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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Microstructure refinement of hot deformed Dy-free NdFeB magnets through a novel cold sintering approach by pressure-assisted spark plasma sintering

Anisotropic fine-grained Dy-free NdFeB high-performance magnets were produced using a novel cold sintering approach by pressure-assisted spark plasma sintering (SPS). The NdFeB nanocrystalline ribbon powders were subjected to cold sintering below 450 °C using pressure-assisted SPS, followed by hot deformation at 710 °C and 810 °C via SPS. Results indicate that cold sintering below 450 °C effectively restricts grain growth in the NdFeB magnets, yielding sub-100 nm scale grains across both fine-grained regions and most coarse-grained regions. The refined grain structure achieved through cold sintering allows for a lower hot deformation temperature as compared with the magnet by conventional sintering, as finer grains allow easier deformation and grain sliding/rotation. This process produces a highly fine-grained and anisotropic microstructure to achieve high magnetic performance (i.e., high intrinsic coercivity, remanence, and maximum energy product) in the magnets. The cold sintering (at 350 °C) and lower hot deformation temperatures required (e.g., 710 °C) help control grain coarsening and limit grain size that is commensurate with the size of a single magnetic domain of the Nd 2 Fe 14 B magnetic matrix phase, resulting in high intrinsic coercivity (H ci =11.4 kOe). Furthermore, the reduced hot deformation temperature mitigates the formation of coarse grain bands, leading to improved magnetic properties, specifically an increased remanence (B r = 14.3 kGs) and a high maximum energy product ((BH) max = 48 MGOe). In conclusion, cold sintered hot deformed NdFeB magnet also shows good thermal stability with reversible temperature coefficient α(B r )= -0.097 %/K and α(H ci )= -0.616 %/K at elevated temperatures up to 400 K.

Cold Sintering↗
DOE OSTI2024

Selective laser sintering and spark plasma sintering of (Zr,Nb,Ta,Ti,W)C compositionally complex carbide ceramics

Abstract Two advanced manufacturing processes, spark plasma sintering (SPS) and selective laser sintering (SLS), have been developed for synthesis of (Zr,Nb,Ta,Ti,W)C compositionally complex carbide (CCC) via reactive sintering of a powder mixture of constitute monocarbides. X‐ray diffraction analysis confirmed that the single‐phase CCC can be formed by both SPS and SLS. While a homogenous microstructure with uniform metal element distributions was developed during SPS, three‐layer microstructures with a thin TiC‐rich layer and two TaC‐rich layers along with a TiO 2 ‐rich surface layer containing W nanoparticles were formed during SLS. In addition, cellular structures with W, Zr, and Ti element segregation and dislocations on cell boundaries were observed in the SLS‐CCC sample, indicating the effect of nonequilibrium conditions on microstructure formation during laser melting followed by rapid cooling and solidification process. Compared to the SPS‐CCC sample, the SLS‐CCC showed enhanced hardness and reduced thermal conductivity, which may be related to their unique cellular structures.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Scaling microstructural processes in the sintering of ionic ceramics

A multi-scale framework, combining a multiphase field formulation and large deformation mechanics, was developed as a stepping stone to perform the data analytics of the microstructural level kinetics of a sintering solid. Relevant microstructural information from this framework, such as grain, stress, and porosity statistics, was scaled up to describe the macroscopic level sintering kinetics. Here, the developed formulation was applied to describe the electric field assisted sintering of Y 2 O 3 . Microstructural inhomogeneities in a multi-granular solid result in the formation of a field of compressive stress networks, which interleave with low compression and weakly tensile regions, defining a scaffolding for sintering concentration regions to develop. A Poisson effect-induced lateral stress network is also naturally self-induced as a result of the mechanical constraints imposed by the sintering apparatus. For long sintering times, localized shear stresses enhancing mass flow along grain boundaries and internal surfaces develop. Three-sided pores are removed by either vacancy transport to the surrounding pores, or move towards the external surfaces through grain boundary diffusion. Four- and higher order-sided pores stabilize because an equal amount of vacancies are gained and lost through the connecting grain boundaries. Grain dewetting contributes to pore coalescence, suggesting that pore kinetics and grain growth are coupled and should be analyzed in concert. The combined sintering and grain growth kinetics define six regimes of sintering behavior: (1) T, the transient regime; (2) E$_Υ$, the surface energy dominated, early sintering regime, where the grain growth exponent, p = 1, and the stress concentration factor, $f$ ~ $1/\hat{ρ}^{4.6}$; (3) E S , the stress dominated, early sintering regime, where p = 1 and $f$ ~ $1/\hat{ρ}^{4}$; (4) I$_Υ$, the surface energy dominated, intermediate sintering regime, where p = 2 and $f$ ~ $1/\hat{ρ}^{4.6}$; (5) I S , the stress dominated, intermediate sintering regime, where p = 2 and $f$ ~ $1/\hat{ρ}^{4}$; and (6) L, the late sintering regime, where p = 3 and $f$ ~ 1. At the macroscopic level, the rapid densification and suppression of grain growth observed in the electric field assisted sintering process is a consequence of the compounding effects of the underlying stress-, transport-, and interfacial-energy-induced energy minimization kinetics, as predicted by the multi-scale framework.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Multi-material direct ink writing and co-sintering of gadolinium oxide – zirconium oxide components

Methods for fabrication of multi-material or functionally graded ceramic composite architectures are of interest for numerous applications. However, conventional co-sintering of multi-material ceramic parts is a challenge because differences in the sintering behavior of the two materials leads to interfacial strain and, ultimately, component failure. Direct ink writing (DIW) is an extrusion-based additive manufacturing process that excels at multi-material printing because multiple extrusion nozzles can be installed on the same gantry system. Furthermore, the use of DIW as a method to fabricate multi-material ceramic green bodies offers an additional variable for controlling and potentially matching sintering kinetics in the slurry formulation used for two dissimilar feedstocks. In the work documented in this manuscript, we explored two strategies to successfully co-sinter multi-material ceramic oxides: slurry optimization to match sintering kinetics and material gradients to step from one material to another. This manuscript also quantifies the allowable mismatch that avoids part cracking in solid solution forming multi-material systems and discusses best strategies to reduce mismatch during co-sintering. Inks composed of gadolinium oxide (Gd 2 O 3 ) and zirconium oxide (ZrO 2 ), a surrogate for uranium oxide (UO 2 ), were thermally matched, which resulted in a sintering mismatch reduction of over 10%. It was found that ~1% mismatch is tolerable during debind cycles and that ~5% mismatch is manageable during sintering cycles after slurry formulations are optimized to match the sintering behavior. Use of continuous gradients is shown to reduce sintering mismatch, although geometric resolution may be lost due to solid solution formation.

Snarr, Patrick L. [Oak Ridge National Laboratory (↗
DOE OSTI2024

Effect of sintering temperature on feature resolution and flexural strength of ceramics fabricated through vat photopolymerization additive manufacturing

Although ceramic additive manufacturing (AM) could be used to fabricate complex, high-resolution parts for diverse, functional applications, one ongoing challenge is optimizing the post-process, particularly sintering, conditions to consistently produce geometrically accurate and mechanically robust parts. This study aims to investigate how sintering temperature affects feature resolution and flexural properties of silica-based parts formed by vat photopolymerization (VPP) AM. Test artifacts were designed to evaluate features of different sizes, shapes and orientations, and three-point bend specimens printed in multiple orientations were used to evaluate mechanical properties. Sintering temperatures were varied between 1000°C and 1300°C. Deviations from designed dimensions often increased with higher sintering temperatures and/or larger features. Higher sintering temperatures yielded parts with higher strength and lower strain at break. Many features exhibited defects, often dependent on geometry and sintering temperature, highlighting the need for further analysis of debinding and sintering parameters. To the best of the authors’ knowledge, this is the first time test artifacts have been designed for ceramic VPP. This work also offers insights into the effect of sintering temperature and print orientation on flexural properties. These results provide design guidelines for a particular material, while the methodology outlined for assessing feature resolution and flexural strength is broadly applicable to other ceramics, enabling more predictable part performance when considering the future design and manufacture of complex ceramic parts.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Compensating for Sintering Distortion in Additively Manufactured Shaped Charge Liners using Physics-Informed Machine Learning

Copper is a challenging material to process using laser-based additive manufacturing due to its high reflectivity and high thermal conductivity. Sintering-based processes can produce solid copper parts without the processing challenges and defects associated with laser melting; however, sintering can also cause distortion in copper parts, especially those with thin walls. In this study, we use physics-informed Gaussian process regression to predict and compensate for sintering distortion in thin-walled copper parts produced using a Markforged Metal X bound powder extrusion (BPE) additive manufacturing system. Through experimental characterization and computational simulation of copper’s viscoelastic sintering behavior, we can predict sintering deformation. We can then manufacture, simulate, and test parts with various compensation scaling factors to inform Gaussian process regression and predict a compensated as-printed (pre-sintered) part geometry that produces the desired final (post-sintered) part.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Enhancing low-temperature sintering in the MgO-LiF system: Mechanistic insights

In the present article, we provide compelling evidence that minor (1 wt%) additions of micron and nanometre-sized LiF particles in MgO decompose leading to free Li diffusing into MgO surfaces enhancing vacancy production during direct current sintering. The addition of nanometre-sized LiF particles leads to a > 500 °C reduction in the sintering temperature and over 99 % theoretical density of final consolidated compacts. Correlating differential scanning calorimetry with in-situ x-ray diffraction, together with Schottky calculations, post sintering electron microscopy and laser induced breakdown spectroscopy, we uncover critical insights into this impressive reduction in sintering temperature. Our quantitative analysis reveals that MgO and LiF interact at low temperatures with the diffusion of Li into the surface of MgO particles due to the intrinsic structural disorder of the LiF and MgO crystallites. Nanometre-sized LiF particles were found to react the most at low temperatures due to their increased structural disorder. Our multimodal characterization points to a Li-promoted densification and sintering mechanism. This impressive reduction in sintering temperature can be harnessed to promote low-temperature fabrication of MgO-based composites for technological applications.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Metal hybridization in dilute-alloy catalysts promotes sintering resistance by decreasing surface mobility

Dilute-metal-alloy nanoparticles exhibit enhanced catalytic performance compared with monometallic nanoparticles for many reactions. Anecdotal reports indicate that very dilute alloying can also slow the sintering rates of supported nanoparticles, although this has not been rigorously assessed and cannot be explained using bulk descriptors such as metal melting temperature. Here, in this study, we utilize methanol synthesis reactivity, microscopy and in situ spectroscopy measurements to demonstrate that 1 atom% Pt addition to ~1–2-nm-diameter Cu (Pt 1 Cu 100 ) nanoparticles supported on SiO 2 dramatically decreases their sintering rates. Minimal sintering of Pt 1 Cu 100 nanoparticles is observed during aging in H 2 up to 700 °C versus 500 °C for Cu nanoparticles. Scanning tunnelling microscopy reveals that the addition of 0.01 monolayer of Pt to a Cu(110) surface decreases the detachment rate of undercoordinated atoms, demonstrating that dilute dopants can locally decrease the rate of the first step in nanoparticle sintering. Density functional theory calculations quantify the stabilization and predict other sinter-resistant dilute alloys. We find that the degree of host–dopant d-state hybridization correlates with decreased surface mobility, providing a mechanistic framework for designing sinter-resistant catalysts.

Finzel, Jordan [Univ. of California, Santa Barbara↗
DOE OSTI2024

Pressureless sintering of lithium hydride

Lithium Hydride is a material of growing importance for addressing technological challenges related to nuclear fusion, long-term human space travel, and thermal energy storage. Pressureless sintering provides a straightforward, scalable approach to produce dense LiH parts of all sizes and shapes. Pressed LiH green compacts were sintered at heating rates from 2.5 to 20 °C/min to 650 °C, yielding densities up to 96 ± 1.4 %, with densification initiating at 500 °C. Here, a validated master sintering curve was constructed with a sintering apparent activation energy of 135 kJ/mol. X-ray diffraction and simultaneous thermal analysis revealed Li 2 O formation from 300 – 550 °C and decomposition of LiH into Li metal at 550 °C, each reflected as deviations in the master sintering curve. Computed tomography after thermal treatment to 550 °C showed the formation of corrosion products, and after thermal treatment to 650 °C LiH reduction to Li most significantly at exposed surfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Thermomechanical Degradation of Sintered Copper Under High-Temperature Thermal Shock

The need for reliable bonded interface materials is critical to realize the performance benefits of wide-bandgap devices in power electronics modules, especially in operating temperatures greater than 150 degrees C. In this paper, we investigate the thermomechanical performance of sintered copper (Cu) as a large-area attachment, bonded between Cu baseplates and active-metal-bonded substrates, under accelerated thermal shock (-40 degrees C to 200 degrees C) conditions. In the fabrication phase of the samples, we used different stencil patterns and found that the grid and stripe patterns resulted in a better outgassing of the residual organics during the sintering process, thereby ensuring a substantially improved bond quality compared to a full-area print. The paste consisted of Cu microflakes, and we performed sintering using a Budatec SP300 sintering press at 275 degrees C with 15 MPa of bonding pressure for 5 minutes in a nitrogen atmosphere. Under accelerated experiments, we monitored the degradation of the sintered Cu bond in the samples through C-mode scanning acoustic microscope (C-SAM) images. To quantify the defect percentage in C-SAM images, we investigated image denoising techniques to exclude the pattern prints. Finally, we cross-sectioned a sample and obtained scanning electron microscope images, which revealed adhesive fracture as the dominant failure mechanism.

ADVANCED PROPULSION SYSTEMS,INORGANIC, ORGANIC, PH↗
DOE OSTI2024

Sintering-based Metal Additive Manufacturing Methods for Magnetic Materials

In this chapter, we review the relationship between solid-state sintering and additive manufacturing (AM) methods for fabricating soft and hard magnetic materials. Heat treatment as a post-processing method has been done in conjunction with AM as a method to improve density and/or mechanical properties. In binder jetting (BJT) of metal powders, sintering is a crucial post-processing step and is necessary for obtaining the final product. This is because the parts are only in the “green” state when they leave the BJT printer, with poor mechanical properties and high porosity. Sintering densifies and strengthens the green part into the final product. A potential industrial application for sintering-based AM is the fabrication of magnetic materials. The motivation for doing so, the process and properties of the AM magnets, and the potential applications of post-sintered AM magnets are explored.

Wang, Haobo↗
DOE OSTI2025

Dynamic Metal–Support Interaction Dictates Cu Nanoparticle Sintering on Al 2 O 3 Surfaces

Nanoparticle sintering remains a critical challenge in heterogeneous catalysis. In this work, we present a unified deep potential (DP) model based on the Perdew–Burke–Ernzerhof approximation of density functional theory for Cu nanoparticles on three Al 2 O 3 surfaces (γ-Al 2 O 3 (100), γ-Al 2 O 3 (110), and α-Al 2 O 3 (0001)). Using DP-accelerated simulations, we reveal that the nanoparticle size-mobility relationship strongly depends on the supporting surface. The diffusion of nanoparticles on the two γ-Al 2 O 3 surfaces is almost independent of the size of the nanoparticle, while the diffusion on α-Al 2 O 3 (0001) decreases rapidly with increasing size. Interestingly, nanoparticles with fewer than 55 atoms diffuse several times faster on α-Al 2 O 3 (0001) than on γ-Al 2 O 3 (100) at 800 K while expected to be more sluggish based on their larger binding energy at 0 K. The diffusion on α-Al 2 O 3 (0001) is facilitated by dynamic metal–support interaction (MSI), where Al atoms move out of the surface plane to optimize contact with the nanoparticle and relax back to the plane as the nanoparticle moves away. In contrast, the MSI on γ-Al 2 O 3 (100) and on γ-Al 2 O 3 (110) is dominated by more stable and directional Cu–O bonds, consistent with the limited diffusion observed on these surfaces. Our extended MD simulations provide insight into the sintering processes, showing that the dispersity of the nanoparticles strongly influences the coalescence driven by nanoparticle diffusion. We observed that the coalescence of Cu 13 nanoparticles on α-Al 2 O 3 (0001) can occur in a short time (10 ns) at 800 K even with an initial internanoparticle distance increased to 3 nm, while the coalescence on the two γ-Al 2 O 3 surfaces are inhibited significantly by increasing the initial internanoparticle distance. These findings demonstrate that the dynamics of the supporting surface is crucial to understanding the sintering mechanism and offer guidance for designing sinter-resistant catalysts by engineering the support morphology.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Improving protonic ceramic electrochemical cell performance via a dual-phase reaction-sintered bilayer electrolyte

Protonic ceramic electrochemical cells (PCCs) are promising energy conversion devices, but their fabrication remains challenging. In particular, the typical electrolytes for PCCs such as BaCe 0.7 Zr 0.1 Y 0.1 Yb 0.1 O 3−δ (7111) and BaCe 0.4 Zr 0.4 Y 0.1 Yb 0.1 O 3−δ (4411) suffer from intrinsic barium evaporation issues during high-temperature sintering. This tendency towards barium loss, combined with their highly refractory nature, leads to a tradeoff between sinterability and chemical stability. To address this tradeoff, we propose a bilayer electrolyte combining layers of 4411 and 7111 materials that is designed to enhance sinterability and conductivity through dual-phase reactive sintering. Our findings demonstrate that the bilayer structure exhibits shrinkage behavior closely matched to that of the fuel electrode substrate, with a higher shrinkage compared to a single-layer 4411 electrolyte. Utilizing this bilayer electrolyte structure, our PCCs achieve a peak power density of 637 mW∙cm −2 in fuel-cell mode and a current density of 1060 mA∙cm −2 at 1.3 V in electrolysis mode at 600 °C. Our PCCs demonstrate high Faradaic efficiency of 83% at 1.3 V and 500 °C. Hybrid distribution of relaxation times (DRT) polarization mapping further reveals that the bilayer structure reduces Ohmic and polarization resistance in both fuel-cell and electrolysis modes.

ceramic processing↗
DOE OSTI2025

Ultrafast Sintering and Dopant Effects in Garnet LLZO Solid Electrolytes

High-throughput, low-cost manufacturing, and optimization of solid electrolytes are necessary for the adoption of solid-state batteries. In this work, garnet-type Li 7 La 3 Zr 2 O 12 (LLZO) with different aliovalent dopants, 𝑇𝑎$_{^·_{𝑍𝑟}}$, 𝐴𝑙$^{··}_{𝐿𝑖}$, and 𝐺𝑎$^{··}_{𝐿𝑖}$, have been ultrafast-sintered with different temperature ramping rates. The densification behavior, phases, their evolution, and surface chemistry of different LLZO have been investigated and linked to their electrochemical performances. It has been shown that LLZO with 𝑇𝑎$_{^·_{𝑍𝑟}}$ dopant demonstrates the highest garnet phase purity and overall best electrochemical performances, and ultrafast sintering further improves densification, ionic conductivity, and electrochemical stability. On the other hand, LLZO doped with 𝐴𝑙$^{··}_{𝐿𝑖}$ and 𝐺𝑎$^{··}_{𝐿𝑖}$ are reaching higher cubic phase purities and ionic conductivities via conventional sintering, indicating undesirable dopant migration and segregation during the ultrafast sintering process. In conclusion, these findings provide insights into the manufacturing of solid electrolyte materials.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Unravelling Adsorbate-Metal-Oxide Interactions: Water Vapor Chemistry on the Growth and Sintering of Ni over Reducible CeO2(111) Thin Films

The role of water in the growth and sintering of Ni particles over well-ordered CeOx(111) (1.5 < x < 2) thin films was investigated through scanning tunneling microscopy (STM) and X-ray photoelectron spectroscopy (XPS) studies, considering ceria-supported Ni attracts great attention as a promising catalyst for reactions such as steam reforming of ethanol and water gas shift reaction, in which water vapor is used as a key reactant. In the study, both fully oxidized CeO2 and partially reduced CeO1.75 thin films were prepared to examine the effect of the oxygen vacancies/Ce3+ sites in ceria supports. Our STM results revealed that dosing water before or after Ni deposition over the CeOx(111) surfaces at room temperature influenced the sintering behavior of Ni nanoparticles with further heating. Exposure of water to Ni nanoparticles that were deposited over both CeO2 and CeO1.75 at 300 K causes the formation of flatter particles with significantly reduced height when heating to the same temperatures compared to Ni/ceria with no water adsorbates. The flatter Ni particles were also observed when water was first dosed over CeO2 at 300 K followed by Ni deposition at room temperature and further heating. Over a partially reduced CeO1.75 surface with predosed water at 300 K, there is an extensive decrease in the particle density upon subsequent Ni deposition at room temperature and a significant increase in the height for Ni nanoparticles with further heating to higher temperatures compared to Ni over a pristine CeO1.75 surface. This is due to the filling of oxygen vacancies caused by the dissociation of water. This creates fewer nucleation sites for Ni on ceria, weakening the metal-oxide interaction and causing significant metal sintering. Our experimental findings suggest distinct adsorbate-metal-oxide interactions are key to the tuning of sintering of Ni nanoparticles over the CeOx(111) surface caused by water exposure. Such interactions are essential for the further modification of Ni-based catalysts for improved reactivity and stability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Sintering protonic zirconate cells with enhanced electrolysis stability and Faradaic efficiency

The emerging applications of steam electrolysis and electrochemical synthesis at 300–600 °C set stringent requirements on the stability of protonic ceramic cells, which cannot be met by Ce-rich electrolytes. A promising candidate is Ce-free BaZr 0.8 Y 0.2 O 3–δ , but its usage has long been hindered due to the high sintering temperatures required for protonic devices. Here we resolved the issue through a co-sintering process, in which the shrinkage stress of a readily sinterable support layer helps to densify the pure BaZr 0.8 Y 0.2 O 3–δ electrolyte membrane at low temperatures. This approach eliminates Ce and harmful sintering aids in the dense zirconate electrolyte membrane, thereby enhancing the Faradaic efficiency and electrochemical stability, especially under harsh operating conditions. Here, the protonic zirconate cells have exceptional performance and demonstrate stable high-steam pressure electrolysis up to 0.7 atm steam pressure, –2 A cm –2 current density and over 800 h of dynamic operation at 600 °C. Our processing breakthrough enables stabilized protonic cells for demanding applications in future energy infrastructure.

25 ENERGY STORAGE↗
DOE OSTI2024

Spark plasma sintering of fuel meats for U 3 O 8 based dispersion fuels

Research and test reactors often use dispersion-type fuel due to its increased thermal conductivity and burn-up capabilities compared to conventional fuel. Al-U 3 O 8 (aluminumtriuranium octaoxide) dispersion fuels have several advantages over their competitors, such as higher service temperature and better stability of oxygen stoichiometry. However, the two-step fabrication of dispersion fuel causes undesirable porosity in cold-pressed fuel meats that is preserved in co-extruded fuel plates. To combat this, spark plasma sintering (SPS) was used for the fabrication of Al-15, 20, and 30 vol% U 3 O 8 and 8 and 12 vol% Mo-U 3 O 8 fuel meats for the Al-U 3 O 8 time. The in situ SPS data was used to construct and validate Master Sintering Curves (MSCs) with accuracies in Al fuels at 0.02 g/cm 3 , and Mo fuels at 0.07 and 0.17 g/cm 3 . The as-sintered fuel meats were characterised using x-ray diffraction (XRD) and scanning electron microscopy (SEM) to understand chemical and physical changes following the SPS process. The pellets exhibited very high relative densities, the U 3 O 8 was observed to undergo reduction to UO 2 .

Aluminium↗