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At least 37 records · Page 2

Binder-jetted AISI M2 tool steel during hot isostatic pressing: Densification and carbide transformation

Binder jetting (BJ) enables fabrication of complex components from high-alloy steels such as AISI M2; however, residual porosity after sintering limits mechanical performance. This study investigates the coupled effects of binder chemistry, sintering conditions, cooling rate, and subsequent hot isostatic pressing (HIP) on densification, microstructure, and mechanical response in binder-jetted M2 tool steel. HIP increased relative density from ∼93 to 95% to >99% and improved compressive strength by ∼40-70%. Densification was governed by initial pore morphology, where closed porosity was effectively eliminated, while interconnected porosity limited full consolidation. Microstructural analysis (XRD, EBSD, SEM) shows that HIP promotes dissolution of metastable carbides and redistribution of alloying elements (W, Mo, V), transforming heterogeneous carbide networks into finer and more uniformly distributed M 2 C, MC, and M 6 C phases through diffusion-assisted homogenization. Among the investigated conditions, the FluidFuse binder combined with sintering at 1270 °C for 60 min and furnace cooling produced the most balanced response, achieving ∼99.7% density, ∼855 HV hardness, ∼4130 MPa compressive strength, and ∼24% strain. In contrast, higher sintering temperatures promoted carbide coarsening, reducing ductility despite high density. HIP reduces microstructural heterogeneity and drives the system toward a near-equilibrium state with reduced sensitivity to prior processing history. A comparative assessment with conventional and additive manufacturing routes (LPBF, DED, EBM, FFF) shows that the BJ-HIP approach achieves competitive densification and mechanical performance. These findings provide a mechanistic basis for controlling densification and microstructure in high-alloy steels processed via BJAM.

AISI M2 tool steel↗

In Situ Microstructure Characterization of Potassium Di-Phosphate (KDP) Densification during Cold Sintering

In order for ceramic additive manufacturing (AM) to achieve its full potential, it is increasingly important to develop a more rigorous understanding of fundamental phenomena that govern the kinetics and thermodynamics of ceramic AM processes. In the case of additive build processes, such as direct ink write and ceramic extrusion, methods for densifying the resulting green-body product need to be considered to complement the efficiencies of ceramics AM, itself. One densification route, at least for monolithic components, built layer-by-layer, is offered by the recently developed cold sintering process, whereby high-density final product is achieved through addition of a small amount of liquid solvent and application of modest uniaxial compressive stress at relatively low temperature. In situ small-angle X-ray scattering methods and X-ray diffraction have been applied to characterize and quantify the pore morphology evolution during cold sintering for a model system: potassium di-phosphate, KH 2 PO 4 (KDP). It is shown that both temperature and applied stress affect the densification rate, but stress has a stronger effect on the evolving morphology. A regime with an approximate linear densification rate can be identified, yielding an effective densification activation energy of ≈90 kJ/mol.

36 MATERIALS SCIENCE↗

Phase Field Modeling of Pressure Induced Densification in Solid Electrolytes

Adoption of dense and homogeneous solid electrolytes can possibly mitigate the propagation of lithium dendrites and enable lithium metal anodes. Application of external pressure helps to minimize the sintering temperature in oxide ceramics and can potentially densify softer sulfide electrolytes even under room temperature conditions. Here, a previously developed phase field-based computational scheme for predicting the high-temperature sintering-induced densification of oxide ceramic solid electrolytes is extended in the present context to capture the influence of external pressure for densifying solid electrolytes. Two different bulk deformation mechanisms, namely, "reorganization" and "creep deformation," are dominant under external pressure, which is different from the surface and grain-boundary diffusion-induced densification of solid electrolytes that occurs during high temperature sintering. External pressure also increases the points of contact between the particles, which further enhances the propensity of diffusion-induced sintering process. Results obtained from simulations indicate that densification under external pressure is independent of the solid electrolyte particle morphology. Finally, a phase map is generated between applied pressure and temperature for achieving complete densification of oxide ceramics, which can possibly guide the synthesis of thin and dense solid electrolyte separators.

25 ENERGY STORAGE↗

Direct in situ observation of electric field assisted densification of ZnO by energy dispersive X-ray diffraction

Electric field assisted sintering techniques are used to enhance the densification process, reducing sintering time and temperature. Here, we report the in situ characterization of non-isothermal densification behavior of zinc oxide under simultaneous application of thermal and electric field by energy dispersive X-ray diffraction. 99% density was achieved under the electric field of 50 V/mm in the 588–843 °C range in a short time without grain growth. The in-situ energy dispersive X-ray diffraction study revealed the abnormal volumetric unit cell expansion of 0.9% at 843 °C associated with the observed sudden rise of the power absorption by the specimen during densification. Furthermore, the variation in peak broadening as a function of time exhibited singularity in the 588–843 °C range implying the formation and rearrangement of defects correlated with densification during electric field assisted sintering.

36 MATERIALS SCIENCE↗

Smaller feature size impairs densification in digital light processing 3D printed ceramic samples

In this study, we investigate how geometric miniaturization affects the sintering densification behavior of alumina cylinders with various wall thicknesses (down to ∼500 µm in green body) fabricated via digital light processing (DLP). As the wall thickness decreased, the density of the sintered samples consistently declined. Microstructural characterization revealed the presence of a crack-rich surface skin that is ∼500 µm thick. As the wall thickness decreases, the skin's volume fraction rises, and its poor local densification increasingly dominates the part average, leading to an overall decrease in the density of the sintered samples. For the thinnest wall (500 µm) cylinder, macroscopic warping occurred during sintering. We suggest that warping further disrupts particle packing and induces through-thickness nonuniformity, further impairing densification in addition to the skin-fraction effect. These results highlight how geometric miniaturization may adversely influence the sintering behavior and final density of DLP-printed ceramics through distinct densification-limiting mechanisms.

Materials science↗

Temperature-induced densification in compressed basaltic glass revealed by in-situ ultrasonic measurements

Abstract Acoustic velocities of a model basalt glass (64 mol% CaMgSi2O6 + 36 mol% CaAl2Si2O8) were measured along different pressure-temperature (P-T) paths. One set of experiments involved isothermal compression-decompression cycles, performed at temperatures of 300, 641, 823, and 1006 K and pressures up to 12.2 GPa. The other set of experiments involved constant-load heating-cooling cycles at temperatures up to 823 K and pressures up to 7.5 GPa. Both sets of experiments were performed in a multi-anvil apparatus using a synchrotron-based ultrasonic technique. Our results show that the glass compressed isothermally at 300 K (cold-compression) displays anomalously decreasing compressional (VP) and shear (VS) wave velocities with increasing pressure until ~8 GPa. Beyond 8 GPa, both VP and VS start to increase sharply with pressure and irreversible densification of the glass occurred, producing large hysteresis loops of velocities upon decompression. However, for the glass compressed isothermally at increasingly higher temperatures (hot-compression), the velocity minima gradually shift to lower pressures. At temperature close to the glass transition temperature Tg, the velocity minima disappear completely, displaying a monotonic increase of velocities during compression and higher VP and VS during decompression. In addition, constant-load heating-cooling experiments show that velocities generally decrease slightly with increasing temperature, but start to increase once heated above a threshold temperature (~650 K). During cooling the velocities increase almost linearly with decreasing temperature, resulting in higher velocities (~1.5–2.5% higher) when returned to 300 K. This implies that a temperature-induced densification may have occurred in the glass at high pressures. Raman spectra on recovered samples show that the hot-compressed and high-P heated glasses contain distinctly densified and depolymerized structural signatures compared to the initial glass and the cold-compressed glass below the velocity transition pressure PT (~8 GPa). Such densification may be attributed to the breaking of bridging oxygen bonds and compaction in the intermediate-range structure. Our results demonstrate that temperature can facilitate glass densification at high pressures and point out the importance of P-T history in understanding the elastic properties of silicate glasses. Comparison with melt velocity suggests that hot-compressed glasses may better resemble the pressure dependence of velocity of silicate melts than cold-compressed glasses, but still show significantly higher velocities than melts. If the abnormal acoustic behaviors of cold-compressed glasses were used to constrain melt fractions in the mantle low-velocity regions, the melt fractions needed to explain a given velocity reduction would be significantly underestimated at high pressures.

Geochemistry & Geophysics↗

Development of Macroscale Models of UO 2 Fuel Sintering and Densification using Multiscale Modeling and Simulation

Light water reactor fuel pellets are fabricated using sintering to final densities of 95% or greater. During reactor operation, the porosity remaining in the fuel after fabrication decreases further due to irradiation-assisted densification. While empirical models have been developed to describe this densification process, a mechanistic model is needed as part of the ongoing work by the NEAMS program to develop a more predictive fuel performance code. In this work we will develop a phase field model of sintering of UO 2 in the MARMOT code, and validate it by comparing to published sintering data. We will then add the capability to capture irradiation effects into the model, and use it to develop a mechanistic model of densification that will go into the BISON code and add another essential piece to the microstructure-based materials models. The final step will be to add the effects of applied fields, to model field-assisted sintering of UO 2 . The results of the phase field model will be validated by comparing to data from field-assisted sintering. Tasks over three years: 1. Develop a sintering model for UO 2 in MARMOT 2. Expand model to account for irradiation effects 3. Develop a mechanistic macroscale model of densification for BISON

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Performance Tests of a Liquid Hydrogen Propellant Densification Ground System for the X33/RLV

A concept for improving the performance of propulsion systems in expendable and single-stage-to-orbit (SSTO) launch vehicles much like the X33/RLV has been identified. The approach is to utilize densified cryogenic liquid hydrogen (LH2) and liquid oxygen (LOX) propellants to fuel the propulsion stage. The primary benefit for using this relatively high specific impulse densified propellant mixture is the subsequent reduction of the launch vehicle gross lift-off weight. Production of densified propellants however requires specialized equipment to actively subcool both the liquid oxygen and liquid hydrogen to temperatures below their normal boiling point. A propellant densification unit based on an external thermodynamic vent principle which operates at subatmospheric pressure and supercold temperatures provides a means for the LH2 and LOX densification process to occur. To demonstrate the production concept for the densification of the liquid hydrogen propellant, a system comprised of a multistage gaseous hydrogen compressor, LH2 recirculation pumps and a cryogenic LH2 heat exchanger was designed, built and tested at the NASA Lewis Research Center (LeRC). This paper presents the design configuration of the LH2 propellant densification production hardware, analytical details and results of performance testing conducted with the hydrogen densifier Ground Support Equipment (GSE).

Tomsik, Thomas M.↗

Evaluating Greenland Surface-Mass-Balance and Firn-Densification Data Using ICESat-2 Altimetry

Surface-mass-balance (SMB) and firn-densification (FD) models are widely used in altimetry studies as a tool to separate atmospheric-driven from ice-dynamics-driven ice-sheet mass changes and to partition observed volume changes into ice-mass changes and firn-air-content changes. Until now, SMB models have been principally validated based on comparison with ice core and weather station data or comparison with widely separated flight radar-survey flight lines. Firn-densification models have been primarily validated based on their ability to match net densification over decades, as recorded in firn cores, and the short-term time-dependent component of densification has rarely been evaluated at all. The advent of systematic ice-sheet-wide repeated ice-surface-height measurements from ICESat-2 (the Ice Cloud, and land Elevation Satellite, 2) allows us to measure the net surface-height change of the Greenland ice sheet at quarterly resolution and compare the measured surface-height differences directly with those predicted by three FD–SMB models: MARv3.5.11 (Modèle Atmosphérique Régional version 3.5.11) and GSFCv1.1 and GSFCv1.2 (the Goddard Space Flight Center FD–SMB models version 1.1 and 1.2). By segregating the data by season and elevation, and based on the timing and magnitude of modelled processes in areas where we expect minimal ice-dynamics-driven height changes, we investigate the models' accuracy in predicting atmospherically driven height changes. We find that while all three models do well in predicting the large seasonal changes in the low-elevation parts of the ice sheet where melt rates are highest, two of the models (MARv3.5.11 and GSFCv1.1) systematically overpredict, by around a factor of 2, the magnitude of height changes in the high-elevation parts of the ice sheet, particularly those associated with melt events. This overprediction seems to be associated with the melt sensitivity of the models in the high-elevation part of the ice sheet. The third model, GSFCv1.2, which has an updated high-elevation melt parameterization, avoids this overprediction.

Benjamin E. Smith↗

Gasification performance of switchgrass pretreated with torrefaction and densification

The purpose of this study was to investigate gasification performance of four switchgrass pretreatments (torrefaction at 230 and 270 °C, densification, and combined torrefaction and densification) and three gasification temperatures (700, 800 and 900 °C). Gasification was performed in a fixed-bed externally heated reactor with air as an oxidizing agent. Switchgrass pretreatment and gasification temperature had significant effects on gasification performance such as gas yields, syngas lower heating value (LHV), and carbon conversion and cold gas efficiencies. With an increase in the gasification temperature, yields of H2 and CO, syngas LHV, and gasifier efficiencies increased whereas CH4, CO2 and N2 yields decreased. Among all switchgrass pretreatments, gasification performance of switchgrass with combined torrefaction and densification was the best followed by that of densified, raw and torrefied switchgrass. Gasification of combined torrefied and densified switchgrass resulted in the highest yields of H2 (0.03 kg/kg biomass) and CO (0.72 kg/kg biomass), highest syngas LHV (5.08 MJ m-3), CCE (92.53%), and CGE (68.40%) at the gasification temperature of 900 °C.

09 BIOMASS FUELS↗

Biomass Blending and Densification: Impacts on Feedstock Supply and Biochemical Conversion Performance

The success of lignocellulosic biofuels and biochemical industries depends on an economic and reliable supply of high-quality biomass. Many research and development efforts, however, have been historically focused on the utilization of agriculturally derived cellulosic feedstocks, without considerations of their low energy density, high variations in compositions and potential supply risks in terms of availability and affordability. This book chapter demonstrated a strategy of feedstock blending and densification to address the supply chain challenges. Blending takes advantage of low cost feedstock to avoid the prohibitive costs incurred through reliance on a single feedstock resource while densification produces feedstocks with increased bulk density and desirable feed handling properties as well as reduced transportation cost. We also review recent research on the blending and densification dealing with various types of feedstocks with a focus on the impacts of these preprocessing steps on biochemical conversion, i.e., various thermochemical pretreatment chemistries and enzymatic hydrolysis, into fermentable sugars for biofuel production.

09 BIOMASS FUELS↗

NUMERICAL MODELING OF CATHODE CONTACT MATERIAL DENSIFICATION

Numerical modeling was used to simulate the constrained sintering process of the cathode contact layer during assembly of solid oxide fuel cells (SOFCs). A finite element model based on the continuum theory for sintering of porous bodies was developed and used to investigate candidate low-temperature cathode contact materials. Constitutive parameters for various contact materials under investigation were estimated from dilatometry screening tests, and the influence of processing time, processing temperature, initial grain size, and applied compressive stress on the free sintering response was predicted for selected candidate materials. The densification behavior and generated stresses within a 5-cell planar SOFC stack during sintering, high temperature operation, and room temperature shutdown were predicted. Insufficient constrained densification was observed in the stack at the proposed heat treatment, but beneficial effects of reduced grain size, compressive stack preload, and reduced thermal expansion coefficient on the contact layer densification and stresses were observed.

30 DIRECT ENERGY CONVERSION↗

Effects of torrefaction and densification on switchgrass pyrolysis products

Abstract The pyrolysis behaviors of four types of pretreated switchgrass (torrefied at 230 and 270 °C, densification, and torrefaction at 270 ºC followed by densification) were studied at three temperatures (500, 600, 700 ºC) using a pyroprobe attached to a gas chromatogram mass spectroscopy (Py-GC/MS). The torrefaction of switchgrass improved its oxygen to carbon ratio and energy content. Contents of anhydrous sugars and phenols in pyrolysis products of torrefied switchgrass were higher than those in pyrolysis products of raw switchgrass. As the torrefaction temperature increased from 230 to 270 °C, the contents of anhydrous sugars and phenols in pyrolysis products increased whereas content of guaiacols decreased. High pyrolysis temperature (600 and 700 °C as compared to 500 °C) enhanced decomposition of lignin and anhydrous sugars, leading to increase in phenols, aromatics and furans. Densification enhanced depolymerization of cellulose and hemicellulose during pyrolysis.

09 BIOMASS FUELS↗

Densification of non-radioactive porous siliceous particles loaded with cesium potassium copper hexacyanoferrate by spark plasma sintering

In the development of a conditioning process for cesium-bearing sorbents from the decontamination of aqueous waste streams, the treatment of a granular material composed of (Cs,K) 2 CuFe(CN) 6 loaded onto mesoporous silica particles has been investigated in an additive-free two-step conditioning process involving (i) calcination at 1000 °C to remove volatile species and (ii) densification by spark plasma sintering. A 92.0 % dense pellet was obtained after 10 min sintering at 850 °C under 100 MPa. Density and microstructural measurements indicate that densification is first driven by the viscous flow of a vitreous phase containing Cs, formed during calcination. Additionally, the density of the sample then increases further during sintering by grain boundary diffusion. However, a limited but non negligible part of cesium is lost during densification.

36 MATERIALS SCIENCE↗

Probing the high-pressure densification of amorphous silica nanomaterials using SBA-15: An investigation into the paradoxical nature of the first sharp diffraction peak

The densification and X-ray scattering of mesoporous silica (SBA-15) were measured simultaneously under gigapascal (GPa) pressures. The results are compared to previous work on amorphous silica (aSiO 2 ) and demonstrate the feasibility of measuring the densification of aSiO 2 nanomaterials with small angle X-ray scattering (SAXS) in-situ in a diamond anvil cell. Compared to fused silica, the position of the SBA-15 first sharp diffraction peak (FSDP) is 7 times more sensitive to pressure and has a transition in its pressure dependance at a lower pressure (~2 GPa vs.~13 GPa). SBA-15 has two densification regimes, low-density amorphous and highdensity amorphous, which have equations of state comparable to low-density amorphous and high-density amorphous fused silica. Further, the transition between these two regimes occurs at a lower pressure than for fused silica (~1.5 GPa vs.~13 GPa). The results suggest that there is no direct relationship between the FSDP position and the aSiO 2 density during compression.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Densification, microstructure and properties of TiB2 ceramics fabricated by spark plasma sintering

Highlights: • Nearly full densification of in-house processed TiB{sub 2} ceramic powders at 1500 °C. • Microstructures revealing the size and shape of TiB{sub 2} grains after SPS. • The effect of sub-micron particles on the densification during SPS. • The effect of sintering pressure on the microstructure. • Microhardness and nano-indentation measurements along with oxidation studies. - Abstract: This study reports the fabrication of high-density TiB{sub 2} ceramics at reduced temperatures (1500 °C) by using field assisted sintering technology/spark plasma sintering (FAST/SPS) technique. In-house processed TiB{sub 2} powders with high purity were employed as starting materials. The effects of SPS conditions on the sintering behavior and microstructure of TiB{sub 2} were investigated. Sub-micron character of TiB{sub 2} particles has a strong influence on the densification during SPS. Microstructural analyses revealed that the high pressure affected both the grain size and the shape of TiB{sub 2} crystallites. Elongated grains with average size of 6 μm were perceived in TiB{sub 2} sample fabricated by SPS at 1500 °C under 60 MPa pressure with a relative density of 96.7%. The microhardness and elastic modulus were measured as 27.4 GPa and 685.2 GPa, respectively. This sample revealed an improved oxidation resistance due to the formation of a thin oxidation layer on the surface when heated up to 1200 °C.

36 MATERIALS SCIENCE↗

More Realistic Intermediate Depth Dry Firn Densification in the Energy Exascale Earth System Model (E3SM)

Abstract Earth system models account for seasonal snow cover, but many do not accommodate the deeper snowpack on ice sheets (aka firn) that slowly transforms to ice under accumulating snowfall. To accommodate and resolve firn depths of up to 60 m in the Energy Exascale Earth System Model's land surface model (ELM), we add 11 layers to its snowpack and evaluate three dry snow compaction equations in multi‐century simulations. After comparing results from ELM simulations (forced with atmospheric reanalysis) with empirical data, we find that implementing into ELM a two‐stage firn densification model produces more accurate dry firn densities at intermediate depths of 20–60 m. Compared to modeling firn using the equations in the (12 layer) Community Land Model (version 5), switching to the two‐stage firn densification model (with 16 layers) significantly decreases root‐mean‐square errors in upper 60 m dry firn densities by an average of 41 kg m −3 (31%). Simulations with three different firn density parameterizations show that the two‐stage firn densification model should be used for applications that prioritize accurate upper 60 m firn air content (FAC) in regions where the mean annual surface temperature is greater than roughly −31°C. Because snow metamorphism, firn density, and FAC are major components in modeling ice sheet surface albedo, melt water retention, and climatic mass balance, these developments advance broader efforts to simulate the response of land ice to atmospheric forcing in Earth system models.

58 GEOSCIENCES↗

Spark Plasma Sintering of Commercial Zirconium Carbide Powders: Densification Behavior and Mechanical Properties

Commercial zirconium carbide (ZrC) powder is consolidated by Spark Plasma Sintering (SPS). Processing temperatures range from 1650 to 2100 °C. Specimens with various density levels are obtained when performing single-die SPS at different temperatures. Besides the single-die tooling setup, a double-die tooling setup is employed to largely increase the actual applied pressure to achieve higher densification in a shorter processing time. In order to describe the densification mechanism of ZrC powder under SPS conditions, a power-law creep constitutive equation is utilized, whose coefficients are determined by the inverse regression of the obtained experimental data. The densification of the selected ZrC powder is shown to be likely associated with grain boundary sliding and dislocation glide controlled creep. Transverse rupture strength and microhardness of sintered specimens are measured to be up to 380 MPa and 24 GPa, respectively. Mechanical properties are correlated with specimens’ average grain size and relative density to elucidate the co-factor dependencies.

36 MATERIALS SCIENCE↗