measuring ablative changes in space vehicle heat shield during reentry phase

ABLATION↗

NASA NTRS1995

Textile technology development

The objectives of this report were to evaluate and select resin systems for Resin Transfer Molding (RTM) and Powder Towpreg Material, to develop and evaluate advanced textile processes by comparing 2-D and 3-D braiding for fuselage frame applications and develop window belt and side panel structural design concepts, to evaluate textile material properties, and to develop low cost manufacturing and tooling processes for the automated manufacturing of fuselage primary structures. This research was in support of the NASA and Langley Research Center (LaRc) Advanced Composite Structural Concepts and Materials Technologies for Primary Aircraft Structures program.

Shah, Bharat M.↗