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All sourcesNASA NTRSDOE OSTI
NASA NTRS1996

Testing of electroformed deposited iridium/powder metallurgy rhenium rockets

High-temperature, oxidation-resistant chamber materials offer the thermal margin for high performance and extended lifetimes for radiation-cooled rockets. Rhenium (Re) coated with iridium (Ir) allow hours of operation at 2200 C on Earth-storable propellants. One process for manufacturing Ir/Re rocket chambers is the fabrication of Re substrates by powder metallurgy (PM) and the application of Ir coatings by using electroformed deposition (ED). ED Ir coatings, however, have been found to be porous and poorly adherent. The integrity of ED Ir coatings could be improved by densification after the electroforming process. This report summarizes the testing of two 22-N, ED Ir/PM Re rocket chambers that were subjected to post-deposition treatments in an effort to densify the Ir coating. One chamber was vacuum annealed, while the other chamber was subjected to hot isostatic pressure (HIP). The chambers were tested on gaseous oxygen/gaseous hydrogen propellants, at mixture ratios that simulated the oxidizing environments of Earth-storable propellants. ne annealed ED Ir/PM Re chamber was tested for a total of 24 firings and 4.58 hr at a mixture ratio of 4.2. After only 9 firings, the annealed ED Ir coating began to blister and spall upstream of the throat. The blistering and spalling were similar to what had been experienced with unannealed, as-deposited ED Ir coatings. The HIP ED Ir/PM Re chamber was tested for a total of 91 firings and 11.45 hr at mixture ratios of 3.2 and 4.2. The HIP ED Ir coating remained adherent to the Re substrate throughout testing; there were no visible signs of coating degradation. Metallography revealed, however, thinning of the HIP Ir coating and occasional pores in the Re layer upstream of the throat. Pinholes in the Ir coating may have provided a path for oxidation of the Re substrate at these locations. The HIP ED Ir coating proved to be more effective than vacuum annealed and as-deposited ED Ir. Further densification is still required to match the integrity of chemically vapor deposited Ir coatings. Despite this, the successful long duration testing of the HIP ED Ir chamber, in an oxidizing environment comparable to Earth-storable propellants, demonstrated the viability of this Ir/Re rocket fabrication process.

Reed, Brian D.↗
NASA NTRS1999

Testing of Densified Liquid Hydrogen Stratification in a Scale Model Propellant Tank

Propellant densification has been identified as a critical technology in the development of a single stage to orbit (SSTO) launch vehicle. The densification of cryogenic propellant through sub-cooling allows more propellant to be stored in a given volume. This allows for higher propellant mass fractions than would otherwise be possible with conventional, normal boiling point, cryogenic fluids. One critical step in determining the viability of densified propellant technology for launch vehicles is to perform the sequential process necessary to load a propellant tank with densified propellants. This paper describes a test program that was conducted at NASA to demonstrate the ability to load densified LH2 into a sub-scale propellant rank. This work was done through a collaborative effort between NASA Lewis Research Center and the Lockheed Martin Michoud Space Systems (LMMSS). The tank, is made from composite materials similar to that to be used on X-33, is formed from two lobes with a center seprum. Test results are shown for data that was collected on filling the sub-scale tank with densified liquid hydrogen propellant that was produced at the NASA Plum Brook Station. Data is compared to analytical predictions.

Greene, W. D.↗
NASA NTRS2009

Gauging Systems Monitor Cryogenic Liquids

Rocket fuel needs to stay cool - super cool, in fact. The ability to store gas propellants like liquid hydrogen and oxygen at cryogenic temperatures (below -243 F) is crucial for space missions in order to reduce their volumes and allow their storage in smaller (and therefore, less costly) tanks. The Agency has used these cryogenic fluids for vehicle propellants, reactants, and life support systems since 1962 with the Centaur upper stage rocket, which was powered with liquid oxygen and liquid hydrogen. During proposed long-duration missions, super-cooled fluids will also be used in space power systems, spaceports, and lunar habitation systems. In the next generation of launch vehicles, gaseous propellants will be cooled to and stored for extended periods at even colder temperatures than currently employed via a process called densification. Densification sub-cools liquids to temperatures even closer to absolute zero (-459 F), increasing the fluid s density and shrinking its volume beyond common cryogenics. Sub-cooling cryogenic liquid hydrogen, for instance, from 20 K (-423 F) to 15 K (-432.4 F) reduces its mass by 10 percent. These densified liquid gases can provide more cost savings from reduced payload volume. In order to benefit from this cost savings, the Agency is working with private industry to prevent evaporation, leakage, and other inadvertent loss of liquids and gases in payloads - requiring new cryogenic systems to prevent 98 percent (or more) of boil-off loss. Boil-off occurs when cryogenic or densified liquids evaporate, and is a concern during launch pad holds. Accurate sensing of propellants aboard space vehicles is also critical for proper engine shutdown and re-ignition after launch, and zero boil-off fuel systems are also in development for the Altair lunar lander.

Source record↗
NASA NTRS2011

High temperature strain gages

A ceramic strain gage based on reactively sputtered indium-tin-oxide (ITO) thin films is used to monitor the structural integrity of components employed in aerospace propulsion systems operating at temperatures in excess of 1500.degree. C. A scanning electron microscopy (SEM) of the thick ITO sensors reveals a partially sintered microstructure comprising a contiguous network of submicron ITO particles with well defined necks and isolated nanoporosity. Densification of the ITO particles was retarded during high temperature exposure with nitrogen thus stabilizing the nanoporosity. ITO strain sensors were prepared by reactive sputtering in various nitrogen/oxygen/argon partial pressures to incorporate more nitrogen into the films. Under these conditions, sintering and densification of the ITO particles containing these nitrogen rich grain boundaries was retarded and a contiguous network of nano-sized ITO particles was established.

Gregory, Otto J.↗
NASA NTRS2009

Experimental Results of Integrated Refrigeration and Storage System Testing

Launch operations engineers at the Kennedy Space Center have identified an Integrated Refrigeration and Storage system as a promising technology to reduce launch costs and enable advanced cryogenic operations. This system uses a close cycle Brayton refrigerator to remove energy from the stored cryogenic propellant. This allows for the potential of a zero loss storage and transfer system, as well and control of the state of the propellant through densification or re-liquefaction. However, the behavior of the fluid in this type of system is different than typical cryogenic behavior, and there will be a learning curve associated with its use. A 400 liter research cryostat has been designed, fabricated and delivered to KSC to test the thermo fluid behavior of liquid oxygen as energy is removed from the cryogen by a simulated DC cycle cryocooler. Results of the initial testing phase focusing on heat exchanger characterization and zero loss storage operations using liquid oxygen are presented in this paper. Future plans for testing of oxygen densification tests and oxygen liquefaction tests will also be discussed. KEYWORDS: Liquid Oxygen, Refrigeration, Storage

Notardonato, W. U.↗
NASA NTRS2015

Methodology for Producing a Uniform Distribution of UO2 in a Tungsten Matrix

Current work at NASA's Marshall Space Flight Center (MSFC) is focused on the development CERMET fuel materials for Nuclear Thermal Propulsion (NTP). The CERMETs consist of uranium dioxide (UO2) fuel particles embedded in a tungsten (W) metal matrix. Initial testing of W-UO2 samples fabricated from fine angular powders performed reasonably well, but suffered from significant fuel loss during repeated thermal cycling due to agglomeration of the UO2 (1). The blended powder mixtures resulted in a non-uniform dispersion of the UO2 particles in the tungsten matrix, which allows rapid vaporization of the interconnected UO2 from the sample edges into the bulk material. Also, the angular powders create areas of stress concentrations due to thermal expansion mismatch, which eventually cracks the tungsten matrix. Evenly coating spherical UO2 particles with chemical vapor deposited (CVD) tungsten prior to consolidation was previously demonstrated to provide improved performance. However, the CVD processing technology is expensive and not currently available. In order to reduce cost and enhance performance, a powder coating process has been developed at MSFC to produce a uniform distribution of the spherical UO2 particles in a tungsten matrix. The method involves utilization of a polyethylene binder during mixing which leads to fine tungsten powders clinging to the larger UO2 spherical particles. This process was developed using HfO2 as a surrogate for UO2. Enough powder was mixed to make 8 discs (2cm diameter x 8mm thickness) using spark plasma sintering. A uniaxial pressure of 50 MPa was used at four different temperatures (2 samples at each temperature). The first two samples were heated to 1400C and 1500C respectively for 5 minutes. Densities for these samples were less than 85% of theoretical, so the time at temperature was increased to 20 minutes for the remaining samples. The highest densities were achieved for the two samples sintered at 1700C (approx. 92% of theoretical). Scanning electron microscopy (SEM) of the mixed powders and the sintered samples along with energy dispersive x-ray analysis was obtained. The SEM of the powders clearly show the fine W powder adhered to the larger HfO2 particles and a uniform distribution of HfO2 particles in a tungsten matrix upon densification. Vicker's Microhardness testing was also performed on all samples using 0.5, 1.0 and 2.0 kg loads. Five indents were made at each load level. All indents were placed in the tungsten matrix to assist as a proxy in measuring densification. The highest hardness value was obtained for the 1700C specimens. The hardness average for these samples was 312.14 MPa. This powder processing method has been applied to W/UO2 powders with the SEM of the powders appearing similar to the W/HfO2 powder images.

Tucker, Dennis S.↗
NASA NTRS2018

Transient Modeling of Large Scale Integrated Refrigeration and Storage Systems

Recently, next generation techniques and designs were demonstrated using Integrated Refrigeration and Storage (IRAS) for large scale storage of liquid hydrogen at NASA Kennedy Space Center (KSC) in Florida. Zero boil-off, densification, and in-situ liquefaction of hydrogen were achieved at various fill levels inside a custom-built 125,000 liter, horizontal-cylindrical IRAS tank, validating the applicability of the concept for large scale cryo-fluid storage architectures. This paper will discuss a number of transient physics models developed to predict the bulk behavior of large IRAS systems, and the comparison of those models to data gathered during the KSC test campaign. In an attempt to extent their usefulness to future IRAS designs, these models were agnostic with respect to stored fluid, tank size and geometry. Behavior during densification testing was examined at three fill levels, and ultimately the depressurization and bulk temperature trends of the KSC tests were predicted with good accuracy.

Swanger, Adam M.↗
NASA NTRS2018

Transient Modeling of Large Scale Integrated Refrigeration and Storage Systems

Recently, next generation techniques and designs were demonstrated using Integrated Refrigeration and Storage (IRAS) for large scale storage of liquid hydrogen at NASA Kennedy Space Center (KSC) in Florida. Zero boil-off, densification, and in-situ liquefaction of hydrogen were achieved at various fill levels inside a custom-built 125,000 liter, horizontal-cylindrical IRAS tank, validating the applicability of the concept for large scale cryo-fluid storage architectures. This paper will discuss a number of transient physics models developed to predict the bulk behavior of large IRAS systems, and the comparison of those models to data gathered during the KSC test campaign. In an attempt to extent their usefulness to future IRAS designs, these models were agnostic with respect to stored fluid, tank size and geometry. Behavior during densification testing was examined at three fill levels, and ultimately the depressurization and bulk temperature trends of the KSC tests were predicted with good accuracy.

Swanger, Adam M.↗
NASA NTRS2018

Large Scale Cryogenic Storage with Active Refrigeration

Storage and transfer of cryogenic liquefied gases on volume scales from under 10 liters for lab use, up to hundreds of millions of liters for industrial applications is of paramount importance across a vast range of industries. Traditionally, these commodities have been stored at or near the normal boiling point due to relative ease of operation and safety-related considerations; however, this also means that some percentage will always be lost due to environmental heat leaking into the vessel and causing boil-off. These losses become more concerning as scales increase, and are of particular importance for high-cost commodities such helium and hydrogen. Additionally, the normal boiling point marks the highest liquid density achievable; which becomes a strong driver of end-use system designs such as space launch vehicles. Recent development and testing of an Integrated Refrigeration and Storage (IRAS) system for liquid hydrogen has proven that next generation cryogenic storage operations such as zero boil-off and densification are feasible on a large scale. This IRAS system married an 850 Watt at 20 Kelvin reverse-Brayton cycle commercial cryogenic refrigerator with a 125,000 liter LH2 storage tank via and internal tubular heat exchanger. This allowed heat to be removed directly from the hydrogen, and by extension, provided a means to control the bulk thermodynamic state. Zero boil-off, in-situ liquefaction, and densification down to the triple point was performed during testing, and data such as fluid temperature profiles and tank pressure were gathered. Details regarding the design, setup, and testing of the IRAS system are discussed herein, and the data used to anchor various physics models created to predict the behavior of the system during transient and steady state operation. It is hoped that these efforts will provide a useful basis for the design and implementation of future large scale IRAS systems across numerous industries.

Swanger, Adam M.↗
NASA NTRS2021

Physics-Based SNOWPACK Model Improves Representation of Near-Surface Antarctic Snow and Firn Density

Estimates of snow and firn density are required for satellite-altimetry-based retrievals of ice sheet mass balance that rely on volume-to-mass conversions. Therefore, biases and errors in presently used density models confound assessments of ice sheet mass balance and by extension ice sheet contribution to sea level rise. Despite this importance, most contemporary firn densification models rely on simplified semi-empirical methods, which are partially reflected by significant modeled density errors when compared to observations. In this study, we present a new drifting-snow compaction scheme that we have implemented into SNOWPACK, a physics-based land surface snow model. We show that our new scheme improves existing versions of SNOWPACK by increasing simulated near-surface (defined as the top 10 m) density to be more in line with observations (near-surface bias reduction from −44.9 to −5.4 kg m−3). Furthermore, we demonstrate high-quality simulation of near-surface Antarctic snow and firn density at 122 observed density profiles across the Antarctic ice sheet, as indicated by reduced model biases throughout most of the near-surface firn column when compared to two semi-empirical firn densification models (SNOWPACK mean bias=−9.7 kg m−3, IMAU-FDM mean bias=−32.5 kg m−3, GSFC-FDM mean bias=15.5 kg m−3). Notably, our analysis is restricted to the near surface where firn density is most variable due to accumulation and compaction variability driven by synoptic weather and seasonal climate variability. Additionally, the GSFC-FDM exhibits lower mean density bias from 7–10 m (SNOWPACK bias=−22.5 kg m−3, GSFC-FDM bias=10.6 kg m−3) and throughout the entire near surface at high-accumulation sites (SNOWPACK bias=−31.4 kg m−3, GSFC-FDM bias=−4.7 kg m−3). However, we found that the performance of SNOWPACK did not degrade when applied to sites that were not included in the calibration of semi-empirical models. This suggests that SNOWPACK may possibly better represent firn properties in locations without extensive observations and under future climate scenarios, when firn properties are expected to diverge from their present state.

Eric Keenan↗
NASA NTRSDate not supplied

Phase Transitions and Melting in the Venusian Basaltic Crust: Implications for Crustal Recycling

Understanding phase transitions and melting in the Venusian crust and the associated changes in density are critical to constrain crustal thickness, recycling, and remelting processes. For example, average surface conditions on Venus of 92 bars and 460 °C correspond to low-grade metamorphic conditions on Earth equivalent to hornfels- and greenschist-facies. Further, the primary igneous mineralogy in the Venusian crust should be replaced by metamorphic minerals over time and potentially melt, as temperatures and pressures increase with depth along geothermal gradients. Here, we use Perple_X (Connolly, 2005), a Gibbs free energy minimization program to calculates table phase equilibria over a range of pressure and temperature conditions for whole-rock compositions of a dry basalt, alkali basalt, and peridotite. Further, we extract mineral abundancies along five geotherms of 5, 10, 15, 20 and 25 °C/km and calculate the rock density after the extraction of melt. On the coldest geotherm of 5 °C/km, melting would start at ~ 197 km and ~121 km in the basalt and alkali basalt, respectively, and therefore at depths that significantly exceed the estimated thickness of the Venusian crust (8-25 km). A density cross-over, where the crustal density would exceed that of the mantle could potentially induce delamination and is estimated to occur at ~ 40 km for both compositions. On the 10 °C/km geotherm, melting of the basalt starts at 65 km and melt extraction only causes a gradual densification due the formation of initially lower melt proportions. In contrast, the alkali basalt starts to melt at a depth of ~ 57 km and the subsequent densification of the residual composition could trigger delamination at ~ 60km depth. For hotter geotherms (i.e., 25 °C/km gradient), melting would occur at shallower depths of 21 – 23 km. However, the basalt will not get significantly denser than the mantle while the residuum of the alkali basalt would reach a density cross-over at 30 km. Hence, differences in Venusian crustal compositions can significantly influence the thickness of the crust on individual geotherms. Our results demonstrate that phase transitions and melting are strongly dependent on the assumed geotherm and could, combined with geodynamic models, further constrain crustal parameters.

Julia Semprich↗
NASA NTRS2022

Simulations of Firn Processes Over the Greenland and Antarctic Ice Sheets: 1980-2021

Conversion of altimetry-derived ice-sheet volume change to mass requires an understanding of the evolution of the combined ice and air content within the firn column. In the absence of suitable techniques to observe the changes to the firn column across the entirety of an ice sheet, the firn column processes are typically modeled. Here, we present new simulations of firn processes over the Greenland and Antarctic ice sheets (GrIS and AIS) using the Community Firn Model and atmospheric reanalysis variables for more than four decades. A data set of more than 250 measured depth–density profiles from both ice sheets provides the basis of the calibration of the dry-snow densification scheme. The resulting scheme results in a reduction in the rate of densification, relative to a commonly used semi-empirical model, through a decreased dependence on the accumulation rate, a proxy for overburden stress. The 1980–2020 modeled firn column runoff, when combined with atmospheric variables from MERRA-2, generates realistic mean integrated surface mass balance values for the Greenland (+390 Gt yr(exp −1)) and Antarctic (+2612 Gt yr(exp −1)) ice sheets when compared to published model-ensemble means. We find that seasonal volume changes associated with firn air content are on average approximately 2.5 times larger than those associated with mass fluxes from surface processes for the AIS and 1.5 times larger for the GrIS; however, when averaged over multiple years, ice and air-volume fluctuations within the firn column are of comparable magnitudes. Between 1996 and 2019, the Greenland Ice Sheet lost nearly 5% of its firn air content, indicating a reduction in the total meltwater retention capability. Nearly all (94 %) of the meltwater produced over the Antarctic Ice Sheet is retained within the firn column through infiltration and refreezing.

Greenland↗
NASA NTRSDate not supplied

Understanding thermal stability in doped zirconia aerogels for high temperature applications

The high porosities and low densities of ceramic aerogels offer outstanding insulative performance in applications where weight is a critical factor. The high surface-to-volume ratios and specific surface areas provide extremely low thermal conductivity, but also contribute to rapid densification of the pore structure at elevated temperatures. This densification diminishes their favorable properties and inhibits use of aerogels in high temperature applications. The purpose of this work is the establishment of a design framework for thermally stable, highly porous materials. Here we will review our recent studies on the effects of synthetic parameters and dopant chemistry on the evolution of zirconia-based aerogels. The structural evolution was studied to 1200 °C using nitrogen physisorption, scanning and transmission electron microscopy, and x-ray diffraction. The role of dopant identity and concentration in thermal stability was elucidated. In context of the design framework, dopant chemistry is an aggregate for many closely related material properties, each of which may contribute to aerogel structural evolution. To develop a truly predictive design framework for ceramic-based aerogels, systematic and comprehensive evaluation of thermodynamic and kinetic properties must be performed in conjunction with studies on structural evolution.

aerogel↗
NASA NTRS2023

An Evaluation of A Physics-Based Firn Model and A Semi-Empirical Firn Model Across the Greenland Ice Sheet (1980–2020)

The Greenland Ice Sheet's (GrIS) firn layer buffers the ice sheet's contribution to sea level rise by storing meltwater in its pore space. However, available pore space and meltwater retention capability is lost due to ablation of the firn layer and refreezing of meltwater as near-surface ice slabs in the firn. Understanding how firn properties respond to climate is important for constraining the GrIS's future contribution to sea level rise in a warming climate. Observations of firn density provide detailed information about firn properties, but they are spatially and temporally limited. Here we use two firn models, the physics-based SNOWPACK model and the Community Firn Model configured with a semi-empirical densification equation (CFM-GSFC), to quantify firn properties across the GrIS from 1980 through 2020. We use an identical forcing (Modern-Era Retrospective Analysis for Research and Applications, version 2 (MERRA-2) atmospheric reanalysis) for SNOWPACK and the CFM-GSFC in order to isolate firn model differences. To evaluate the models, we compare simulated firn properties, including firn air content (FAC), to measurements from the Surface Mass Balance and Snow on Sea Ice Working Group (SUMup) dataset of snow and firn density. Both models perform well (mean absolute percentage errors of 14 % in SNOWPACK and 16 % in the CFM-GSFC), though their performance is hindered by the spatial resolution of the atmospheric forcing. In the ice-sheet-wide simulations, the 1980–1995 average spatially integrated FAC (i.e., air volume in the firn) for the upper 100 m is 34 645 km 3 from SNOWPACK and 28 581 km 3 from the CFM-GSFC. The discrepancy in the magnitude of the modeled FAC stems from differences in densification with depth and variations in the sensitivity of the models to atmospheric forcing. In more recent years (2005–2020), both models simulate substantial depletion of pore space. During this period, the spatially integrated FAC across the entire GrIS decreases by 3.2 % (−66.6 km 3 yr −1 ) in SNOWPACK and 1.5 % (−17.4 km 3 yr −1 ) in the CFM-GSFC. These differing magnitudes demonstrate how model differences propagate throughout the FAC record. Over the full modeled record (1980–2020), SNOWPACK simulates a loss of pore space equivalent to 3 mm of sea level rise buffering, while the CFM-GSFC simulates a loss of 1 mm. The greatest depletion in FAC is along the margins and especially along the western margin where observations and models show the formation of near-surface, low-permeability ice slabs that may inhibit meltwater storage.

Megan Thompson-Munson↗
NASA NTRS2023

Thermal Stability of M x O y Doped Zirconia Aerogels (M = Y, Yb, Gd, Ce, Ca) Studied Through 1200°C

The high porosities and low densities of ceramic aerogels offer outstanding insulative performance in applications where weight is a critical factor. The high surface area-to-volume ratios and specific surface areas provide extremely low thermal conductivity, but also contribute to rapid densification of the pore structure at elevated temperatures. This densification diminishes their favorable properties and inhibits use of aerogels in high temperature applications. This work contributes to a design framework for thermally stable aerogels via the study of dopant chemistry (Y, Yb, Gd, Ca, Ce) in zirconia aerogels. The structural evolution was studied to 1200°C using nitrogen physisorption, scanning electron microscopy, and x-ray diffraction. The role of dopant identity and concentration in thermal stability was elucidated. In context of the design framework, dopant chemistry is an aggregate for many closely related material properties, each of which may contribute to aerogel structural evolution. To develop a truly predictive design framework for ceramic-based aerogels, systematic and comprehensive evaluation of thermodynamic and kinetic properties must be performed in conjunction with studies on structural evolution.

aerogel↗
NASA NTRSDate not supplied

Improved Treatment of Snow Over Ice Sheets in the NASA GISS Climate Model: Towards Ice Sheet–Climate Coupling

Representing the interactions between ice sheets and climate is essential for more accurate prediction of climate change and sea level rise. Ice sheets interact with the overlying atmosphere via the accumulation of snow and its compaction into firn, then ice, as well as the melting of surface snow and ice and the creation of runoff water. Getting an adequate representation of heat transfer, compaction, and melting processes is essential for an accurate representation of snow on land ice in global climate models. We are implementing an improved snow model on top of land ice as part of an effort to couple the NASA GISS climate model with the PISM ice sheet model. The new snow model includes additional layers and processes that are not currently incorporated (e.g., liquid water retention, percolation and refreezing, and snow densification), and mass and energy transfer methods that are consistent with both static ice sheets (with implicit iceberg fluxes) and interactive ice sheets (with explicit dynamics). We are tuning the densification scheme of this snow model with temperature and density data from common FirnCover and SumUp observations at locations in the accumulation zone of Greenland, and we compare the resulting density profiles to other SumUp density profiles in Greenland and Antarctica. We will assess the impact of this new snow model in climate model simulations with a static ice sheet compared with the previous (simpler) 2-layer snow model. Finally, we aim to use the non-coupled simulations as a baseline to assess the impact of dynamic coupling with an interactive ice sheet model.

snow↗
DOE OSTI2018

Development of Hot-Isostatic Pressing for Treatment of UK ILW Radioactive Wastes - 18280

Hot-Isostatic Pressing (HIPing) has been proposed as an improved method for the treatment of radioactive wastes in the UK. Sludges and slurries housed on the Sellafield site are a prime candidate for HIP treatment due to their large volumes and issues associated with the use of the baseline cementation strategy. Options have been developed by GeoRoc Ltd to co-process these wastes, including a detailed conceptual plant design. This paper will describe research and development aimed at demonstrating the viability of the concept presented in this design. This paper summarizes two studies performed to address the knowledge gaps identified for treatment of these wastes using HIP technology. The first study related to the poorly characterized nature of the wastes, which requires any treatment option to be flexible in terms of the chemical and physical properties of the waste feed. The second study involved demonstrating that HIPing can be effectively utilized at a scale applicable to treat a waste inventory estimated to be in excess of 5,000 m{sup 3}. The first section of this paper presents a summary of research carried out to determine where variation in the waste stream composition may affect the processing and wasteform produced when HIPing Magnox sludges. This study aimed to qualify where restrictions on the process envelope may exist due to poorly defined waste-stream characteristics. A baseline wasteform was selected with the aim of achieving significant waste volume reduction, while producing a physically and chemically stable wasteform. A glass-bonded magnesium-titanate/magnesium-silicate wasteform was selected as the preferred option for the Magnox sludge wastes. A series of studies investigated the densification and phase formation of waste-forms by altering key variables in the Magnox sludge simulant. To test the extremes of the processable waste loading, samples were produced and characterized at 100 wt% waste-loading for Magnox sludge, Site-Ion Exchange Plant (SIXEP) sand/clinoptilolite and a 50:50 mix of the two waste-streams. Further studies involved a) altering the waste loading to additive mass ratio (to simulate changes in the waste loading/sludge solids content), b) varying the particle size distribution from the datum to include only small or large particulates in the sludge feed; and c) introducing up to 20 wt% metallic Magnox alloy, organic species or carbonate materials (to determine how their inclusion may affect the processing and densification of the materials). A U{sub 3}O{sub 8} loaded sample was also produced using the baseline Magnox sludge formulation. All the tests performed were shown to produce monolithic, well densified waste-forms with substantial volume reductions. Minimal variations from the baseline were noted but the waste-forms produced with these deviations was determined to be of comparable quality to of the baseline product. U{sub 3}O{sub 8} was shown to behave in a similar fashion to the ZrO{sub 2} surrogate used to simulate it in the process envelope studies and was encapsulated in the magnesium titanate/magnesium silicate matrix. This work demonstrates that HIP technology can successfully produce waste-forms across the broad process envelope expected in the Magnox sludge inventory. It is also possible to produce monolithic waste-forms at 100 wt% waste loading from Magnox sludges, SIXEP sand clinoptilolite slurries or a co-processed mixture of the two. The second part of this paper summarizes a commercially relevant demonstration of HIP technology for the treatment of sludge and slurry wastes housed at the Sellafield site (UK). This study culminated in production of the largest HIPed wasteform successfully produced to date. This study was performed in a series of stages. Investigations into formulation and properties of waste-forms were performed at a lab scale to evaluate suitable wasteform systems and identify suitable combinations of additives and waste loadings. Scale up demonstrations were then performed in stages with custom-designed HIP canisters. Scale-up and characterization of key wasteform properties were successfully performed with initial canister volumes of 50 ml, 400 ml and 8 L. Suitable front-end unit operations to produce a granular, free-flowing calcined simulant were demonstrated at an engineering scale. The demonstration was successful in processing a HIP canister with an initial starting volume in excess of 100 L. A 75 % volume reduction from the raw sludge was achieved at scale while demonstrating that HIP is applicable at suitably large scale for immobilization of ILW waste. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Atmospheric plasma-sprayed BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ ($\mathrm{BZCYYb}$) electrolyte membranes for intermediate-temperature solid oxide fuel cells

The high co-sintering temperature of BZCYYb electrolyte membranes supported by anode substrates usually causes a series of problems including undesirable electrolyte-anode reactions/diffusion and Ba-evaporation, posing a challenge for seeking alternative fabrication approaches. Here in this study, BZCYYb electrolyte membranes supported by anode substrates are fabricated by a large-scale and cost-effective atmospheric plasma spraying (APS) process. The 25 µm thick BZCYYb membrane has negligible electrolyte-anode reactions/diffusion due to the APS process free of high-temperature co-firing. The Ba-evaporation problem is also resolved during APS process because of the adoption of large-grained BZCYYb feedstock powders. After 15 cycles of post-densification treatment by infiltrating, the plasma-sprayed BZCYYb membrane is dense enough for electrolyte application. The single cell based on dense plasma-sprayed BZCYYb electrolyte membrane shows a peak power density of 0.35 W cm -2 at 750 °C using 3 vol% humidified H 2 as fuel and ambient air as oxidant.

36 MATERIALS SCIENCE↗