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Protective coating containing a plasma arc sprayed mixture of hafnium oxide and zirconium diboride will withstand high temperatures in an oxygen rich atmosphere. Used on a homogeneous tungsten thermocouple, it does not flake or crack on subsequent cooling and reheating, and does not degrade the thermocouple response time.
Description of the reference materials selected for the major components of the unit cell of a thermionic pile element (TFE), the out-of-pile and in-pile test results, and current efforts for improving the life and performance of thermionic fuel elements. The component materials are required to withstand the fuel burnup and fast neutron fluence dictated by the thermionic reactor system. Tungsten was selected as the cladding material because of its compatibility with both the carbide and the oxide fuel materials. Niobium was selected as the collector material because its thermal expansion coefficient matches closely with that of the thin aluminum oxide layer used to electrically insulate the collector from the TFE sheath. An unfueled converter has performed stably over 41,000 hr. Accelerated irradiation tests have attained burnups equivalent to that for 40,000 hr of the thermionic reactor under consideration.
Tungsten and molybdenum alloy silicide slurry applied and vacuum sintered on tantalum and niobium alloys for protection from oxidation
Materials problems related to electric arc jets
A directionally solidified multivariant eutectic gamma + beta nickel-base superalloy casting having improved high temperature strength and oxidation resistance properties is provided. This comprises a two phase eutectic structure containing, on a weight percent basis, 5.0-15.0 tungsten, 8.5-14.5 aluminum, 0.0-35.0 cobalt and the balance being nickel. Embedded within the gamma phase nickel-base matrix are aligned eutectic beta phase (primarily (NiCo)Al reinforcing lamellae.
Tungsten alloy fiber reinforced Ni-base superalloy composites evaluated for high temperature turbojet engine applications, considering stress-rupture strength, oxidation and impact resistance
This program demonstrated the feasibility of fabricating fiber-reinforced MMC (niobium matrix) turbine blades to net shape by chemical vapor infiltration (CVI). A controllable, repeatable niobium infiltration process was developed, and the kinetics of both deposition and infiltration were studied. Several continuous refractory fibers (Nicalon, Nextel 440, FP-Al2O3, HPZ, and tungsten mesh) were investigated as potential reinforcements for strengthening niobium. Thermodynamic and experimental evaluation indicated FP-Al2O3 and tungsten to be the most chemically compatible with niobium, while Nicalon, FP-Al2O3, and tungsten were found to be best with regard to reinforcing capability. Finally, a protective coating for iridium was found to provide substantial oxidation protection to the niobium blade matrix.
Thermal fatigue and oxidation data were obtained on 36 specimens, representing 18 distinct variations (including the base systems) of TAZ-8A and M22 alloys. Double-edge wedge specimens for these systems were cycled between fluidized beds maintained at 1088 C and 316 C with a 180 s immersion in each bed. The systems included alloys TAZ-8A, M22, and 16 variations of these alloys. Each alloy variation consisted of a unique composition with an alternation in the percentage of carbon (C1 and C2), molydenum (M1 and M2), tungsten (W1 and W2), columbium (CB1, CB2, and CB3), tantalium (T1, T2, and T3), or boron (B1, B2, and B3) present. All of the alloys showed little weight change due to oxidation compared with other alloys previously tested in fluidized beds. Only both C1 alloy variation specimens survived 3500 cycles without cracking in the small radius, although substantial cracks were present, emanating from the end notches which were used for holding the specimens.
The optical constants of samples of six different metals (Al, Cu, Ni, Ta, W, and Zr) exposed to space on the Long Duration Exposure Facility (LDEF) were studied by variable angle spectroscopic ellipsometry. Measurements were also carried out on portions of each sample which were shielded from direct exposure by a metal bar. A least-squares fit of the data using an effective medium approximation was then carried out, with thickness and composition of surface films formed on the metal substrates as variable parameters. The analysis revealed that exposed portions of the Cu, Ni, Ta, and Zr samples are covered with porous oxide films ranging in thickness from 500 to 1000 A. The 410 A thick film of Al2O3 on the exposed Al sample is practically free of voids. Except for Cu, the shielded portions of these metals are covered by thin non-porous oxide films characteristic of exposure to air. The shielded part of the Cu sample has a much thicker porous coating of Cu2O. The tungsten data could not be analyzed.
Tungsten fiber reinforced superalloy composite (TFRS) impingement cooled turbine blade inlet gas temperatures were calculated taking into account material spanwise strength, thermal conductivity, material oxidation resistance, fiber-matrix interaction, and coolant flow. Measured values of TFRS thermal conductivities are presented. Calculations indicate that blades made of 30 volume percent fiber content TFRS having a 12,000 N-m/kg stress-to-density ratio while operating at 40 atmospheres and a 0.06 coolant flow ratio could permit a turbine blade inlet gas temperature of over 1900K. This is more than 150K greater than similar superalloy blades.
This research program was used to further develop the existing W-Ta generator and to evaluate alternative adsorbents, preferably inorganic materials, as supports for the generator. During the first half year, combinations of non-complexing eluents and a variety of adsorbents, both inorganic and organic, were evaluated. Some of these adsorbents were synthetic, such as chelate resins that could be specific for tungsten. In the second half of the year, the stress was mainly on the use of complexing eluents because of the high affinity of hydrous oxides for tantalum, on the synthesis of chelate resins and on the use novel techniques (electrolytic) to solve the tantalum-adsorption problem.
Tungsten fiber-reinforced superalloy composite (TFRS) impingement-cooled turbine blade inlet gas temperatures were calculated taking into account material spanwise strength, thermal conductivity, material oxidation resistance, fiber-matrix interaction, and coolant flow. Measured values of TFRS thermal conductivities are presented. Calculations indicate that blades made of 30 volume percent fiber content TFRS having a 12,000 N-m/kg stress-to-density ratio while operating at 40 atm and a 0.06 coolant flow ratio could permit a turbine blade inlet gas temperature of over 1900 K. This is more than 150 K greater than similar superalloy blades.
High-velocity xenon ions used to drill holes of controlled size and distribution through tungsten layer that sheaths surface of controlled-porosity dispenser cathode of traveling wave-tube electron emitter. Controlled-porosity dispenser cathode employs barium/calcium/ aluminum oxide mixture that migrates through pores in cathode surface, thus coating it and reducing its work function. Rapid, precise drilling technique applied to films of other metals and used in other applications where micron-scale holes required. Method requires only few hours, as opposed to tens of hours by prior methods.
Tungsten/tungsten-26 percent rhenium thermocouples for Apollo heat shield temperature measurement
This is the Monthly Letter Progress Report for the eighth month of a twelve month technical study directed toward the following objectives: A. Determining analytically and experimentally the feasibility and attractiveness of using free-standing pyrolytic graphite for a radiation cooled liquid rocket thrust chamber and exit nozzle for space application. B. Establishing through analysis and experimental demonstration, a set of design principles to facilitate the design of a reliable pyrolytic graphite thrust chamber assembly for a specific range of operating conditions. C. Demonstrate by means of test firings of complete thrust chamber assemblies, the validity of the design data and principles developed during the program. Preparations have been completed for test firing the two 100 lb. thrust Boron Pyralloy chambers at Marquardt during the first week in March 1962. These two chambers will first be static pressure checked with water to a pressure of 135 psig. The chambers will then be test fired with N204/N2H4-MMH propellants . Test samples of eleven different pyrolytic carbide and nitride materials have been ordered for high temperature oxidation tests and should be delivered by the end of March for evaluation in the plasma torch facility. The specific materials ordered in free- standing condition in thicknesses from 0.030 inch to 0.065 inch were as follows: (a) Pyrolytic graphite (on hand) (b) Pyrolytic graphite-boron alloy (on hand) (c) Pyrolytic graphite-tungsten alloy (d)Boron nitride (e) Titanium nitride (f) Silicon carbide (g) Titanium carbide (h) Zirconium carbide (i) Hafnium carbide (j) Niobium carbide (k) Tantalum carbide (l) High density (1 1-90) graphite (m) High density graphite (heat treated) These materials were ordered from Raytheon, HTM, and American Meta 1 Products . A summary of the available data on the oxidation rates of pyrolytic materials under slow air and rocket motor conditions is shown in Figure 1. High Temperature Materials, Inc. has been contacted relative to providing Pyrographite thrust chambers with extra-thick walls . They believe they can deliver chambers with substantially thicker walls than were possible a short time ago. Such a configuration, with acceptable residual stresses, would provide a longer firing life since it is ultimately limited by the oxidation rate of the chamber wall material. Stress and structural studies have continued. The analytical stress studies point out some of the problems associated with the experimental determination of the elastic constants of this highly anisotropic material. Further analysis may shed light on improved techniques for making these experimental determinations. The large potential weight saving available with the use of pyrolytic graphite as a thrust chamber wall material in a radiation cooled rocket motor has been calculated and is shown graphically in Figure 2. Figure A presents the program progress schedule and the actual expenditures as of 7 February 1962.
In the literature to date on thermophotovoltaic (TPV) generators, two types of infrared emitter's have been emphasized : gray body emitters and rare earth oxide selective emitters. The gray body emitter is defined as an emitter with a spectral emissivity independent of wavelength whereas the rare earth oxide selective emitter is idealized as a delta function emitter with a high emissivity at a select wavelength and a near zero emissivity at all other wavelengths. Silicon carbide is an example of a gray body emitter and ER-YAG is an example of a selective emitter. The Welsbach mantle in a common lantern is another example of an oxide selective emitter. Herein, we describe an alternative type of selective emitter, a selective metallic emitter. These metallic emitters are characterized by a spectral emissivity curve wherein the emissivity monotonically increases with shorter infrared wavelengths as is shown. The metal of curve "A", tungsten, typifies this class of selective metallic emitter's. In a thermophotovoltaic generator, a photovoltaic cell typically converts infrared radiation to electricity out to some cut-off wavelength. For example, Gallium Antimonide (GaSb) TPV cells respond out to 1.7 microns. The problem with gray body emitters is that they emit at all wavelengths. Therefore, a large fraction of the energy emitted will be outside of the response band of the TPV cell. The argument for the selective emitter is that, ideally, all the emitted energy can be in the cells response band. Unfortunately, rare earth oxide emitters are not ideal. In order to suppress the emissivity toward zero away from the select wavelength, the use of thin fiber's is necessary. This leads to a fragile emitter typical of a lantern mantle. Even given a thin ER-YAG emitter, the measured emissivity at the select wavelength of 1.5 microns has been reported to be 0.6 while the off wavelength background emissivity falls to only 0.2 at 5 microns. This gives a selectivity ratio of only 3. Another problem with a delta function selective emitter is its low power density at practical temperatures because of its narrow emission bandwidth. The concept of selectivity can be generalized by noting that we simply wish to maximize the ratio of in-cell-band power to out-of-cell-band power. Using this generalized selectivity concept and assuming a GaSb cell covered by a simple dielectric filter, we note that the emissivity selectivity ratio for tungsten is 0.3 (at 1.5 microns) / 0.07 (at 5 microns) = 4.3. In the folloy4ng sections, we note that the selective metallic emitters can be valuable in both radioisotope TPV generators in space and in hydrocarbon fired TPV generators here on earth.
Uranium losses during thermal cycling of tungsten - uranium dioxide composites to 2500° C in flowing purified hydrogen for specimens initially containing 35 volume percent uranium dioxide were reduced by the use of thorium dioxide, calcium oxide, or yttrium oxide as additives in solid solution with the uranium dioxide. The effectiveness of the additives decreased in the order yttrium oxide, calcium oxide, and thorium dioxide. Stabilization of uranium dioxide by calcium oxide or yttrium oxide can be explained in part on the basis of the introduction of oxygen vacancies into the fluorite lattice and the associated lowered partial molar free energy of oxygen. The difference in the effectiveness of calcium oxide and yttrium oxide is discussed, and a possible explanation of the observed behavior is proposed. Of the concentrations of yttrium oxide tested (i.e., 2. 5, 5, and 10 mole percent), 10 mole percent of yttrium oxide was the most effective in pre venting loss of uranium from composities.
Processing techniques were developed for applying several diffusion barriers to TD-Ni and TD-NiCr. Barrier coated specimens of both substrates were clad with Ni-Cr-Al and Fe-Cr-Al alloys and diffusion annealed in argon. Measurement of the aluminum distribution after annealing showed that, of the readily applicable diffusion barriers, a slurry applied tungsten barrier most effectively inhibited the diffusion of aluminum from the Ni-Cr-Al clad into the TD-alloy substrates. No barrier effectively limited interdiffusion of the Fe-Cr-Al clad with the substrates. A duplex process was then developed for applying Ni-Cr-Al coating compositions to the tungsten barrier coated substrates. A Ni-(16 to 32)Cr-3Si modifier was applied by slurry spraying and firing in vacuum, and was then aluminized by a fusion slurry process. Cyclic oxidation tests at 2300 F resulted in early coating failure due to inadequate edge coverage and areas of coating porosity. EMP analysis showed that oxidation had consumed 70 to 80 percent of the aluminum in the coating in less than 50 hours.