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Ru(sub 1)Si(sub 1)O(sub 4) thin films were deposited on Si and oxidized Si substrates by reactive rf magnetron sputtering of a Ru(sub 1)Si(sub 1) target in an argon/oxygen gas mixture.
A multilayer thin film strain sensor for large temperature range use is under development using a reactively-sputtered process. The sensor is capable of being fabricated in fine line widths utilizing the sacrificial-layer lift-off process that is used for micro-fabricated noble-metal sensors. Tantalum nitride films were optimized using reactive sputtering with an unbalanced magnetron source. A first approximation model of multilayer resistance and temperature coefficient of resistance was used to set the film thicknesses in the multilayer film sensor. Two multifunctional sensors were fabricated using multilayered films of tantalum nitride and palladium chromium, and tested for low temperature resistivity, TCR and strain response. The low temperature coefficient of resistance of the films will result in improved stability in thin film sensors for low to high temperature use.
Nanolaminate manufacturing (NLM) is a new way of developing materials whose properties can far exceed those of homogeneous materials. Traditional alloys, composites and bulk laminates tend to average the properties of the materials from which they were made. With nanostructured materials, the high density of interfaces between dissimilar materials results in novel material properties. For example, materials made -from alternating nanoscale layers of metals and oxides have exhibited thermal conductivities far below those of the oxides themselves. Also, metallic nanolaminates can have peak strengths 100 times lager than the bulk constituent metals. Recent work at MSFC has focused on the development of nickel/aluminum oxide (Ni/Al2O3)) nanolaminates. Ni/Al2O3 nanolaminates are expected to have better strength, creep and fatigue resistance, oxygen compatibility, and corrosion resistance than the traditional metal-matrix composites of this material, which has been used in a variety of aerospace applications. A chemical vapor deposition (CW) system has been developed and optimized for the deposition of nanolaminates. Nanolaminates with layer thicknesses between 10 and 300 nm have been successfully grown and characterization has included scanning electron microscopy (SEM) and atomic force microscopy (AFM) Nanolaminates have a large variety of potential applications. They can be tailored to have both very small and anisotropic thermal conductivities and are promising as thermal coatings for both rock$ engine components and aerobraking structures. They also have the potential to be used in aerospace applications where strength at high temperatures, corrosion resistance or resistance to hydrogen embrittlement is important. Both CVD and magnetron sputtering facilities are available for the deposition of nanolayered materials. Characterization equipment includes SEM, AFM, X-ray diffraction, transmission electron microscopy, optical profilometry, and mechanical tensile pull testing.
We have prepared transparent films with a sheet relativity of 10(exp 1) to 10(exp 12) ohm/square by co-depositing a transparent conducting oxide (TCO) with magnesium fluoride, using two independently controlled RF magnetron sputter guns to facilitate adjustment of the film composition, Co-deposited indium tin oxide (ITO) and MgF2 on quartz and flexible polymeric substrate exhibited reasonably stable sheet resistivity over several months' time, with substantially lower optical reflectance than that of pure ITO. However, exposure to low-intensity blue light reduces sheet resistivity by as much as two orders of magnitude. Our results suggest this photoconductivity effect may be present in all InO(x)-based materials. We find that sheet resistivity can by "tuned" by admitting a small amount of high-purity air during deposition offering the possibility of closed loop process control.
Electrically insulating spacecraft surfaces are vulnerable to nonuniform charge buildup due to particles emitted by the sun. On Mars, insulating surfaces of exploration vehicles and structures will be affected by dust coatings possibly held in place by triboelectric surface charge. Application of a conductive film may be a solution to the charging problem, but the coating must be highly transparent if used on solar panels, lenses, etc. Sheet resistivity requirements depend on the application and are in the range 10(exp 2) - 10(exp 8) ohms/square. Co-deposited indium tin oxide (ITO) and MgF2 is promising, with high transparency, tailorable electrical properties, and durability to atomic oxygen. Due to ITO's relatively narrow bandgap (approximately 3.5 eV), the film might absorb enough ultraviolet to protect polymeric substrates. Recent work on dual-magnetron-sputtered ITO-MgF2 showed that a variety of polymeric substrates can be coated at room temperature. However, the sheet resistivity is very sensitive to composition, suggestive of a percolation transition. This could be a serious problem for large-scale coating production. We will report on attempts to control film composition by plasma emission monitoring of the ITO and MgF2 guns.
Highly transparent, slightly conductive films of co-deposited indium tin oxide (ITO) and MgF, have possible applications for environmental protection of exterior surfaces of spacecraft. Reliable preparation of films with the desired sheet resistivity (approximately 10(exp 8) ohms/square) is difficult because the electrical properties of ITO-Mg F, are highly dependent on film composition. We have investigated the use of plasma emission monitoring to improve the reproducibility of films prepared by RF magnetron sputtering. While considerable improve ment was observed, it appears that some in-situ electrical or optica l characterization will be needed for reliable production coating wit h ITO-MgF,. We have also done further evaluation of a possibly undesi rable photoconductive effect previously observed in these films.
The increased role of unmanned aerial vehicles (UAV) in NASA's suborbital program has created a strong interest in the development of instruments with new capabilities, more compact sizes and reduced weights than the instruments currently operated on manned aircrafts. There is a strong demand and tremendous potential for using high altitude UAV (HUAV) to carry weather radars for measurements of reflectivity and wind fields from tropical storms. Tropical storm genesis frequently occurs in ocean regions that are inaccessible to piloted aircraft due to the long off shore range and the required periods of time to gather significant data. Important factors of interest for the study of hurricane genesis include surface winds, profiled winds, sea surface temperatures, precipitation, and boundary layer conditions. Current satellite precipitation and surface wind sensors have resolutions that are too large and revisit times that are too infrequent to study this problem. Furthermore, none of the spaceborne sensors measure winds within the storm itself. A dual beam X-band Doppler radar, UAV Radar (URAD), is under development at the NASA Goddard Space Flight Center for the study of tropical storms from HUAV platforms, such as a Global Hawk. X-band is the most desirable frequency for airborne weather radars since these can be built in a relatively compact size using off-the-shelf components which cost significantly less than other higher frequency radars. Furthermore, X-band radars provide good sensitivity with tolerable attenuation in storms. The low-cost and light-weight URAD will provide new capabilities for studying hurricane genesis by analyzing the vertical structure of tropical cyclones as well as 3D reflectivity and wind fields in clouds. It will enable us to measure both the 3D precipitation structure and surface winds by using two antenna beams: fixed nadir and conical scanning each produced by its associated subsystem. The nadir subsystem is a magnetron based radar modified from a marine radar transceiver. It is capable of measuring vertical reflectivity and velocity profile while being a lower-cost, smaller size, and lighter weight version of the NASA ER-2 Doppler Radar (EDOP), which has flown during many NASA field campaigns and has provided valuable scientific information on hurricanes and weather phenomena. Unfortunately, EDOP is too large and heavy for most UAV platforms, but the experience gained with this instrument provided us with the heritage to build a new low-cost, light-weight, smaller system that will be capable of flying on UAVs. The scanning subsystem uses a TWT transmitter and provides measurements of 3D reflectivity/wind fields in-clouds. Conical scanning of the radar beam at a 35 deg. incidence angle will also provide information of surface wind speed and direction derived from the surface return over a single 360 deg. sweep. URAD data system will be Linux based with the capability of autonomous operation. It will utilize cutting edge digital receiver and FPGA technologies to carry out the data acquisition and processing tasks. High speed navigation data from the aircraft will also be captured and saved along with radar data for 3D measurement field reconstruction and aircraft motion correction. There is a tremendous potential for UAVs to carry down-looking weather radars for measurements of reflectivity, horizontal and vertical winds from tropical storms. With operation from HUAV platforms, the dual beam X-band radar under development promises to provide greatly needed information for tropical storm research.
Composite films of multicomponent materials, such as oxides and nitrides, e.g., lead zirconate titanate, are deposited by dc magnetron sputtering, employing a rotating substrate holder, which rotates relative to a plurality of targets, one target for each metal element of the multicomponent material. The sputtering is carried out in a reactive atmosphere. The substrates on which the layers are deposited are at ambient temperature. Following deposition of the composite film, the film is heated to a temperature sufficient to initiate a solid state reaction and form the final product, which is substantially single phase and substantially homogeneous.
A high conductivity, n-doped semiconductor film is produced from zinc, or Zn and Cd, and group VI elements selected from Se, S and Te in a reactive magnetron sputtering system having a chamber with one or two targets, a substrate holder, means for heating the substrate holder, and an electric field for ionizing gases in the chamber. Zinc or a compound of Zn and Cd is placed in the position of one of the two targets and doping material in the position of the other of the two targets. Zn and Cd may be placed in separate targets while a dopant is placed in the third target. Another possibility is to place an alloy of Zn and dopant, or Zn, Cd and dopant in one target, thus using only one target. A flow of the inert gas is ionized and directed toward said targets, while a flow of a reactant gas consisting of hydrides of the group VI elements is directed toward a substrate on the holder. The targets are biased to attract negatively ionized inert gas. The desired stochiometry for high conductivity is achieved by controlling the temperature of the substrate, and partial pressures of the gases, and the target power and total pressure of the gases in the chamber.
Nanophase nickel-zirconium alloys have been investigated for use as electrically conductive coatings and catalyst supports in fuel cells. Heretofore, noble metals have been used because they resist corrosion in the harsh, acidic fuel cell interior environments. However, the high cost of noble metals has prompted a search for less-costly substitutes. Nickel-zirconium alloys belong to a class of base metal alloys formed from transition elements of widely different d-electron configurations. These alloys generally exhibit unique physical, chemical, and metallurgical properties that can include corrosion resistance. Inasmuch as corrosion is accelerated by free-energy differences between bulk material and grain boundaries, it was conjectured that amorphous (glassy) and nanophase forms of these alloys could offer the desired corrosion resistance. For experiments to test the conjecture, thin alloy films containing various proportions of nickel and zirconium were deposited by magnetron and radiofrequency co-sputtering of nickel and zirconium. The results of x-ray diffraction studies of the deposited films suggested that the films had a nanophase and nearly amorphous character.
MoO3 has shown promise as a cathode material that can extend the upper limit of operating temperature of rechargeable lithium thin-film electrochemical cells. Cells of this type are undergoing development for use as energy sources in cellular telephones, wireless medical sensors, and other, similarly sized portable electronic products. The LiCoO2 and LiMn2O4 cathodes heretofore used in these cells exhibit outstanding cycle lives (of the order of hundreds of thousands of cycles) at room temperature, but operation at higher temperatures reduces their cycle lives substantially: for example, at a temperature of 150 C, cells containing LiCoO2 cathodes lose half their capacities in 100 charge/discharge cycles. The superiority of MoO3 as a cathode material was demonstrated in experiments on lithium thin-film cells fabricated on glass slides. Each cell included a layer of Ti (for adhesion to the glass slide), a patterned layer of Pt that served as a cathode current collector, a cathode layer of MoO3, a solid electrolyte layer of Li3.3 PO3.8 N0.22 ("LiPON"), and an anode layer of Li. All the layers were deposited by magnetron sputtering except for the Li layer, which was deposited by thermal evaporation. These cells, along with similar ones containing LiCoO2 cathodes, were subjected to several tests, including measurements of specific capacity in charge/discharge cycling at a temperature of 150 C. The results of these measurements, plotted in the figure, showed that whereas specific capacity of the cells containing LiCoO2 cathodes faded to about half its initial value after only 100 cycles, the specific capacity of the cells containing the MoO3 cathodes faded only slightly during the first few hundred cycles and thereafter not only recovered to its initial value but continued to increase up to at least 5,500 cycles.
L1(sub 0)-ordered FePd epitaxial thin films were prepared using dc magnetron sputter deposition on MgO (001) substrates. The films were grown with varying thickness and degree of chemical order to investigate the interplay between the microstructure, magnetic anisotropy, and magnetic domain structure. The experimentally measured domain size/period and magnetic anisotropy in this high perpendicular anisotropy system were found to be correlated following the analytical energy model proposed by Kooy and Enz that considers a delicate balance between the domain wall energy and the demagnetizing stray field energy.
In support of NASA's efforts to advance methane technology for future exploration missions, two different igniter concepts were developed and tested at NASA's Marshall Space Flight Center for ignition of oxygen/methane propellants. The first type of igniter, an impinging injection, spark-initiated torch igniter (impinging igniter), used traditional spark plug technology to produce a small, but very intense, pulsed plasma as the ignition source. The second type of igniter, a microwave-generated plasma igniter (microwave igniter), used a microwave magnetron to produce a continuous, larger-volume plasma as the ignition source. Two new designs for both types of igniters were leveraged off past oxygen/methane igniter designs that were tested at MSFC and documented in a 2008 JANNAF paper. In this most recent work, the two new igniters were to be tested at the component level as well as inside a liquid oxygen/liquid methane (LOX/LCH4) 40-element swirl coaxial injector. Although the microwave igniter achieved ignition in every test, it encountered technical difficulties that prevented it from being tested with the injector. The impinging igniter required several design iterations as well as testing at different mixture ratios and mass flow rates before reliable operation with minimal ignition delay was achieved. The final design of the impinging igniter was successfully tested in the LOX/LCH4 injector. The same igniter was later re-configured and component-tested to demonstrate reliable ignition of oxygen/hydrogen propellants. Future tests of the impinging igniter will include ignition of a LOX/hydrogen two-stage swirl injector, which is one of several injector concepts being tested in the Lunar Lander Descent Engine Test Bed at MSFC. All igniter and injector tests have been funded by the Propulsion & Cryogenics Advanced Development project managed by Glenn Research Center and sponsored by NASA s Exploration Technology Development Program.
A plasma-enhanced chemical vapor deposition (PECVD) growth technique has been developed where the choice of starting substrate was found to influence the electrical characteristics of the resulting carbon nanofiber (CNF) tubes. It has been determined that, if the tubes are grown on refractory metallic nitride substrates, then the resulting tubes formed with dc PECVD are also electrically conducting. Individual CNFs were formed by first patterning Ni catalyst islands using ebeam evaporation and liftoff. The CNFs were then synthesized using dc PECVD with C2H2:NH3 = [1:4] at 5 Torr and 700 C, and approximately equal to 200-W plasma power. Tubes were grown directly on degenerately doped silicon <100> substrates with resistivity rho approximately equal to 1-5 meterohm-centimeter, as well as NbTiN. The approximately equal to 200-nanometer thick refractory NbTiN deposited using magnetron sputtering had rho approximately equal to 113 microohm-centimeter and was also chemically compatible with CNF synthesis. The sample was then mounted on a 45 beveled Al holder, and placed inside a SEM (scanning electron microscope). A nanomanipulator probe stage was placed inside the SEM equipped with an electrical feed-through, where tungsten probes were used to make two-terminal electrical measurements with an HP 4156C parameter analyzer. The positive terminal nanoprobe was mechanically manipulated to physically contact an individual CNF grown directly on NbTiN as shown by the SEM image in the inset of figure (a), while the negative terminal was grounded to the substrate. This revealed the tube was electrically conductive, although measureable currents could not be detected until approximately equal to 6 V, after which point current increased sharply until compliance (approximately equal to 50 nA) was reached at approximately equal to 9.5 V. A native oxide on the tungsten probe tips may contribute to a tunnel barrier, which could be the reason for the suppressed transport at low biases. Currents up to approximately 100 nA could be cycled, which are likely to propagate via the tube surface, or sidewalls, rather than the body, which is shown by the I-V in figure (a). Electrical conduction via the sidewalls is a necessity for dc NEMS (nanoelectromechanical system) applications, more so than for the field emission applications of such tubes. During the tests, high conductivity was expected, because both probes were shorted to the substrate, as shown by curve 1 in the I-V characteristic in figure (b). When a tube grown on NbTiN was probed, the response was similar to the approximately equal to 100 nA and is represented by curve 2 in figure (b), which could be cycled and propagated via the tube surface or the sidewalls. However, no measureable currents for the tube grown directly on Si were observed as shown by curve 3 in figure (b), even after testing over a range of samples. This could arise from a dielectric coating on the sidewalls for tubes on Si. As a result of the directional nature of ion bombardment during dc PECVD, Si from the substrate is likely re-sputtered and possibly coats the sidewalls.
In this investigation sputtered silicon carbide annealed at 300 C for one hour is used as a conformal thin film package. A RF magnetron sputterer was used to deposit 500 nm silicon carbide films on gold metal structures on alumina wafers. To determine the reliability and resistance to immersion in harsh environments, samples were submerged in gold etchant for 24 hours, in BOE for 24 hours, and in an O2 plasma etch for one hour. The adhesion strength of the thin film was measured by a pull test before and after the chemical immersion, which indicated that the film has an adhesion strength better than 10(exp 8) N/m2; this is similar to the adhesion of the gold layer to the alumina wafer. MIM capacitors are used to determine the dielectric constant, which is dependent on the SiC anneal temperature. Finally, to demonstrate that the SiC, conformal, thin film may be used to package RF circuits and sensors, an LC resonator circuit was fabricated and tested with and without the conformal SiC thin film packaging. The results indicate that the SiC coating adds no appreciable degradation to the circuits RF performance. Index Terms Sputter, silicon carbide, MIM capacitors, LC resonators, gold etchants, BOE, O2 plasma
A process that employs silicon-on-insulator (SOI) substrates and silicon (Si) micromachining has been devised for fabricating wide-intermediate-frequency-band (wide-IF) superconductor/insulator/superconductor (SIS) mixer devices that result in suspended gold beam leads used for radio-frequency grounding. The mixers are formed on 25- m-thick silicon membranes. They are designed to operate in the 200 to 300 GHz frequency band, wherein wide-IF receivers for tropospheric- chemistry and astrophysical investigations are necessary. The fabrication process can be divided into three sections: 1. The front-side process, in which SIS devices with beam leads are formed on a SOI wafer; 2. The backside process, in which the SOI wafer is wax-mounted onto a carrier wafer, then thinned, then partitioned into individual devices; and 3. The release process, in which the individual devices are separated using a lithographic dicing technique. The total thickness of the starting 4-in. (10.16-cm)-diameter SOI wafer includes 25 m for the Si device layer, 0.5 m for the buried oxide (BOX) layer, and 350 m the for Si-handle layer. The front-side process begins with deposition of an etch-stop layer of SiO2 or AlN(x), followed by deposition of a Nb/Al- AlN(x) /Nb trilayer in a load-locked DC magnetron sputtering system. The lithography for four of a total of five layers is performed in a commercial wafer-stepping apparatus. Diagnostic test dies are patterned concurrently at certain locations on the wafer, alongside the mixer devices, using a different mask set. The conventional, self-aligned lift-off process is used to pattern the SIS devices up to the wire level.
The figure depicts the planned Actuated Hybrid Mirror Telescope (AHMT), which is intended to demonstrate a new approach to the design and construction of wide-aperture spaceborne telescopes for astronomy and Earth science. This technology is also appropriate for Earth-based telescopes. The new approach can be broadly summarized as using advanced lightweight mirrors that can be manufactured rapidly at relatively low cost. More specifically, it is planned to use precise replicated metallic nanolaminate mirrors to obtain the required high-quality optical finishes. Lightweight, dimensionally stable silicon carbide (SiC) structures will support the nanolaminate mirrors in the required surface figures. To enable diffraction- limited telescope performance, errors in surface figures will be corrected by use of mirror-shape-control actuators that will be energized, as needed, by a wave-front-sensing and control system. The concepts of nanolaminate materials and mirrors made from nanolaminate materials were discussed in several previous NASA Tech Briefs articles. Nanolaminates constitute a relatively new class of materials that can approach theoretical limits of stiffness and strength. Nanolaminate mirrors are synthesized by magnetron sputter deposition of metallic alloys and/or compounds on optically precise master surfaces to obtain optical-quality reflector surfaces backed by thin shell structures. As an integral part of the deposition process, a layer of gold that will constitute the reflective surface layer is deposited first, eliminating the need for a subsequent and separate reflective-coating process. The crystallographic textures of the nanolaminate will be controlled to optimize the performance of the mirror. The entire deposition process for making a nanolaminate mirror takes less than 100 hours, regardless of the mirror diameter. Each nanolaminate mirror will be bonded to its lightweight SiC supporting structure. The lightweight nanolaminate mirrors and SiC supporting structures will be fabricated from reusable master molds. The mirror-shape-control actuators will be low-power, high-capacitance lead magnesium niobate electrostrictive actuators that will be embedded in the SiC structures. The mode of operation of these actuators will be such that once power was applied, they will change in length and once power was removed, they will maintain dimensional stability to nanometer precision. This mode of operation will enable the use of low-power, minimally complex electronic control circuitry. The wave-front-sensing and control system will be designed and built according to a two-stage architecture. The first stage will be implemented by a Shack- Hartmann (SH) sensor subsystem, which will provide a large capture range. The second, higher-performance stage will be implemented by an image-based wave-front-sensing subsystem that will include a phase-retrieval camera (PRC), and will utilize phase retrieval and other techniques to measure wavefront error directly. Phase retrieval is a process in which multiple images of an unresolved object are iterated to estimate the phase of the optical system that acquired the images. The combination of SH and phase-retrieval sensors will afford the virtues of both a dynamic range of 105 and an accuracy of <10 nm.
The purpose of this investigation is to develop the fundamental materials and fabrication technology for field-controlled spectrally active optics that are essential for industry, NASA, and DOD applications such as: membrane optics, filters for LIDARs, windows for sensors, telescopes, spectroscopes, cameras, flat-panel displays, etc. ScN and AlN thin films were fabricated on c-axis Sapphire (0001) or quartz substrate with the RF and DC magnetron sputtering. The crystal structure of AlN in fcc (rocksalt) and hcp (wurtzite) were controlled. Advanced electrical characterizations were performed, including I-V and Hall Effect Measurement. ScN film has a free carrier density of 5.8 x 10(exp 20)/per cubic centimeter and a conductivity of 1.1 x 10(exp 3) per centimeter. The background ntype conductivity of as-grown ScN has enough free electrons that can readily interact with the photons. The high density of free electrons and relatively low mobility indicate that these films contain a high level of shallow donors as well as deep levels. Also, the UV-Vis spectrum of ScN and AlN thin films with rare earth elements (Er or Ho) were measured at room temperature. Their optical band gaps were estimated to be about 2.33eV and 2.24eV, respectively, which are obviously smaller than that of undoped thin film ScN (2.4eV). The red-shifted absorption onset gives direct evidence for the decrease of band gap (Eg) and the energy broadening of valence band states are attributable to the doping. As the doped elements enter the ScN crystal lattices, the localized band edge states form at the doped sites with a reduction of Eg. Using a variable angle spectroscopic ellipsometer, the decrease in refractive index with applied field is observed with a smaller shift in absorption coefficient.