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High temperature materials characterization

A lab facility for measuring elastic moduli up to 1700 C was constructed and delivered. It was shown that the ultrasonic method can be used to determine elastic constants of materials from room temperature to their melting points. The ease in coupling high frequency acoustic energy is still a difficult task. Even now, new coupling materials and higher power ultrasonic pulsers are being suggested. The surface was only scratched in terms of showing the full capabilities of either technique used, especially since there is such a large learning curve in developing proper methodologies to take measurements into the high temperature region. The laser acoustic system does not seem to have sufficient precision at this time to replace the normal buffer rod methodology.

Workman, Gary L.↗

Density fluctuations and radiated noise for a high-temperature supersonic jet

Experimental data on density fluctuations were obtained by the laser Schlieren method in a supersonic jet which at the nozzle exit had a Mach number of 1.43 and a stagnation temperature of about 1090 K. The jet emerged into the ambient atmosphere in an anechoic chamber, correctly expanded from a nozzle which had an exit diameter of 10.8 cm. Using the information on the density fluctuations and the mean shear obtained by probes, the autocorrelation of the radiated noise was calculated by a theory that is suitable for Mach wave emission. This theory is a modification of that developed by Ffowcs Williams and Maidanik (1965). The calculated noise field agrees well with that obtained by using microphones outside the jet.

Parthasarathy, S. P.↗

Computational simulation of microfracture in high temperature metal matrix composites

A computational simulation procedure, using three-dimensional finite element method and global strain energy release rates, is described to predict the microfracture process and identify/quantify the hierarchy of respective fracture modes in metal matrix composites. The procedure is used to predict the microfracture in unidirectional composites under longitudinal loads and accounts for the interphase strength in the in situ state. A novel procedure to computationally simulate the fiber pushthrough process is also described. In this simulation, the interface material is replaced by an anisotropic material with greatly reduced shear modulus in order to simulate the fiber pushthrough process using a linear analysis. Such a procedure is easily implemented and is computationally very effective.

Mital, Subodh K.↗

High performance miniature hygrometer and method thereof

An uncoated interdigitated transducer is cooled from a temperature above the dew point to a temperature below the dew point, while a parameter of a signal of the transducer is measured. The reduction in temperature causes a monotonic change in transducer signal because that signal is sensitive primarily to the water loading of the transducer surface as water forms on that surface due to the reduction in temperature. As the dew point is approached with temperature reduction, the slope of the curve of transducer signal with respect to temperature, remains relatively constant. However, as the dew point is reached the slope of that curve increases and because of changes in the structure of the water layer on the surface of the transducer, at the dew point the transducer responds with a clear shift in the rate at which the transducer signal changes. The temperature at which the second derivative of signal vs. temperature peaks can be readily used to identify with extreme accuracy, the precise dew point. The measurement technique employed by the present invention is relatively immune to surface contamination which remains significantly unchanged during the brief measurement period.

VanZandt, Thomas R.↗

High-temperature, high-pressure optical cells

For measuring the thermal diffusivity of HgCdTe melts by the laser-pulse method, an infrared transparent cell with flat windows of sufficient strength to withstand the high-vapor pressure of mercury had to be developed. Since mercury telluride expands on freezing, certain difficulties arose in returning the cell to room temperature without cracking it. T08 commercial fused silica is used in the construction of the cell, and the cells are transparent for wavelengths from about 3.5 microns in the infrared to 260 nm in the ultraviolet. The construction procedure for the required cells has been laborious. However, the obtained cell has routinely withstood internal pressures in excess of 60 atm at 900 C. Attention is given to the design of the windows, aspects of cell construction, and questions of loading.

Holland, L. R.↗

Feasibility of Coupling Between a Single-Mode Elliptical-Core Fiber and a Single Mode Rib Waveguide Over Temperature

To determine the feasibility of coupling the output of an optical fiber to a rib waveguide in a temperature environment ranging from 20 C to 300 C, a theoretical calculation of the coupling efficiency between the two was investigated. This is a significant problem which needs to be addressed to determine whether an integrated optic device can function in a harsh temperature environment. Because the behavior of the integrated-optic device is polarization sensitive, a polarization-preserving optic fiber, via its elliptical core, was used to couple light with a known polarization into the device. To couple light energy efficiently from an optical fiber into a channel waveguide, the design of both components should provide for well-matched electric field profiles. The rib waveguide analyzed was the light input channel of an integrated-optic pressure sensor. Due to the complex geometry of the rib waveguide, there is no analytical solution to the wave equation for the guided modes. Approximation or numerical techniques must be utilized to determine the propagation constants and field patterns of the guide. In this study, three solution methods were used to determine the field profiles of both the fiber and guide: the effective-index method (EIM), Marcatili's approximation, and a Fourier method. These methods were utilized independently to calculate the electric field profile of a rib channel waveguide and elliptical fiber at two temperatures, 20 C and 300 C. These temperatures were chosen to represent a nominal and a high temperature that the device would experience. Using the electric field profile calculated from each method, the theoretical coupling efficiency between the single-mode optical fiber and rib waveguide was calculated using the overlap integral and results of the techniques compared. Initially, perfect alignment was assumed and the coupling efficiency calculated. Then, the coupling efficiency calculation was repeated for a range of transverse offsets at both temperatures. Results of the calculation indicate a high coupling efficiency can be achieved when the two components were properly aligned. The coupling efficiency was more sensitive to alignment offsets in the y direction than the x, due to the elliptical modal profile of both components. Changes in the coupling efficiency over temperature were found to be minimal.

Tuma, Margaret L.↗

High Temperature Mechanical Behavior of Polycrystalline Alumina from Mixed Nanometer and Micrometer Powders

Sintered aluminum oxide materials were formed using commercial methods from mechanically mixed powders of nano-and micrometer alumina. The powders were consolidated at 1500 and 1600 C with 3.2 and 7.2 ksi applied stress in argon. The conventional micrometer sized powders failed to consolidate. While 100 percent nanometer-sized alumina and its mixture with the micrometer powders achieved less than 99 percent density. Preliminary high temperature creep behavior indicates no super-plastic strains. However high strains (less than 0.65 percent) were generated in the nanometer powder, due to cracks and linked voids initiated by cavitation.

Goldsby, Jon C.↗

Extraction of amino acids from soils and sediments with superheated water

A method of extraction for amino acids from soils and sediments involving superheated water has been investigated. About 75-97 per cent of the amino acids contained in four soils of a soil profile from Illinois were extracted by this method. Deep penetration of water into soil aggregates and partial hydrolysis of peptide bonds during this extraction by water at high temperature are likely mechanisms responsible for the release of amino acids from samples. This extraction method does not require subsequent desalting treatments when analyses are carried out with an ion-exchange amino acid analyzer.

Cheng, C. N.↗

Survivability of Affordable High Temperature Polymer Matrix Composites for Propulsion Engine Components

PMR-type polyimides are regarded as state of the art high temperature polymers, due to their excellent thermo-mechanical properties and thermo-oxidative stability. One of their drawbacks, however is the inability to process them using cost-effective processing methods such as Resin Transfer Molding (RTM) and Resin Film Infusion (RFI). Development of low viscosity, high temperature polymers has been the subject of intense research. Recently, a new generation of low viscosity polyimides were synthesized by the introduction of twisted biphenyl or binapthyl groups into the backbone. This report details the progress for Year 1, which has involved acquiring samples and initiating Phases I and II of the proposed research. Specifically, studies of the process-property relationships of a series of polymers using oligomers based on 2,3,3' ,4'-biphenyltertracarboxylic dianhydride (PBDA) and a mixture of a diamine, BAX and a triamine, 1,3,5-Tris (4-aminophenoxybenzene), TAB, where the amount of TAB was varied have been initiated. The sample containing 10 percent TAB possesses a slightly higher degree of crystalline order versus that of the 20 percent TAB sample, based on x-ray diffraction studies of the b-staged oligomers. Both systems lose all of the crystalline order upon curing, however. The chemorheology has been studied as a function of the TAB content. While the magnitude of the viscosity is essentially the same for both systems, the cure kinetics of the 10 percent TAB system is faster than that for the 20 percent TAB system. The sample exhibits a melting-recrystallization-remelting behavior before the crosslinking commences. Correlation of other kinetic parameters, such as the activation energies for curing, the Tg and mechanical properties to the structure of these systems is underway. Future studies will involve characterization of mechanical and thermal properties of the pure resins and the fabrication of fiber reinforced composites using these materials.

Dean, Derrick↗

Comparison of two methods of performing the Thellier experiment

Two methods for performing the Thellier experiment on paleointensity determinations are compared. The first method is essentially that of Coe (1967) and the second is a slight modification of it. Prepared samples containing different species of magnetic particles are used, and both methods are always performed on the same sample. The study is designed to accent procedural differences between the two methods. It is shown that only the Coe method yields linear PNRM-PTRM (Partial ThermoRemanent Magnetization) plots for single domain and pseudo-single domain particles, because it maintains the symmetry between high-temperature VRM (Viscous Remanent Magnetization) and spontaneous decay, whereas for the modified Coe method the spontaneous decay is enhanced. For multidomain remanence, even the Coe method yields a nonlinear concave-up PNRM-PTRM plot. Paleointensity determinations employing only the ratio NRM/TRM provide no means of evaluating the reliability of the results.

Levi, S.↗

Measurement of Seebeck coefficient using a light pulse

A high-temperature (1900 K) Seebeck coefficient apparatus is described in which small thermal gradients are generated in a sample by light pulses transmitted via light pipes. By employing an analog subtraction circuit, the Seebeck coefficient is displayed directly on an X-Y recorder. This technique presents a convenient, accurate, and rapid method for measuring the Seebeck coefficient in highly doped semiconductors as a function of temperature. The nature of the resulting display (X-Y recording) is a valuable tool in determining validity of the data. A straight line results (i.e., a minimum of hysteresis) only if all potential experimental errors are minimized. Under these conditions, the error of measurements of the Seebeck coefficient is estimated to be less than + or - 1 percent.

Wood, C.↗

Mechanical Properties of T650-35/AFR-PE-4 at Elevated Temperatures for Lightweight Aeroshell Designs

Considerable efforts have been underway to develop multidisciplinary technologies for aeroshell structures that will significantly increase the allowable working temperature for the aeroshell components, and enable the system to operate at higher temperatures while sustaining performance and durability. As part of these efforts, high temperature polymer matrix composites and fabrication technologies are being developed for the primary load bearing structure (heat shield) of the spacecraft. New high-temperature resins and composite material manufacturing techniques are available that have the potential to significantly improve current aeroshell design. In order to qualify a polymer matrix composite (PMC) material as a candidate aeroshell structural material, its performance must be evaluated under realistic environments. Thus, verification testing of lightweight PMC's at aeroshell entry temperatures is needed to ensure that they will perform successfully in high-temperature environments. Towards this end, a test program was developed to characterize the mechanical properties of two candidate material systems, T650-35/AFR-PE-4 and T650-35/RP46. The two candidate high-temperature polyimide resins, AFR-PE-4 and RP46, were developed at the Air Force Research Laboratory and NASA Langley Research Center, respectively. This paper presents experimental methods, strength, and stiffness data of the T650-35/AFR-PE-4 material as a function of elevated temperatures. The properties determined during the research test program herein, included tensile strength, tensile stiffness, Poisson s ratio, compressive strength, compressive stiffness, shear modulus, and shear strength. Unidirectional laminates, a cross-ply laminate and two eight-harness satin (8HS)-weave laminates (4-ply and 10-ply) were tested according to ASTM standard methods at room and elevated temperatures (23, 316, and 343 C). All of the relevant test methods and data reduction schemes are outlined along with mechanical data. These data contribute to a database of material properties for high-temperature polyimide composites that will be used to identify the material characteristics of potential candidate materials for aeroshell structure applications.

Whitley, Karen S.↗

FaceSheet Push-off Tests to Determine Composite Sandwich Toughness at Cryogenic Temperatures

A new novel test method, associated analysis, and experimental procedures are developed to investigate the toughness of the facesheet-to-core interface of a sandwich material at cryogenic temperatures. The test method is designed to simulate the failure mode associated with facesheet debonding from high levels of gas pressure in the sandwich core. The effects of specimen orientation are considered, and the results of toughness measurements are presented. Comparisons are made between room and liquid nitrogen (-196 C) test temperatures. It was determined that the test method is insensitive to specimen facesheet orientation and strain energy release rate increases with a decrease in the test temperature.

Gates, Thomas S.↗

Strain gage performance above 1033 K

Study provides compendium of test methods and results which may be used in evaluating high temperature environment gage behavior. Tests include resistance to ground and drift rate and gage factor variation as temperature function. Variation ranged from zero at room temperature (297 K) to 14.5 percent at 1053 K.

Nichols, D. W.↗

Dryden Flight Research Center hot structures research

The facilities, testing techniques, and design methods are described for NASA Dryden Flight Research Center. High temperature strain gage technology, realistic flight hardware fabrication, and structural analysis are discussed. A considerable amount of experimental work on hot structure concepts for hypersonic vehicles was performed; all the work is not complete, and there are still problem areas that need to be resolved.

Fields, R. A.↗

Graphite/Polyimide Composites

Technology developed under the Composites for Advanced Space Transportation System Project is reported. Specific topics covered include fabrication, adhesives, test methods, structural integrity, design and analysis, advanced technology developments, high temperature polymer research, and the state of the art of graphite/polyimide composites.

Dexter, H. B.↗

Reduced hydrogen permeability at high temperatures

CO and CO2 reduce hydrogen loss through iron, nickel, and cobalt based alloy tubes. Method is based on concept that oxide film on metal surface reduces hydrogen permeability through metal; adding CO or CO2 forms oxide films continuously during operation, and hydrogen containment is improved. Innovation enhances prospects for Stirling engine system utilization.

Stephens, J. R.↗