Results for “MATERIALS, SINTERED” — Page 21

DOE OSTI2023

Shrinkage, microstructure, and mechanical properties of sintered 3D-printed silica via stereolithography

Stereolithography has been used to create ceramic parts with complex geometry that is difficult to achieve with conventional fabrication techniques. Here this study used stereolithography to print silica honeycomb structures with a commercial Formlabs Form2 printer. The printed samples were sintered at different temperatures, and the print shape was retained up to 1300°C, but significant distortion from partial melting occurred at 1400°C. Higher sintering temperatures lead to more shrinkage, but it is non-uniform among directions, with the open cell plane shrinking more than the dense plane of the sample. As expected, the density of samples also increases with the sintering temperature. At higher sintering temperatures, there is an increase in cristobalite and a decrease in quartz, tridymite, and amorphous silica. Regarding mechanical properties, the out-of-plane compressive strength is approximately one order of magnitude higher than the in-plane compressive strength. When compressed along the out-of-plane direction, the samples sintered at lower temperatures surprisingly exhibit higher strength, which is explained by the micro-cracking mechanism. As expected, the samples sintered at higher temperatures display higher strength when compressed along the in-plane direction.

36 MATERIALS SCIENCE↗

NASA NTRS2018

Development of New Rocket Engine Liner Materials Based on Copper Alloys with Diamond Particle Additions

Novel copper-diamond materials containing particulate dispersions of diamond within a copper alloy matrix have been produced as next-generation rocket engine combustion chamber liner materials. These Copper-Diamond (Cu-D) composite materials have significantly higher thermal conductivity than conventional liner materials and have the potential to increase the engine performance significantly. Liner fabrication techniques include hot pressing and spark plasma sintering (SPS), which are capable of scale up to full-size production parts. The materials have been evaluated for thermal cycling resistance and ease of manufacturing. The results indicate great promise of these materials and associated economics to replace state-of-the-art combustion chamber liner materials such as GRCop-84 and NARloy-Z. Combustion chamber fabrication processes are also discussed, including SPS and additive manufacturing.

Bhat, Biliyar N.↗

DOE OSTI2022

Bonded Interfaces for High-Temperature Power Electronics

Wide-bandgap devices have pushed the operational limit of semiconductor devices in automotive power electronics packages to higher temperatures (>200 degrees C). While a higher efficiency can be achieved through the use of wide-bandgap devices, the entire package must be re-designed with components that can withstand the higher temperature limits. Sintered silver and transient liquid phase bonds are potential candidates as bonded materials for use in higher temperatures however, the underlying mechanics of deformation under thermal loads and the resulting failure mechanisms in these materials are not well understood. Furthermore, thermomechanical modeling plays a key role in understanding the degradation behavior of bonded interface materials and for design optimization of power electronics packages.

ADVANCED PROPULSION SYSTEMS,DIRECT ENERGY CONVERSI↗

DOE OSTI2021

Compositions and methods for thermoelectric ceramics

In one aspect, the disclosure relates to thermoelectric ceramic oxide compositions comprising a CaMnO 3 ceramic. In a further aspect, the disclosed thermoelectric ceramic oxide compositions can dramatically increase the energy conversion efficiency of thermoelectric through a combination of modifying the chemistry of precursor materials, and simultaneously introducing a metal oxide liquid phase during sintering. In a further aspect, the present disclosure pertains to thermoelectric ceramic oxide compositions comprising a metal doped CaMnO 3 having with a metal oxide grain boundary phase; wherein the metal is selected from group 13, group 14, group 15, group 16, or a rare earth element. In a still further aspect, the disclosure relates to methods for making the thermoelectric ceramic oxide materials. This abstract is intended as a scanning tool for purposes of searching in the particular art and is not intended to be limiting of the present disclosure.

Song, Xueyan↗

NASA NTRS2020

Effect of Material Porosity on Residual Stress in an Additive Manufacturing Simulation using the Generalized Method of Cells

The effect of material porosity on final part distortion and residual stresses in a selective laser sintering manufacturing simulation is presented here. A time-dependent thermo-mechanical model is used with the open-source FEA software CalculiX. Effective homogenized material properties for Inconel 625 are precomputed using NASA’s Micromechanics Analysis Code with the Generalized Method of Cells. The evolving porosity of the material is estimated with each pass of the laser beam during simulation runtime. A comparison with a homogenous model and the evolving model shows that the model with evolving porosity predicts larger distortions with greater residual stresses.

Additive Manufactuirng↗

DOE OSTI2024

Tuning the spontaneous exchange bias effect in La 1.5 Sr 0.5 CoMnO 6 with sintering temperature

Here, in this study, we present a study of the influence of microstructure on the magnetic properties of polycrystalline samples of the La 1.5 Sr 0.5 CoMnO 6 double perovskite, with primary attention to the spontaneous exchange bias effect, a fascinating recently discovered phenomena for which some materials exhibit unidirectional magnetic anisotropy after being cooled in zero magnetic fields. By sintering La 1.5 Sr 0.5 CoMnO 6 at different temperatures, we obtained samples with distinct average grain sizes, ranging from 1.54-6.65 μm. A detailed investigation of the material's structural, morphologic, electronic, and magnetic properties using x-ray powder diffraction, powder neutron diffraction, x-ray absorption near edge structure spectroscopy, scanning electron microscopy, and ac and dc magnetometry has revealed a systematic enhancement of the exchange bias effect with increasing the average grain size. This evolution is discussed in terms of changes in the material's porosity and grain morphology and its influence on the exchange couplings at the magnetic interfaces.

14 SOLAR ENERGY↗

DOE OSTI2025

Additive manufacturing of mullite ceramic by digital light processing

Mullite material was successfully additively manufactured using digital light processing (DLP). The printed geometry involves a one-step process of pyrolysis, de-binding, and sintering under a plain atmosphere to achieve an average of 76 % ceramic yield and linear shrinkage of 12 %. Furthermore, the thermal profile was carefully controlled to obtain consistent phases in which the XRD shows a mullite phase. Here, in addition, the Weibull analysis was conducted on the sintered flexural specimens, showing a Weibull modulus (m) of 13.05 with a characteristic strength (σ 0 ) of 94.96 MPa. Synchrotron microtomography was performed on the sintered specimens, which showed two distinct porosity distributions (small and large). Large porosity (non-spherical elongated) is the primary cause of decreased material strength, while small porosity (spherical) is the sintering product. The measured thermal conductivity of the specimens was in the range of 2.7–3.1 W/m∙k and decreased with an increase in temperature. Lastly, large-scale prototypes were printed concurrently with a fine resolution of 25 μm without any compromise on the predetermined design and structure.

Additive manufacturing↗

NASA NTRS2004

Processing Techniques Developed to Fabricate Lanthanum Titanate Piezoceramic Material for High-Temperature Smart Structures

Piezoelectric ceramic materials are potential candidates for use as actuators and sensors in intelligent gas turbine engines. For piezoceramics to be applied in gas turbine engines, they will have to be able to function in temperatures ranging from 1000 to 2500 F. However, the maximum use temperature for state-of-the-art piezoceramic materials is on the order of 300 to 400 F. Research activities have been initiated to develop high-temperature piezoceramic materials for gas turbine engine applications. Lanthanum titanate has been shown to have high-temperature piezoelectric properties with Curie temperatures of T(sub c) = 1500 C and use temperatures greater than 1000 C. However, the fabrication of lanthanum titanate poses serious challenges because of the very high sintering temperatures required for densification. Two different techniques have been developed at the NASA Glenn Research Center to fabricate dense lanthanum titanate piezoceramic material. In one approach, lower sintering temperatures were achieved by adding yttrium oxide to commercially available lanthanum titanate powder. Addition of only 0.1 mol% yttrium oxide lowered the sintering temperature by as much as 300 C, to just 1100 C, and dense lanthanum titanate was produced by pressure-assisted sintering. The second approach utilized the same commercially available powders but used an innovative sintering approach called differential sintering, which did not require any additive.

Goldsby, Jon C.↗

DOE OSTI2023

Sensitivity of UO 2 fuel performance to microstructural evolutions driven by dilute additives

Use of dilute additives to nuclear fuel is being considered to increase the security of commercial fuel management through traceability of fabricated fuel elements. Taggants, as additives are denoted when included for traceability purposes, may also improve fuel performance, as demonstrated in Cr-containing uranium dioxide as described in the literature, and they may also improve fuel safety. In fact, studies have shown that some additives affect fuel material properties such as grain size and density after sintering. Given the possible range of elements that could be used as additives, the impact of such fuel property variations on the fuel’s thermomechanical behavior becomes relevant. These effects can be evaluated through a sensitivity study of standard fuel models to analyze changes in these properties using a fuel performance code. In this work, the BISON code is being used to investigate these effects through a 2D axisymmetric model of smeared UO 2 fuel pellets and ZIRLO® cladding under realistic pressurized water reactor core irradiation conditions. Here, randomly sampled densities and grain sizes within specified ranges are used as input parameters in the simulations, and several fuel model-related outputs are evaluated. The thermomechanical response of the cladding is also addressed in this study. The simultaneous variation of both input parameters offers a more comprehensive path to identify key sensitivities. Outputs explored include temperature, fission gas release, creep, and radial stress. Results show that although most of these outputs are sensitive to grain size to a certain extent, density mainly affects fuel temperature and elastic strain. Furthermore, sensitivities can vary depending on the radial position within the fuel pellet.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1992

Development of high T(sub c) (greater than 110 K) Bi, Tl, and Y-based materials as superconducting circuit elements

Experimental work has continued on the development and characterization of bulk and hot pressed powders and tapecast materials in the Bi-Sr-Ca-Cu-O and Tl-Ba-Ca-Cu-O systems. A process for producing warp-free, sintered, superconducting tapes of Bi composition Bi2Sr2Ca2Cu3O(x) with a mixed oxide process was established. This procedure required a triple calcination at 830 C for 24 hours and sintering at 845 C from 20 to 200 hours. Hot pressing the triple calcined powder at 845 C for 6 hours at 5000 psi yielded a dense material which on further heat treatment at 845 C for 24 hours exhibited a Tc of 108.2 K. A further improvement in the processing of the bismuth materials was achieved via a chemical coprecipitation process wherein the starting nitrate materials were coprecipitated with oxalic acid, thus yielding a more chemically homogeneous, more reactive powder. With the coprecipitated powders, only one calcine at 830 C for 12 hours and a final sinter at 845 C for 30 hours was sufficient to produce a bulk superconducting material with a Tc of 108.4 K. SAFIRE-type grounding links were successfully fabricated from sintered, tapecast, coprecipitated BSCCO 2223 powders. Compositional and processing investigations were continued on the Tl-based superconductors. Manganese and lithium additions and sintering temperature and time were examined to determine their influence on superconducting properties. It was found that lithium substitutions for copper enhance the transition temperatures while manganese additions produced deleterious effects on the superconducting properties. A suitable procedure for producing reproducible bulk and tapecast material of Tl composition Tl2Ba2Ca2Cu3O(x) was developed and used in fabricating uniform superconducting tapes. The highest transition temperature for Tl-based tapes was measured at 110.2 K. Thallium superconducting SAFIRE-type grounding links were fabricated from the tapes.

Haertling, Gene H.↗

NASA NTRS2014

Sintering Characteristics of Multilayered Thermal Barrier Coatings Under Thermal Gradient and Isothermal High Temperature Annealing Conditions

Pyrochlore oxides have most of the relevant attributes for use as next generation thermal barrier coatings such as phase stability, low sintering kinetics and low thermal conductivity. One of the issues with the pyrochlore oxides is their lower toughness and therefore higher erosion rate compared to the current state-of-the-art TBC material, yttria (6 to 8 wt%) stabilized zirconia (YSZ). In this work, sintering characteristics were investigated for novel multilayered coating consisted of alternating layers of pyrochlore oxide viz Gd2Zr2O7 and t' low k (rare earth oxide doped YSZ). Thermal gradient and isothermal high temperature (1316 C) annealing conditions were used to investigate sintering and cracking in these coatings. The results are then compared with that of relevant monolayered coatings and a baseline YSZ coating.

Thermal Barrier Coatings↗

NASA NTRSDate not supplied

Vacuum Sintering of Highland Simulant CSM-LHT-1G

Sintering of lunar regolith is a process of interest to consolidate the ubiquitous granular material in durable structures on the lunar surface such as platforms, landing/launch pads, roads, and foundations for long-term robotic and human activities. Many publications do not report quantitative assessment of the effects of processing conditions on the strength properties of the sintered products. The work presented is an investigation into such effects on a carefully selected simulant, CSM-LHT-1G prepared for high temperature processing to eliminate undesired components that would not be present from lunar materials. Careful experiments under vacuum were conducted to identify the relevant factors that dominate the properties and the quality of the sintered product. CSM-LHT-1G simulant is a variant of the CSM-LHT-1 lunar highland simulant produced by Colorado School of Mines. The original mineralogical composition of CSM-LHT-1 (70 wt.% Greenspar, 30 wt.% Merriam Crater basalt) was modified to obtain a 30 wt.% glass content with the addition of NU-LHT-5M glass balanced with pyroxene (augite) to yield CSM-LHT-1G.

Vacuum Sintering↗

DOE OSTI2021

Self-regeneration of supported transition metals by a high entropy-driven principle

The sintering of Supported Transition Metal Catalysts (STMCs) is a core issue during high temperature catalysis. Perovskite oxides as host matrix for STMCs are proven to be sintering-resistance, leading to a family of self-regenerative materials. However, none other design principles for self-regenerative catalysts were put forward since 2002, which cannot satisfy diverse catalytic processes. Herein, inspired by the principle of high entropy-stabilized structure, a concept whether entropy driving force could promote the self-regeneration process is proposed. To verify it, a high entropy cubic Zr 0.5 (NiFeCuMnCo) 0.5 O x is constructed as a host model, and interestingly in situ reversible exsolution-dissolution of supported metallic species are observed in multi redox cycles. Notably, in situ exsolved transition metals from high entropy Zr 0.5 (NiFeCuMnCo) 0.5 O x support, whose entropic contribution (TΔS config = T$\star$12.7 J mol -1 K -1 ) is predominant in ΔG, affording ultrahigh thermal stability in long-term CO 2 hydrogenation (400 °C, >500 h). Current theory may inspire more STWCs with excellent sintering-resistance performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2012

Regolith Derived Heat Shield for Planetary Body Entry and Descent System with In Situ Fabrication

This NIAC project investigated an innovative approach to provide heat shield protection to spacecraft after launch and prior to each EDL thus potentially realizing significant launch mass savings. Heat shields fabricated in situ can provide a thermal-protection system for spacecraft that routinely enter a planetary atmosphere. By fabricating the heat shield with space resources from materials available on moons and asteroids, it is possible to avoid launching the heat-shield mass from Earth. Regolith has extremely good insulating properties and the silicates it contains can be used in the fabrication and molding of thermal-protection materials. Such in situ developed heat shields have been suggested before by Lewis. Prior research efforts have shown that regolith properties can be compatible with very-high temperature resistance. Our project team is highly experienced in regolith processing and thermal protection systems (TPS). Routine access to space and return from any planetary surface requires dealing with heat loads experienced by the spacecraft during reentry. Our team addresses some of the key issues with the EDL of human-scale missions through a highly innovative investigation of heat shields that can be fabricated in space by using local resources on asteroids and moons. Most space missions are one-way trips, dedicated to placing an asset in space for economical or scientific gain. However, for human missions, a very-reliable heat-shield system is necessary to protect the crew from the intense heat experienced at very high entry velocities of approximately 11 km/s at approximately Mach 33 (Apollo). For a human mission to Mars, the return problem is even more difficult, with predicted velocities of up to 14 km/s, at approximately Mach 42 at the Earth-atmosphere entry. In addition to human return, it is very likely that future space-travel architecture will include returning cargo to the Earth, either for scientific purposes or for commercial reasons. Platinum, titanium, helium 3, and other metals, elements and minerals are all high-value commodities in limited supply on Earth, and it may be profitable to mine these substances throughout the Solar System and return them to Earth, if an economical method can be found. To date, several private corporations have been launched to pursue these goals. Because the heat shield is the last element to be used in an Earth-return mission, a high penalty is paid in the propellant mass required to carry the heat shield to the destination and back. If the heat shield could be manufactured in space, and then outfitted on the spacecraft prior to the reentry at Earth, then significant propellant and mass savings could be achieved during launch and space operations. Preliminary mission architecture scenarios are described, which explain the potential benefits that may be derived from using an in-situ fabricated regolith heat shield. In order to prove that this is a feasible technology concept, this project successfully fabricated heat shield materials from mineral simulant materials of lunar and Martian regolith by two methods: 1) Sintering and 2) Binding the simulant with a "room-temperature vulcanizing" (RTV) silicone formulated to withstand high temperatures. Initially a third type of fabrication was planned using the hot waste stream from regolith ISRU processes. This fabrication method was discarded since the resulting samples would be too dense and brittle for heat shields. High temperature flame tests at KSC and subsequent arc jet tests at Ames Research Center (ARC) have proved promising. These coupon tests show favorable materials properties and have the potential to be a new way of fabricating heat shields for space entry into planetary atmospheres.

Hogue, Michael D.↗

NASA NTRS2013

Regolith Derived Heat Shield for Planetary Body Entry and Descent System with In Situ Fabrication

This NIAC project investigated an innovative approach to provide heat shield protection to spacecraft after launch and prior to each EDL thus potentially realizing significant launch mass savings. Heat shields fabricated in situ can provide a thermal-protection system for spacecraft that routinely enter a planetary atmosphere. By fabricating the heat shield with space resources from materials available on moons and asteroids, it is possible to avoid launching the heat-shield mass from Earth. Regolith has extremely good insulating properties and the silicates it contains can be used in the fabrication and molding of thermal-protection materials. Such in situ developed heat shields have been suggested before by Lewis. Prior research efforts have shown that regolith properties can be compatible with very-high temperature resistance. Our project team is highly experienced in regolith processing and thermal protection systems (TPS). Routine access to space and return from any planetary surface requires dealing with heat loads experienced by the spacecraft during reentry. Our team addresses some of the key issues with the EDL of human-scale missions through a highly innovative investigation of heat shields that can be fabricated in space by using local resources on asteroids and moons. Most space missions are one-way trips, dedicated to placing an asset in space for economical or scientific gain. However, for human missions, a very-reliable heat-shield system is necessary to protect the crew from the intense heat experienced at very high entry velocities of approximately 11 km/s at approximately Mach 33 (Apollo). For a human mission to Mars, the return problem is even more difficult, with predicted velocities of up to 14 km/s, at approximately Mach 42 at the Earth-atmosphere entry. In addition to human return, it is very likely that future space-travel architecture will include returning cargo to the Earth, either for scientific purposes or for commercial reasons. Platinum, titanium, helium 3, and other metals, elements and minerals are all high-value commodities in limited supply on Earth, and it may be profitable to mine these substances throughout the Solar System and return them to Earth, if an economical method can be found. To date, several private corporations have been launched to pursue these goals. Because the heat shield is the last element to be used in an Earth-return mission, a high penalty is paid in the propellant mass required to carry the heat shield to the destination and back. If the heat shield could be manufactured in space, and then outfitted on the spacecraft prior to the reentry at Earth, then significant propellant and mass savings could be achieved during launch and space operations. Preliminary mission architecture scenarios are described, which explain the potential benefits that may be derived from using an in-situ fabricated regolith heat shield. In order to prove that this is a feasible technology concept, this project successfully fabricated heat shield materials from mineral simulant materials of lunar and Martian regolith by two methods: 1) Sintering and 2) Binding the simulant with a "room-temperature vulcanizing" (RTV) silicone formulated to withstand high temperatures. Initially a third type of fabrication was planned using the hot waste stream from regolith ISRU processes. This fabrication method was discarded since the resulting samples would be too dense and brittle for heat shields. High temperature flame tests at KSC and subsequent arc jet tests at Ames Research Center (ARC) have proved promising. These coupon tests show favorable materials properties and have the potential to be a new way of fabricating heat shields for space entry into planetary atmospheres.

Hogue, Michael D.↗

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 OSTI2020

Solid-State Sintering of Core-Shell Ceramic Powders Fabricated by Particle Atomic Layer Deposition

The properties of technical ceramics are highly dependent on their microstructure, which evolves during sintering. Sintering is the process by which ceramic parts are subjected to high temperatures to activate chemical diffusion and the consumption of porosity. During the initial stage of sintering, interparticle necks between neighboring particles form and subsequently increase in size, consuming porosity as the particle centers move closer together. To experimentally determine how this process depends on particle surface composition, particle atomic layer deposition (ALD) was used to deposit a thin film of amorphous aluminum oxide (Al2O3) onto yttria-stabilized tetragonal zirconia (3YSZ) particles, producing core-shell structured powders. The uniformity of the Al2O3 film was confirmed with transmission electron microscopy and energy dispersive spectroscopy. Scanning electron microscopy was used to observe microstructural evolution during sintering, and the dihedral angles of Al2O3 and 3YSZ grains were measured to determine the ratio of interfacial energies between the 3YSZ|3YSZ, 3YSZ|Al2O3, and Al2O3|Al2O3 interfaces. Analysis of the densification kinetics revealed that the initial stage of densification is dependent on the material at the surface of the particles (ie, the Al2O3 film) and is controlled by the diffusion of Al3+ cations through Al2O3. Once the Al2O3 film has coalesced, the sintering behavior is controlled by the densification of the core material (3YSZ). Thus, core-shell powders fabricated by particle ALD sinter by a two-step process where the kinetics are dependent on the material present at interparticle contacts.

alumina↗

DOE OSTI2020

Novel High Temperature Carbide and Boride Ceramics for Direct Power Extraction Electrode Applications. Final report

The current project aims to develop new carbide and boride ceramic materials that incorporate different metal elements (e.g., (Hf 1-x Zr x )B 2 , also called ceramic solid solutions) and understand the fundamental composition-processing-structure-property relationships for such materials. Specifically, nano powders and related nano-composites for selected mixed metal carbide and boride materials are synthesized from nano-scale mixed precursors obtained from solution-based processing via heat treatment in inert atmosphere. The obtained fine powders were then consolidated into dense ceramics via a novel flash sintering process. The mechanical properties and thermal oxidation resistance for the obtained materials were evaluated for these materials. It was found that different synthesis routes produced powders with somewhat different characteristics in terms of composition and microstructure, which then led to different properties for the final ceramics. The synthesis and processing methods demonstrated in this study might be adopted for developing other similar high temperature ceramics, while the mixed metal or solid solution ceramic materials obtained from this study might be used as hot electrodes for direction power extraction and other energy-related applications.

20 FOSSIL-FUELED POWER PLANTS↗