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High-Temperature RF Probe Station For Device Characterization Through 500 deg C and 50 GHz

A high-temperature measurement system capable of performing on-wafer microwave testing of semiconductor devices has been developed. This high temperature probe station can characterize active and passive devices and circuits at temperatures ranging from room temperature to above 500 C. The heating system uses a ceramic heater mounted on an insulating block of NASA shuttle tile material. The temperature is adjusted by a graphical computer interface and is controlled by the software-based feedback loop. The system is used with a Hewlett-Packard 8510C Network Analyzer to measure scattering parameters over a frequency range of 1 to 50 GHz. The microwave probes, cables, and inspection microscope are all shielded to protect from heat damage. The high temperature probe station has been successfully used to characterize gold transmission lines on silicon carbide at temperatures up to 540 C.

Schwartz, Zachary D.

Characterization of Ni19.5Ti50.5Pd25Pt5 High-Temperature Shape Memory Alloy Springs and their Potential Application in Aeronautics

Shape memory alloys (SMAs) have been used as actuators in many different industries since the discovery of the shape memory effect, but the use of SMAs as actuation devices in aeronautics has been limited due to the temperature constraints of commercially available materials. Consequently, work is being done at NASA's Glenn Research Center to develop new SMAs capable of being used in high temperature environments. One of the more promising high-temperature shape memory alloys (HTSMAs) is Ni19.5Ti50.5Pd25Pt5. Recent work has shown that this material is capable of being used in operating environments of up to 250 C. This material has been shown to have very useful actuation capabilities, demonstrating repeatable strain recoveries up to 2.5% in the presence of an externally applied load. Based on these findings, further work has been initiated to explore potential applications and alternative forms of this alloy, such as springs. Thus, characterization of Ni19.5Ti50.5Pd25Pt5 springs, including their mechanical response and how variations in this response correlate to changes in geometric parameters, are discussed. The effects of loading history, or training, on spring behavior were also investigated. A comparison of the springs with wire actuators is made and the benefits of using one actuator form as opposed to the other discussed. These findings are used to discuss design considerations for a surge-control mechanism that could be used in the centrifugal compressor of a T-700 helicopter engine.

Stebner, Aaron

Technical evaluation report of the Specialists Meeting on Characterization of Low Cycle High Temperature Fatigue by the Strainrange Partitioning Method

The ability of the Strainrange Partitioning Method SRP was evaluated to correlate the creep-fatigue behavior of gas turbine materials and to predict the creep fatigue life of laboratory specimens subjected to complex cycling conditions. A reference body of high temperature creep fatigue data which can be used in the evaluation of other SRP and low cycle high temperature fatigue predictive techniques was provided.

Drapier, J. M.

Sensor Lead Wires Positioned on SiC-based Monolithic Ceramic and Fiber- reinforced Ceramic Matrix Composite Subcomponents with Flat and Curved Surfaces

There is strong interest in the development of silicon carbide-based monolithic ceramic and composite materials and components for demanding, high-temperature applications. Thorough characterization of material properties, including high-temperature testing under simulated or actual operating conditions, is a high priority for programs involved in developing these silicon carbide- (SiC) based materials and components. Members of the Sensors and Electronics Technology Branch at the NASA Lewis Research Center are developing minimally intrusive methods of measuring the properties (such as the surface temperature, strain, and heat flux characteristics) of components and subelements that are being tested or operated in hostile, high-temperature environments. Their primary goal is to instrument the test article or operating component with durable sensors that have a minimal effect on test conditions such as the gas flow across the surface of the item and the material response (including the through-thickness conduction of heat). Therefore, the main thrust of their work has been the development of thin-film sensors (e.g., thermocouples or strain gauges) for use on various advanced material test articles, including SiC/SiC composite components. There was a need for a better method of securing sensor lead wires on SiC-based components and subelements that would be tested at temperatures to 1000 C (or higher), to enhance the durability of the overall minimally intrusive sensor system. To address this need, Lewis researchers devised an alternative approach for positioning the sensor lead wires (which are connected to the thin-film sensors) on SiC or SiC/SiC components. A reaction-forming method of joining was used to strongly bond hoop-shaped monolithic SiC and SiC/SiC composite attachments of various sizes to both flat and curved surfaces of SiC/SiC composite subelements (see the photos). This approach is based on an affordable, robust ceramic joining technology, named ARCJoinT, which was developed at Lewis for the joining of SiC-based ceramics and fiber-reinforced composites.

Kiser, James D.

Characterization of polybenzimidazole (PBI) film at high temperatures

Polybenzimidazole, a linear thermoplastic polymer with excellent thermal stability and strength retention over a wide range of temperatures, was evaluated for its potential use as the main dielectric in high temperature capacitors. The film was characterized in terms of its dielectric properties in a frequency range of 50 Hz to 100 kilo-Hz. These properties, which include the dielectric constant and dielectric loss, were also obtained in a temperature range from 20 C to 300 C with an electrical stress of 60 Hz, 50 V/mil present. The alternating and direct current breakdown voltages of silicone oil impregnated films as a function of temperature were also determined. The results obtained indicate that while the film remained relatively stable up to 200 C, it exhibited an increase in its dielectric properties as the temperature was raised to 300 C. It was also found that conditioning of the film by heat treatment at 60 C for six hours tended to improve its dielectric and breakdown properties. The results are discussed and conclusions made concerning the suitability of the film as a high temperature capacitor dielectric.

Hammoud, Ahmad N.

A high-temperature Rutherford Backscattering Spectrometry apparatus for in situ material characterization

A new methodology for high-temperature Rutherford Backscattering Spectrometry (HT-RBS) has been developed to enable in situ material characterization at elevated temperatures. A 3.5 MeV proton beam penetrates a 10-µm-thick 316L stainless steel foil mounted on a graphite substrate, with backscattered signals detected using an HT-RBS system. Conventional semiconductor detectors, primarily based on silicon, suffer significant performance degradation at temperatures higher than ~ 60 °C due to increased leakage current and noise, leading to signal distortion and failure. Here, to preserve spectral quality, a 5 µm aluminum foil shields the detector from thermal radiation, allowing reliable operation up to 900 °C at the target. A rotatable shutter provides additional thermal isolation during data collection pauses. In situ measurements of areal density changes of 316L stainless steel were conducted to validate the technique, revealing consistency with the known thermal expansion coefficient. The method facilitates seamless switching between irradiation and analysis, enabling continuous studies. This approach supports in situ investigations of diffusion, void swelling, creep, and corrosion, offering a versatile tool for advanced materials research.

36 MATERIALS SCIENCE

Solar Total Energy Project (STEP) Performance Analysis of High Temperature Energy Storage Subsystem

The 1982 milestones and lessons learned; performance in 1983; a typical day's operation; collector field performance and thermal losses; and formal testing are highlighted. An initial test that involves characterizing the high temperature storage (hts) subsystem is emphasized. The primary element is on 11,000 gallon storage tank that provides energy to the steam generator during transient solar conditions or extends operating time. Overnight, thermal losses were analyzed. The length of time the system is operated at various levels of cogeneration using stored energy is reviewed.

Moore, D. M.

Characterizing the Chemical Stability of High Temperature Materials for Application in Extreme Environments

The chemical stability of high temperature materials must be known for use in the extreme environments of combustion applications. The characterization techniques available at NASA Glenn Research Center vary from fundamental thermodynamic property determination to material durability testing in actual engine environments. In this paper some of the unique techniques and facilities available at NASA Glenn will be reviewed. Multiple cell Knudsen effusion mass spectrometry is used to determine thermodynamic data by sampling gas species formed by reaction or equilibration in a Knudsen cell held in a vacuum. The transpiration technique can also be used to determine thermodynamic data of volatile species but at atmospheric pressures. Thermodynamic data in the Si-O-H(g) system were determined with this technique. Free Jet Sampling Mass Spectrometry can be used to study gas-solid interactions at a pressure of one atmosphere. Volatile Si(OH)4(g) was identified by this mass spectrometry technique. A High Pressure Burner Rig is used to expose high temperature materials in hydrocarbon-fueled combustion environments. Silicon carbide (SiC) volatility rates were measured in the burner rig as a function of total pressure, gas velocity and temperature. Finally, the Research Combustion Lab Rocket Test Cell is used to expose high temperature materials in hydrogen/oxygen rocket engine environments to assess material durability. SiC recession due to rocket engine exposures was measured as a function of oxidant/fuel ratio, temperature, and total pressure. The emphasis of the discussion for all techniques will be placed on experimental factors that must be controlled for accurate acquisition of results and reliable prediction of high temperature material chemical stability.

Opila, Elizabeth

Development of an Extreme High Temperature n-type Ohmic Contact to Silicon Carbide

We report on the initial demonstration of a tungsten-nickel (75:25 at. %) ohmic contact to silicon carbide (SiC) that performed for up to fifteen hours of heat treatment in argon at 1000 C. The transfer length method (TLM) test structure was used to evaluate the contacts. Samples showed consistent ohmic behavior with specific contact resistance values averaging 5 x 10-4 -cm2. The development of this contact metallization should allow silicon carbide devices to operate more reliably at the present maximum operating temperature of 600 C while potentially extending operations to 1000 C. Introduction Silicon Carbide (SiC) is widely recognized as one of the materials of choice for high temperature, harsh environment sensors and electronics due to its ability to survive and continue normal operation in such environments [1]. Sensors and electronics in SiC have been developed that are capable of operating at temperatures of 600 oC. However operating these devices at the upper reliability temperature threshold increases the potential for early degradation. Therefore, it is important to raise the reliability temperature ceiling higher, which would assure increased device reliability when operated at nominal temperature. There are also instances that require devices to operate and survive for prolonged periods of time above 600 oC [2, 3]. This is specifically needed in the area of hypersonic flight where robust sensors are needed to monitor vehicle performance at temperature greater than 1000 C, as well as for use in the thermomechanical characterization of high temperature materials (e.g. ceramic matrix composites). While SiC alone can withstand these temperatures, a major challenge is to develop reliable electrical contacts to the device itself in order to facilitate signal extraction

Evans, Laura J.

Characterization of Ternary NiTiPt High-Temperature Shape Memory Alloys

Pt additions substituted for Ni in NiTi alloys are known to increase the transformation temperature of the alloy but only at fairly high Pt levels. However, until now only ternary compositions with a very specific stoichiometry, Ni50-xPtxTi50, have been investigated and then only to very limited extent. In order to learn about this potential high-temperature shape memory alloy system, a series of over twenty alloys along and on either side of a line of constant stoichiometry between NiTi and TiPt were arc melted, homogenized, and characterized in terms of their microstructure, transformation temperatures, and hardness. The resulting microstructures were examined by scanning electron microscopy and the phase compositions quantified by energy dispersive spectroscopy."Stoichiometric" compositions along a line of constant stoichiometry between NiTi to TiPt were essentially single phase but by any deviations from a stoichiometry of (Ni,Pt)50Ti50 resulted in the presence of at least two different intermetallic phases, depending on the overall composition of the alloy. Essentially all alloys, whether single or two-phase, still under went a martensitic transformation. It was found that the transformation temperatures were depressed with initial Pt additions but at levels greater than 10 at.% the transformation temperature increased linearly with Pt content. Also, the transformation temperatures were relatively insensitive to alloy stoichiometry within the range of alloys examined. Finally, the dependence of hardness on Pt content for a series of Ni50-xPtxTi50 alloys showed solution softening at low Pt levels, while hardening was observed in ternary alloys containing more than about 10 at.% Pt. On either side of these "stoichiometric" compositions, hardness was also found to increase significantly.

Rios, Orlando

Electrical characterization of glass, teflon, and tantalum capacitors at high temperatures

Dielectric materials and electrical components and devices employed in radiation fields and the space environment are often exposed to elevated temperatures among other things. Therefore, these systems must withstand the high temperature exposure while still providing good electrical and other functional properties. Experiments were carried out to evaluate glass, teflon, and tantalum capacitors for potential use in high temperature applications. The capacitors were characterized in terms of their capacitance and dielectric loss as a function of temperature up to 200 C. At a given temperature, these properties were obtained in a frequency range of 50 Hz to 100 kHz. The DC leakage current measurements were also performed in a temperature range from 20 to 200 C. The obtained results are discussed and conclusions are made concerning the suitability of the capacitors investigated for high temperature applications.

Hammoud, A. N.

Energy-Based Tetrahedron Sensor for High-Temperature, High-Pressure Environments

An acoustic energy-based probe has been developed that incorporates multiple acoustic sensing elements in order to obtain the acoustic pressure and three-dimensional acoustic particle velocity. With these quantities, the user can obtain various energy-based quantities, including acoustic energy density, acoustic intensity, and acoustic impedance. In this specific development, the probe has been designed to operate in an environment characterized by high temperatures and high pressures as is found in the close vicinity of rocket plumes. Given these capabilities, the probe is designed to be used to investigate the acoustic conditions within the plume of a rocket engine or jet engine to facilitate greater understanding of the noise generation mechanisms in those plumes. The probe features sensors mounted inside a solid sphere. The associated electronics for the probe are contained within the sphere and the associated handle for the probe. More importantly, the design of the probe has desirable properties that reduce the bias errors associated with determining the acoustic pressure and velocity using finite sum and difference techniques. The diameter of the probe dictates the lower and upper operating frequencies for the probe, where accurate measurements can be acquired. The current probe design implements a sphere diameter of 1 in. (2.5 cm), which limits the upper operating frequency to about 4.5 kHz. The sensors are operational up to much higher frequencies, and could be used to acquire pressure data at higher frequencies, but the energy-based measurements are limited to that upper frequency. Larger or smaller spherical probes could be designed to go to lower or higher frequency range

Gee, Kent L.

Thermal Gradient Effects on Redox Evolution and Volatility-Driven Fractionation in Ternary U/Ce/Cs Condensates

Understanding how thermal history influences redox evolution and chemical fractionation is essential for characterizing high-temperature condensation in complex materials, including nuclear debris. Here, we tested the hypothesis that distinct thermal regimes in a plasma flow reactor influence redox pathways and elemental partitioning in ternary U/Ce/Cs systems. A configurable plasma flow reactor was modified with an external tube furnace to impose two distinct thermal gradients: continuous ambient cooling and a furnace-assisted thermal hold-up near 1400 K followed by rapid cooling. Transmission electron microscopy characterized phase identity, morphology, and nanoscale element distributions, while inductively coupled plasma-mass spectrometry quantified bulk elemental ratios. Across both thermal regimes, uranium and cerium condensed as UO 2 and CeO 2 as dominant refractory oxide products. Uranium partially oxidized to α-UO 3 during extended ambient cooling, while furnace-assisted hold-up preserved UO 2 and produced partial reduction of cerium to Ce 2 O 3 . Cesium remained volatile upstream and condensed later in the reactor, forming Cs 2 O and Cs-uranate phases with the highest incorporation after thermal hold-up. Bulk ICP-MS measurements supported these observations. U/Ce ratios remained comparatively stable and Cs displayed delayed and apparent transient enrichment that matched the nanoscale measurements. This integrated approach provides a quantitative method for linking thermal gradients to redox evolution and volatility-driven fractionation. These results show how the plasma flow reactor can identify where equilibrium descriptions remain adequate and where kinetic effects from residence time and temperature history must be considered when interpreting condensation behavior in multicomponent systems.

and nuclear chemistry

Ab initio Computations of the Electronic, Mechanical, and Thermal Properties of Ultra High Temperature Ceramics (UHTC) ZrB2 and HfB2

Refractory materials such as metallic borides, often considered as ultra high temperature ceramics (UHTC), are characterized by high melting point, high hardness, and good chemical inertness. These materials have many applications which require high temperature materials that can operate with no or limited oxidation. Ab initio, first principles methods are the most accurate modeling approaches available and represent a parameter free description of the material based on the quantum mechanical equations. Using these methods, many of the intrinsic properties of these material can be obtained. We performed ab initio calculations based on density functional theory for the UHTC materials ZrB2 and HfB2. Computational results are presented for structural information (lattice constants, bond lengths, etc), electronic structure (bonding motifs, densities of states, band structure, etc), thermal quantities (phonon spectra, phonon densities of states, specific heat), as well as information about point defects such as vacancy and antisite formation energies.

Lawson, John W.

Simulated Reentry Heating by Torching

The two first order reentry heating parameters are peak heating flux (W/cm2) and peak heat load (kJ/cm2). Peak heating flux (and deceleration, gs) is higher for a ballistic reentry and peak heat load is higher for a lifting reentry. Manned vehicle reentries are generally lifting reentries at nominal 1-5 gs so that personnel will not be crushed by high deceleration force. A few off-nominal manned reentries have experienced 8 or more gs with corresponding high heating flux (but below nominal heat load). The Shuttle Orbiter reentries provide about an order of magnitude difference in peak heating flux at mid-bottom (TPS tiles, approximately 6 W/cm2 or 5 BTU/ft2- sec) and leading edge (RCC, approximately 60 W/cm2 or 50 BTU/ft2- sec). Orion lunar return and Mars sample lander are of the same order of magnitude as orbiter leading edge peak heat loads. Flight temperature measurements are available for some orbiter TPS tile and RCC locations. Return-to-Flight on-orbit tile-repair-candidate-material-heating performance was evaluated by matching propane torch heating of candidate-materials temperatures at several depths to orbiter TPS tile flight-temperatures. Char and ash characteristics, heat expansion, and temperature histories at several depths of the cure-in-place ablator were some of the TPS repair material performance characteristics measured. The final char surface was above the initial surface for the primary candidate (silicone based) material, in contrast to a receded surface for the Apollo-type ablative heat shield material. Candidate TPS materials for Orion CEV (LEO and lunar return), and for Mars sample lander are now being evaluated. Torching of a candidate ablator material, PICA, was performed to match the ablation experienced by the STARDUST PICA heat shield. Torching showed that the carbon fiberform skeleton in a sample of PICA was inhomogeneous in that sample, and allowed measurements (of the clumps and voids) of the inhomogeneity. Additional reentry heating-performance characterizations of high temperature insulation materials were performed.

Harvey, Gale A.

Simulated Reentry Heating by Torching

The two first order reentry heating parameters are peak heating flux (W/square cm) and peak heat load (kJ/square cm). Peak heating flux (and deceleration, gs) is higher for a ballistic reentry and peak heat load is higher for a lifting reentry. Manned vehicle reentries are generally lifting reentries at nominal 1-5 gs so that personnel will not be crushed by high deceleration force. A few off-nominal manned reentries have experienced 8 or more gs with corresponding high heating flux (but below nominal heat load). The Shuttle Orbiter reentries provide about an order of magnitude difference in peak heating flux at mid-bottom (TPS tiles, approximately 6 W/square cm or 5 BTU/square ft - sec) and leading edge (RCC, approximately 60 W/square cm or 50 BTU/square ft- sec). Orion lunar return and Mars sample lander are of the same order of magnitude as orbiter leading edge peak heat loads. Flight temperature measurements are available for some orbiter TPS tile and RCC locations. Return-to-Flight on-orbit tile-repair-candidate-material-heating performance was evaluated by matching propane torch heating of candidate-materials temperatures at several depths to orbiter TPS tile flight-temperatures. Char and ash characteristics, heat expansion, and temperature histories at several depths of the cure-in-place ablator were some of the TPS repair material performance characteristics measured. The final char surface was above the initial surface for the primary candidate (silicone based) material, in contrast to a receded surface for the Apollo-type ablative heat shield material. Candidate TPS materials for Orion CEV (LEO and lunar return), and for Mars sample lander (MSL) are now being evaluated. Torching of a candidate ablator material, PICA, was performed to match the ablation experienced by the STARDUST PICA heat shield. Torching showed that the carbon fiberform skeleton in a sample of PICA was inhomogeneous in that sample, and allowed measurements (of the clumps and voids) of the inhomogeneity. Additional reentry heating-performance characterizations of high temperature insulation materials were performed.

Harvey, Gale A.

Finite Element Analysis of Active and Sensory Thermopiezoelectric Composite Materials

Analytical formulations are developed to account for the coupled mechanical, electrical, and thermal response of piezoelectric composite materials. The coupled response is captured at the material level through the thermopiezoelectric constitutive equations and leads to the inherent capability to model both the sensory and active responses of piezoelectric materials. A layerwise laminate theory is incorporated to provide more accurate analysis of the displacements, strains, stresses, electric fields, and thermal fields through-the-thickness. Thermal effects which arise from coefficient of thermal expansion mismatch, pyroelectric effects, and temperature dependent material properties are explicitly accounted for in the formulation. Corresponding finite element formulations are developed for piezoelectric beam, plate, and shell elements to provide a more generalized capability for the analysis of arbitrary piezoelectric composite structures. The accuracy of the current formulation is verified with comparisons from published experimental data and other analytical models. Additional numerical studies are also conducted to demonstrate additional capabilities of the formulation to represent the sensory and active behaviors. A future plan of experimental studies is provided to characterize the high temperature dynamic response of piezoelectric composite materials.

Lee, Ho-Jun

Characterization of a Ultra-high Temperature Ceramic Composite

Ultra-high temperature ceramics (UHTC) are of interest for hypersonic vehicle leading edge applications. Monolithic UHTCs are of concern because of their low fracture toughness and brittle behavior. UHTC composites (UHTCC) are being investigated as a possible approach to overcome these deficiencies. In this study a small sample of a UHTCC was evaluated by limited mechanical property tests, furnace oxidation exposures, and oxidation exposures in a flowing environment. The composite was prepared from a carbon fiber perform using ceramic particulates and a preceramic polymer. The as-received composite plate was non-uniform from front to back surface. Plate dimensions were 150 x 150 x 6 mm. The back surface had a fibrous, uniform appearance; XRD analysis revealed the presence of Sic and C. The front surface was smooth and non-uniform in appearance with evidence of a coarse grain structure produced by a liquid phase; XRD analysis revealed the presence of HfB2. Microcracks were present throughout the thickness as one might expect from a carbon fiber reinforced composite with attendant large thermal expansion mismatch between the matrix phases and the fibers. The HfB2 phase on the front surface was comparable in thickness to a fiber ply or about 0.6 mm, and surface microcracks were evident. Limited four point flexural tests were carried out at span to depth ratios of approximately 14 and 16 with markedly different results. Tests were run with the front or the back surface in tension. At the shorter span to depth failures occurred under a loading pin for both orientations. At a span to depth of 16 failures occurred in the center of the span with fracture clearly initiating from a tensile failure. Ultimate flexural strength, strain at ultimate stress, stress and strain at deviation from linear elastic behavior are reported. Strains at ultimate stress ranged from about 0.6 to 0.7 % for the back surface in tension, and 0.4 to 0.6 for the front surface in tension. At constant span to depth the strain at ultimate stress was about 0.2% greater for the back surface in tension and the ultimate strength was also higher. Strengths were in line with predictions from theory. Furnace oxidation studies were carried out at 1627 and 1927OC in a static furnace environment using ten minute cycles and one, five, and ten cycles. Limited oxidation studies were also carried out in a flowing oxyacetylene torch environment. Specimens were photographed, and weight and dimensional changes were determined. XRD and SEM characterizations were performed. Weight losses were attributed primarily to carbon fiber oxidation. The composite survived the torch test with little visible distress. Further details will be determined once metallographic studies are completed.

Levine, Stanley R.