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At least 163 records · Page 9

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DOE OSTI2022

Selective Laser Sintering of High-Temperature Thermoset Polymer

Thermoplastic materials such as PA12 and PA6 have been extensively employed in Selective Laser Sintering (SLS) 3D printing applications due to their printability, processability, and crystalline structure. However, thermoplastic-based materials lack polymer inter-chain bonding, resulting in inferior mechanical and thermal properties and relatively low fatigue behavior. Therefore, 3D printing of high-performance crosslinked thermosets using SLS technology is paramount to pursue as an alternative to thermoplastics. In this work, a thermoset resin was successfully 3D printed using SLS, and its thermal stability of printed parts after a multi-step post-curing process was investigated. Dimensionally stable and high glass transition temperature (Tg: ~300 °C) thermoset parts were fabricated using SLS. The polymer crosslinking mechanism during the printing and curing process was investigated through FTIR spectra, while the mechanical stability of the SLS 3D-printed thermoset was characterized through compression tests. It is found that 100% crosslinked thermoset can be 3D printed with 900% higher compressive strength than printed green parts.

Hassan, Md Sahid (ORCID:0000000304665395)↗

NASA NTRS1988

Effect of high-temperature hydrogen exposure on sintered alpha-SiC

Sintered alpha-silicon carbide was exposed to pure, dry hydrogen at high temperatures for times up to 500 hr. Weight loss and corrosion were seen after 50 hr at temperatures as low as 1000 C. Corrosion of SiC by hydrogen produced grain boundary deterioration at 1100 C and a mixture of grain and grain boundary deterioration at 1300 C. Statistically significant strength reductions were seen in samples exposed to hydrogen for times greater than 50 hr and temperatures above 1100 C. Critical fracture origins were identified by fractography as either general grain boundary corrosion at 1100 C or as corrosion pits at 1300 C. A maximum strength decrease of approximately 33 percent was seen at 1100 and 1300 C after 500 hr exposure to hydrogen. A computer assisted thermodynamic program was also used to predict possible reaction species of SiC and hydrogen.

Hallum, Gary W.↗

DOE OSTI2024

Thermomechanical Degradation of Sintered Copper Under High-Temperature Thermal Shock

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

ADVANCED PROPULSION SYSTEMS,INORGANIC, ORGANIC, PH↗

DOE OSTI2022

Reliability and Lifetime Prediction Model of Sintered Silver Under High-Temperature Cycling

Although excellent reliability has been reported for sintered silver as a die-attach material under both thermal and power cycling loads in power electronics applications, the promise of this material as a large-area attachment at temperatures beyond 200 degrees C needs to be investigated. This paper presents insights into the thermomechanical behavior and reliability of sintered silver under extreme thermal cycling conditions. In this study, we bonded sintered silver samples and subjected it to a thermal cycling profile of -40 °C to 200 °C with high ramp rates. We periodically monitored samples under thermal cycling to detect the presence of any failure mechanisms using a scanning acoustic microscope. We also included 95Pb5Sn solder in the study to obtain reference data. Results show the occurrence of cracks in sintered silver followed by a rapid rate of crack growth that exceeded the failure criterion in just 50 cycles. The predominant failure mechanism we observed was adhesive failure. As a large-area attachment, solder exhibited a higher reliability than sintered silver but failed within 100 cycles. Finally, we performed thermomechanical modeling to compute strain energy density values and correlated these with the experimentally observed crack growth rates to formulate a lifetime prediction model for sintered silver.

30 DIRECT ENERGY CONVERSION↗

NASA NTRS1992

Making High-Temperature Superconductors By Melt Sintering

Melt-sintering technique applied to YBa2Cu3O7-x system and to Bi/Ca/Sr/Cu-oxide system to produce highly oriented bulk high-temperature-superconductor materials extending to macroscopically usable dimensions. Processing requires relatively inexpensive and simple equipment. Because critical current two orders of magnitude greater in crystal ab plane than in crystal c direction, high degree of orientation greatly enhances critical current in these bulk materials, making them more suitable for many proposed applications.

Golben, John P.↗

NASA NTRS1992

Tribological and mechanical comparison of sintered and hipped PM212: High temperature self-lubricating composites

Selected tribological, mechanical and thermophysical properties of two versions of PM212 (sintered and hot isostatically pressed, HIPped) are compared. PM212, a high temperature self-lubricating composite, contains 70 wt percent metal bonded chromium carbide, 15 wt percent CaF2/BaF2 eutectic and 15 wt percent silver. PM212 in the sintered form is about 80 percent dense and has previously been shown to have good tribological properties from room temperature to 850 C. Tribological results of a fully densified, HIPped version of PM212 are given. They are compared to sintered PM212. In addition, selected mechanical and thermophysical properties of both types of PM212 are discussed and related to the tribological similarities and differences between the two PM212 composites. In general, both composites display similar friction and wear properties. However, the fully dense PM212 HIPped composite exhibits slight lower friction and wear than sintered PM212. This may be attributed to its generally higher strength properties. The sintered version displays stable wear properties over a wide load range indicating its promise for use in a variety of applications. Based upon their properties, both the sintered and HIPped PM212 have potential as bearing and seal materials for advanced high temperature applications.

Dellacorte, Christopher↗

NASA NTRS1992

Tribological and mechanical comparison of sintered and HIPped PM212 - High temperature self-lubricating composites

Dellacorte, Christopher↗

DOE OSTI2024

Bayesian Optimization of Low-Temperature Nonthermal Plasma Jet Sintering of Nanoinks

Not provided.

Materials Science↗

DOE OSTI2025

Development of direct ink write radially graded alumina/zirconia

Functionally graded materials (FGMs) are of interest in multiple fields, yet many materials combinations are limited by coefficient of thermal expansion (CTE) mismatch. Here, a radially graded alumina/yttria-doped zirconia (Al 2 O 3 /8YZ) FGM is used to demonstrate processing strategies to mitigate CTE and sintering behavior differences between these oxides. FGM materials are especially sensitive to ink stability during printing, as all components (in this case, Al 2 O 3 and 8YZ) must be stabilized in the same dispersant or additive solution. Thus, this system is also ideal to demonstrate ink optimization best practices. Materials were characterized throughout processing to correlate the effects of common additives on both the ceramic particle suspensions and final sintered components. Aggregation observed in the initial additive-containing suspensions were present in the sintered component. The differences in sintering onset temperature and shrinkage rate resulted in internal stresses within the sintered component, which ultimately caused mechanical failure of the component under low stress. In conclusion, a processing strategy was recommended to mitigate the sintering behavior mismatch of alumina and 8 wt% yttria-stabilized zirconia.

Lamm, Benjamin W. [Oak Ridge National Laboratory (↗

NASA NTRS2002

New High-Performance SiC Fiber Developed for Ceramic Composites

Sylramic-iBN fiber is a new type of small-diameter (10-mm) SiC fiber that was developed at the NASA Glenn Research Center and was recently given an R&D 100 Award for 2001. It is produced by subjecting commercially available Sylramic (Dow Corning, Midland, MI) SiC fibers, fabrics, or preforms to a specially designed high-temperature treatment in a controlled nitrogen environment for a specific time. It can be used in a variety of applications, but it currently has the greatest advantage as a reinforcement for SiC/SiC ceramic composites that are targeted for long-term structural applications at temperatures higher than the capability of metallic superalloys. The commercial Sylramic SiC fiber, which is the precursor for the Sylramic-iBN fiber, is produced by Dow Corning, Midland, Michigan. It is derived from polymers at low temperatures and then pyrolyzed and sintered at high temperatures using boron-containing sintering aids (ref. 1). The sintering process results in very strong fibers (>3 GPa) that are dense, oxygen-free, and nearly stoichiometric. They also display an optimum grain size that is beneficial for high tensile strength, good creep resistance, and good thermal conductivity (ref. 2). The NASA-developed treatment allows the excess boron in the bulk to diffuse to the fiber surface where it reacts with nitrogen to form an in situ boron nitride (BN) coating on the fiber surface (thus the product name of Sylramic-iBN fiber). The removal of boron from the fiber bulk allows the retention of high tensile strength while significantly improving creep resistance and electrical conductivity, and probably thermal conductivity since the grains are slightly larger and the grain boundaries cleaner (ref. 2). Also, as shown in the graph, these improvements allow the fiber to display the best rupture strength at high temperatures in air for any available SiC fiber. In addition, for CMC applications under oxidizing conditions, the formation of an in situ BN surface layer creates a more environmentally durable fiber surface not only because a more oxidation-resistant BN is formed, but also because this layer provides a physical barrier between contacting fibers with oxidation-prone SiC surface layers (refs. 3 and 4). This year, Glenn demonstrated that the in situ BN treatment can be applied simply to Sylramic fibers located within continuous multifiber tows, within woven fabric pieces, or even assembled into complex product shapes (preforms). SiC/SiC ceramic composite panels have been fabricated from Sylramic-iBN fabric and then tested at Glenn within the Ultra-Efficient Engine Technology Program. The test conditions were selected to simulate those experienced by hot-section components in advanced gas turbine engines. The results from testing at Glenn demonstrate all the benefits expected for the Sylramic-iBN fibers. That is, the composites displayed the best thermostructural performance in comparison to composites reinforced by Sylramic fibers and by all other currently available high-performance SiC fiber types (refs. 3 and 5). For these reasons, the Ultra-Efficient Engine Technology Program has selected the Sylramic-iBN fiber for ongoing efforts aimed at SiC/SiC engine component development.

DiCarlo, James A.↗

DOE OSTI2022

Power Electronics Materials and Bonded Interfaces - Reliability and Lifetime

Wide-bandgap devices have pushed the operational limit of semiconductor devices in automotive power electronics packages to higher temperatures (>200 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. Accelerated experiments conducted at NREL reveal that high-lead solder joints have better reliability than sintered silver under extreme thermal cycling conditions. Furthermore, efforts to develop a crack propagation model for the high-temperature materials are described.

ADVANCED PROPULSION SYSTEMS↗

NASA NTRS1986

High-temperature effect of hydrogen on sintered alpha-silicon carbide

Sintered alpha-silicon carbide was exposed to pure, dry hydrogen at high temperatures for times up to 500 hr. Weight loss and corrosion were seen after 50 hr at temperatures as low as 1000 C. Corrosion of SiC by hydrogen produced grain boundary deterioration at 1100 C and a mixture of grain and grain boundary deterioration at 1300 C. Statistically significant strength reductions were seen in samples exposed to hydrogen for times greater than 50 hr and temperatures above 1100 C. Critical fracture origins were identified by fractography as either general grain boundary corrision at 1100 C or as corrosion pits at 1300 C. A maximum strength decrease of approximately 33 percent was seen at 1100 and 1300 C after 500 hr exposure to hydrogen. A computer assisted thermodynamic program was also used to predict possible reaction species of SiC and hydrogen.

Hallum, G. W.↗

NASA NTRS1991

Phase Transformations In Mullite-Precursor Xerogels

Report describes experimental study of phase transformations occurring in monophasic and diphasic xerogels of overall stoichiometric mullite composition during thermal treatment. Mullite valued as refractory material because of relatively high mechanical strength, excellent resistance to thermal shock, high resistance to creep, low density, low thermal conductivity, and stability at high temperature. Part of continuing effort to develop precursor materials transformed into mullite and sintered at temperatures low enough to avoid degradation of non-mullite reinforcing fibers in manufacture of mullite/fiber composites.

Hyatt, Mark J.↗

DOE OSTI2023

Nonthermal plasma synthesis of silicon carbonitride

Abstract The use of a low‐temperature plasma for the synthesis of amorphous silicon carbonitride (SiCN) nanoparticles enables the realization of sintered bulk samples with high thermal stability. Amorphous SiCN nanoparticles are produced from a mixture of silane, methane, and ammonia utilizing a mid‐pressure, radio‐frequency, continuous flow reactor. Particle characterization shows that the nanoparticles are largely amorphous with some crystalline silicon and silicon carbide domains <10 nm in size. Compositional tuning, controlled by varying the precursor flow rates, coupled with the uniform mixing of elements at the nanoscale, results in samples that resist crystallization even when sintered at temperatures as high as 2000°C. This study suggests that the low‐temperature plasma synthesis of nanoparticles has great potential to produce bulk structural materials for application in harsh environments.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS1984

Strength evaluation test of pressureless-sintered silicon nitride at room temperature

In order to study strength characteristics at room temperature and the strength evaluating method of ceramic materials, the following tests were conducted on pressureless sintered silicon nitride specimens: bending tests, the three tensile tests of rectangular plates, holed plates, and notched plates, and spin tests of centrally holed disks. The relationship between the mean strength of specimens and the effective volume of specimens are examined using Weibull's theory. The effect of surface grinding on the strength of specimens is discussed.

Matsusue, K.↗

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↗

NASA NTRS1953

Effect of Prestraining of Recrystallization Temperature and Mechanical Properties of Commercial, Sintered, Wrought Molybdenum

Given three presumably identical lots of commercial, sintered, wrought molybdenum, the 1-hour recrystallization temperature of one lot remained above 2900 F by limiting the amount of effective restraining to 35 percent or less. Different recrystallization temperatures were obtained in various atmospheres, the highest in argon and the lowest in hydrogen. Metal thus fabricated and then stress-relieved possessed an ultimate tensile strength at room temperature within 10 percent of metal swaged 99 percent and also possessed equivalent ductility. At 1800 F, equivalent strength and ductility was obtained irrespective of the amount of swaging over the range of 10 to 99 percent. The amount of swaging greatly influenced the recrystallized grain size but the difference in grain size is not the major controlling factor which determines whether recrystallized molybdenum is ductile or brittle at room temperature.

MATERIALS, PROPERTIES - TENSILE↗

NASA NTRS1991

FNAS materials processing and characterization

Research on melt-sintered high temperature superconducting materials is presented. The vibrating sample magnetometer has become a useful characterization tool for the study of high temperature superconductors. Important information regarding the superconducting properties of a sample can be obtained without actually making contact with the sample itself. A step toward microgravity processing of high temperature superconductors was taken. In the future, the samples need to be optimized prior to this processing of the sample before the specific effects of the microgravity environment can be isolated. A series of melt-sintered samples show that bulk processing of high temperature superconductors is getting better.

Golben, John P.↗