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At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

A Double-side Cooled SiC MOSFET Power Module with Sintered-silver Interposers: I. Design, Simulation, Fabrication, and Performance Characterization

Planar, double-side cooled power modules are emerging in electric-drive inverters because of their low profile, better heat extraction, and lower package parasitic inductances. However, there is still concern about their reliability due to the rigid interconnection between the device chips and two substrates of the power module. In this paper, a porous interposer made of low-temperature sintered silver is introduced to reduce the thermo-mechanical stresses in the module. A double-side cooled half-bridge module consisting of two 1200 V, 149 A SiC MOSFETs was designed, fabricated, and characterized. By using the sintered-Ag instead of solid copper interposers, our simulation results showed that at a total power loss of 200 W, the thermo-mechanical stress at the most vulnerable interfaces (interposer-attach layer) was reduced by 42 % and in the SiC MOSFET by 50 % with a trade-off of only 3.6 % increase in junction temperature. The sintered-Ag interposers were readily fabricated into desired dimensions without post-machining and did not require any surface finishing for die-bonding and substrate interconnection by silver sintering. Here, the porous interposers were also deformable under a low force or pressure, which helped to accommodate chip thickness and/or substrate-to-substrate gap variations in the planar module structure, thus simplifying module fabrication. Experimental results on the electrical performance of the fabricated SiC modules validated the success of using the porous silver interposers for fabricating planar, double-side cooled power modules.

42 ENGINEERING↗
DOE OSTI2020

Magnetic and mechanical properties of grain-refined Dy-free Nd-Fe-B sintered magnets

In this work, the effects of grain size on magnetic and mechanical properties of Dy-free Nd-Fe-B sintered magnets were studied. The grain size of the sintered magnets was varied by using different sized Dy-free Nd-Fe-B alloy feedstock powders which were ball milled to different extents. Increasing the ball milling time from 7 to 11 h caused the average particle size of the powders to decrease from 3.6 to 2.1 µm, while the average grain size of the corresponding sintered magnets decreased from 5.0 to 4.0 µm. The intrinsic coercivity Hcj and maximum energy product (BH) max of these magnets increased from 11.6 to 13.7 kOe and 41.6 to 43.6 MGOe, respectively. The finer grain magnets exhibited better thermal stability, as indicated by a smaller temperature coefficient of H cj (-0.71%/°C). With extending ball milling time to 15 h, the magnetic properties of the magnets deteriorate, while the flexural strengths first decrease and then increase. The flexural strength improvement is attributed to the increased Oxygen content in the magnets due to finer grains. The coercivity enhancement by reduction of grain size is a promising approach to develop Dy-free Nd-Fe-B sintered magnets with better thermal stability. It is important to control the Oxygen contents in the magnets to compromise both magnetic and mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Chemically Inert Hydrocarbon-Based Slurries for Rapid Laser Sintering of Thin Proton-Conducting Ceramics

The process of rapid laser sintering of thin BaZrO 3 –BaCeO 3 -based proton-conducting electrolytes is being developed for easy fabrication of ceramic fuel cells and electrolyzers. However, cracks on the electrolytes caused by volume change due to chemical reactions between the basic ceramic constituents and the polar solvents during wet processing has been problematic. In order to address this issue, the use of chemically inert saturated-hydrocarbon-based slurries comprised of hexadecane, polybutene, and a long-chain saturated fatty acid were investigated in this work. By optimizing slurry composition and laser sintering conditions, a 20 mm long, 4 mm wide, 13.5-μm-thick and 97%-dense BaCe 0.7 Zr 0.1 Y 0.07 Sm 0.13 O 3-d membrane showing proton conductivity on the order of 10 –4 S•cm –1 at 600 °C was successfully prepared in just three seconds by laser sintering. As a result, the use of saturated-hydrocarbon-based slurries will facilitate wet processing and rapid laser sintering of proton-conducting ceramic electrolytes.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Transformation of a ceramic precursor to a biomedical (metallic) alloy: Part I – sinterability of Ta 2 O 5 and TiO 2 mixed oxides

Mixed Ta 2 O 5 – TiO 2 binary system was studied by a combination of differential thermal analysis (DTA), scanning electron microscopy-energy dispersive spectrometry (SEM-EDS), X-ray diffraction (XRD) and in situ high temperature X-ray diffraction (HT-XRD) techniques. Different compositions of the mixed oxide powders were fabricated by ball–milling the powdered compositions, pelletizing the homogenized composite powders, and heating the green pellets in air at different temperatures for fixed time intervals. The sintered pellets were evaluated and characterized with respect to porosity, morphology, and phase distribution. DTA runs of the un-sintered powders indicated the onset temperatures for both exothermic and endothermic changes in the binary system. Significant amount of sintering was observed to take place at temperatures higher than 900 °C. Both room and high temperature X-ray diffraction patterns exhibited consistency in phase formation. A ternary compound (TaTiO 4 ) and a ternary solid solution (Ti 0.33 Ta 0.67 O 2 ) were observed to form in both room and high temperatures in addition to the respective binary phases (Ta 2 O 5 and TiO 2 ). A sintering temperature in the range 900–1000 °C was observed to be adequate to achieve the requisite mechanical strength and optimum internal porosity (40–48%) for subsequent electrochemical polarization experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Extraordinary Thermal Stability and Sinter Resistance of Sub-2 nm Platinum Nanoparticles Anchored to a Carbon Support by Selenium

Nanoparticle sintering has long been a major challenge in developing catalytic systems for use at elevated temperatures. Here we report an in situ electron microscopy study of the extraordinary sinter resistance of a catalytic system comprised of sub-2 nm Pt nanoparticles on a Se-decorated carbon support. When heated to 700 °C, the average size of the Pt nanoparticles only increased from 1.6 to 2.2 nm, while the crystal structure, together with the {111} and {100} facets, of the Pt nanoparticles was well retained. Our electron microscopy analyses suggested that the superior resistance against sintering originated from the Pt–Se interaction. Confirmed by energy-dispersive X-ray elemental mapping and electron energy loss spectra, the Se atoms surrounding the Pt nanoparticles could survive the heating. This work not only offers an understanding of the physics behind the thermal behavior of this catalytic material but also sheds light on the future development of sinter-resistant catalytic systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
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 OSTI2021

Evaluation of Low-Pressure-Sintered Multi-Layer Substrates for Medium-Voltage SiC Power Modules: Preprint

Direct-bonded aluminum (DBA) multi-layer substrates have been fabricated using low-pressure silver sintering. These multi-layer substrates can be used to reduce the peak electric field strength inside power modules. This benefit is particularly important for medium-voltage silicon carbide (SiC) MOSFETs due to their higher operating voltages. The voiding content and defect density of the bond used to create the multi-layer substrate stackup is critical to the thermal performance and reliability of the power module. This work two low-pressure-assisted sintering techniques; one using nano-silver preform and the other using nano-silver paste to bond 23 mm by 49 mm DBA substrates. Scanning acoustic microscopy (C-SAM) is used to evaluate the bond quality after sintering. To evaluate the reliability of the sintered multi-layer substrates, passive thermal cycling from –40 °C to 200 °C was performed. Cross-sections were cut at pre-determined intervals and imaged with Scanning Electron Microscopy (SEM). After 1,000 thermal cycles, minor cracking was observed, but no failures have occurred.

28 EE - Advanced Manufacturing Office (EE-5A)↗
DOE OSTI2023

New Materials and an Efficient Processing Approach for Materials for Harsh Environments – Continuous Electric Field Assisted Sintering

Electric-field assisted sintering (EFAS) is an advanced manufacturing method for the consolidation and processing of ceramic and metal materials. It is a particularly excellent candidate for efficient materials processing as it has greater than 90% energy cost savings and improved CO2 emissions compared to traditional sintering in a furnace. This is due to direct rapid heating of the materials and molds leveraging an electrification phenomenon called Joule heating where electrical current is passed through the sample/mold assemblies causing direct heating. The technique does have limitations though as it is traditionally a batch-process and suffers from scale up difficulties. To overcome this, researchers at Idaho National Laboratory changed the form factor of traditional EFAS instruments to develop and construct a continuous rolling electric-field assisted sintering (CEFAS) device. Its unique design creates highly localized electrical, thermal, and mechanical process parameters for continuous samples of limitless length. Advanced core shell powder materials were also created using fluidized powder bed atomic layer deposition of core/shell solid oxide electrochemical electrode/electrolyte BaCe0.7Zr0.1Y0.1Yb0.1O3 (BCZYYb) and yttrium doped BaZrO3 (BZY) to be a feedstock for the new CEFAS instrument. The innovative core/shell powder is hypothesized to have high protonic conductivity with enhanced environmental resistance. The completed project covers innovations in process control and design enabled by control theory, finite element modeling and mechanical design, three dimensionally printed carbon-carbon composite manufacturing and utilization, and green materials processing techniques.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Multi-scale modeling of the electric field assisted sintering process

The electric field assisted sintering (EFAS) process involves tightly coupled physics that influence microstructural evolution in the particles being compacted. It is also an inherently multi-scale phenomenon, with the microstructure of the compact influencing the subsequent engineering-scale response of the sintering system. To improve understanding of how processing parameters influence microstructural evolution, we have developed a multi-scale modeling approach that couples a continuum-level model of the sintering system with a phase-field model for microstructural evolution of particles within the compact. The phase-field model couples the effect of chemical and electrical driving forces on microstructural evolution and includes the effect of charged defect segregation to surfaces and grain boundaries; this segregation leads to enhanced defect transport and heat generation at these interfaces in response to applied electric field. The effect of enhanced heat generation on particle neck growth and the influence of microstructural evolution on the engineering-scale model are demonstrated.

36 - MATERIALS SCIENCE↗
DOE OSTI2023

A Limit to Accelerated Free-Sintering: Nano-Phase Separation Interferes With Organic Debinding

Nano-phase separating Ni–12 at. pct Ag powders are processed via high-energy ball milling and brought into a supersaturated state with a reduction of the grain size to the nanocrystalline scale, a combination that is designed to encourage rapid densification by phase separation upon heating. This unstable powder is then characterized by dilatometry, in-situ x-ray diffraction, thermogravimetry and microstructure analysis for sintering cycles up to 940 °C. However, these powder compacts exhibit excessive pore evolution and significant macroscopic swelling caused by removal of the organic process additives. This competition of organic removal with densification is known in nanocrystalline metals, but the present study adds an additional dimension of phase separation, which shifts the dominant swelling mechanism as the formation of the second phase traps the volatilizing organics and hinders the debinding process. The creep swelling and overall loss in relative density is then dominated by the creep deformation of the second Ag phase. The interference between organic removal and low-temperature onset of consolidation represents a new challenge to efforts aimed at rapid free sintering and should guide the design of rapidly sintering alloys; specifically, the present work emphasizes the need to select alloys that have their sintering-accelerating phase separation temperature above the range where gases are evolved.

36 MATERIALS SCIENCE↗
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↗
DOE OSTI2025

Induction ultrafast sintering

This study proposes and demonstrates induction ultrafast sintering (IUS), which enables rapid densification of refractory and other materials via two contactless modalities: direct IUS (d-IUS), where heating occurs through electromagnetic coupling with the sample, and susceptor IUS (s-IUS), where heating is achieved indirectly via an induction-heated metal case. Ultrahigh heating rates of ∼75 to >450 °C/s and temperatures exceeding 2500 °C are readily achieved. Both d-IUS and s-IUS densify molybdenum to high densities within 120 s, with only ∼1–3 % porosity observed by image analysis. Similarly, 3 mol % yttria-stabilized zirconia (3YSZ) reaches ∼97 % relative density in 30 s via s-IUS. This study further demonstrates ultrafast reactive sintering of two difficult-to-sinter materials: a refractory compositionally complex alloy–carbide (RCCA–CCC) composite, NbMoTaW–(Nb 0.37 Mo 0.11 Ta 0.39 W 0.13 ) 2 C, using d-IUS, and a compositionally complex silicide (CCS), (Mo 1/3 Nb 1/3 Zr 1/3 )Si 2 , using s-IUS. This IUS platform offers a versatile route for high-throughput materials discovery and energy-efficient fabrication of bulk refractory materials.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Demonstration of the Reproducibility Challenges in the Sintering Behavior of Lithium‐Stuffed Garnets in Scaling up Synthesis

Lithium-stuffed garnets, such as Li 7 La 3 Zr 2 O 12 (LLZO), are promising candidates for next-generation solid-state batteries because of their high room-temperature ionic conductivity and chemical stability against lithium metal anodes, which are crucial for achieving higher energy density. However, realizing LLZO's potential in practical devices requires synthesis methods that can be scaled reliably to large batch sizes for manufacturing. Herein, we investigate the sintering reproducibility of LLZO synthesized at larger scales using ultrasonic spray pyrolysis, a cost-effective and scalable synthesis route. Two 100 g batches of Al-doped LLZO are prepared and their sintering behavior is examined in detail. Both Al-LLZO batches contain over 90 wt.% cubic-phase LLZO, and both batches exhibit room temperature conductivities greater than 1 × 10 −4 S cm −1 at a relative density above 0.8. However, variations in secondary phases and subtle differences in Al content lead to significant differences in densification and microstructure. These results demonstrate that LLZO's sintering behavior is highly sensitive to small changes in secondary phases and Al content, creating reproducibility challenges when moving from laboratory- to manufacturing-scale synthesis.

36 MATERIALS SCIENCE↗
DOE OSTI2023

In situ probing of interfacial roughness and transient phases during ceramic cold sintering process

The ceramic cold sintering process (CSP) offers an eco-friendly approach to producing fully dense ceramics at low temperatures. However, an incomplete mechanistic understanding hinders its optimization and widespread adoption. In this study, we analyze the microstructural and structural changes in ZnO, a model CSP system, using in situ synchrotron-based high-energy small-angle X-ray scattering and X-ray diffraction techniques. Our results reveal the time evolution of ZnO particles' surface area and roughness, reflecting the dissolution and re precipitation processes that enable densification. The in situ measurements supply valuable kinetic data for these stages of CSP. Alongside microstructural changes and densification, we observed the evolution of secondary phases representing reaction products between ZnO and acetic acid, the solvent used. The initial ZnO/solvent mixture's dominant secondary phase is attributed to zinc acetate, which is gradually replaced by a zinc soap-type structure during CSP. This structure has a large (≈ 21 Å) lattice parameter and is assumed to have a layered nature. The formation of this soap phase, which is retained in the sintered product as an intergranular component, appears to be a signature of successful cold sintering as it facilitates mass transport, leading to densification. Here, our study underscores the potential of in situ synchrotron characterization for revealing microstructural and phase-evolution details during CSP. These findings, which would be challenging to obtain through ex situ measurements, provide crucial data to guide and validate theoretical models, ultimately enhancing CSP's effectiveness and adoption.

36 MATERIALS SCIENCE↗