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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Unconventional Materials Processing Using Spark Plasma Sintering

Spark plasma sintering (SPS) has gained recognition in the last 20 years for its rapid densification of hard-to-sinter conventional and advanced materials, including metals, ceramics, polymers, and composites. Herein, we describe the unconventional usages of the SPS technique developed in the field. The potential of various new modifications in the SPS technique, from pressureless to the integration of a novel gas quenching system to extrusion, has led to SPS’ evolution into a completely new manufacturing tool. The SPS technique’s modifications have broadened its usability from merely a densification tool to the fabrication of complex-shaped components, advanced functional materials, functionally gradient materials, interconnected materials, and porous filter materials for real-life applications. The broader application achieved by modification of the SPS technique can provide an alternative to conventional powder metallurgy methods as a scalable manufacturing process. The future challenges and opportunities in this emerging research field have also been identified and presented.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Methods of forming silicon carbide by spark plasma sintering

A method of forming silicon carbide by spark plasma sintering comprises loading a powder comprising silicon carbide into a die and exposing the powder to a pulsed current to heat the powder at a rate of between about 50.degree. C./min and about 200.degree. C./min to a peak temperature while applying a pressure to the powder. The powder is exposed to the peak temperature for between about 30 seconds and about 5 minutes to form a sintered silicon carbide material and the sintered silicon carbide material is cooled. Related structures and methods are disclosed.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Methods of forming articles including silicon carbide by spark plasma sintering

A method of forming silicon carbide by spark plasma sintering comprises loading a powder comprising silicon carbide into a die and exposing the powder to a pulsed current to heat the powder at a rate of between about 50° C./min and about 200° C./min to a peak temperature while applying a pressure to the powder. The powder is exposed to the peak temperature for between about 30 seconds and about 5 minutes to form a sintered silicon carbide material and the sintered silicon carbide material is cooled. Related structures and methods are disclosed.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Performance and Reliability of Bonded Interfaces for High-Temperature Packaging. Annual Report

Current generation automotive power electronics packages utilize silicon devices and lead-free solder alloys. To meet stringent technical targets for 2020 and beyond (for cost, power density, specific power, efficiency and reliability), wide-bandgap devices are being considered since they offer advantages such as operation at higher frequencies, voltages, and temperatures. Traditional power electronics packages must be redesigned to utilize the full potential of wide-bandgap devices, and the die- and substrate-attach layers are key areas where new material development and validation is required. Present solder alloys do not meet the performance requirements for these new package designs while also meeting cost and hazardous substance restrictions. Sintered silver (Ag) promises to meet the needs for die- and substrate-attach interfaces but synthesis optimization and reliability evaluation must be completed. Sintered Ag material was proposed as an alternative solution in power electronics packages almost 20 years back. However, synthesis pressure requirements up 40 MPa caused a higher complexity in the production process and more stringent flatness specifications for the substrates. Recently, several manufacturers have developed sintered Ag materials that require lower (3-5 MPa) or even no bonding pressures. Degradation mechanisms for these sintered Ag materials are not well known and need to be addressed. We are addressing these aspects to some extent in this project. We are developing generalized (i.e., independent of geometry) stress intensity factor versus cycles-to-failure relations for sintered Ag. Because sintered Ag is a relatively new material for automotive power electronics, the industry currently does not have a good understanding of recommended synthesis parameters or expected reliability under prescribed conditions. It is an important deliverable of this project to transfer findings to industry to eliminate barriers to using sintered Ag as a viable and commercialized die- and substrate-attach material. Only a few manufacturers produce sintered Ag pastes and may consider some processing conditions as proprietary. It is the goal of this project to openly explore and define best practices in order to impact the maximum number of power electronics module manufacturers and suppliers.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2018

The physical chemistry and materials science behind sinter-resistant catalysts

Catalyst sintering, a main cause of the loss of catalytic activity and/or selectivity at high reaction temperatures, is a major concern and grand challenge in the general area of heterogeneous catalysis. Although all heterogeneous catalysts are inevitably subjected to sintering during their operation, the immediate and drastic consequences can be mitigated by carefully engineering the catalytic particles and their interactions with the supports. In this tutorial review, we highlight recent progress in understanding the physical chemistry and materials science involved in sintering, including the discussion of advanced techniques, such as in situ microscopy and spectroscopy, for investigating the sintering process and its rate. We also discuss strategies for the design and rational fabrication of sinter-resistant catalysts. To conclude, we showcase recent success in improving the thermal stability and thus sinter resistance of supported catalytic systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Power Electronics Materials and Bonded Interfaces - Reliability and Lifetime

Advanced packaging technologies are currently being designed and developed by the power electronics industry however, the maximum operating temperature is still limited to 175 degrees Celsius for the silicon carbide devices. Bonded materials such as sintered copper and polymeric materials are potential candidates for high temperature operation, but it is critical to characterize and evaluate its reliability under harsh operating conditions. In this project, we discuss the results of the accelerated experiments conducted on sintered copper and polymeric materials. Additionally, a novel framework to develop the lifetime prediction model of bonded interfaces through employing statistical and machine learning models are described. In this task, scanning acoustic microscope images of bonded interfaces obtained under thermal cycling experiments are used as the data.

ENGINEERING↗
NASA NTRS1989

External artery heat pipe

An improved heat pipe with an external artery. The longitudinal slot in the heat pipe wall which interconnects the heat pipe vapor space with the external artery is completely filled with sintered wick material and the wall of the external artery is also covered with sintered wick material. This added wick structure assures that the external artery will continue to feed liquid to the heat pipe evaporator even if a vapor bubble forms within and would otherwise block the liquid transport function of the external artery.

Gernert, Nelson J.↗
DOE OSTI2016

Cold Sintering Process of Composites: Bridging the Processing Temperature Gap of Ceramic and Polymer Materials

Co-sintering ceramic and thermoplastic polymer composites in a single step with very high volume fractions of ceramics seems unlikely, given the vast differences in the typical sintering temperatures of ceramics versus polymers. These processing limitations are overcome with the introduction of a new sintering approach, namely “cold sintering process” (CSP). CSP utilizes a transient low temperature solvent, such as water or water with dissolved solutes in stoichiometric ratios consistent with the ceramic composition, to control the dissolution and precipitation of ceramics and effect densification between room temperature and ≈200 °C. Under these conditions, thermoplastic polymers and ceramic materials can be jointly formed into dense composites. Three diphasic composite examples are demonstrated to show the overall diversity of composite material design between organic and inorganic oxides, including the microwave dielectric Li 2 MoO 4 –(-C 2 F 4 -) n , electrolyte Li 1.5 Al 0.5 Ge 1.5 (PO 4 ) 3 –(-CH 2 CF 2 -) x [-CF2CF(CF3)-] y, and semiconductor V 2 O 5 –poly(3,4-ethylenedioxythiophene) polystyrene sulfonate composites. Cold sintering is more general and shall have a major impact on the processing of composite materials for many different applications, mechanical, thermal, and electronic, to mention a few possibilities. CSP concepts open up new composite material design and device integration schemes, impacting a wide variety of applications.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The Effect of Porosity and Grain Size on the Phase Composition and Mechanical Properties of Zirconium-Dioxide-Based Ceramic

ZrO{sub 2}(Y) ceramic with embedded particles of a pore-forming agent—ultrahigh molecular weight polyethylene—has been studied. It has been shown that the porosity of samples after sintering changed from 2 to 42 vol % and the grain size changed from 0.5 to 1.55 μm depending on sintering regime. The strength of materials with minimum porosity was 3000 ± 200 MPa, while the strength of materials with maximum porosity was 100 ± 20 MPa, regardless of grain size. It has been shown that the tetragonal to monoclinic martensitic phase transformation related to mechanical stresses takes place in the material without any effect on the macrostrength of the material. Internal microscopic stresses decreasing with an increase in porosity and ceramic grain size are the main factor causing this transformation in a porous material.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Implementation of a spark plasma sintering facility in a hermetic glovebox for compaction of toxic, radiotoxic, and air sensitive materials

Spark plasma sintering (SPS) is a rapidly developing method for densification of powders into compacts. It belongs to the so-called “field assisted sintering techniques” that enable rapid sintering at much lower temperatures than the classical approaches of pressureless sintering of green pellets or hot isostatic pressing. In this paper, we report the successful integration of a SPS device into a hermetic glovebox for the handling of highly radioactive material containing radioisotopes of U, Th, Pu, Np, and Am. The glovebox implantation has been facilitated by the replacement of the hydraulic system to apply pressure with a compact electromechanical unit. The facility has been successfully tested using UO{sub 2} powder. Pellets with 97% of the theoretical density were obtained at 1000 °C for 5 min, significantly lower than the ∼1600 °C for 5-10 h used in conventional pellet sintering.

36 MATERIALS SCIENCE↗
NASA NTRS1985

Iron impurities in Si3N4 processing

The atomic environment of iron impurities is investigated during the processing cycle of reaction-bonding silicon nitride (RBSN). Several analysis techniques are utilized, including X-ray photoelectron spectroscopy (XPS), extended X-ray absorption fine structure (EXAFS), and electron spin resonance (ESR), to examine iron impurities in the starting silicon powder, in sintered silicon compacts, and in RBSN materials. Results indicate that iron impurities in as-received metallurgical grade silicon powder are incorporated in the silicon bulk as a highly distorted FeSi2 compound. No surface iron or iron-based particulate is observed in the starting material. Upon sintering, the iron environment becomes an ordered FeSi2 structure. In the RBNS material, the FeSi2 structure is again distorted, as observed by both EXAFS and ESR.

Bouldin, C. E.↗
DOE OSTI2010

Thermoelectric properties of HPHT sintered In-doped Pb{sub 0.5}Sn{sub 0.5}Te

The thermoelectric properties of Pb{sub 0.5}Sn{sub 0.5}Te doped with In at 1.0, 2.0, and 3.0x10{sup 19}/cm{sup 3} and sintered at a high pressure and high temperature (HPHT) of 4.0 GPa and 800 or 900 {sup o}C, respectively, have been studied. All samples show p-type semiconducting behavior with positive thermopower. We find that HPHT sintering of conventionally synthesized materials improves their thermoelectric properties. The highest power factor is obtained for In doping of 2.0x10{sup 19}/cm{sup 3} with 13.5 {mu}W/cm K{sup 2} at 230 {sup o}C. The corresponding figure of merit is 1.43x10{sup -3}/K. This represents a twofold improvement in thermoelectric figure of merit, compared to the conventionally sintered materials reported in the literature. When exposed to 400 {sup o}C for 10 days, samples sintered at 900 {sup o}C exhibit more stable thermoelectric properties, while the properties of those sintered at 800 {sup o}C deteriorated. These results demonstrate that HPHT sintering is a viable and controllable way of tuning the thermoelectric properties of PbTe-based materials. - Graphical abstract: A twofold improvement in thermoelectric figure of merit (ZT) is achieved for HPHT sintered In-doped Pb{sub 0.5}Sn{sub 0.5}Te, when compared to the conventionally sintered materials of similar composition reported in the literature.

36 MATERIALS SCIENCE↗
NASA NTRS1986

Improved silicon carbide for advanced heat engines

Work performed to develop silicon carbide materials of high strength and to form components of complex shape and high reliability is described. A beta-SiC powder and binder system was adapted to the injection molding process and procedures and process parameters developed capable of providing a sintered silicon carbide material with improved properties. The initial effort has been to characterize the baseline precursor materials (beta silicon carbide powder and boron and carbon sintering aids), develop mixing and injection molding procedures for fabricating test bars, and characterize the properties of the sintered materials. Parallel studies of various mixing, dewaxing, and sintering procedures have been carried out in order to distinguish process routes for improving material properties. A total of 276 MOR bars of the baseline material have been molded, and 122 bars have been fully processed to a sinter density of approximately 95 percent. The material has a mean MOR room temperature strength of 43.31 ksi (299 MPa), a Weibull characteristic strength of 45.8 ksi (315 MPa), and a Weibull modulus of 8.0. Mean values of the MOR strengths at 1000, 1200, and 14000 C are 41.4, 43.2, and 47.2 ksi, respectively. Strength controlling flaws in this material were found to consist of regions of high porosity and were attributed to agglomerates originating in the initial mixing procedures. The mean stress rupture lift at 1400 C of five samples tested at 172 MPa (25 ksi) stress was 62 hours and at 207 MPa (30 ksi) stress was 14 hours. New fluid mixing techniques have been developed which significantly reduce flaw size and improve the strength of the material. Initial MOR tests indicate the strength of the fluid-mixed material exceeds the baseline property by more than 33 percent.

Whalen, T. J.↗
DOE OSTI2017

Performance and Reliability of Bonded Interfaces for High-temperature Packaging: Annual Progress Report

As maximum device temperatures approach 200 °Celsius, continuous operation, sintered silver materials promise to maintain bonds at these high temperatures without excessive degradation rates. A detailed characterization of the thermal performance and reliability of sintered silver materials and processes has been initiated for the next year. Future steps in crack modeling include efforts to simulate crack propagation directly using the extended finite element method (X-FEM), a numerical technique that uses the partition of unity method for modeling discontinuities such as cracks in a system.

30 DIRECT ENERGY CONVERSION↗
NASA NTRS2003

Sintering Behavior of Diboride Based Materials

A brief history of diboride research, an overview of processing, and sintering studies are covered in this viewgraph presentation. UHTCs are a family of ceramic materials, including diborides of Hf and Zr, with extremely high melting temperatures. Spark Plasma Sintering (SPS) is a novel processing technique useful in consolidating difficult materials. The presentation also contains microphotographs of the microstructure of HfB2 and ZrB2 processed in different ways.

Gasch, Matt↗
NASA NTRS1986

Improved silicon carbide for advanced heat engines

The development of silicon carbide materials of high strength was initiated and components of complex shape and high reliability were formed. The approach was to adapt a beta-SiC powder and binder system to the injection molding process and to develop procedures and process parameters capable of providing a sintered silicon carbide material with improved properties. The initial effort was to characterize the baseline precursor materials, develop mixing and injection molding procedures for fabricating test bars, and characterize the properties of the sintered materials. Parallel studies of various mixing, dewaxing, and sintering procedures were performed in order to distinguish process routes for improving material properties. A total of 276 modulus-of-rupture (MOR) bars of the baseline material was molded, and 122 bars were fully processed to a sinter density of approximately 95 percent. Fluid mixing techniques were developed which significantly reduced flaw size and improved the strength of the material. Initial MOR tests indicated that strength of the fluid-mixed material exceeds the baseline property by more than 33 percent. the baseline property by more than 33 percent.

Whalen, Thomas J.↗
NASA NTRS1970

Contact material for pressure-sintering ferrites

Pressure-sintering, in which the unfired laminated ferrite plane is placed between two flat punches and pressed during firing, reduces lateral firing shrinkage to less than one percent. A decrease in thickness of the laminate produces the required volume shrinkage. Phlogopite is the most suitable contact material investigated.

Wentworth, C.↗
DOE OSTI2024

High-pressure high-temperature synthesis and characterization of B 10 C

The boron-rich boron carbide materials have been traditionally synthesized by adding boron powder to B 4 C material and subjecting it to hot pressing sintering for materials composition containing 8.8–20 at. % carbon in boron (composition range of B 10.4 C to B 4 C). Our study explores a synthesis route for B 10 C starting from high-purity boron and carbon and direct conversion under high pressure and high temperature (HPHT) conditions of 2000 °C and 6–8 GPa. Synthesis was verified via x-ray diffraction analysis, showing the conversion of the high-purity boron and carbon powder mixture into a hexagonal B 10 C structure (R-3m space group) with lattice parameters of a = b = 5.6115 Å and c = 12.197 Å. The concentration of boron was measured through x-ray photoelectron spectroscopy, confirming the B 10 C ratio. The measured nanoindentation mean hardness of B 10 C was 40 GPa. Raman spectroscopy of the HPHT synthesized sample shows characteristic vibrational breathing modes of boron icosahedron and an additional intense band at a vibrational frequency of 380 cm –1 . This Raman band, which appears notably weaker in earlier studies and B 4 C samples, is assigned to the linear chain of B–B–B and attributed to the maximal incorporation of boron within the hexagonal structure.

36 MATERIALS SCIENCE↗