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NASA NTRS1989

Densification and coarsening during solid state sintering of ceramics: A review of the models. II - Grain growth

Two processes occur simultaneously during the sintering of a ceramic powder compact: densification and coarsening (or grain growth). Both processes have as their driving force the reduction of the excess free surface energy of the powder particles. Several different mechanisms of atom transport, operating concurrently or consecutively, may be responsible for the two processes. Algebraic, geometric and topological models have been proposed and refined in attempts to determine the mechanism, or mechanisms, responsible for densification under defined processing conditions. These efforts have met with varying degrees of success. Recently, it has become apparent that more attention must be paid to the coarsening processes during sintering. The models for both densification and coarsening during solid state sintering are reviewed with particular emphasis on their applicability to engineering ceramics.

Shaw, Nancy J.↗

NASA NTRS1991

Application of powder densification models to the consolidation processing of composites

Unidirectional fiber reinforced metal matrix composite tapes (containing a single layer of parallel fibers) can now be produced by plasma deposition. These tapes can be stacked and subjected to a thermomechanical treatment that results in a fully dense near net shape component. The mechanisms by which this consolidation step occurs are explored, and models to predict the effect of different thermomechanical conditions (during consolidation) upon the kinetics of densification are developed. The approach is based upon a methodology developed by Ashby and others for the simpler problem of HIP of spherical powders. The complex problem is devided into six, much simpler, subproblems, and then their predicted contributions are added to densification. The initial problem decomposition is to treat the two extreme geometries encountered (contact deformation occurring between foils and shrinkage of isolated, internal pores). Deformation of these two geometries is modelled for plastic, power law creep and diffusional flow. The results are reported in the form of a densification map.

Wadley, H. N. G.↗

NASA NTRS1999

Propellant Densification for Launch Vehicles: Simulation and Testing 1999

One of the many key technologies required to make single-stage to orbit an actuality, the technology of sub-cooling cryogenic propellants below their normal saturation temperatures and thereby making them more dense, is unquestionably on its way towards full and practical realization. The technology of Propellant Densification has been the subject of an extensive research and development program overseen by Lockheed Martin Michoud Space Systems and NASA Glenn Research Center over the past several years. This paper presents a status report of this research and development. Specifically examined within this paper is the status of the current and continuing efforts on the mathematical simulation of the in-tank propellant densification process currently baselined for the Lockheed Martin VentureStar Reusable Launch Vehicle (RLV). Keys to this modeling effort are an understanding and quantification of the effects of thermal stratification and the ability to capture the complex and unique multiple section tank geometries being proposed for future launch vehicles. A simulation that properly captures these phenomena has been developed by Lockheed Martin. Also discussed is the significant test program that has been undertaken in coordination with NASA Glenn Research Center. In this testing, the liquid hydrogen recirculation and densification process was simulated and the thermal stratification of the densified propellant was recorded throughout the tank. This testing marks the first time that such a process has been carried out within a multiple-lobe, flight-similar tank. The results from this testing have gone a long way towards grounding the mathematical models and towards demonstrating the readiness of the technology for near-term use. A further and even more ambitious test program examining the production and utilization of densified propellants is being planned for late-autumn 1999. An overview of these plans is presented.

Knowles, Timothy E.↗

NASA NTRS2010

Liquid Oxygen Propellant Densification Production and Performance Test Results With a Large-Scale Flight-Weight Propellant Tank for the X33 RLV

This paper describes in-detail a test program that was initiated at the Glenn Research Center (GRC) involving the cryogenic densification of liquid oxygen (LO2). A large scale LO2 propellant densification system rated for 200 gpm and sized for the X-33 LO2 propellant tank, was designed, fabricated and tested at the GRC. Multiple objectives of the test program included validation of LO2 production unit hardware and characterization of densifier performance at design and transient conditions. First, performance data is presented for an initial series of LO2 densifier screening and check-out tests using densified liquid nitrogen. The second series of tests show performance data collected during LO2 densifier test operations with liquid oxygen as the densified product fluid. An overview of LO2 X-33 tanking operations and load tests with the 20,000 gallon Structural Test Article (STA) are described. Tank loading testing and the thermal stratification that occurs inside of a flight-weight launch vehicle propellant tank were investigated. These operations involved a closed-loop recirculation process of LO2 flow through the densifier and then back into the STA. Finally, in excess of 200,000 gallons of densified LO2 at 120 oR was produced with the propellant densification unit during the demonstration program, an achievement that s never been done before in the realm of large-scale cryogenic tests.

Tomsik, Thomas M.↗

NASA NTRS2011

Frost Growth and Densification in Laminar Flow Over Flat Surfaces

One-dimensional frost growth and densification in laminar flow over flat surfaces has been theoretically investigated. Improved representations of frost density and effective thermal conductivity applicable to a wide range of frost circumstances have been incorporated. The validity of the proposed model considering heat and mass diffusion in the frost layer is tested by a comparison of the predictions with data from various investigators for frost parameters including frost thickness, frost surface temperature, frost density and heat flux. The test conditions cover a range of wall temperature, air humidity ratio, air velocity, and air temperature, and the effect of these variables on the frost parameters has been exemplified. Satisfactory agreement is achieved between the model predictions and the various test data considered. The prevailing uncertainties concerning the role air velocity and air temperature on frost development have been elucidated. It is concluded that that for flat surfaces increases in air velocity have no appreciable effect on frost thickness but contribute to significant frost densification, while increase in air temperatures results in a slight increase the frost thickness and appreciable frost densification.

Kandula, Max↗

NASA NTRS2018

Hydrogen Densification for Nuclear Thermal Propulsion Missions

Propellant densification is cooling the propellant below the normal boiling point; Densified propellants can either be saturated or subcooled. Propellant densification has two potential benefits; Increased density for more mass in a given volume (more propellant), Decrease temperature for thermal energy buffer (extended storage). Two primary methods for producing densified propellants; Vapor pumping for pressure control, Refrigeration for temperature control. SpaceX has been flying densified liquid oxygen for several years. NASA has developed and tested hydrogen densification systems but have never been used in an operational mission

densified propellants↗

NASA NTRS2023

Simulations of Zero Boiloff, Densification, and Solidification in a Large-Scale Liquid Hydrogen Tank

The current research utilizes an Energy of Fluid (EOF) approach to develop a finite volume-based Computation Fluid Dynamic (CFD) model to create a benchmark simulation of the densification of liquid hydrogen (LH2) in an experimental Integrated Refrigeration and Storage (IRAS) tank at the Kennedy Space Center (KSC). The computational code will incorporate the FLUENT pressure-based model with User Defined Functions (UDF) to implement the EOF model. The enhanced model will solve the energy equation in terms of internal energy and provide temperature and pressure calculations for a given tank geometry. Specifically, a convection term will be added to an already existing code for a more accurate simulation of LH2 densification. However, currently the research focuses on utilizing User Defined Scalars (UDS) with FLUENT to show the built-in solvers are as accurate as the written UDS. This will reduce the computational time down significantly by utilizing an already built in solver for the momentum equation. A custom UDF has been written to solve transient and steady state conduction, and results obtained using the UDF agree with results obtained using the built-in FLUENT solver. Currently, a convection UDF is being added and will be verified using known solutions for solidification and validated with the experimental results from the Cryogenics Test Laboratory (CTL) at KSC for the IRAS densification process.

Colin Philip Mahony↗

NASA NTRS2023

A New Model of Dry Firn Densification Constrained By Continuous Strain Measurements Near South Pole

Converting measurements of ice-sheet surface elevation change to mass change requires measurements of accumulation and knowledge of the evolution of the density profile in the firn. Most firn-densification models are tuned using measured depth-density profiles, a method which is based on an assumption that the density profile in the firn is invariant through time. Here we present continuous measurements of firn-compaction rates in 12 boreholes near the South Pole over a two-year period. To our knowledge, these are the first continuous measurements of firn compaction on the Antarctic Plateau. We use the data to derive a new firn-densification algorithm framed as a constitutive relationship. We also compare our measurements to compaction rates predicted by several existing firn densification models. Results indicate that an activation energy of 60 kJ mol (−1), a value within the range used by current models, best predicts the seasonal cycle in compaction rates on the Antarctic Plateau. Our results suggest models can predict firn-compaction rates with at best 7% uncertainty and cumulative firn compaction on a two year timescale with at best 8% uncertainty.

C. Max Stevens↗

DOE OSTI2023

Densification and microstructure features of lithium hydride fabrication

The manufacturing of lithium hydride (LiH) utilizing uniaxial pressing, which offers fabrication with tailorable properties via microstructure control, can lead to the expansion in application of LiH while bypassing the challenges presented by historical casting manufacturing techniques. Through control of consolidation conditions such as pressure, temperature, dwell time and powder load, the presented work highlights the densification of LiH, with an emphasis on quantifying oxygen content, for applications requiring a specific density range necessary for optimized material performance. Karl Fischer Titration and X-ray Diffraction proved useful in determining oxygen and phase content while Computed Tomography and Scanning Electron Microscopy provided structural analysis. The temperature dependent densification of LiH fit with an Arrhenius term resulted in an activation energy of 21.2 kJ/mol. Images of fractured surfaces of LiH pressed at 500 °C revealed drastic grain coarsening, aided by the presence of oxygen impurities.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Enhancing biomass flowability for entrained flow Gasification: The role of densification and torrefaction

Gasification presents a key strategy in addressing future energy demands while minimizing environmental impact. This has been recognized as a promising method to convert biomass to higher value products such as biofuels or hydrogen. Among gasification technologies, high-temperature and high-pressure reactors, particularly the R-GAS® system, emerge as an advanced option boasting superior conversion efficiency. However, akin to conventional high-temperature and high-pressure gasifiers, R-GAS® necessitates small particle sizes for optimal carbon conversion, a requirement yet to be fully explored for biomass. Hence, this study investigated the effectiveness of combined mechanical and thermal preprocessing techniques in modifying the physicochemical properties of biomass to suit gasification systems. Mechanical techniques including densification and pulverization, alongside thermal techniques such as torrefaction and steam explosion, were examined. The results demonstrate that torrefaction fosters producing of uniform granular material, enhancing flowability and reducing energy requirements for pulverization compared to steam explosion. Notably, torrefied corn stover exhibited lower internal friction angles and effective cohesion (40.09 ± 0.22° and 0.56 ± 0.01 kPa, respectively) compared to steam exploded corn stover (41.87 ± 0.65° and 0.83 ± 0.06 kPa, respectively), indicative of improved flowability. Additionally, pulverization of torrefied corn stover required approximately 16 % less energy than steam exploded corn stover and 91 % less energy than raw corn stover. Furthermore, the torrefaction-induced alterations in particle size, shape, and packing densities emphasize its potential to optimize flow and handling processes for gasification. These findings underline that densification followed by torrefaction effectively addresses biomass variability, leading to more efficient and sustainable energy conversion.

09 - BIOMASS FUELS↗

NASA NTRS2025

Simulations of Large-Scale Zero Boiloff, Densification, and Solidification of Hydrogen

An Integrated Refrigeration and Storage (IRAS) experimental system called the Ground Operations and Demonstration Unit for Liquid Hydrogen (GODU-LH2) demonstrated the ability store cryogens in a zero boiloff (ZBO) process, and to densify liquid hydrogen by reducing the temperature and pressure down to the triple point resulting in solidification. The incompressible Navier-Stokes was utilized to simulate ZBO, densification, and solidification of liquid hydrogen (LH2) in the IRAS tank. The simulations were performed using a commercially available Computational Fluid Dynamics (CFD) pressure-based mass and momentum flow model and an enthalpy-porosity energy model. Results demonstrated the simulation’s ability to predict time-dependent flow and temperature fields and solid-liquid phase locations for hydrogen during ZBO, densification, and solidification. The simulations showed good agreement with experimental data, with errors within acceptable ranges for temperature and pressure predictions, provided detailed insights into natural convection and solid-liquid phase change dynamics. These findings are critical for the design of future cryogenic fluid management systems.

Computational Fluid Dynamics↗

DOE OSTI2021

Powder spreading, densification, and part deformation in binder jetting additive manufacturing

Binder jetting additive manufacturing (AM) can print complex structures in economical and scalable manner. Binder jetting AM comprises of deposition and weak binding of particles, known as green part, at room temperature and subsequent binder removal and sintering densification at high temperatures. However, during the densification (i.e., sintering), the part significantly deforms due to volume shrinkage. The deformation during sintering is difficult to predict, which prevents the widespread application of this technology. In this research, powder spreading simulation using discrete element method (DEM) was performed first to capture local variations in powder bed configuration. Second, finite element method (FEM) with a phenomenological continuum constitutive model was used to predict part shrinkage during the sintering process. DEM simulation showed variations in packing density, particle segregation, formation of uneven powder bed surface, and shift in particle size distribution (PSD). The sintering simulation modeled part deformation with a reasonable accuracy of 3% for solid-state sintering and intermediate liquid phase sintering. A demonstration case with non-uniform initial packing density showed that inhomogeneous green part density and PSD should be accounted for prediction of part deformation in binder jetting AM.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Densification of the entropy stabilized oxide (Mg 0.2 Co 0.2 Ni 0.2 Cu 0.2 Zn 0.2 )O

The first entropy-stabilized oxide, (Mg 0.2 Co 0.2 Ni 0.2 Cu 0.2 Zn 0.2 )O, was reported in 2015. Initial studies synthesized this material using solid state processing and were limited to densities < 80%. Here, we report a straightforward solid state route to sinter samples to densities up to 98% of the theoretical by identifying the role of oxygen and promoting the resulting mechanisms in densification. Previous works have studied effects of cation stoichiometry on the entropy-driven reaction to form a single phase, but few have explored the associated effects of anion stoichiometry and/or redox chemistry on both phase stability and densification. We demonstrate here that tuning heating rate and pO 2 during heating of initially-homogeneous calcined powders can enhance densifying diffusion processes and enable reliable sintering of dense (Mg 0.2 Co 0.2 Ni 0.2 Cu 0.2 Zn 0.2 )O samples.

MATERIALS SCIENCE↗

DOE OSTI2023

Concurrent reaction-bonded joining and densification of additively manufactured silicon carbide by liquid silicon infiltration

Here, in this study, additive-manufactured silicon carbide preforms were joined and densified by reaction bonding via liquid silicon infiltration. The silicon carbide preforms were first printed by binder jetting additive manufacturing. To demonstrate concurrent joining and densification, two preforms with carbon or parchment papers at the interface were concurrently joined and infiltrated by liquid silicon. Results showed a robust interface with thicknesses ranging from 150 to 500 µm, depending on the paper type and the number of paper layers. High-energy synchrotron X-ray revealed that β-phase silicon carbide was formed inside the interface. Finally, two additively manufactured samples with complicated channel geometry were successfully joined. Energy dispersive spectroscopy of the interface of the channeled samples showed a consistent and robust joining. This concurrent approach of joining and densification enables efficiency improvement of fabricating silicon carbide parts with complicated geometries and widens geometry freedom for additive manufacturing of silicon carbide.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Densification and Immobilization of AgI-Containing Iodine Waste Forms Using Spark Plasma Sintering

Here in this study, porous Ag-xerogel (Ag-Xero), Ag-faujasite (Ag-FAU) zeolite, and Ag-mordenite (Ag-MOR) zeolite sorbents were loaded with iodine gas [I 2 (g)] under saturated conditions at 150 °C for 24 h, followed by densification and consolidation into monolithic waste forms using spark plasma sintering (SPS). For Ag-Xero materials, SPS pellets were made with as-loaded samples, while others were made with preheated (PH; 500 °C for 2 h) samples to help with densification. SPS processing was conducted at 50 MPa under different temperatures (T = 200–800 °C) for different times (t = 0.5–30 min), where eleven AgI-Xero samples, five AgI-FAU, and two AgI-MOR separate samples were produced. The primary goal was to look for the optimum processing parameters for each material to yield pellets with high iodine retentions, high densities, and low porosities while preventing AgI decomposition. The Ag-Xero showed the highest iodine loadings (qe = 470 mg g –1 ) compared to Ag-FAU (qe = 368 mg g –1 ) and Ag-MOR (qe = 108 mg g –1 ). Measured iodine concentrations were the highest in AgI-Xero pellets without PH, followed by AgI-Xero with PH, AgI-FAU, and then AgI-MOR. Silver utilization (I/Ag on a mol % basis) values were in the order of AgI-MOR ≈ AgI-Xero (no PH) > AgI-Xero (PH) > AgI-FAU. Chemical durabilities of SPS-densified AgI-Xero (PH) pellets were very favorable, with lower releases than SPS pellets made from AgI-Xero samples without PH. These results show promise for iodine waste form production.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1975

Silicon nitride-aluminum oxide solid solution (SiAION) formation and densification by pressure sintering

Stirred-ball-mill-blended Si3N4 and Al2O3 powders were pressure sintered in order to investigate the mechanism of solid solution formation and densification in the Si3N4-Al2O3 system. Powder blends with Si3N4:Al2O3 mole ratios of 4:1, 3:2, and 2:3 were pressure sintered at 27.6-MN/sq m pressure at temperatures to 17000 C (3090 F). The compaction behavior of the powder blends during pressure sintering was determined by observing the density of the powder compact as a function of temperature and time starting from room temperature. This information, combined with the results of X-ray diffraction and metallographic analyses regarding solutioning and phase transformation phenomena in the Si3N4-Al2O3 system, was used to describe the densification behavior.

Yeh, H. C.↗

NASA NTRS1975

Effect of additions of coarse grains and fibers on the densification of a sinterable SiC

This note reports the effects on densification of independent additions of coarse equiaxed SiC grains and fibrous SiC that were mixed with fine beta-SiC to develop a duplex microstructure with improved toughness. The fine-matrix SiC did not contain excess boron and carbon. The equiaxed CVD beta-SiC was introduced in the fine beta-SiC matrix material in amounts of 5 and 10 wt%. Results indicate that the CVD beta-SiC, which is quite coarse, exhibits little indication of sinterability. The effect of these coarse-grained and fibrous additions on the sinterability of fine beta-SiC may result from a geometric type of interaction. This interpretation is reinforced by X-ray diffraction of the powders and sintered pellets via monochromatic CuK-alpha radiation; the diffraction patterns of the sintered composite structures are virtually a combination of those of the components. The addition of nonsinterable SiC to the sinterable material slightly reduces sinterability, the larger particles interacting geometrically with the fine matrix material to prevent complete densification.

Abe, H.↗

NASA NTRS1987

Localized Densification of Tile for Impact Resistance

Densification process increases impact resistance of lightweight, porous silica tile without appreciably raising weight. Colloidal suspension of silica used to increase density of small portion of tile to be strengthened. Process controls penetration of suspension laterally and vertically so densification limited to volume where needed. Insures weight increased only minimally. See also "Attaching Metal Fasteners to Silica Tiles" (MSC-20537).

Smiser, Laurence W.↗