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DOE OSTI2024

Solar Thermochemical Carbon Dioxide Splitting Using Ceria and Iron Aluminate Foam Devices and Simulation of a Plant System for Demonstration

An international research project has been undertaken to integrate a unique solar thermal processing reactor system with ceria and iron aluminate as active redox materials for CO2 splitting. Experimental investigations for CO2 splitting were conducted using a solar simulator and tube furnace at Niigata University, followed by demonstrations using a high-flux solar furnace (HFSF) at the National Renewable Energy Laboratory (NREL) in Golden, CO. Each experimental setup consisted of foam devices composed of reticulated porous ceramic (RPC). The RPC has a full ceria or iron aluminate body. It fabricated using the replica method and subjected to a two-step redox reaction, which iteratively separated a stream of CO2 into O2 and CO. Reactivity was evaluated using CO production per mass of the reactive material. The tubular furnace yielded a CO production of 6.41 mL/g at a reduction temperature of 1600degrees C, showcasing a higher CO production rate and total amount than those obtained from experiments conducted with solar simulators and solar furnace setups. For iron aluminate RPC, the productivity was measured as 3.57 mL/g using HFSF at a reduction temperature of 1450degrees C. These results are somewhat higher than those of the previous experiment at lower reduction temperatures of 1400degrees C-1500degrees C. Additionally, the production of CO in the case of ceria RPC was compared with the steady flow model simulation, which assumed chemical equilibrium at various levels of oxygen partial pressure during the reduction process. On the basis of these results, this study proposes a solar fuel system with an open receiver that uses a high-temperature heat transfer fluid.

carbon dioxide thermochemical splitting↗

NASA NTRS1999

Monte Carlo Simulation of Nanoparticle Encapsulation in Flames

Two critical challenges facing the application of flames for synthesis of nanopowder materials are: (1) overcoming formation of agglomerates and (2) ensuring that the highly reactive nanopowders that are synthesized in flames can be produced in such a manner that their purity is maintained during subsequent processing. Agglomerates are produced in flames because particle formation occurs in a high temperature and high number density environment. They are undesirable in most advanced applications of powders. For example, agglomerates have a deleterious effect on compaction density, leading to voids when nanopowders are consolidated. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Powder purity must also be maintained during subsequent handling of nanopowders and this poses a significant challenge for any synthesis route because nanopowders, particularly metals and non-oxide ceramic powders, are inherently reactive. Impurities acquired during handling of nanopowders have slowed the advancement of the nanostructured materials industry. One promising approach that has been proposed to address these problems is nano-encapsulation. In this approach, the core particles are encapsulated in a removable material while they are within the flame but before excessive agglomeration has occurred. Condensation can be very rapid so that core particles are trapped within the condensed material and agglomeration is limited. Nano-encapsulation also addresses the handling concerns for post-synthesis processing. Results have shown that when nano-encapsulated powders are exposed to atmosphere the core particles are protected from oxidation and/or hydrolysis. Thus, handling of the powders does not require extreme care. If, for example, at the time of consolidation the encapsulation material is removed by vacuum annealing, the resulting powder remains unagglomerated and free of impurities. In this work, we described a novel aerosol model that has been developed to simulate particle encapsulation in flames. The model will ultimately be coupled to a one-dimensional spherical flame code and compared to results from microgravity flame experiments.

Sun, Z.↗

DOE OSTI2019

Infiltration studies of additive manufacture of WC with Co using binder jetting and pressureless melt method

Additive manufacturing (AM) of tungsten carbide-cobalt (WC-Co) is explored starting with WC preforms shaped with binder jet additive manufacturing (BJAM) followed by melt infiltration of Co. The research objective is to demonstrate the ability to net-shape WC-Co composites through BJAM of a WC preform followed by backfilling with cobalt via pressureless infiltration. This method also has the potential to minimize shrinkage and grain growth compared to other AM techniques. The effects of sintering, Co content, and infiltration time on the net shaping and properties of processed composites are shown. The best shaped material had an average grain size of 5.1 μm, 32 vol.% Co, density of 98.54% theoretical, fracture toughness of 23.2 MPa m 1/2 , and hardness of 9.0 GPa. Data presented illustrates that the proposed approach results in favorable ceramic-metal (cermet) properties and is viable for fabricating cermets of other material combinations. Furthermore successful AM of cermets provides complex geometries, high throughout, and low costs.

36 MATERIALS SCIENCE↗

DOE OSTI2018

In situ observations of cracking in constrained sintering

Here in this article, we examine the long-standing problem of cracking during constrained sintering of a powder aggregate. Using binder jet 3D printing, we prepare ceramic green bodies in the form of center-notched panels, then use in situ imaging to observe how cracks nucleate and grow from the notch as the material sinters under restraint. Quantitative image analysis allows us to identify important characteristics of the sinter-cracking process, indicating a framework for analyzing the problem and developing methods for avoiding it, including representation of sinter-cracking as a creep crack growth process, use of fracture mechanics parameters to design specimen geometries that do not exceed critical stress intensities, and the possibility of exploiting the inherently ductile nature of sinter-cracking to mitigate damage.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Theory and modeling of active brazing.

Active brazes have been used for many years to produce bonds between metal and ceramic objects. By including a relatively small of a reactive additive to the braze one seeks to improve the wetting and spreading behavior of the braze. The additive modifies the substrate, either by a chemical surface reaction or possibly by alloying. By its nature, the joining process with active brazes is a complex nonequilibrium non-steady state process that couples chemical reaction, reactant and product diffusion to the rheology and wetting behavior of the braze. Most of the these subprocesses are taking place in the interfacial region, most are difficult to access by experiment. To improve the control over the brazing process, one requires a better understanding of the melting of the active braze, rate of the chemical reaction, reactant and product diffusion rates, nonequilibrium composition-dependent surface tension as well as the viscosity. This report identifies ways in which modeling and theory can assist in improving our understanding.

van Swol, Frank B.↗

DOE OSTI2015

Laboratory optimization tests of technetium decontamination of Hanford Waste Treatment Plant low activity waste melter off-gas condensate simulant

The Hanford Waste Treatment and Immobilization Plant (WTP) Low Activity Waste (LAW) vitrification facility will generate an aqueous condensate recycle stream (LAW Off-Gas Condensate) from the off-gas system. The baseline plan for disposition of this stream is to send it to the WTP Pretreatment Facility, where it will be blended with LAW, concentrated by evaporation and recycled to the LAW vitrification facility again. Alternate disposition of this stream would eliminate recycling of problematic components, and would enable simplified operation of the LAW melter and the Pretreatment Facilities. Eliminating this stream from recycling within WTP would also decrease the LAW vitrification mission duration and quantity of glass waste.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS1985

Fabrication of ceramic components for advanced gas turbine engines

The AGT101 ceramic gas turbine engine feasibility study has made use of the slip casting of silicon or silicon nitride powders to produce either reaction-bonded or sintered components such as turbine rotors, turbine shrouds, and inner and outer diffusers. Attention is given to the effects of processing parameters on the microstructure and properties of the finished components; the parameters encompass powder particle size distribution, casting slip viscosity, pH, and solid content fraction. The green slip cast components were consolidated by nitriding, sintering, or sinter/HIPping.

Liu, F.↗

NASA NTRS1995

Thermally Stable, Piezoelectric and Pyroelectric Polymeric Substrates and Method Relating Thereto

Production of an electric voltage in response to mechanical excitation (piezoelectricity) or thermal excitation (pyroelectricity) requires a material to have a preferred dipole orientation in its structure. This preferred orientation or polarization occurs naturally in some crystals such as quartz and can be induced into some ceramic and polymeric materials by application of strong electric or mechanical fields. For some materials, a combination of mechanical and electrical orientation is necessary to completely polarize the material. The only commercially available piezoelectric polymer is poly(vinylidene fluoride) (PVF2). However, this polymer has material and process limitations which prohibit its use in numerous device applications where thermal stability is a requirement. By the present invention, thermally stable, piezoelectric and pyroelectric polymeric substrates were prepared from polymers having a softening temperature greater than 1000C. A metal electrode material is deposited onto the polymer substrate and several electrical leads are attached to it. The polymer substrate is heated in a low dielectric medium to enhance molecular mobility of the polymer chains. A voltage is then applied to the polymer substrate inducing polarization. The voltage is then maintained while the polymer substrate is cooled 'freezing in' the molecular orientation. The novelty of the invention resides in the process of preparing the piezoelectric and pyroelectric polymeric substrate. The nonobviousness of the invention is found in heating the polymeric substrate in a low dielectric medium while applying a voltage.

Simpson, Joycelyn O.↗

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 OSTI2017

Consumable core for manufacture of composite articles and related method

Systems, methods and devices adapted to ease manufacture of composite articles (e.g., ceramic composite articles), particularly composite articles which include a hollow feature are disclosed. In one embodiment, a system includes: a consumable core formed to be disposed within an inner portion of a composite precursor, the consumable core adapted to convert into an infiltrant during a manufacturing process and infiltrate the composite precursor.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Creep Performance of Novel Composite Heating Elements for Reheat Furnace Electrification

The iron and steel industry is critical for the modern world but is also very energy intensive and is a low margin industry. Hot rolling requires reheating steel slabs to ~1250 °C for hot rolling and involves yield loss due to scale formation. Electrification of this process using resistive heating could improve yield but is currently not possible due to the poor creep resistance of MoSi2 heating elements, which need to be operated well below their maximum temperatures when mounted horizontally. To solve this problem, novel MoSi2 composite heating elements with SiBCN ceramic reinforcements are being developed using high energy ball milling and spark plasma sintering. The creep performance of different heating elements and their corresponding microstructures and electrical properties will be presented.

36 - MATERIALS SCIENCE↗

NASA NTRS2017

MSRR Rack Materials Science Research Rack

The Materials Science Research Rack (MSRR) is a research facility developed under a cooperative research agreement between NASA and the European Space Agency (ESA) for materials science investigations on the International Space Station (ISS). The MSRR is managed at the Marshall Space Flight Center (MSFC) in Huntsville, AL. The MSRR facility subsystems were manufactured by Teledyne Brown Engineering (TBE) and integrated with the ESA/EADS-Astrium developed Materials Science Laboratory (MSL) at the MSFC Space Station Integration and Test Facility (SSITF) as part of the Systems Development Operations Support (SDOS) contract. MSRR was launched on STS-128 in August 2009, and is currently installed in the U. S. Destiny Laboratory Module on the ISS. Materials science is an integral part of developing new, safer, stronger, more durable materials for use throughout everyday life. The goal of studying materials processing in space is to develop a better understanding of the chemical and physical mechanisms involved, and how they differ in the microgravity environment of space. To that end, the MSRR accommodates advanced investigations in the microgravity environment of the ISS for basic materials science research in areas such as solidification of metals and alloys. MSRR allows for the study of a variety of materials including metals, ceramics, semiconductor crystals, and glasses. Materials science research benefits from the microgravity environment of space, where the researcher can better isolate chemical and thermal properties of materials from the effects of gravity. With this knowledge, reliable predictions can be made about the conditions required on Earth to achieve improved materials. MSRR is a highly automated facility with a modular design capable of supporting multiple types of investigations. Currently the NASA-provided Rack Support Subsystem provides services (power, thermal control, vacuum access, and command and data handling) to the ESA developed Materials Science Laboratory (MSL) which accommodates interchangeable Furnace Inserts (FI). Two ESA-developed FIs are presently available on the ISS: the Low Gradient Furnace (LGF) and the Solidification and Quenching Furnace (SQF). Sample-Cartridge Assemblies (SCAs), each containing one or more material samples, are installed in the FI by the crew and can be processed at temperatures up to 1400 C. Once an SCA is installed, the experiment can be run by automatic command or science conducted via telemetry commands from the ground. This facility is available to support materials science investigations through programs such as the US National Laboratory, Technology Development, NASA Research Announcements, and others. TBE and MSFC are currently developing NASA Sample Cartridge Assemblies (SCA's) with a planned availability for launch in 2017.

Reagan, Shawn↗

NASA NTRS2018

Cracking Problems and Mechanical Characteristics of PME and BME Ceramic Capacitors

Most failures in MLCCs are caused by cracking that create shorts between opposite electrodes of the parts. A use of manual soldering makes this problem especially serious for space industry. Experience shows that different lots of ceramic capacitors might have different susceptibility to cracking under manual soldering conditions. This simulates a search of techniques that would allow revealing capacitors that are most robust to soldering-induced stresses. Currently, base metal electrode (BME) capacitors are introduced to high-reliability applications as a replacement of precious metal electrode (PME) parts. Understanding the difference in the susceptibility to cracking between PME and BME capacitors would facilitate this process. This presentation gives a review of mechanical characteristics measured in-situ on MLCCs that includes flexural strength, Vickers hardness, indentation fracture toughness, and the board flex testing and compare characteristics of BME and PME capacitors. A history case related to cracking in PME capacitors that caused flight system malfunctions and mechanisms of failure are considered. Possible qualification tests that would allow evaluation of the resistance of MLCCs to manual soldering are suggested and perspectives related to introduction of BME capacitors discussed.

Reliability↗

DOE OSTI2019

Thermodynamic assessment of the hollandite high‐level radioactive waste form

Abstract Hollandite has been studied as a candidate ceramic waste form for the disposal of high‐level radioactive waste due to its inherent leach resistance and ability to immobilize alkaline‐earth metals such as Cs and Ba at defined lattice sites in the crystallographic structure. The chemical and structural complexity of hollandite‐type phases developed for high‐level waste immobilization limits the systematic experimental research that is required to understand phase development due to the large number of potential additives and compositional ranges that must be evaluated. Modeling the equilibrium behavior of the complex hollandite‐forming oxide waste system would aid in the design and processing of hollandite waste forms by predicting their thermodynamic stability. Thus, a BaO–Cs 2 O–TiO 2 –Cr 2 O 3 –Al 2 O 3 –Fe 2 O 3 –FeO–Ga 2 O 3 thermodynamic database was developed in this work according to the CALPHAD methodology. The compound energy formalism was used to model solid solution phases such as hollandite while the two‐sublattice partially ionic liquid model characterized the oxide melt. Results of model optimizations are presented and discussed including a 1473 K isothermal BaO–Cs 2 O–TiO 2 pseudo‐ternary diagram that extrapolates phase equilibrium behavior to regions not experimentally explored.

Utlak, Stephen A.↗

DOE OSTI2016

Biological Sampling Variability Study

There are many sources of variability that exist in the sample collection and analysis process. This paper addresses many, but not all, sources of variability. The main focus of this paper was to better understand and estimate variability due to differences between samplers. Variability between days was also studied, as well as random variability within each sampler. Experiments were performed using multiple surface materials (ceramic and stainless steel), multiple contaminant concentrations (10 spores and 100 spores), and with and without the presence of interfering material. All testing was done with sponge sticks using 10-inch by 10-inch coupons. Bacillus atrophaeus was used as the BA surrogate. Spores were deposited using wet deposition. Grime was coated on the coupons which were planned to include the interfering material (Section 3.3). Samples were prepared and analyzed at PNNL using CDC protocol (Section 3.4) and then cultured and counted. Five samplers were trained so that samples were taken using the same protocol. Each sampler randomly sampled eight coupons each day, four coupons with 10 spores deposited and four coupons with 100 spores deposited. Each day consisted of one material being tested. The clean samples (no interfering materials) were run first, followed by the dirty samples (coated with interfering material). There was a significant difference in recovery efficiency between the coupons with 10 spores deposited (mean of 48.9%) and those with 100 spores deposited (mean of 59.8%). There was no general significant difference between the clean and dirty (containing interfering material) coupons or between the two surface materials; however, there was a significant interaction between concentration amount and presence of interfering material. The recovery efficiency was close to the same for coupons with 10 spores deposited, but for the coupons with 100 spores deposited, the recovery efficiency for the dirty samples was significantly larger (65.9% - dirty vs. 53.6% - clean) (see Figure 4.1). Variance component analysis was used to estimate the amount of variability for each source of variability. There wasn’t much difference in variability for dirty and clean samples, as well as between materials, so these results were pooled together. There was a significant difference in amount of concentration deposited, so results were separated for the 10 spore and 100 spore deposited tests. In each case the within sampler variability was the largest with variances of 426.2 for 10 spores and 173.1 for 100 spores. The within sampler variability constitutes the variability between the four samples of similar material, interfering material, and concentration taken by each sampler. The between sampler variance was estimated to be 0 for 10 spores and 1.2 for 100 spores. The between day variance was estimated to be 42.1 for 10 spores and 78.9 for 100 spores. Standard deviations can be calculated in each case by taking the square root of the variance.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2024

UZrCN Formation via Arc Melting – A Novel Synthesis Study

The next generation of nuclear reactors for both power production and space nuclear propulsion require fuel that is more durable, thermally stable, and more thermally conductive to support rapid heat transfer. High temperature gas reactors (HTGR), advanced gas reactors (AGR), and space-based nuclear thermal propulsion (NTP) are advanced reactor concepts that require a fuel type that can withstand high temperatures (1000-2900K) and flow of corrosive gas coolants such as helium, hydrogen, and carbon dioxide. One fuel with the potential to meet these demanding requirements is uranium-zirconium-carbonitride (UZrCN). UZrCN has many favorable fuel qualities compared to other eligible fuel forms such as uranium dioxide (UO2) and uranium mononitride (UN) that could support the aforementioned reactor concepts. UZrCN has an exceptionally high operating temperature and thermal conductivity which are highly desirable to improve reactor economics and safety. It far exceeds the properties of UO2 which is the most common fuel form in the United States. UZrCN also surpasses UN in terms of thermal conductivity and operating temperature by eliminating the dissociation problem UN has at 1700K. UZrCN could improve gas reactor performance and enable NTP technologies; however, it is an under-researched fuel that lacks rigorous scientific study. In recent efforts by the Idaho National Laboratory, a variety of novel methods to produce this fuel composition have been explored. One such method is via arc melting of uranium, zirconium, and carbon under a nitrogen atmosphere. Alloy fabrication using arc melting has been utilized for close to 150 years now and is well-understood as a method for rapid alloy prototyping. This process will be used to perform in-situ nitriding to form UZrCN.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Update on ASME AG-1 and Revision of the DOE Nuclear Air Cleaning Handbook - 20536

The American Society of Mechanical Engineers AG-1 Code on Nuclear Air and Gas Treatment is updated every two years. This paper provides an overview of issues being discussed within AG-1 committee meetings and revisions that will be included in the next version of the code. Additional information is provided on issues being discussed ranging from media velocity limits, control of airflow using actual versus and standard cubic feet per minute. Navigation and identification of applicable high-efficiency particulate air (HEPA) filter code sections can be confusing for those unfamiliar with AG-1. A general reorganization of filtration code sections clarifies geometry, flow, and performance envelopes for nuclear grade HEPA filters. The initial step consists of establishment of Section FN covering qualification of conventional, ceramic, metal, and high strength fibrous glass media. Future filter sections are currently expected to be characterized by geometry and flow direction (axial vs. radial). The Department of Energy's (DOE) Nuclear Air Cleaning Handbook (NACH) is also undergoing revision. An update on the status of that effort, along with issues and changes being considered. The original charter of the AG-1 Code was specific to commercial nuclear power plants, and to safety-related air cleaning systems. This has evolved over the years to include normal non-safety ventilation systems and process gas systems. Corollary guidance for DOE facilities has been available in several editions of the Nuclear Air Cleaning Handbook, starting with ORNL-NSIC 65. The latest edition of the Handbook, 2003, is undergoing revision and modifications. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Accurate additive manufacturing of lightweight and elastic carbons using plastic precursors

Despite groundbreaking advances in the additive manufacturing of polymers, metals, and ceramics, scaled and accurate production of structured carbons remains largely underdeveloped. This work reports a simple method to produce complex carbon materials with very low dimensional shrinkage from printed to carbonized state (less than 4%), using commercially available polypropylene precursors and a fused filament fabrication-based process. The control of macrostructural retention is enabled by the inclusion of fiber fillers regardless of the crosslinking degree of the polypropylene matrix, providing a significant advantage to directly control the density, porosity, and mechanical properties of 3D printed carbons. Using the same printed plastic precursors, different mechanical responses of derived carbons can be obtained, notably from stiff to highly compressible. This report harnesses the power of additive manufacturing for producing carbons with accurately controlled structure and properties, while enabling great opportunities for various applications.

36 MATERIALS SCIENCE↗

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