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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 OSTI2017

Contact Drying of Printed Sinterable-Silver Paste

We report that drying of stencil-, screen-, or dispense-printed paste is a crucial, yet taken-for-granted, presintering step for sinterable-silver (SS) interconnect processing and ultimately its reliability. If the paste’s solvent is not sufficiently removed during drying, then entrapped gas can result, and that leads to the formation of thermal-, strength-, and reliability-limiting defects in the later-sintered interconnect layer. Presently advocated drying strategies for wet silver paste cause either a limit of associated size or area or require pressure assistance during subsequent sintering. Alternatively, open-face contact drying (OContDry) from contact heating or conductive heating (a method used in industrial processes) offers the potential to overcome those limitations with SS paste. However, satisfactory strength of its final sintered structure must be proven prior to any potential adoption. In this paper, the achievement of a combination of relatively large shear failure stress with low scatter for OContDry SS was demonstrated. Lastly, this is significant because OContDry enables greater processing versatility with SS interconnects and several other advantages too.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Characteristic properties of macroporous silicon sintering in an argon atmosphere

The temperature and time dependences of the sintering of macroporous silicon in Ar or Ar + 3% H{sub 2} are studied. The contribution of various mechanisms governing this process is determined. The specific features of the sintering of macroporous silicon are examined by means of isochronous and isothermal annealing of the samples with ordered and random macropores in the temperature range 1000–1225°C. It is found that the sintering of macroporous silicon under atmospheric pressure in an inert gas flow containing 2 × 10–4% O{sub 2} is greatly affected by thermal etching. Thermal etching competes with the substance-transfer processes characteristic of sintering and hinders the formation of a defect-free surface crust. The reason for etching consists in that gaseous silicon monoxide is generated and then carried away by the gas flow. The etching effect is dominant in the low-temperature range and is independent of whether H{sub 2} is added. The values obtained for the activation energy of the silicon diffusion coefficient, E{sub a} = 2.57 eV, and for the exponent n = 3.31–3.74 in the time dependence of the pore radius, r ~ t{sup 1/n} are indicative of a mixed substance-transfer mechanism via the surface and volume diffusion of silicon atoms.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Influence of the Sintering Temperature on the Thermoelectric Properties of the Bi 1.9 Gd 0.1 Te 3 Compound

The regularities of the influence of the sintering temperature (750, 780, 810, and 840 K) on the elemental composition, crystal-lattice parameters, electrical resistivity, Seebeck coefficient, total thermal conductivity, and thermoelectric figure of merit of the Bi 1.9 Gd 0.1 Te 3 compound are investigated. It is established that the elemental composition of the samples during high-temperature sintering varies due to intense tellurium evaporation, which can lead to the formation of various point defects (vacancies and antisite defects) affecting the majority carrier (electron) concentration and mobility. The sintering temperature greatly affects the electrical resistivity of the samples, while the influence on the Seebeck coefficient and total thermal conductivity is much weaker. The largest thermoelectric figure of merit (ZT ≈ 0.55) is observed for the sample sintered at 750 K.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2010

Improvement of Sintering, Thermal Behavior, and Electrical Properties of Calcium- and Transition Metal-Doped Yttrium Chromite

The A-site calcium doped yttrium chromite was additionally doped with various transition metals on the B-site to improve the sintering, thermal behavior and electrical properties of these ceramics for future use as an interconnect material in high temperature solid oxide fuel cells (SOFC). With 10 % addition of Co, Cu, Ni, Fe, and Mn, the single phase orthorhombic perovskite structure remained stable over a wide range of oxygen partial pressures, as confirmed by X-ray diffraction. The substitution of Cu for chromium remarkably improved the sinterability and allowed full densification in air by sintering at 1400 degrees C. The substitution of Co and Ni significantly improved the electrical conductivity of yttrium chromites in both oxidizing and reducing environments. This was explained by the increase of charge carrier density with nickel and cobalt doping, as confirmed by Seebeck measurements. With 10% of nickel dopant, the electrical conductivity of Y0.8Ca0.2CrO3±δ increased from 12 to 38 S/cm in air and from 2 to 15 S/cm in reducing atmosphere at 950 degrees C. Mn doping had a negative effect on the sintering and electrical conductivity.

30 DIRECT ENERGY CONVERSION↗

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 OSTI2012

Processing of U-2.5Zr-7.5Nb and U-3Zr-9Nb alloys by sintering process

To minimize the risk of nuclear proliferation, there is worldwide interest in reducing fuel enrichment of research and test reactors. To achieve this objective while still guaranteeing criticality and cycle length requirements, there is need of developing high density uranium metallic fuels. Alloying elements such as Zr, Nb and Mo are added to uranium to improve fuel performance in reactors. In this context, the Centro de Desenvolvimento da Tecnologia Nuclear (CDTN) is developing the U-2.5Zr-7.5Nb and U-3Zr-9Nb (weight %) alloys by the innovative process of sintering that utilizes raw materials in the form of powders. The powders were pressed at 400 MPa and then sintered under a vacuum of about 1x10{sup -4} Torr at temperatures ranging from 1050 deg. to 1500 deg.C. The densities of the alloys were measured geometrically and by hydrostatic method and the phases identified by X ray diffraction (XRD). The microstructures of the pellets were observed by scanning electron microscopy (SEM) and the alloying elements were analyzed by energy dispersive X-ray spectroscopy (EDS). The results obtained showed the fuel density to slightly increase with the sintering temperature. The highest density achieved was approximately 80% of theoretical density. It was observed in the pellets a superficial oxide layer formed during the sintering process. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2016

In-pile investigation results of re-sintering for uranium dioxide fuel with large grain size at temperature 650-700 C

When determining the radiation creep of nuclear fuel, apart from deformation caused by axial compressive stress, there is a shrinkage process induced by radiation re-sintering, which may contribute in total value of in-pile deformation. The aim of this work was to study re-sintering for large grain size fuel of uranium dioxide. WWER fuel pellets with grain size greater than 25 μm have been piled up in a special device and irradiated in the channel number 7 of the RBT-6 pool-type reactor. The height of the fuel column was continuously measured during the irradiation. The average temperature value in the fuel column center was 682 Celsius degrees and the total time of irradiation reached 1800 hours which corresponds to a specific burnup of 2.5 MWd/KgU, taking into account fission density and initial fuel stoichiometry. The results show that re-sintering throughout the height equals to 0.08% which correlates well with thermal re-sintering test and does not have an impact on the steady-state creep rate.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

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 OSTI2019

Water-Mediated Surface Diffusion Mechanism Enables the Cold Sintering Process: A Combined Computational and Experimental Study

The cold sintering process (CSP) densifies ceramics at much lower temperatures than conventional sintering processes. Several ceramics and composite systems have been successfully densified under cold sintering. For the grain growth kinetics of zinc oxide, reduced activation energies are shown, and yet the mechanism behind this growth is unknown. In this work, we investigate these mechanisms in more detail with experiments and ReaxFF molecular dynamics simulations. We investigated the recrystallization of zinc cations under various acidic conditions and found that their adsorption to the surface can be a rate-limiting factor for cold sintering. In conclusion, our studies show that surface hydroxylation in CSP does not inhibit crystallization; in contrast, by creating a surface complex, it creates an orders of magnitude acceleration in surface diffusion, and in turn, accelerates recrystallization.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Phase Transformations and Formation of Ultra-Fine Microstructure During Hydrogen Sintering and Phase Transformation (HSPT) Processing of Ti-6Al-4V

The hydrogen sintering and phase transformation (HSPT) process is a novel powder metallurgy method for producing Ti alloys, particularly the Ti-6Al-4V alloy, with ultra-fine microstructure in the as-sintered state. The ultra-fine microstructure is obtained as a direct result of the use of H-2 gas during sintering. The refinement of the microstructure during HSPT is similar to that of thermal hydrogen processing (THP) of bulk Ti alloys. For both THP and HSPT of Ti-6Al-4V alloy, the mechanisms of the grain refinement depend on the phase equilibria and phase transformations in the presence of hydrogen, which are surprisingly still not well established to date and are still subjected to research and debate. In recent work by the present authors, a pseudo-binary phase diagram of (Ti-6Al-4V)-H has been determined by using in situ synchrotron XRD and TGA/DSC techniques. Aided by this phase diagram, the current paper focuses on the series of phase transformations during sintering and cooling of Ti-6Al-4V in a hydrogen atmosphere and the mechanisms for the formation of the ultra-fine microstructures obtained. Using experimental techniques, including in situ synchrotron XRD, SEM, EBSD, and TEM, the microstructural refinement was found to be the result of (1) the precipitation of ultra-fine alpha/alpha(2) within coarse beta grains during an isothermal hold at intermediate temperatures, and (2) the eutectoid transformation of beta -> alpha + delta d at approximately 473 K (200 degrees C). (C) The Minerals, Metals & Materials Society and ASM International 2015

Sun, Pei↗

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 OSTI2018

Porous Titanium Parts Fabricated by Sintering of TiH{sub 2} and Ti Powder Mixtures

A new simple powder metallurgy process by sintering TiH{sub 2} powders was used to manufacture porous Ti components. The effects of the processing parameters (pressure of cold isostatic pressing and sintering temperature) and the TiH{sub 2}/Ti ratio in the powder mixtures on the impurities, the linear shrinkage and the pore properties (including overall and open porosities) were comprehensively determined. The addition of TiH{sub 2} as a reactant has been found beneficial for the synthesis of porous Ti components. The formation mechanisms of pores were demonstrated based on the dehydrogenation process of TiH{sub 2} during sintering, resulting in highest reactivity due to the “in statu nascendi” generation of the metal. In addition, the hardness and corrosion resistance of all the sintered samples were evaluated, related to the overall and open porosities. As a result, an optimal composition of Ti-40 wt.% TiH{sub 2} was defined, as its maximum open porosity was about 23%.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Phosphate glass matrix composites incorporating trisilanol phenyl polyhedral oligomeric silsesquioxane prepared by viscous flow sintering method with enhanced benefits

The effect of mixing and sintering processes to prepare tin fluorophosphate glass (Pglass) matrix composites incorporating trisilanol phenyl polyhedral oligomeric silsesquioxane (TSP-POSS) was investigated by comparing manual and suspension mixing, one-step and stepwise sintering processes to explore the structure dynamics and physical properties in the composites as a function of the different process conditions used. Energy Dispersive X-ray analysis confirmed optimal homogeneous dispersion of the TSP-POSS molecules in the composites prepared by the suspension method. The observed increase of glass transition temperature and the reduction of non-bridging bonds in the composites are believed to be the reason for the effective dispersion of TSP-POSS molecules in the composites. The chemical reaction between the TSP-POSS and Pglass was strongly influenced by the mixing/dispersion and sintering processes investigated. 13 C cross polarized magic angle spinning (CP MAS) solid state nuclear magnetic resonance (NMR) spectroscopy confirmed the chemical stability of the TSP-POSS during the sintering process at elevated temperatures. In addition, a chemical reaction between the TSP-POSS and Pglass was evidenced by 29 Si CP MAS NMR analysis. Here, this study will provide a better fundamental understanding of the effective dispersion mechanism of the TSP-POSS molecules in the Pglass matrix that will facilitate tailoring the physicochemical properties of the composites with addition of various small concentrations of TSP-POSS for a number of applications where the pure Pglass is not applicable due to the intrinsic properties of the Pglass.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Evaluation of sintering effects on SiC incorporated UO2 kernels under Ar and Ar-4%H2 environments

Silicon carbide (SiC) is suggested as an oxygen getter in UO2 kernels used for TRISO particle fuels to lower oxygen potential and prevent kernel migration during irradiation. Scanning electron microscopy and X-ray diffractometry analyses performed on sintered kernels verified that internal gelation process can be used to incorporate SiC in urania fuel kernels. Sintering in either Ar or Ar-4%H2 at 1500 C lowered the SiC content in the UO2 kernels to some extent. Formation of UC was observed as the major chemical phase in the process, while other minor phases such as U3Si2C2, USi2, U3Si2, and UC2 were also identified. UC formation was presumed to be occurred by two reactions. The first was the SiC reaction with its protective SiO2 oxide layer on SiC grains to produce volatile SiO and free carbon that subsequently reacted with UO2 to form UC. The second process was direct UO2 reaction with SiC grains to form SiO, CO, and UC, especially in Ar-4%H2. A slightly higher density and UC content was observed in the sample sintered in Ar-4%H2, but the use of both atmospheres produced kernels with ~95% of theoretical density. It is suggested that incorporating CO in the sintering gas would prevent UC formation and preserve the initial SiC content.

Silicon carbide uranium oxide↗

DOE OSTI2020

U 3 Si 2 and UO 2 composites densified by spark plasma sintering for accident-tolerant fuels

This work reports the synthesis and characterization of the U 3 Si 2 and UO 2 composites sintered by spark plasma sintering (SPS) with controlled microstructures for accident-tolerant fuel application. The U 3 Si 2 and UO 2 composites with different silicide and oxide ratios were synthesized by SPS at temperatures from 1000 to 1300 °C for 5 minutes. The microstructure and phase composition of the SPS densified composite fuels were characterized with scanning electron microscopy, X-ray diffraction (XRD), and energy dispersed spectroscopy (EDS). A systematic study of the thermal and mechanical properties was conducted using microhardness testing and laser flash apparatus, along with oxidation resistance measurements using thermogravimetric analysis (TGA). The results show that the synthesis of composite fuels can be achieved with a 90% theoretical density (TD) at 1000 °C and over 95% TD when sintered at 1300 °C. XRD and EDS results confirmed that the dominant phases in the composites are U 3 Si 2 and UO 2 . Improved physical density generally leads to improved hardness, fracture toughness, thermal diffusivity, and onset temperature during the oxidation process. U 3 Si 2 was found to play a dominant role in determining the mechanical and oxidation properties of the composite fuels, whereas UO 2 had a more important impact on controlling the thermal diffusivity of the composites. The composite with 50 wt% UO 2 sintered at 1300 °C displayed the onset oxidation temperature of 500 °C by dynamic oxidation testing using TGA at a ramp degree of 10 °C/min. The composite also achieved a high fracture toughness of ~3.5 MPa m ½ . Finally, these results highlight the potential of composite fuel forms densified by SPS with simultaneously enhanced fissile element density, fracture toughness, thermal transport properties, and oxidation resistance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2015

Microstructure and mechanical properties of NiCoCrAlYTa alloy processed by press and sintering route

Nickel-based superalloys such as NiCoCrAlY are widely used in high-temperature applications, such as gas turbine components in the energy and aerospace industries, due to their strength, high elastic modulus, and high-temperature oxidation resistance. However, the processing of these alloys is complex and costly, and the alloys are currently used as a bond coat in thermal barrier coatings. In this work, the effect of cold press and sintering processing parameters on the microstructure and mechanical properties of NiCoCrAlY alloy were studied using the powder metallurgy route as a new way to obtain NiCoCrAlYTa samples from a gas atomized prealloyed powder feedstock. High mechanical strength and adequate densification up to 98% were achieved. The most suitable compaction pressure and sintering temperature were determined for NiCoCrAlYTa alloy through microstructure characterization. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and energy dispersive spectroscopy microanalysis (EDS) were performed to confirm the expected γ-Ni matrix and β-NiAl phase distribution. Additionally, the results demonstrated the unexpected presence of carbides and Ni–Y-rich zones in the microstructure due to the powder metallurgy processing parameters used. Thus, microhardness, nanoindentation and uniaxial compression tests were conducted to correlate the microstructure of the alloy samples with their mechanical properties under the different studied conditions. The results show that the compaction pressure did not significantly affect the mechanical properties of the alloy samples. In this work, the compaction pressures of 400, 700 and 1000 MPa were used. The sintering temperature of 1200 °C for NiCoCrAlYTa alloy was preferred; above this temperature, the improvement in mechanical properties is not significant due to grain coarsening, whereas a lower temperature produces a decrease in mechanical properties due to high porosity and poor solid-state diffusion. - Graphical abstract: Display Omitted - Highlights: • We made NiCoCrAlYTa alloy by a conventional powder metallurgy route. • High densification and adequate strength were observed. • The presence of unexpected carbides found along γ/γ and γ/β grain boundaries was detected. • The effect of cold press and sintering processing parameters on the microstructure and mechanical properties were studied.

36 MATERIALS SCIENCE↗