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Advanced Aerogel Technology

The JPL Aerogel Laboratory has made aerogels for NASA flight missions, e.g., Stardust, 2003 Mars Exploration Rovers and the 2011 Mars Science Laboratory, as well as NASA research projects for the past 14 years. During that time it has produced aerogels of a range of shapes, sizes, densities and compositions. Research is ongoing in the development of aerogels for future sample capture and return missions and for thermal insulation for both spacecraft and scientific instruments. For the past several years, the JPL Aerogel Laboratory has been developing, producing and testing a new composite material for use as the high temperature thermal insulation in the Advanced Sterling Radioisotope Generator (ASRG) being developed by Lockheed Martin and NASA. The composite is made up of a glass fiber felt, silica aerogel, Titania powder, and silica powder. The oxide powders are included to reduce irradiative heat transport at elevated temperatures. These materials have thermal conductivity values that are the same as the best commercially produced high temperature insulation materials, and yet are 40% lighter. By greatly reducing the amount of oxide powder in the composite, the density, and therefore for the value of the thermal conductivity, would be reduced. The JPL Aerogel Laboratory has experimented with using glass fiber felt, expanded glass fiber felt and loose fibers to add structural integrity to silica aerogels. However, this work has been directed toward high temperature applications. By conducting a brief investigation of the optimal combination of fiber reinforcement and aerogel density, a durable, extremely efficient thermal insulation material for ambient temperature applications would be produced. If a transparent thermal insulation is desired, then aerogel is an excellent candidate material. At typical ambient temperatures, silica aerogel prevents the transport of heat via convection and conduction due to its highly porous nature. To prevent irradiative thermal transport, silica aerogel can be used in conjunction with a transparent polymeric material that blocks infrared radiation. The transparency of silica aerogel is typically greater than 90% for visible wavelengths from 500 nm to 900 nm for a 5 mm long path length.

reduce irradiative heat transport↗

Effects of Microgravity on the Formation of Aerogels

This paper describes research to investigate fundamental aspects of the effects of microgravity on the formation of the microstructure of metal oxide alcogels and aerogels. We are studying the role of gravity on pore structure and gel uniformity in collaboration with Marshall Space Flight Center (MSFC) on gelling systems under microgravity conditions. While this project was just initiated in May 1998, related research performed earlier is described along with the plans and rationale for the current microgravity investigation to provide background and describe newly developing techniques that should be useful for the current gellation studies. The role of gravity in materials processing must be investigated through the study of well-mastered systems. Sol-gel processed materials are near-perfect candidates to determine the effect of gravity on the formation and growth of random clusters from hierarchies of aggregated units. The processes of hydrolysis, condensation, aggregation and gellation in the formation of alcogels are affected by gravity and therefore provide a rich system to study under microgravity conditions. Supercritical drying of the otherwise unstable wet alcogel preserves the alcogel structure produced during sol-gel processing as aerogel. Supercritically dried aerogel provides for the study of material microstructures without interference from the effects of surface tension, evaporation, and solvent flow. Aerogels are microstructured, low density open-pore solids. They have many unusual properties including: transparency, excellent thermal resistance, high surface area, very low refractive index, a dielectric constant approaching that of air, and extremely low sound velocity. Aerogels are synthesized using sol-gel processing followed by supercritical solvent extraction that leaves the original gel structure virtually intact. These studies will elucidate the effects of microgravity on the homogeneity of the microstructure and porosity of aerogel. The presence of poorly controlled microporosity in aerogel leads to material non-uniformity that gives rise to increased light scattering. Investigation of the effect of gravity driven solute flows within microclusters and their effect on condensation and agglomeration reactions will enable us to improve the preparation and properties of aerogel. Increased clarity of images viewed through aerogel and decreased scattering from the pores of aerogel will significantly improve the prospects for large-scale adoption of aerogel in such applications as transparent insulating windows, high performance thermal insulation, and Cherenkov detectors.

Hunt, A. J.↗

Analysis of Thermal Radiation Effects on Temperatures in Turbine Engine Thermal Barrier Coatings

Thermal barrier coatings are important, and in some instances a necessity, for high temperature applications such as combustor liners, and turbine vanes and rotating blades for current and advanced turbine engines. Some of the insulating materials used for coatings, such as zirconia that currently has widespread use, are partially transparent to thermal radiation. A translucent coating permits energy to be transported internally by radiation, thereby increasing the total energy transfer and acting like an increase in thermal conductivity. This degrades the insulating ability of the coating. Because of the strong dependence of radiant emission on temperature, internal radiative transfer effects are increased as temperatures are raised. Hence evaluating the significance of internal radiation is of importance as temperatures are increased to obtain higher efficiencies in advanced engines.

Siegel, Robert↗

Fluorinated Poly(Phenylene Ether Ketones)

Fluorinated poly(phenylene ether ketones) are colorless, transparent, low-dielectric-constant, highly thermally stable polymers. Particularly suitable for use as film and coating materials in electronic and thermal-control applications such as; passivant insulating coats and interlevel dielectrics in microelectronic circuits, or as protective transparent coats on solar cells or mirrors. Solubility and transparency of 12F-PEK along with its lower dielectric constant and other properties make it more useful as dielectric film and coating material in many applications.

St. Clair, Anne K.↗

Mechanical Properties of Aerogels

Aerogels are extremely low density solids that are characterized by a high porosity and pore sizes on the order of nanometers. Their low thermal conductivity and sometimes transparent appearance make them desirable for applications such as insulation in cryogenic vessels and between double paned glass in solar architecture. An understanding of the mechanical properties of aerogels is necessary before aerogels can be used in load bearing applications. In the present study, the mechanical behavior of various types of fiber-reinforced silica aerogels was investigated with hardness, compression, tension and shear tests. Particular attention was paid to the effects of processing parameters, testing conditions, storage environment, and age on the aerogels' mechanical response. The results indicate that the addition of fibers to the aerogel matrix generally resulted in softer, weaker materials with smaller elastic moduli. Furthermore, the testing environment significantly affected compression results. Tests in ethanol show an appreciable amount of scatter, and are not consistent with results for tests in air. In fact, the compression specimens appeared to crack and begin to dissolve upon exposure to the ethanol solution. This is consistent with the inherent hydrophobic nature of these aerogels. In addition, the aging process affected the aerogels' mechanical behavior by increasing their compressive strength and elastic moduli while decreasing their strain at fracture. However, desiccation of the specimens did not appreciably affect the mechanical properties, even though it reduced the aerogel density by removing trapped moisture. Finally, tension and shear test results indicate that the shear strength of the aerogels exceeds the tensile strength. This is consistent with the response of brittle materials. Future work should concentrate on mechanical testing at cryogenic temperatures, and should involve more extensive tensile tests. Moreover, before the mechanical response of reinforced aerogels can be fully understood, more tests of unreinforced aerogels are necessary. Unreinforced aerogels are of particular use because their birefringent nature allows for visual determination of stress fields during mechanical testing. The success of any future tests depends on the availability of a large supply of quality specimens with well-documented preparation and storage histories.

Parmenter, Kelly E.↗

Thermal Field Imaging Using Ultrasound

It is often desirable to be able to determine the temperature field in the interiors of opaque fluids forced into convection by externally imposed temperature gradients. To measure the temperature at a point in an opaque fluid in the usual fashion requires insertion of a probe, and to determine the full field therefore requires either the ability to move this probe or the introduction of multiple probes. Neither of these solutions is particularly satisfactory, although they can lead to quite accurate measurements. As an alternative we have investigated the use of ultrasound as a relatively non-intrusive probe of the temperature field in convecting opaque fluids. The temperature dependence of the sound velocity can be sufficiently great to permit a determination of the temperature from timing the traversal of an ultrasound pulse across a chamber. In this paper we will present our results on convecting flows of transparent and opaque fluids. Our experimental cells consist of relatively narrow rectangular cavities made of thermally insulating materials on the sides, and metal top and bottom plates. The ultrasound transducer is powered by a pulser/receiver, the signal output of which goes to a very high speed signal averager. The average of several hundred to several thousand signals is then sent to a computer for storage and analysis. The experimental procedure is to establish a convective flow by imposing a vertical temperature gradient on the chamber, and then to measure, at several regularly spaced locations, the transit time for an ultrasound pulse to traverse the chamber horizontally (parallel to the convecting rolls) and return to the transducer. The transit time is related to the temperature of the fluid through which the sound pulse travels. Knowing the relationship between transit time and temperature (determined in a separate experiment), we can extract the average temperature across the chamber at that location. By changing the location of the transducer it is then possible to find the average temperature at different locations along the chamber, thereby determining the temperature profile along the system. (In the future we will construct an array of transducers. This will give us the capability to determine the temperature profile much more rapidly than at present, an important consideration if time-dependent phenomena are to be studied.) To validate our procedure we introduced encapsulated liquid crystal particles into glycerol. The liquid crystal particles' color varies depending on the temperature of the fluid. A photograph of the fluid through transparent sidewalls therefore gives a picture of the temperature field of the convecting fluid, independent of our ultrasound imaging. A representative result is shown in the Figure 1, which reveals a very satisfying correspondence between the two techniques. Therefore we have a great deal of confidence that the ultrasound imaging approach is indeed measuring the actual temperature profile of the fluid. The technique has also been applied to convecting liquid metal flows, and representative data will be presented from those experiments as well.

Andereck, D.↗

Conducting a thermal conductivity survey

A physically transparent approximate theory of phonon decay rates is presented starting from a pair potential model of the interatomic forces in an insulator or semiconductor. The theory applies in the classical regime and relates the 3-phonon decay rate to the third derivative of the pair potential. Phonon dispersion relations do not need to be calculated, as sum rules relate all the needed quantities directly to the pair potential. The Brillouin zone averaged phonon lifetime turns out to involve a dimensionless measure of the anharmonicity multiplied by an effective density of states for 3-phonon decay. Results are given for rare gas and alkali halide crystals. For rare gases, the results are in good agreement with more elaborate perturbation calculations. Comparison to experimental data on phonon linewidths and thermal conductivity are made.

Allen, P. B.↗

Saltless Solar Ponds

Problems associated with heat storage in solar ponds eliminated by transparent insulating cover at surface of pond. Cover makes unnecessary salt gradient that suppresses natural convection within pond to promote thermal storage.

Lin, E. I.↗

Polyimides Made From PDMDA

Thermally stable linear aromatic polyimides with improved optical, electrical, and processing characteristics made from 3,3'-bis(3,4-dicarboxyphenoxy)diphenylmethane dianhydride (PDMDA). Made in form of powders that can be dissolved to cast thin films. Potentially useful as coating and matrix materials. Films made vary from transparent to pale yellow. Greater degrees of transparency and lower dielectric constants make these polyimides more suitable for use in some electronic and optical applications; e.g., as insulating materials on wires and protective films on solar photovoltaic cells.

St. Clair, Anne K.↗

Thermal characterization of reusable external insulation for the space shuttle.

Thermal protection systems utilizing reusable ceramic external insulations are under study for application to the orbiter vehicle of NASA's space shuttle system which is to be launched by an expendable booster, remain in orbit for a week or two, reenter the earth's atmosphere, and land like a conventional aircraft. The required reuse capability is for 100 missions. The thermal characterization of the reusable external insulation (REI) is described. Thermal conductivity measurements are described for a series of mullite-based REIs with densities ranging from 100 to 300 kg/cu m, including opacified variations of the mullite material designed for reduction of the radiant component of heat transport. The results of thermal conductivity measurements performed on guarded-hot-plate equipment from 150 to above 1200 K in different vacuum and gaseous environments are described. Measurements were also made with exceptionally large temperature differences to detect transparency effects in the unopacified REIs. These measurements were made to provide design data for the flight conditions, and to aid in theoretical computations aimed at separating and optimizing the heat transport components.

Brazel, J. P.↗

Single layer multi-color luminescent display and method of making

The invention is a multi-color luminescent display comprising an insulator substrate and a single layer of host material, which may be a phosphor deposited thereon that hosts one or more different impurities, therein forming a pattern of selected and distinctly colored phosphors such as blue, green, and red phosphors in a single layer of host material. Transparent electrical conductor means may be provided for subjecting selected portions of the pattern of colored phosphors to an electric field, thereby forming a multi-color, single layer electroluminescent display. A method of forming a multi-color luminescent display includes the steps of depositing on an insulator substrate a single layer of host material, which itself may be a phosphor, with the properties to host varying quantities of different impurities and introducing one or more of said different impurities into selected areas of the said single layer of host material by thermal diffusion or ion implantation to form a pattern of phosphors of different colors in the said single layer of host material.

Robertson, James B.↗

Alternate Approach to Multi Layer Insulation Modeling to Reduce Node Count

For models with a limitation on the overall node count, the typical approach to Multi-Layer Insulation (MLI) modeling may generate nodes that are necessary for the analysis, but do not represent components of particular interest. This leaves fewer nodes that can be utilized to model components of greater importance than the MLI. A common approach to modeling MLI is to include a separate MLI node representing the outer layer of the insulation and a radiative coupling based on the area multiplied by an effective emissivity. Therefore, wherever insulation is included, one node is needed for the underlying surface and another node for the insulation. Since many spacecraft and instruments include MLI covering a sizable portion of their designs, this may result in a considerable number of nodes being used for MLI. An alternate method to MLI modeling was developed that eliminates the MLI node, while still preserving the effect of the insulation for the underlying surface, thereby increasing the available nodes that could be used elsewhere in the model. This approach relies on preserving the baseline reflectivity, while reducing the absorptivity (based on the blanket effective emittance) and including a transparency. An inactive second surface is placed just behind the base surface that fully absorbs any energy that is transmitted without including its effect in the model. In essence, this approach applies only the energy that makes it through the blanket to the underlying surface. This method was tested out on the Roman Space Telescope model in local areas in preparation for its use in the generation of a launch model, which is constrained in the allowable node count. This paper documents the performance of the method and presents a comparison between the One-Node MLI method and the traditional two node MLI approach.

Thermal↗

Space Environmentally Stable Polyimides and Copolyimides

Polyimides with a unique combination of properties including low color in thin films, atomic oxygen (AO), ultra-violet (UV) radiation resistance, solubility in organic solvents in the imide form, high glass transition (T(sub g)) temperatures and high thermal stability have been prepared and characterized. The polymers were prepared by reacting a novel aromatic diamine with aromatic dianhydrides in a polar aprotic solvent. The solubility of the polymers in the imide form as well as the color density of thin films were dependent upon the chemical structure of the dianhydride. Several thin films (25-50 mm thick) prepared by solution casting of amide acid or imide solutions exhibited very low color and high optical transparency (approximately 90%) as determined by UV/visible spectroscopy. The polymers exhibited T(sub g)s >200 C depending upon the structure of the dianhydride and temperatures of 5% weight loss approximately 500C in air as determined by dynamic thermogravimetric analysis. Thin films coated with silver/inconel were exposed to a high fluence of AO and 1000 equivalent solar hours of UV radiation. The effects of these exposures on optical properties were minor. These space environmentally durable polymers are potentially useful in a variety of applications on spacecraft such as thin film membranes on antennas, second-surface mirrors, thermal/optical coatings and multi-layer thermal insulation (MLI) blanket materials. The chemistry, physical and mechanical properties of the polymers as well as their responses to AO and UV exposure will be discussed.

Watson, Kent A.↗

Temperature Distribution in a Composite of Opaque and Semitransparent Spectral Layers

The analysis of radiative transfer becomes computationally complex for a composite when there are multiple layers and multiple spectral bands. A convenient analytical method is developed for combined radiation and conduction in a composite of alternating semitransparent and opaque layers. The semi- transparent layers absorb, scatter, and emit radiation, and spectral properties with large scattering are included. The two-flux method is used, and its applicability is verified by comparison with a basic solution in the literature. The differential equation in the two-flux method Is solved by deriving a Green's function. The solution technique is applied to analyze radiation effects in a multilayer zirconia thermal barrier coating with internal radiation shields for conditions in an aircraft engine combustor. The zirconia radiative properties are modeled by two spectral bands. Thin opaque layers within the coating are used to decrease radiant transmission that can degrade the zirconia insulating ability. With radiation shields, the temperature distributions more closely approach the opaque limit that provides the lowest metal wall temperatures.

Siegel, Robert↗

The PCM is Dead! Long Live O-PCM!

The ability to reconfigure the optical behavior of a device enables free-space applications ranging from imaging to sensing and signal control. Such optical devices can be compacted via meta-surfaces, patterned structures with feature sizes below the incident wavelength. Leveraging geometry in addition to material properties and CMOS fabrication techniques has allowed meta-surfaces for lenses, holograms, beam steerers and more. To incorporate multiple optical functions into one device, various methods of device control have been implemented, such as stretching of flexible substrates, tuning the refractive index of the comprising meta-atoms via the electro-optic or the thermo-optic effects, phase transition materials such as VO2 and more. Chalcogenide glasses used as optical phase change materials, such as Ge¬2Sb2Te5 (GST), have gained increased traction in the optics community for potential use in the near infrared (NIR) and mid infrared (MIR) bands, including the telecom bands. Various chalcogenides such as Sb2Se3, Sb2S3, Ge2Sb¬2Se5 and Ge2Sb2Se4Te (GSST) have been investigated due to their broad NIR or MIR transparency window and large changes in refractive index. In their amorphous phase, these materials usually display a lower refractive index and low absorption when compared to their crystalline state which display a higher refractive index and typically larger extinction coefficients. The amorphous-crystalline reversible switching can be done via fast melt-quenching thermal processes triggered by laser or electrical impulses, relying on a substrate as a heat sink. The potential of PCMs in photonic devices can be limited by intrinsic material limitations as well as by device fabrication issues. To explore the cyclability of GSST, a PCM with large refractive index contrast and on-chip electrothermal switching on a silicon-on-insulator platform has been done to analyze potential failure mechanisms from both a material and device perspective. A brief outline of the instrumentation and phase change contrast analysis is provided. Dewetting of the PCM, delamination of and damage in the PECVD SiNx protective layer, elemental migration in the PCM and optical contrast decay have been observed in cycled GSST devices. Guidelines for device performance improvement are proposed, and an improved design with larger endurance is shown in progress.

reconfigurable photonics↗

Depth-Penetrating Measurements Developed for Thermal Barrier Coatings Incorporating Thermographic Phosphors

The insulating properties of thermal barrier coatings (TBCs) provide highly beneficial thermal protection to turbine engine components by reducing the temperature sustained by those components. Therefore, measuring the temperature beneath the TBC is critical for determining whether the TBC is performing its insulating function. Currently, noncontact temperature measurements are performed by infrared pyrometry, which unfortunately measures the TBC surface temperature rather than the temperature of the underlying component. To remedy this problem, the NASA Glenn Research Center, under the Information Rich Test Instrumentation Project, developed a technique to measure the temperature beneath the TBC by incorporating a thin phosphor layer beneath the TBC. By performing fluorescence decay-time measurements on light emission from this phosphor layer, Glenn successfully measured temperatures from the phosphor layer up to 1100 C. This is the first successful demonstration of temperature measurements that penetrate beneath the TBC. Thermographic phosphors have a history of providing noncontact surface temperature measurements. Conventionally, a thermographic phosphor is applied to the material surface and temperature measurements are performed by exciting the phosphor with ultraviolet light and then measuring the temperature-dependent decay time of the phosphor emission at a longer wavelength. The innovative feature of the new approach is to take advantage of the relative transparency of the TBC (composed of yttria-stabilized zirconia) in order to excite and measure the phosphor emission beneath the TBC. The primary obstacle to achieving depth-penetrating temperature measurements is that the TBCs are completely opaque to the ultraviolet light usually employed to excite the phosphor. The strategy that Glenn pursued was to select a thermographic phosphor that could be excited and emit at wavelengths that could be transmitted through the TBC. The phosphor that was selected was yttria doped with europia (Y2O3:Eu), which has a minor excitation peak at 532 nm (green) and an emission peak at 611 nm (red)--both are wavelengths that exhibit significant transmission through the TBC. The measurements were performed on specimens consisting of a 25- m-thick phosphor layer beneath a 100- m-thick TBC. The 532-nm (green) excitation light was provided by a frequency-doubled YAG:Nd (yttrium-aluminum-garnet:neodymium) laser, and the fluorescence decay time measurements were acquired with a modified Raman microscope. The preceding graph compares the intensity of the phosphor emission of the phosphor layer above the TBC versus that of the phosphor layer beneath the TBC. Although there was considerable attenuation of the phosphor signal (a factor of 30), the phosphor emission at the reduced intensity was more than sufficient to perform fluorescence decay time measurements. The following graph shows the fluorescence lifetime temperature dependency for the Y2O3:Eu phosphor layers both above and below the TBC. These curves show an excellent match and indicate that, despite the attenuation due to the overlying TBC, the phosphor layer beneath the TBC still functions as an effective temperature indicator.

Eldridge, Jeffrey I.↗

Corner-Cube Retroreflector Instrument for Advanced Lunar Laser Ranging

A paper describes how, based on a structural-thermal-optical-performance analysis, it has been determined that a single, large, hollow corner cube (170- mm outer diameter) with custom dihedral angles offers a return signal comparable to the Apollo 11 and 14 solid-corner-cube arrays (each consisting of 100 small, solid corner cubes), with negligible pulse spread and much lower mass. The design of the corner cube, and its surrounding mounting and casing, is driven by the thermal environment on the lunar surface, which is subject to significant temperature variations (in the range between 70 and 390 K). Therefore, the corner cube is enclosed in an insulated container open at one end; a narrow-bandpass solar filter is used to reduce the solar energy that enters the open end during the lunar day, achieving a nearly uniform temperature inside the container. Also, the materials and adhesive techniques that will be used for this corner-cube reflector must have appropriate thermal and mechanical characteristics (e.g., silica or beryllium for the cube and aluminum for the casing) to further reduce the impact of the thermal environment on the instrument's performance. The instrument would consist of a single, open corner cube protected by a separate solar filter, and mounted in a cylindrical or spherical case. A major goal in the design of a new lunar ranging system is a measurement accuracy improvement to better than 1 mm by reducing the pulse spread due to orientation. While achieving this goal, it was desired to keep the intensity of the return beam at least as bright as the Apollo 100-corner-cube arrays. These goals are met in this design by increasing the optical aperture of a single corner cube to approximately 170 mm outer diameter. This use of an "open" corner cube allows the selection of corner cube materials to be based primarily on thermal considerations, with no requirements on optical transparency. Such a corner cube also allows for easier pointing requirements, because there is no dependence on total internal reflection, which can fail off-axis.

Turyshev, Slava G.↗