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All sourcesNASA NTRSDOE OSTI
NASA NTRS2003

Structural Anomalies Detected in Ceramic Matrix Composites Using Combined Nondestructive Evaluation and Finite Element Analysis (NDE and FEA)

Most reverse engineering approaches involve imaging or digitizing an object and then creating a computerized reconstruction that can be integrated, in three dimensions, into a particular design environment. The rapid prototyping technique builds high-quality physical prototypes directly from computer-aided design files. This fundamental technique for interpreting and interacting with large data sets is being used here via Velocity2 (an integrated image-processing software, ref. 1) using computed tomography (CT) data to produce a prototype three-dimensional test specimen model for analyses. A study at the NASA Glenn Research Center proposes to use these capabilities to conduct a combined nondestructive evaluation (NDE) and finite element analysis (FEA) to screen pretest and posttest structural anomalies in structural components. A tensile specimen made of silicon nitrite (Si3N4) ceramic matrix composite was considered to evaluate structural durability and deformity. Ceramic matrix composites are being sought as candidate materials to replace nickel-base superalloys for turbine engine applications. They have the unique characteristics of being able to withstand higher operating temperatures and harsh combustion environments. In addition, their low densities relative to metals help reduce component mass (ref. 2). Detailed three-dimensional volume rendering of the tensile test specimen was successfully carried out with Velocity2 (ref. 1) using two-dimensional images that were generated via computed tomography. Subsequent, three-dimensional finite element analyses were performed, and the results obtained were compared with those predicted by NDE-based calculations and experimental tests. It was shown that Velocity2 software can be used to render a three-dimensional object from a series of CT scan images with a minimum level of complexity. The analytical results (ref. 3) show that the high-stress regions correlated well with the damage sites identified by the CT scans and the experimental data. Furthermore, modeling of the voids collected via NDE offered an analytical advantage that resulted in more accurate assessments of the material s structural strength. The top figure shows a CT scan image of the specimen test section illustrating various hidden structural entities in the material and an optical image of the test specimen considered in this study. The bottom figure represents the stress response predicted from the finite element analyses (ref .3 ) for a selected CT slice where it clearly illustrates the correspondence of the high stress risers due to voids in the material with those predicted by the NDE. This study is continuing, and efforts are concentrated on improving the modeling capabilities to imitate the structural anomalies as detected.

Abdul-Aziz, Ali↗
NASA NTRS2005

Thermodynamics of Volatile Species in the Silicon-Oxygen-Hydrogen System Studied

The volatilization of silica (SiO2) to silicon hydroxides and oxyhydroxides because of reaction with water vapor is important in a variety of high-temperature corrosion processes. For example, the lifetimes of silicon carbide (SiC) and silicon nitride (Si3N4) - based components in combustion environments are limited by silica volatility. To understand and model this process, it is essential to have accurate thermodynamic data for the formation of volatile silicon hydroxides and oxyhydroxides.

Jacobson, Nathan S.↗
NASA NTRS2007

Array of Bolometers for Submillimeter- Wavelength Operation

A feed-horn-coupled monolithic array of micromesh bolometers is undergoing development for use in a photometric camera. The array is designed for conducting astrophysical observations in a wavelength band centered at 350 m. The bolometers are improved versions of previously developed bolometers comprising metalized Si3N4 micromesh radiation absorbers coupled with neutron- transmutation-doped Ge thermistors. Incident radiation heats the absorbers above a base temperature, changing the electrical resistance of each thermistor. In the present array of improved bolometers (see figure), the thermistors are attached to the micromesh absorbers by indium bump bonds and are addressed by use of lithographed, vapor-deposited electrical leads. This architecture reduces the heat capacity and minimizes the thermal conductivity to 1/20 and 1/300, respectively, of earlier versions of these detectors, with consequent improvement in sensitivity and speed of response. The micromesh bolometers, intended to operate under an optical background set by thermal emission from an ambient-temperature space-borne telescope, are designed such that the random arrival of photons ("photon noise") dominates the noise sources arising from the detector and readout electronics. The micromesh is designed to be a highly thermally and optically efficient absorber with a limiting response time of about 100 s. The absorber and thermistor heat capacity are minimized in order to give rapid speed of response. Due to the minimization of the absorber volume, the dominant source of heat capacity arises from the thermistor.

Bock, James↗
NASA NTRS2010

Microstructural and Mechanical Evaluation of a Cu-Based Active Braze Alloy to Join Silicon Nitride Ceramics

Self-joining of St. Gobain Si3N4 (NT-154) using a ductile Cu-Al-Si-Ti active braze (Cu-ABA) was demonstrated. A reaction zone approx.2.5-3.5 microns thick) developed at the interface after 30 min brazing at 1317 K. The interface was enriched in Ti and Si. The room temperature compressive shear strengths of Si3N4/Si3N4 and Inconel/Inconel joints (the latter created to access baseline data for use with the proposed Si3N4/Inconel joints) were 140+/-49MPa and 207+/-12MPa, respectively. High-temperature shear tests were performed at 1023K and 1073 K, and the strength of the Si3N4/Si3N4 and Inconel/Inconel joints were determined. The joints were metallurgically well-bonded for temperatures above 2/3 of the braze solidus. Scanning and transmission electron microscopy studies revealed a fine grain microstructure in the reaction layer, and large grains in the inner part of the joint with interfaces being crack-free. The observed formation of Ti5Si3 and AlN at the joint interface during brazing is discussed.

Singh, M.↗
NASA NTRS2012

Static Indentation Load Capacity of the Superelastic 60NiTi for Rolling Element Bearings

The nickel-rich, binary nickel-titanium alloys, such as 60NiTi (60Ni-40Ti by wt%), are emerging as viable materials for use in mechanical components like rolling element bearings and gears. 60NiTi is a superelastic material that simultaneously exhibits high hardness and a relatively low elastic modulus (approx.100 GPa). These properties result in the potential to endure extremely high indentation loads such as those encountered in bearings, gears and other mechanical components. In such applications, quantifying the load that results in permanent deformation that can affect component performance and life is important. In this paper, the static load capacity is measured by conducting indentation experiments in which 12.7 mm diameter balls made from the ceramic Si3N4 are pressed into highly polished, hardened 60NiTi flat plates. Hertz stress calculations are used to estimate contact stress. The results show that the 60NiTi surface can withstand an approximately 3400 kN load before significant denting (>0.6 microns deep) occurs. This load capacity is approximately twice that of high performance bearing steels suggesting that the potential exists to make highly resilient bearings and components from such materials.

DellaCorte, Christopher↗
NASA NTRS2013

The Effect of Pre-Stressing on the Static Indentation Load Capacity of the Superelastic 60NiTi

Superelastic nickel-titanium alloys, such as 60NiTi (60Ni-40Ti by wt.%), are under development for use in mechanical components like rolling element bearings and gears. Compared to traditional bearing steels, these intermetallic alloys, when properly heat-treated, are hard but exhibit much lower elastic modulus (approx.100 GPa) and a much broader elastic deformation range (approx.3 percent or more). These material characteristics lead to high indentation static load capacity, which is important for certain applications especially space mechanisms. To ensure the maximum degree of elastic behavior, superelastic materials must be pre-stressed, a process referred to as "training" in shape memory effect (SME) terminology, at loads and stresses beyond expected use conditions. In this paper, static indentation load capacity tests are employed to assess the effects of pre-stressing on elastic response behavior of 60NiTi. The static load capacity is measured by pressing 12.7 mm diameter ceramic Si3N4 balls into highly polished, hardened 60NiTi flat plates that have previously been exposed to varying levels of pre-stress (up to 2.7 GPa) to determine the load that results in shallow but measurable (0.6 m, 25 in. deep) permanent dents. Hertz stress calculations are used to estimate contact stress. Without exposure to pre-stress, the 60NiTi surface can withstand an approximately 3400 kN load before significant denting (>0.4 m deep) occurs. When pre-stressed to 2.7 GPa, a static load of 4900 kN is required to achieve a comparable dent, a 30 percent increase. These results suggest that stressing contact surfaces prior to use enhances the static indentation load capacity of the superelastic 60NiTi. This approach may be adaptable to the engineering and manufacture of highly resilient mechanical components such as rolling element bearings.

DellaCorte, Christopher↗
NASA NTRS2013

Wear and Reactivity Studies of Melt infiltrated Ceramic Matrix Composite

As interest grows in the use of ceramic matrix composites (CMCs) for critical gas turbine engine components, the effects of the CMCs interaction with the adjoining structure needs to be understood. A series of CMC/material couples were wear tested in a custom elevated temperature test rig and tested as diffusion couples, to identify interactions. Specifically, melt infiltrated silicon carbide/silicon carbide (MI SiC/SiC) CMC was tested in combination with a nickel-based super alloy, Waspaloy, a thermal barrier coating, Yttria Stabilized Zirconia (YSZ), and a monolithic ceramic, silicon nitride (Si3N4). To make the tests more representative of actual hardware, the surface of the CMC was kept in the as-received state (not machined) with the full surface features/roughness present. Test results include: scanning electron microscope characterization of the surfaces, micro-structural characterization, and microprobe analysis.

Jarmon, David C.↗
NASA NTRS2014

The Effect of Indenter Ball Radius on the Static Load Capacity of the Superelastic 60NiTi for Rolling Element Bearings

Static load capacity is a critical design parameter for rolling element bearings used in space mechanisms because of the potential for Brinell (surface dent) damage due to shock and vibration loading events during rocket launch. Brinell damage to bearing raceways can lead to torque variations (noise) and reduced bearing life. The growing use of ceramic rolling elements with high stiffness in hybrid bearings exacerbates the situation. A new family of hard yet resilient materials based upon nickel-titanium is emerging to address such bearing challenges. 60NiTi is a superelastic material that simultaneously exhibits high hardness and a relatively low elastic modulus (approx. 100 GPa) and has been shown to endure higher indentation loads than conventional and high performance steel. Indentation load capacity has been reported for relatively large (12.7 mm diameter) ceramic (Si3N4) indenter balls pressed against flat plates of 60NiTi. In order to develop damage load threshold criteria applicable to a wide range of bearing designs and sizes, the effects of indenter ball radius and the accuracy of interpolation of the Hertz contact stress relations for 60NiTi must be ascertained. In this paper, results of indentation tests involving ceramic balls ranging from 6.4 to 12.7 mm in diameter and highly polished 60NiTi flat plates are presented. When the resulting dent depth data for all the indenter ball sizes are normalized using the Hertz equations, the data (dent depth versus stress) are comparable. Thus when designing bearings made from 60NiTi, the Hertz stress relations can be applied with relative confidence over a range of rolling element sizes and internal geometries.

bearings↗
NASA NTRS2014

Behavior of Particle Depots in Molten Silicon During Float-Zone Growth in Strong Static Magnetic Fields

In the photovoltaics industry, the largest market share is represented by solar cells made from multicrystalline silicon, which is grown by directional solidification. During the growth process, the silicon melt is in contact with the silicon nitride coated crucible walls and the furnace atmosphere which contains carbon monoxide. The dissolution of the crucible coating, the carbon bearing gas, and the carbon already present in the feedstock, lead to the precipitation of silicon carbide, and silicon nitride, at later stages of the growth process. The precipitation of Si3N4 and SiC particles of up to several hundred micrometers in diameter leads to severe problems during the wire sawing process for wafering the ingots. Furthermore the growth of the silicon grains can be negatively influenced by the presence of particles, which act as nucleation sources and lead to a grit structure of small grains and are sources for dislocations. If doped with Nitrogen from the dissolved crucible coating, SiC is a semi conductive material, and can act as a shunt, short circuiting parts of the solar cell. For these reasons, the incorporation of such particles needs to be avoided. In this contribution we performed model experiments in which the transport of intentionally added SiC particles and their interaction with the solid-liquid interface during float zone growth of silicon in strong steady magnetic fields was investigated. SiC particles of 7μm and 60μm size are placed in single crystal silicon [100] and [111] rods of 8mm diameter. This is achieved by drilling a hole of 2mm diameter, filling in the particles and closing the hole by melting the surface of the rod until a film of silicon covers the hole. The samples are processed under a vacuum of 1x10(exp -5) mbar or better, to prevent gas inclusions. An oxide layer to suppress Marangoni convection is applied by wet oxidation. Experiments without and with static magnetic field are carried out to investigate the influence of melt convection on the distribution of particles and their incorporation into the crystal. The field strengths applied by a superconducting magnet are 1T, 3T, 4.5T, and 5T. The increase in field strength dampens the melt flow, and so this study provides comparative data to the crystal growth experiment to be carried out onboard the sounding rocket mission TEXUS 51, where purely diffusive growth condition will be achieved under microgravity conditions.

Jauss, T.↗
NASA NTRS2014

Behavior of Particle Depots in Molten Silicon During Float-Zone Growth in Strong Magnetic Fields

Solar cells made from directionally solidified silicon cover 57% of the photovoltaic industry's market [1]. One major issue during directional solidification of silicon is the precipitation of foreign phase particles. These particles, mainly SiC and Si3N4, are precipitated from the dissolved crucible coating, which is made of silicon nitride, and the dissolution of carbon monoxide from the furnace atmosphere. Due to their hardness and size of several hundred micrometers, those particles can lead to severe problems during the wire sawing process for wafering the ingots. Additionally, SiC particles can act as a shunt, short circuiting the solar cell. Even if the particles are too small to disturb the wafering process, they can lead to a grit structure of silicon micro grains and serve as sources for dislocations. All of this lowers the yield of solar cells and reduces the performance of cells and modules. We studied the behaviour of SiC particle depots during float-zone growth under an oxide skin, and strong static magnetic fields. For high field strengths of 3T and above and an oxide layer on the sample surface, convection is sufficiently suppressed to create a diffusive like regime, with strongly dampened convection [2, 3]. To investigate the difference between atomically rough phase boundaries and facetted growth, samples with [100] and [111] orientation were processed.

Jauss, T.↗
NASA NTRS2014

The Effect of Indenter Ball Radius on the Static Load Capacity of the Superelastic 60NiTi for Rolling Element Bearings

Static load capacity is a critical design parameter for rolling element bearings used in space mechanisms because of the potential for Brinell (surface dent) damage due to shock and vibration loading events during rocket launch. Brinell damage to bearing raceways can lead to torque variations (noise) and reduced bearing life. The growing use of ceramic rolling elements with high stiffness in hybrid bearings exacerbates the situation. A new family of hard yet resilient materials based upon nickel-titanium is emerging to address such bearing challenges. 60NiTi is a superelastic material that simultaneously exhibits high hardness and a relatively low elastic modulus (~100GPa) and has been shown to endure higher indentation loads than conventional and high performance steel. Indentation load capacity has been reported for relatively large (12.7mm diameter) ceramic (Si3N4) indenter balls pressed against flat plates of 60NiTi. In order to develop damage load threshold criteria applicable to a wide range of bearing designs and sizes, the effects of indenter ball radius and the accuracy of interpolation of the Hertz contact stress relations for 60NiTi must be ascertained. In this paper, results of indentation tests involving ceramic balls ranging from 6.4 to 12.7mm in diameter and highly polished 60NiTi flat plates are presented. When the resulting dent depth data for all the indenter ball sizes are normalized using the Hertz equations, the data (dent depth vs. stress) are comparable. Thus when designing bearings made from 60NiTi, the Hertz stress relations can be applied with relative confidence over a range of rolling element sizes and internal geometries.

bearings↗
NASA NTRS2014

The Effect of Indenter Ball Radius on the Static Load Capacity of the Superelastic 60NiTi for Rolling Element Bearings

Static load capacity is a critical design parameter for rolling element bearings used in space mechanisms because of the potential for Brinell (surface dent) damage due to shock and vibration loading events during rocket launch. Brinell damage to bearing raceways can lead to torque variations (noise) and reduced bearing life. The growing use of ceramic rolling elements with high stiffness in hybrid bearings exacerbates the situation. A new family of hard yet resilient materials based upon nickel-titanium is emerging to address such bearing challenges. 60NiTi is a superelastic material that simultaneously exhibits high hardness and a relatively low elastic modulus (approx. 100 GigaPascals) and has been shown to endure higher indentation loads than conventional and high performance steel. Indentation load capacity has been reported for relatively large (12.7 millimeters diameter) ceramic (Si3N4) indenter balls pressed against flat plates of 60NiTi. In order to develop damage load threshold criteria applicable to a wide range of bearing designs and sizes, the effects of indenter ball radius and the accuracy of interpolation of the Hertz contact stress relations for 60NiTi must be ascertained. In this paper, results of indentation tests involving ceramic balls ranging from 6.4 to 12.7 mm in diameter and highly polished 60NiTi flat plates are presented. When the resulting dent depth data for all the indenter ball sizes are normalized using the Hertz equations, the data (dent depth versus stress) are comparable. Thus when designing bearings made from 60NiTi, the Hertz stress relations can be applied with relative confidence over a range of rolling element sizes and internal geometries.

materials↗
NASA NTRS2016

Processing and Characterization of Thousand-Hour 500 C Durable 4H-SiC JFET Integrated Circuits

This work reports fabrication and testing of integrated circuits (ICs) with two levels of interconnect that consistently achieve greater than 1000 hours of stable electrical operation at 500 C in air ambient. These ICs are based on 4H-SiC junction field effect transistor (JFET) technology that integrates hafnium ohmic contacts with TaSi2 interconnects and SiO2 and Si3N4 dielectric layers over approximately 1-micrometer scale vertical topology. Following initial burn-in, important circuit parameters remain stable for more than 1000 hours of 500 C operational testing. These results advance the technology foundation for realizing long-term durable 500 C ICs with increased functional capability for sensing and control combustion engine, planetary, deep-well drilling, and other harsh-environment applications.

Microelectronics↗
NASA NTRS2016

Processing and Characterization of Thousand-Hour 500 C Durable 4H-SiC JFET Integrated Circuits

This work reports fabrication and testing of integrated circuits (ICs) with two levels of interconnect that consistently achieve greater than 1000 hours of stable electrical operation at 500 C in air ambient. These ICs are based on 4H-SiC junction field effect transistor (JFET) technology that integrates hafnium ohmic contacts with TaSi2 interconnects and SiO2 and Si3N4 dielectric layers over 1-m scale vertical topology. Following initial burn-in, important circuit parameters remain stable for more than 1000 hours of 500 C operational testing. These results advance the technology foundation for realizing long-term durable 500 C ICs with increased functional capability for sensing and control combustion engine, planetary, deep-well drilling, and other harsh-environment applications.

JFET↗
NASA NTRS2019

Experimental Study on Mitigation of Lifetime-Limiting Dielectric Cracking in Extreme Temperature 4H-SiC JFET Integrated Circuits

While NASA Glenn Research Center's "Generation 10" 4H-SiC Junction Field Effect Transistor (JFET) integrated circuits (ICs) have uniquely demonstrated 500 °C electrical operation for durations of over a year, this experimental work has also revealed that physical cracking of chip dielectric passivation layers ultimately limits extreme-environment operating lifetime [1-3]. The prevention of such dielectric passivation cracks should therefore improve IC high temperature durability and yield, leading to more beneficial technology adoption into aerospace, automotive, and energy systems. This report describes Generation 10.2, 11.1, and 11.2 die tested under unbiased and unpackaged accelerated age testing at 500 °C, 600 °C, 720 °C, and 800 °C in air-atmosphere ovens for 100- and 200-hour duration. Additional samples were separately subjected to 10 thermal cycles between the same high temperatures (with 10-hour high-temperature soak each cycle) and 50 °C. It is shown that having two stoichiometric Si3N4 layers in the interconnect dielectric stack substantially decreases the amount of dielectric cracking observed following these oven tests.

Spry, D. J.↗
NASA NTRS2021

Effect of High-K Dielectric Layer on 1/f Noise Behavior in Graphene Field-Effect Transistors

We report the 1/f noise characteristics at low-frequency in graphene field-effect transistors that utilized a high- dielectric tantalum oxide encapsulated layer (a few nanometers thick) placed by atomic layer deposition on Si3N4. A low-noise level of ~ 2.2  10-10 Hz-1 has been obtained at f = 10 Hz. The origin and physical mechanism of the noise can be interpreted by the McWhorter context, where fluctuations in the carrier number contribute dominantly to the low-frequency noise. Optimizing fabrication processes reduced the number of charged impurities in the graphene field-effect transistors. The study has provided insights into the underlying physical mechanisms of the noise at low-frequency for reducing the noise in graphene-based devices.

Yifei Wang↗
DOE OSTI2022

Properties and microstructure evolution of silicon nitride and zirconium nitride following Ni ion irradiation

We report that silicon nitride and zirconium nitride have been proposed as potential materials for multiple nuclear applications (inert matrix fuels, accident tolerant fuels, space nuclear power, fusion reactor design), yet knowledge on their behavior under irradiation remains limited. Ion irradiations were performed using 15 MeV Ni 5+ ions on Si 3 N 4 and ZrN samples, with midrange doses (around 3 µm) from 1 to 50 dpa and temperatures from 300 to 700°C. Volumetric lattice swelling was determined by grazing incidence X-ray diffraction, defect production and evolution were tracked using Transmission Electron Microscopy, and nanoindentation was performed to quantify the ceramics’ mechanical properties evolution. The results from these irradiation studies on nitride ceramics help fill the current gap present in the literature. Behavior consistent with past work on irradiated Si 3 N 4 was observed with respect to mechanical properties and defect formation up to 15 dpa and 500°C. Failure of the grain boundary sintering aid in Si 3 N 4 was observed above these conditions. Different behavior was observed in both nitrides at 50 dpa and 700°C, where lattice swelling increased past potential saturation values. Unreported cavity formation was witnessed in both materials under all irradiation conditions, with stable number density and slight size increase above 15 dpa. The mechanism for the cavity formation remains to be determined.

36 MATERIALS SCIENCE↗