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NASA NTRS1984

Reaction of amorphous Ni-W and Ni-N-W films with substrate silicon

Wiley et al. (1982) have studied sputtered amorphous films of Nb-Ni, Mo-Ni, Si-W, and Si-Mo. Kung et al. (1984) have found that amorphous Ni-Mo films as diffusion barriers between multilayer metallizations on silicon demonstrate good electrical and thermal stability. In the present investigation, the Ni-W system was selected because it is similar to the Ni-Mo system. However, W has a higher silicide formation temperature than Mo. Attention is given to aspects of sample preparation, sample characterization, the interaction between amorphous Ni-W films and Si, the crystallization of amorphous Ni(36)W(64) films on SiO2, amorphous Ni-N-W films, silicide formation and phase separation, and the crystallization of amorphous Ni(36)W(64) and Ni(30)N(21)W(49) layers.

Zhu, M. F.↗

NASA NTRS1985

Summary of process research analysis efforts

A summary of solar-cell process research analysis efforts was presented. Process design and cell design are interactive efforts where technology from integrated circuit processes and other processes are blended. The primary factors that control cell efficiency are: (1) the bulk parameters of the available sheet material, (2) the retention and enhancement of these bulk parameters, and (3) the cell design and the cost to produce versus the finished cells performance. The process sequences need to be tailored to be compatible with the sheet form, the cell shape form, and the processing equipment. New process options that require further evaluation and utilization are lasers, robotics, thermal pulse techniques, and new materials. There are numerous process control techniques that can be adapted and used that will improve product uniformity and reduced costs. Two factors that can lead to longer life modules are the use of solar cell diffusion barriers and improved encapsulation.

Burger, D. R.↗

NASA NTRS1985

Process development

An overview is given of seven process development activities which were presented at this session. Pulsed excimer laser processing of photovoltaic cells was presented. A different pulsed excimer laser annealing was described using a 50 w laser. Diffusion barrier research focused on lowering the chemical reactivity of amorphous thin film on silicon. In another effort adherent and conductive films were successfully achieved. Other efforts were aimed at achieving a simultaneous front and back junction. Microwave enhanced plasma deposition experiments were performed. An updated version of the Solar Array Manufacturing Industry Costing Standards (SAMICS) was presented, along with a life cycle cost analysis of high efficiency cells. The last presentation was on the evaluation of the ethyl vinyl acetate encapsulating system.

Bickler, D. B.↗

NASA NTRS1985

Amorphous metallic films in silicon metallization systems

Diffusion barrier research was focussed on lowering the chemical reactivity of amorphous thin films on silicon. An additional area of concern is the reaction with metal overlays such as aluminum, silver, and gold. Gold was included to allow for technology transfer to gallium arsenide PV cells. Amorphous tungsten nitride films have shown much promise. Stability to annealing temperatures of 700, 800, and 550 C were achieved for overlays of silver, gold, and aluminum, respectively. The lower results for aluminum were not surprising because there is an eutectic that can form at a lower temperature. It seems that titanium and zirconium will remove the nitrogen from a tungsten nitride amorphous film and render it unstable. Other variables of research interest were substrate bias and base pressure during sputtering.

So, F.↗

NASA NTRS1987

Interactions of amorphous Ta(x)Cu(1-x) (x = 0.93 and 0.80) alloy films with Au overlayers and GaAs substrates

Amorphous Ta(93)Cu(7) and Ta(80)Cu(20) alloy films are prepared by cosputtering of pure Ta and pure Cu targets with a rotating sample holder table. To investigate the possible application of these materials as diffusion barriers for the Au-GaAs system, vacuum annealings are made in the temperature range from 200 to 800 C. Resistivity change, X-ray diffraction, and Auger electron spectroscopy measurements are performed to find the chemical and metallurgical stabilities of these materials in this system. The reaction temperature for Ta(x)Cu(1-x) in contact with GaAs lies between 500 and 700 C. For Au in contact with Ta(x)Cu(1-x) the reaction occurs at about 600 C. Amorphous Ta(93)Cu(7) shows different interdiffusion characteristics with surrounding elements than does Ta(80)Cu(20).

Oh, Jae E.↗

NASA NTRS1988

Electrochemical Growth Of Crystals In Gels

Nucleation and growth rates readily controlled. Technique developed to grow crystals by controlling rate of transfer of one component into crystallization volume. Method involves electrochemically controlled generation of one of precipitation species, coupled with diffusion barrier. New procedure, developed in connection with formation of lead tin telluride by reaction in gels of metal ions with telluride ions.

Barber, Patrick G.↗

NASA NTRS1990

Interfacial reactions in high temperature metallic and intermetallic matrix composites - A status review

Interdiffusion and interdiffusion-related phenomena in metal and intermetallic matrix composites can be of crucial interest for the prolonged application of these systems at high temperature. The level of complication that these effects can have can vary significantly from system to system. Reviewed herein are recent efforts to address interdiffusion and reaction kinetics for both a simple system, the single phase W/Nb system, and more complex systems such as tungsten fiber reinforced superalloys (TFRS) and beryllide reinforced aluminides. Additionally, recent work on inhibiting interdiffusion in MMCs via ion-implanted diffusion barriers will be presented.

Tien, J. K.↗

NASA NTRS1987

Soft x ray window encapsulant for HgI2 detectors

HgI2 is an excellent semiconductor material for a low energy, room temperature x-ray spectrometer. The high values of the atomic numbers for its constituent elements gives high x-ray and gamma ray stopping power. The band gap of HgI2 is significantly higher than other commonly used semiconductors. Owing to the large value band gap, the leakage current for HgI2 devices is smaller, thus allowing low noise performance. Devices fabricated from HgI2 crystals have demonstrated energy resolution sufficient to distinguish the x-ray emission from the neighboring elements on the periodic table. Also the power requirements of HgI2 are very low. These characteristics make a HgI2 spectrometer an ideal component in a satellite based detection system. Unfortunately, HgI2 crystals tend to deteriorate with time, even if protected by standard semiconductor encapsulants. This degradation ruins the performance of the device in terms of its energy resolution and pulse amplitude. The degrading mechanism is believed to be material loss occurring from below the electrodes, due to high vapor pressure of HgI2 at room temperature. To address this major obstacle to rapid expansion of HgI2 technology, a research program aimed at improving device stability by encapsulation with inert polymeric materials was carried out. The program focused specifically on optimizing the encapsulant materials and their deposition techniques. The principal objectives for this program were device encapsulation, device testing, and accelerated testing to ensure very long term stability of these high resolution sensors. A variety of encapsulants were investigated with the selection criteria based on their chemical diffusion barrier properties, mechanical stability, reactivity, and morphology of encapsulant films. The investigation covered different classes of encapsulants including solvent based encapsulants, vapor deposited encapsulants, and plasma polymerized encapsulants. A variety of characterization techniques were employed to examine their effectiveness in stabilizing HgI2 devices; these included permeability evaluation, vacuum and heat testing, scanning electron microscopy (SEM) as well as studying the detector performance of coated detectors. The plasma polymerized films appear to have entirely solved the HgI2 degradation problem. Another achievement of this program was the development of an accelerated testing technique which correlates extremely well with long term tesing.

Entine, G.↗

NASA NTRS1990

Micromechanical thermal analysis of interphase region in a titanium aluminide MMC

The high reactivity between the fiber and matrix in silicon carbide/titanium aluminide MMCs leads to the formation of brittle reaction products at the fiber/matrix (F/M) interface. Also, the high thermal expansion coefficient mismatch between the fiber and matrix leads to high tensile residual stresses at the F/M interface, and this can lead to premature cracking during cooldown. One solution to these problems is the use of a metallic fiber coating like Ta which acts as an F/M diffusion barrier and reacts with the matrix to form a beta stabilized compliant layer. A finite element micromechanics analysis was performed to study the effects of Ta and beta interphase layers on the thermal residual stresses during consolidation. A 5-micron-thick beta layer reduced cool-down stresses by 8 percent compared to a 2 percent reduction computed for a Ta layer of the same thickness. Plastic yielding in the Ta was not effective in reducing cool-down stresses. Compliant alpha-2 particles next to the stiffer gamma particles reduced stresses in the gamma particles by less than 2 percent. A simple closed form analysis was developed to calculate thermal residual stresses in a fiber/interphase/matrix system. A 2-micron-thick Ag interphase layer was found to reduce residual stresses by about 11 percent.

Naik, R. A.↗

NASA NTRS1992

Materials, structures, and devices for high-speed electronics

Advances in materials, devices, and instrumentation made under this grant began with ex-situ null ellipsometric measurements of simple dielectric films on bulk substrates. Today highly automated and rapid spectroscopic ellipsometers are used for ex-situ characterization of very complex multilayer epitaxial structures. Even more impressive is the in-situ capability, not only for characterization but also for the actual control of the growth and etching of epitaxial layers. Spectroscopic ellipsometry has expanded from the research lab to become an integral part of the production of materials and structures for state of the art high speed devices. Along the way, it has contributed much to our understanding of the growth characteristics and material properties. The following areas of research are summarized: Si3N4 on GaAs, null ellipsometry; diamondlike carbon films; variable angle spectroscopic ellipsometry (VASE) development; GaAs-AlGaAs heterostructures; Ta-Cu diffusion barrier films on GaAs; GaAs-AlGaAs superlattices and multiple quantum wells; superconductivity; in situ elevated temperature measurements of III-V's; optical constants of thermodynamically stable InGaAs; doping dependence of optical constants of GaAs; in situ ellipsometric studies of III-V epitaxial growth; photothermal spectroscopy; microellipsometry; and Si passivation and Si/SiGe strained-layer superlattices.

Woollam, John A.↗

NASA NTRS1995

Tensile Behavior of Al2o3/feal + B and Al2o3/fecraly Composites

The feasibility of Al2O3/FeAl + B and Al2O3/FeCrAlY composites for high-temperature applications was assessed. The major emphasis was on tensile behavior of both the monolithics and composites from 298 to 1100 K. However, the study also included determining the chemical compatibility of the composites, measuring the interfacial shear strengths, and investigating the effect of processing on the strength of the single-crystal Al2O3 fibers. The interfacial shear strengths were low for Al203/FeAl + B and moderate to high for Al203/FeCrAlY. The difference in interfacial bond strengths between the two systems affected the tensile behavior of the composites. The strength of the Al203 fiber was significantly degraded after composite processing for both composite systems and resulted in poor composite tensile properties. The ultimate tensile strength (UTS) values of the composites could generally be predicted with either rule of mixtures (ROM) calculations or existing models when using the strength of the etched-out fiber. The Al2O3/FeAl + B composite system was determined to be unfeasible due to poor interfacial shear strengths and a large mismatch in coefficient of thermal expansion (CTE). Development of the Al2O3/FeCrAlY system would require an effective diffusion barrier to minimize the fiber strength degradation during processing and elevated temperature service.

Draper, S. L.↗

NASA NTRS2000

Fabrication of an Aluminum Based Hot Electron Mixer for Terahertz Applications

Aluminum based diffusion cooled hot electron bolometers (HEB) mixers, predicted to have better noise, bandwidth and to require less LO power than Nb based diffusion cooled HEBs, have been fabricated. Preliminary DC tests were performed. The bolometer elements consisted of short (0.1 to 0.3 micron), narrow (0.08 to 0. 15 micron) and thin (11 nm) aluminum wires connected to large contact pads consisting of a novel trilayer Al/Ti/Au. The patterns were defined by electron beam lithography and the metal deposition involved a double angle process, the Aluminum wires being deposited straight on and the pads being deposited at a 45 degree angle without breaking vacuum. The Al/Ti/Au trilayer was developed to provide a way of making contact between the aluminum wire and the gold antenna. The Titanium layer acts as a diffusion barrier to avoid damage of the Aluminum contact and bolometer wire and to lower the transition temperature of the pads to below that of the bolometer wire. The Au layer avoids the formation of an oxide on the Ti layer and provides good electrical contact to the IF/antenna structure. The resistance of the bolometers as a function of temperature was measured. It is clear that below the transition temperature of the wire (1.8K) but above the transition temperature of the contact pads (0.6K), the proximity effect drives most of the bolometer wire normal, causing a very broad transition. This effect should not affect the performance of the bolometers since they will be operated at a temperature below the TC of the pads. This is evident from the IV characteristics measured at 0.3K. RF characterization tests will begin shortly.

Echternach, P. M.↗

NASA NTRS1966

Development of Protective Coatings for Chromium-Base Alloys

Chromium alloy sheet was clad with 5 to 10-mil-thick oxidation-resistant nickel-base alloy foils. Specimens also contained 1/2 to 1-mil-thick intermediate layers of platinum, tungsten, and/or W-25Re. Cladding was done by the isostatic hot gas-pressure bonding,.process. The clad chromium-alloy specimens were cyclic oxidation tested at 2100 F and 2300 F for up to 200 hours to determine the effectiveness of these metal claddings in protecting the chromium alloy Cr-5W from oxidation and contamination. Cladding systems consisting of 5-mil-thick Ni-20Cr-20W modified with 3 to 5 weight percent aluminum and containing a 1 /2-mil tungsten diffusion barrier demonstrated potential for long-time service at temperatures as high as 2300 F.

English, J. J.↗

NASA NTRS2000

Triaxial Burke-Schumann Flames with Applications to Flame Synthesis

The problem of a flame generated by three coaxial flows is solved by extending the Burke-Schumann methodology to include a third stream. The solution is particularly relevant to flame synthesis wherein multiple tubes are often employed either to introduce inert as a diffusion barrier or to introduce more than two reactants. The general problem is solved where the inner and outer tubes contain reactants and the middle tube contains either an inert or a third reactant. Relevant examples are considered and the results show that the triaxial Burke-Schumann flame can be substantially more complicated than the traditional Burke-Schumann flame. When the middle flow is inert the flame temperature is no longer constant but increases axially, reaching a maximum at the flame centerline. At the exit the flame does not sit on the tube exit but instead resides between the inner and outer tubes, resulting in an effective barrier for particle build-up on the burner rim. For the case of a third reactant in the middle flow, synthesis chemistry where the inner reaction is endothermic and the outer reaction is exothermic is considered. In addition to showing the flame temperature and flame shape, the results identify conditions wherein reaction is not possible due to insufficient heat transfer from the outer flame to support the inner flame reaction.

Chao, B. H.↗

NASA NTRS2003

Flame Spray Strain Gages with Improved Durability and Lifetimes

The focus of this APP research program was to improve the bond coats used in the fabrication of flame sprayed instrumentation. Typically. a bond coat is applied to a superalloy surface prior to the application of a thin dielectric coating onto which instrumentation is placed. After affixing the instrumentation, a much thicker ceramic topcoat is typically applied to protect the instrumentation from harsh environments. The fatigue life of NiCoCrAlY coated superalloys was extended beyond current state-of-the-art by relatively simple and cost effective means. Heat treatment in reduced oxygen partial pressures at 1750 to 1800 F effectively doubled the fatigue life of NiCoCrAlY coated substrates relative to as-sprayed substrates and when used in conjunction with platinum diffusion barriers yielded a four fold increase in the fatigue life of NiCoCrAlY coated substrates. Further improvements in the fatigue life of thermally sprayed coatings were made by employing intermediate coatings, which minimized thermal expansion differences between the bond coat and top coat. Combinatorial chemistry experiments yielded an optimum composition for an intermediate TCE matching coating that showed considerable promise in extending the fatigue life of thermal spray instrumentation. The intermediate coating had two functions: to reduce the surface roughness of the peaks and valleys associated with the as-sprayed NiCoCrAlY bond coat, and to produce a thin layer of a mixture of Al2O3 and NiCoCrAlY that exhibited an intermediate TCE. The optimal composition of the intermediate coating consisted of 60 wt% Al2O3 and 40 wt% NiCoCrAlY, as determined by energy dispersive analysis of x-rays (EDS). Intermediate coatings having this composition were prepared by physical vapor deposition and the resulting coating systems are being evaluated in our test facility.

Fralick, Gustave↗

NASA NTRS2004

Volatility of Common Protective Oxides in High-Temperature Water Vapor: Current Understanding and Unanswered Questions

Many structural materials rely on the formation of chromia, silica or alumina as a protective layer when exposed in high temperature oxidizing environments. The presence of these oxide layers provides a protective diffusion barrier which slows down further oxidation. In atmospheres containing water vapor, however, reactions to form volatile hydroxide species occur which remove the surface oxide, thus, lowering the protective capability of the oxide scale. This paper summarizes the current understanding of volatility of chromia, silica and alumina in water vapor containing combustion environments. In addition unanswered questions in each system are discussed. Th current paper represents an update on the considerable information learned in the past five years for these systems.

Opila, Elizabeth J.↗

NASA NTRS2000

Metabolic activity of permafrost bacteria below the freezing point

Metabolic activity was measured in the laboratory at temperatures between 5 and -20 degrees C on the basis of incorporation of (14)C-labeled acetate into lipids by samples of a natural population of bacteria from Siberian permafrost (permanently frozen soil). Incorporation followed a sigmoidal pattern similar to growth curves. At all temperatures, the log phase was followed, within 200 to 350 days, by a stationary phase, which was monitored until the 550th day of activity. The minimum doubling times ranged from 1 day (5 degrees C) to 20 days (-10 degrees C) to ca. 160 days (-20 degrees C). The curves reached the stationary phase at different levels, depending on the incubation temperature. We suggest that the stationary phase, which is generally considered to be reached when the availability of nutrients becomes limiting, was brought on under our conditions by the formation of diffusion barriers in the thin layers of unfrozen water known to be present in permafrost soils, the thickness of which depends on temperature.

NASA Center ARC↗

NASA NTRS1997

Rhenium Rocket Manufacturing Technology

The NASA Lewis Research Center's On-Board Propulsion Branch has a research and technology program to develop high-temperature (2200 C), iridium-coated rhenium rocket chamber materials for radiation-cooled rockets in satellite propulsion systems. Although successful material demonstrations have gained much industry interest, acceptance of the technology has been hindered by a lack of demonstrated joining technologies and a sparse materials property data base. To alleviate these concerns, we fabricated rhenium to C-103 alloy joints by three methods: explosive bonding, diffusion bonding, and brazing. The joints were tested by simulating their incorporation into a structure by welding and by simulating high-temperature operation. Test results show that the shear strength of the joints degrades with welding and elevated temperature operation but that it is adequate for the application. Rhenium is known to form brittle intermetallics with a number of elements, and this phenomena is suspected to cause the strength degradation. Further bonding tests with a tantalum diffusion barrier between the rhenium and C-103 is planned to prevent the formation of brittle intermetallics.

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